Production of Acetaldehyde

Chapter 1
INTRODUCTION
Production of Acetaldehyde | Chapter 1 1

1.1 HISTORY
Acetaldehyde, CH3CHO, was first prepared by Scheele in 1774, by the action of manganese
dioxide and sulfuric acid on ethanol. The structure of acetaldehyde was established by Liebig in
1835 when he prepared a pure sample by oxidizing the ethanol with chromic acid. Liebig named
the compound aldehyde from the Latin words translated as al (cohal) dehyde (originated). The
formation of acetaldehyde by the addition of water to acetylene was observed by Kutscherow in
1881.
Acetaldehyde was first prepared from ethyl alcohol by Davy (1817) who employed a platinum
black catalyst and passed a mixture of alcohol and air over it at a lower temperature. More
thorough studies of the air oxidation of ethanol, employing various catalyses, were made by
Kuhlman in 1839, Strecker (1855) and Grimax (1886). Not until the work of Trillatt (1902) and
Orloff (1901), however, were any quantitative data reported. More recently Faith and Keyes
(1931) carried out extensive investigation of this reaction and found that the silver gauze was the
best catalyst. Employing a flow rate of 0.57 liter of alcohpl vapors per minute over a heated
silver gauze, 12 mm. in diameter and 15 mm. long, maintaining a temp. Fairly constant at 515°C,
they observed 80.6% conversion of ethanol to acetaldehyde with losses of 13.3% to C02 and 3.2
to acetic acid.
Shrieve (1945) and Faith, Keyes, Clark (1950) have reported slightly higher yields of 85 to 95%
by the air oxidation of ethanol to acetaldehyde by use of silver catalyst at a temp of 550 - 5700C
and a conversion per pass of 50 to 55%.
However, Groggins (1947) reporting results from a similar process claims only 70-80% of the
theoretical yield of acetaldehyde under identical conditions.
The production pattern for acetaldehyde has undergone two significant changes since 1940. At
that time, principal industrial routs to acetaldehyde were hydration of acetylene and oxidation of
ethyl alcohol. However, increasing acetylene costs made this feed stock economically
unattractive and the industry turned to the oxidation of ethanol. The production of acetaldehyde
based on ethanol increased from 63.5 kilotons per years in 1940 to 403 kilo tons per years in
1960.
In 1960, the two aldehyde Wacker-Hoechst G.M.B.H. processes for the liquid phase oxidation of
ethylene to acetaldehyde began commercial operation. By 1963, more acetaldehyde was
produced by the direct oxidation of ethylene using the Wacker process than from ethanol, and

since then, production via the Wacker process has increased while production from ethanol has
declined.
1.2 PHYSICAL PROPERTIES
Acetaldehyde is a colorless, mobile liquid having a pungent suffocating odor that is somewhat
fruity and pleasant in dilute concentrations. Some physical properties of acetaldehyde are given
in table, the vapor pressure of acetaldehyde and its aqueous solutions in tables and the solubility
of acetylene, C02 and N2 in liquid acetaldehyde in table. The freezing points of aqueous
solutions of acetaldehyde are as follows:
4.8 wt. % - 2.5ºC; 13.5 wt. % - 7.8ºC; & 31.0 wt. % - 23.0ºC
Acetaldehyde is miscible in all proportions with water and most common organic solvents;
acetone, benzene, ethyl alcohol, ethyl ether, gasoline, paraldehyde, toluene, xylene, tarpentine
and acetic acid.

Table-1.1: Physical Properties of Acetaldehyde
Formula weight 44.052
Melting point, °C -123.5
Boiling point at 760 mm, °C 20.16
Density 0.7730
Vapor density (air = 1) 1.52
Surface tension at 20 OC, dyne/cm 21.2
Absolute viscosity at 15°C (cgs units) 0.02456
Specific heat, cal/(°C)(g) at 0 ºC 0.522
at 25°C 0.336
Latent heat of fusion, cal/g 17.6
Latent heat of vaporization, cal/g 139.5
Heat of combustion of liquid at constant Pressure Kcal/mol 379.2
Heat of formation at 273 K 39.55
Free energy of formation at 273 K, Kcal/mole -32.60
Critical temp, ºC 181.5
Critical pressure, (atm.) 63.2
Dissociation constant, Ka, at 0ºC 0.7(10-14)
Flash point, closed cup, °C -38
Ignition temperature in air, ºC 135
Explosive limits of mixtures with air, % acetaldehyde by volume 4-57

Table-1.2: Vapor Pressure of Acetaldehyde
Temperature °C Vapor Pressure mmHg Temperature °C Vapor Pressure mmHg
-50 19 20 755
-20 123 20.16 760
0 330 30 1069
5 411 50 3096
10 508 70 3696
15 622 100 3607
Table-1.3: Vapor Pressure of Aqueous solutions of Acetaldehyde
Temperature °C Vapor Pressure mmHg Temperature °C Vapor Pressure mmHg
10 4.9 4.9 74.5
10 10.5 10.5 139.8
20 5.4 5.4 125.2
20 12.9 12.9 259.2

Table 1.4: Solubility of Gases in Liquid Acetaldehyde at 760 mm (Volume of gas
[NTP] dissolved in one volume of acetaldehyde)
Temperature °C Acetylene Carbon Dioxide Nitrogen
-6 27 11
0 17 6.6
0.15
12 7.3 2.45
16 5 1.5
1.3 CHEMICAL PROPERTIES
In a study of the spontaneous ignition of fuels injected into hot air streams, it was found that
acetaldehyde was the least ignitable of the aldehydes examined.
Acetaldehyde reactivity of condensation, Conditions, the is a highly reactive compound

exhibiting the general aldehydes (qv). Acetaldehyde undergoes numerous addition, and
polymerization reaction; under suitable oxygen or any of the hydrogen can be replaced.
1.3.1 Decomposition
Acetaldehyde decomposes at temperatures above 4000C, forming principally methane and

carbon monoxide. The activation energy of the pyrolysis reaction is 97.7 kJ/mol (408.8
kcal/mol). There have been many investigations of the photolytic and radical induced
decomposition of acetaldehyde and deuterated acetaldehyde.
1.3.2 The Hydrate and Enol Form
In aqueous solutions, acetaldehyde exists in equilibrium with the acetaldehyde hydrate,

(CH3CH(OH)2. The degree of hydration can be computed from an equation derived by Bell and
Clunie Hydration, the mean heat of which is2 1.34 kJ/mol (-89.29 kcal/mol), has been attributed
to hyper conjugation. The enol form, vinyl alcohol (CH2=CHOH) exists in equilibrium with
acetaldehyde to the extent of approximately one molecule per 30,000. Acetaldehyde enol has
been acetylated with ketene to form vinyl acetate.

1.3.3 Oxidation
Acetaldehyde is readily oxidized with oxygen or air to acetic acid, acetic anhydride, and per
acetic acid, the principal product depends on the reaction conditions.
Low temperature oxidation of acetaldehyde in the presence of metal salts, Ultraviolet irradiation,
or ozone yields acetaldehyde mono per acetate, which can be decomposed to per acetic acid and
acetaldehyde (36). Per acetic acid can also be formed directly by liquid-phase oxidation at 5-
50°C with a cobalt salt catalyst (see Peroxides and per oxy compounds) Nitric acid oxidation of
acetaldehyde yields glyoxal. Oxidation of p-xylene to terephthalic acid and of ethanol to acetic
acid is activated by acetaldehyde.
1.3.4 Reduction
Acetaldehyde is readily reduced to ethanol. Suitable catalysts for vapor-phase hydrogenation of

acetaldehyde are supported nickel and copper oxide the kinetics of the hydrogenation of
acetaldehyde over a commercial nickel catalyst has been studied.
1.3.5 Polymerization
Paraldehyde, 2,4,6- trimethyl -1,3,5 trioxance, a cyclic trimer of acetaldehyde, is formed when a
mineral acid, such as sulfuric phosphoric, or hydrochloric acid is added to acetaldehyde.
Paraldehyde can also be formed continuously by feeding liquid acetaldehyde at 15- 20°C over an
acid ion-exchange resin.
Paraldehyde is a colorless liquid, boiling at 125.35°C at l0l kPa ( l atm).
1.4 CHEMICAL REACTIONS
Metaldehyde [9002-91-9], a cyclic tetramer of acetaldehyde, is formed at temperatures below 0C

in the presence of dry hydrogen chloride or pyridine-hydrogen bromide. The metaldehyde
crystallizes from solution and is separated from the paraldehyde by filtration. Metaldehyde melts
in a sealed tube at 246.2°C and sublimes at 115°C with partial depolymerization.
1.4.1 Reactions with Aldehydes and Ketones
The base-catalyzed self-addition of acetaldehyde leads to formation of the dimmer, acetaldol,

which can be hydrogenated to form 1,3- butanediol or dehydrated to form crotonaldehyde.
Crotonaldehyede (qv) can also be made directly by the vapor phase condensation of
acetaldehyde over a catalyst.

Acetaldehyde forms aldols with other carbonyl compounds containing active hydrogen atoms.
A hexyl alcohol, 2-ethyl-1 butanol is produced industrially by the condensation of acetaldehyde

and butyraldehyde in dilute caustic solution followed by hydrogenation of the enal intermediate.
Condensation of acetaldehyde in the presence o dimethyl amine hydrochloride yields polyenals

which can be hydrogenated to a mixture of alcohols containing from 4-22 carbon atoms.
The base-catalyzed reaction of acetaldehyde with excess formaldehyde is the commercial route
to penta erythritol. The aldol condensation of three I moles of formaldehyde with one mole of
acetaldehyde is followed by a crossed Cannizzaro reaction between penta erythrose, the
intermediate product, formaldehyde to give penta erythritol. The proces.s proceeds to completion
without isolation of the intermediate.
Ethyl acetate is produced commercially by the Tischenko condensation of acetaldehyde using an

aluminum ethoxide catalyst.
1.4.2 Reaction with Ammonia and Amities
Acetaldehyde readily adds ammonia to form acetaldehyde ammonia. Diethyl amine is obtained
when acetaldehyde is added to a saturated aqueous or alcoholic solution of ammonia and the
mixture is heated to 50-75°C in the presence of a nickel catalyst and hydrogen at 1.2 (12 atm)
Pyridine and pyridine derivatives are made from paraldehyde and aqueous ammonia in the
presence of a catalyst at elevated temperatures.
1.4.3 Reactions with Alcohols, Mercaptants, and Phenols
Alcohols add readily to acetaldehyde in the presence of trace quantities of mineral acid to form
acetals; e.g., ethanol and acetaldehyde form diethyl acetal. Similarly cyclic acetals are formed by
reactions with glycols and other poiy hydroxy compounds; e.g. ethylene glycol and acetaldehyde
give 2-methyl -13 dioxolane.
MercaptalS, CH3CH(SR)2, are formed in a like manner by the addition of mercaptants. The
formation of acetals by non catalytic vapor-phase reactions of acetaldehyde and various alcohols
at 35°C has been reported. Butadiene can be made by the reaction of acetaldehyde. and ethyl
alcohol at temperatures above 3000C over a tantala-silica catalyst.

1.4.4 Reactions with Halogens and Halogens Compounds
Halogens readily replace the hydrogen atoms of the acetaldehyde’s methyl group.. Chlorine
reacts with acetaldehyde or-paraldehyde at room temperature to give chloro acetaldehyde.
Increasing the temperature to 7-80°C gives dichioro acetaldehyde and at a temperature of 80-
90°C chloral is formed.
Acetyl chloride has been prepared by the gas-phase reaction of acetaldehyde and chlorine.
Acetaldehyde reacts with phosphorus pentachioride to produce 1,1 - dichiorol ethane and with
hypochiorite a hypoiodite to yield chloroform and iodoform respectively. Phosgene [75-44-5] is
produced by the reaction of carbon tetrachioride with acetaldehyde in the presence of anhydrous
aluminum chloride. Chloroform reacts with acetaldehyde in the presence of potassium hydroxide
and sodium amide to form 1,1,1 - trichloro—2 propanol.
1.5 SHIPPING, HANDLING AND STORAGE
Acetaldehyde appears to paralyze the respiratory muscles and causes panic. It has a general
narcotic action which prevents coughing. It causes irritation of the eyes and mucous membranes,
and accelerates heart action.
When breathed in high concentration, it causes headache and sore throat. Carbon dioxide
solutions in acetaldehyde are particularly pernicious because the acetaldehyde odor is weakened
by the carbon dioxide. Prolonged exposure causes a decrease of red and white blood cell; there is
also a sustained rise in blood pressure. The maximum allowable concentration of acetaldehyde in
air is 200 ppm. In normal industrial operations there is no health hazard in handling acetaldehyde
provided normal precautions are taken.
Mixture of Acetaldehyde vapor with air is flammable if the concentration of Acetaldehyde and
oxygen are higher than 4 and 9% respectively. Acetaldehyde is very volatile, has a low flash
point, oxidizes readily and may form highly explosive peroxides.
1.5.1 Handling
In handling acetaldehyde one has to remember that it is an extremelY reactive compound that
can be easily oxidized, reduced, or polymerized and is highly reactive with oxygen, it has to be
treated as a volatile, flammable and toxic materiaL The following is a list of precautions
recommended when handling acetaldehyde.

1) Nitrogen or other inert gases should be used as a blanketing material whenever expo’sure
to air is possibility.
2) Safety goggles should be used.
3) Transfers should be made in open air structures or using suitable gas mask or self
contained breathing equipment if necessary.
4) Drums should be stored out of doors, avoiding direct exposure to sunlight.
5) Acetaldehyde should be chilled before transferring and a nitrogen blanket should be used,
1.5.2 Shipping and Storage
Acetaldehyde is shipped in 5,10 or 55 gal drums. Insulated tank trucks and insulated tank cars.
Acetaldehyde in the liquid state is non corrosive to most metals, but it can be easily oxidized to
acetic, especially in the vapor stage. Suitable materials of constructions are stainless steel and
Aluminium. Drums coated with phenolic resins have also been used. If a darker color and some
iron contaminations are not objectionable, carbon steel may be used. Because acetaldehyde is
classed as a flammable liquid, it requires a red DOT (Department of Transportation) shipped
label.Bulk storage held at low temperature and pressure is recommended over storage in a
pressure vessel.
1.6 CAPACITY AND CONSUMPTION
No accurate data are available for world production. Production data are difficult to obtain
because most of the acetaldehyde produced is consumed internally by the manufacturer and
because most acetaldehyde derivatives can be and are produced from other starting materials.
Therefore estimated world production is only crude and should be taken with caution.
1.7 ECONOMIC ASPECTS AND FUTURE TRENDS
The production pattern for acetaldehyde has undergone two significant changes since 1940. At
that time, the principal industrial routes to acetaldehyde were hydration of acetylene and
oxidation of ethyl alcohol. However, increasing acetylene costs made this feed stock
economically unattractive and the industry turned to the oxidation of ethyl alcohol. The
production of acetaldehyde based ethyl alcohol increased from 63.5 kilotons per year in 1940 to
48 kilotons /year in 1960.

Acetaldehyde production is linked with the demand for acetic acid, acetic anhydride, cellulose
acetate, vinyl acetate resins and per acetic acid.
Increased prices for hydrocarbon cracking feed stock beginning in late 1973 resulted in higher
costs for ethylene and concurrent higher costs for acetaldehyde. The future of acetaldehyde
growth appears to depend on the development of a lower cost process based on synthesis gas and
an increase in demand for processes on acetaldehyde activation techniques and per acetic acid.
1.8 USES OF ACETALDEHYDE
About 95% of the Acetaldehyde produced is used internally by the manufacturers as an

intermediate for the production of other organic chemicals. Imports and exports of Acetaldehyde
are negligible.
Acetic acid and anhydride are the major derivatives of Acetaldehyde (45%) followed by n-
butanol (9%) and 2 ethyl hexanol (17%). Twenty percent of the Acetaldehyde is consumed in a
variety of other products, the most important being penta erythrital, Trimethylol propane,
Pyridines, per acetic acid, Crotonaldehyde, chloral, 1,3-butylene glycol and Lactic acid. The
proportion of Acetaldehyde used in the manufacture of acetic acid and acetic anhydride will tend
to increase in near future, and the proportion used in the synthesis of n-butanol and 2-
ethyihexanol will decrease. Acetaldehyde is competing with propylene and x-olefins as the raw
material for the production of nbutanol and higher alcohols. The future growth of Acetaldehyde
will be mainly dictated by the Acetic acid and anhydride picture and the growth of the other
minor derivatives. The largest use of acetaldehyde is as a chemical intermediate for the
production of acetic acid. The production of esters, principally ethyl acetate and isobutyl acetate,
is the second most significant use. It is also used as an intermediate for a number of other
chemicals, including pyridine and pyridine bases, penta erythritol, per acetic acid, 1,3butylene
glycol, and chioral.
Acetaldehyde is also used in silvering mirrors; hardening gelatin fibers; denaturing alcohol; and
in the manufacture of disinfectants, dyes, drugs, explosives, flavorings, phenolic and urea resins,
rubber accelerators and antioxidants, varnishes, and yeast.
Production of Acetaldehyde | 11
Chapter 2
MANUFACTURING PROCESSES

The economics of the various processes for the manufacture of Acetaldehyde are strongly
dependent on the price of the feed stock used since 1960 the liquid phase oxidation of ethylene
has been the process however; there is still commercial production by the partial oxidation
alcohol and the hydration of acetylene.
Acetaldehyde is also formed as a co product in the high temperature oxidation of butane. A

recently developed palladium catalyzed process produces acetaldehyde from carbonylation of
methyl acetate with acetic acid as byproduct.
2.1 OXIDATION OF ETHYLENE
The direct liquid phase oxidation of ethylene was developed in 1957- 9 by Waker-Chemie and
Farbwerke Hoechst. The catalyst is an aqueous solution of PdC12 and CuC12. Phillips observed
the reaction of ethylene with an aqueous Palladium chloride solution to form acetaldehyde.
C2H4+PDCl2+H2O CH3CHO+Pd+2HC1
The metallic palladium is reoxidized to PdC12 with CUC12 and the cuprous chloride formed is
reoxidized with oxygen air
Pd + 2CuC12 PdCl2+ CuC1
2CuC1+ 1/2O2 + 2HC1 2CuC12 + H20
The net result is a process in which ethylene is oxidized continuously through a series of
oxidation reduction reaction.
C2H4 + 1/2O2 CH3CHO
2.2 OXIDATION ETHYL ALCOHOL
Acetaldehyde is produced commercially by the catalytic oxidation of ethyl alcohol. The

oxidation is carried out by passing alcohol vapors and preheated air over a silver catalyst at
480°C
CH3CH2OH + 1/2O2 CH3CHO+H20
With a multitubular reactor, conversions of 74-82% per pass can be obtained while generating
steam to be used elsewhere in the process.

2.3 HYDRATION OF ACETYLENE
Acetaldehyde has been produced commercially by the hydration of Acetylene since 1916.
However the development of the process for the direct oxidation of ethylene in the 1960’s has
almost completely replaced the acetylene-based processes and in 1976 there was only small
volume production in few European countries. In the order processes, acetylene of high purity, is
passed under a pressure of 13.4 k pa (15 psi) into a vertical reactor containing a mercury catalyst
dissolved in 18-25% sulfuric acid at 70-90°C
HC=CH + H2O CH3CHO
2.4 OXIDATION OF SATURATED HYDROCARBONS
Acetaldehyde is formed as a coproduct in the vapor phase oxidation of saturated hydrocarbons,

such as butane or mixtures containing butane, with air or, in higher yield, oxygen. Oxidation of
butane yield acetaldehyde, formaldehyde, methanol, acetone and mixed solvents as major
products; other aldehydes, alcohols, ketones, glycols, acetals, epoxides and organic acids are
formed in smaller concentrations. This is of historic interest. Unlike the acetylene route, it has
almost no chance to be used as a major process.
2.5 FROM SYNTHESIS GAS
A rhodium catalyzed process capable o converting synthesis gas directly into acetaldehyde in a
single step was reported in 1974.
The Process comprises passing synthesis gas over 5% rhodium on SiO2 at 300°C and 2.0 MPa
(20 atm). The principal coproducts are acetaldehyde, 24% Acetic acid, 20%; and ethanol, 16%. If
there will be a substantial degree of coal gasification, the interest in the use of synthesis gas as a
raw material for acetaldehyde production will increase.
2.6 HYDROCARBONYLATION OF METHYL ACETATE
Acetaldehyde is formed in vapor phase. It is hydrocarbonylation process in which methyl acetate

reacts with carbon monoxide and hydrogen gas in boiling reaction zone. The reaction takes place
in the presence of iodine moiety and palladium acetate catalyst.
Low operating conditions 160°C and 310KPa makes the process more economical. Side
reactions are avoided by maintaining the ratio of carbon monoxide and hydrogen i.e.CO:H2=1:5

2.7 COMPARISON OF ACETALDEHYDE PROCESSES
Process Reaction Temp Pressure Catalyst Conversion Yield

phase (ºC) (atm) metal per pass% %
Hydration of Liquid 70-100 1 Mercury, iron 50-60 93-98

acetylene
Partial oxidation of Vapor 480 1 Silver or 70-85 85-95

ethyl alcohol copper
Dehydrogenation of Vapor 260-290 1 Chromium, 30-50 90+

ethyl alcohol copper
Oxidation of Vapor 450 6-7 None 25-35 90

butane
Oxidation of Liquid 100-130 3 Palladium 75 93-95

ethylene
Hydrocarbonylation Vapor 160 3 Palladium 85 85-98

of Methyl acetate
Chapter 3
PROCESS DESCRIPTION

3.1 PROCESS DESCRIPTION
The flow sheet shows the process for conversion of methyl acetate to acetaldehyde. Methyl
acetate, methyl iodide, carbon monoxide and hydrogen are fed to continuous stirred tank reactor.
Methyl acetate, carbon monoxide and hydrogen react in the presence of iodine moiety (methyl
iodide) and catalyst palladium acetate at temperature 160°C and pressure 310KPa.The liquid
reaction mixture being maintained under continuous boiling conditions, whereby a vaporous
product mixture is produced from the boiling liquid reaction mixture. The non-volatile palladium
catalyst remains all times in the reaction zone as a component of boiling liquid body and the
effluent from the reactor in the vapor phase consist only acetaldehyde, acetic acid, methyl
acetate, methyl iodide, carbon monoxide and hydrogen.
The vapor effluent is cooled to condense its condensable components in condenser. Then effluent
is sent to 2-phase separator. As feed is flashed from high pressure 210KPa to low pressure
289KPa, vapor is produced and reaches equilibrium with the remaining liquid. Carbon monoxide
and hydrogen are separated from the methyl acetate, methyl iodide, acetaldehyde and acetic acid.
The vapor stream of 2-phase separator is send to absorber .water is used as solvent for absorption
because acetaldehyde is infinitely soluble in water. Caron monoxide, hydrogen along with small
amount of acetaldehyde and water is sent to atmosphere and can be flared. The bottom stream of
absorber and 2-phase separator are mixed together in static mixer.
The outlet stream of mixer is brought to saturation temperature and sent to distillation column. In
first distillation column acetaldehyde is distilled from acetic acid. Thus acetic acid which is our
by product is recovered in this column. To achieve the required purity the top stream of first
distillation column is pumped to second distillation column .The top product of this column is
acetaldehyde of 99% purity while the bottom stream is methyl acetate containing small amount
of water, acetaldehyde and methyl iodide.
3.2 RAW MATERIAL USAGE
Theoretical yield of methyl acetate is 100mol%.The actual yield of methyl acetate is 85mol%.At
85mol% yield the methyl acetate consumption would be 1977.8Kg/1000Kg acetaldehyde
produced.

3.3 UTILITY REQUIREMENTS
The major energy requirements in the production of acetaldehyde from methyl acetate are to
maintain the reaction temperature, condense the vapor effluent of continuous stirred tank reactor,
and maintain the temperature of flash drum. Other energy requirements include the steam and
water require for heating and cooling purposes in different heat exchangers used in the process.
3.4 TYPICAL ADVANTAGES
The production of acetaldehyde from methyl acetate requires very low operating conditions
i.e.160°C and 310KPa.This process is distinguished from conventional processes wherein the
product effluent is withdrawn as liquid stream. The boiling zone is also distinguished from a
vapor phase zone wherein the reactants and reaction products are essentially in the vapor phase
all times. Under the conditions of continuous boiling the selectivity of acetaldehyde approaches
to 100%.Under these conditions selectivity of acetaldehyde approaches to its theoretical
maximum.

PROCESS FLOW DIAGRAM
P-15
10
12
7
C-100 13
2
9
6
E-100 V-102
V-1
3
8
11
14
4
R-100 16
P-6 E-101
18 15
M-100
P-100 17
5
19 33
1
26
E-102 36
27
30
28
V-100 E-105
V-101 20 37
29
P-101 E-104 34 35
P-23
C-101 P-49
C-102
32
21
38
31
24 41
E-103 E-106
25 39 42
22
40
23

Chapter 4
MATERIAL BALANCE

4.1 MATERIAL BALANCE ACROSS REACTOR R-100
Reactions:
Main Reaction
CH3COOCH3+CO+H2 CH3CHO+CH3COOH
Reaction Steps
(1) CH3COOCH3+CO (CH3CO)2O
(2) (CH3CO)2O+H2 CH3CHO+CH3COOH
(3) CH3CHO+(CH3CO)2O C6H10O4
Side Reaction
Reaction (3) is side reaction which is controlled by maintaining the H2: CO ratio 1:5
Basis: 4897.52 ton/year (514.69 Kg/h) CH3CHO of 97.88% purity
Assumption: 5.326% CH3CHO lost in the process
 1% in Absorber (C-100)
 3.28% in first distillation column (C-101)
 1.05% in second distillation column (C-102)
100% CH3CHO produced = 514.69 x 0.9788 = 503.78 Kg/h
Loss = 503.78 x 0.05326 = 26.831 Kg/h
100% CH3CHO produced = 503.78 + 26.831 = 530.61 Kg/h
= 530.61/44.05 = 12.05 Kg mol/h
CH3COOH produced = 12.05 Kg mol/h
= 12.05 x 60.05 = 723.34 Kg/h
Selectivity=Kg mol of CH3CHO produced / Kg mol of CH3COOCH3 reacted
The theoretical selectivity of the process is 100% so
Kg mol of CH3COOCH3reacted = 12.05 Kg mol/h

= 12.05 x7 4.08
= 892.34 Kg/h
Molar conversion of CH3COOCH3is 85% hence
100% CH3COOCH3 supplied = 12.05/0.85 = 14.17 Kg mol/h
= 14.17 x 74.08 = 1049.82 Kg/h
99.8% CH3COOCH3 supplied = 14.17/0.998 = 14.20 Kg mol/h
= 14.20 x 74.08 = 1051.92Kg/h
CH3COOCH3 Un reacted = 14.20 – 14.17 = 2.15 Kg mol/h
= 2.15 x 74.08 = 59.58 Kg/h
CO reacted = 12.05 Kg mol/h
= 12.05 x 28 = 337.28 Kg/h
100% CO supplied = 12.05/0.85 = 14.17Kgmol/h
99.8% CO supplied = 12.05/.998 = 14.20Kgmol
= 314.20 x 28 = 397.59Kg/h
CO un reacted = 14.20 -12.05 = 2.15 Kg mol/h
= 2.15 x 28 = 60.32 Kg/h
(CH3CO)2O formed = 12.05 Kg mol/h
((CH3CO)2O consumed = 12.05 Kg mol/h
The Hydrogen to carbon monoxide ratio is maintained to control the side reaction H2: CO=1:5
H2 reacted = 12.05 Kg mol/h
H2 supplied = 12.05 x 5 = 71 Kg mol/h
= 71 x 2 = 142Kg/h
H2 un reacted = 71 – 12.05 = 58.95 Kg mol/h
= 58.95 x 2 = 117.91 Kg/h
Catalyst and Promoter
CH3COOPd and CH3I are used as catalyst and P(C4H9)3 is used as promoter
CH3I used = CH3COOCH3 supplied x 0.2
= 14.17 x 0.2 = 2.83 Kg mol/h
= 2.83 x 141.94 = 402.3 Kg/h
CH3COOPd used = 0.01% of liquid reaction mixture
Liquid reaction mixture = CH3COOCH3+CH3I
= 1051.92 + 402.3 = 1454.22 Kg/h
CH3COOPd used = (0.01/100) x 1454.22 = 0.15 Kg/h
= 0.15/224.5 = 6.48x10-3Kg mol/h
P(C4H9)3 used = Kg mol of CH3COOPd x 2
= 6.48x10-3 x 2
= 0.001296 Kg mol/h
= 0.001296 x 202.32 = 0.26 Kg/h
The inlet and outlet flows of different components are shown below in tabulate form.
Stream Inlet Streams Outlet Stream
Stream name liquid Bottom Vapor
Stream Flow rate Kg/h Kg mol/h Kg/h Kg mol/h Kg/h Kg mol/h
CH3COOCH3 1051.92 14.20 0.00 0.00 159.58 2.15
CH3I 402.30 2.83 0.00 0.00 402.30 2.83
CO 0.00 0.00 396.80 14.20 60.32 2.15
H2 0.00 0.00 142.00 71.00 117.91 58.95
CH3CHO 0.00 0.00 0.00 0.00 530.61 12.05
CH3COOH 0.00 0.00 0.00 0.00 723.34 12.05
Total 1454.22 17.03 538.80 85.20 1994.05 90.19
4.2 MATERIAL BALANCE ACROSS 2-PHASE SEPARATOR
Two phase separator is operating at 94°C and 289Kpa.Overall balance across separator is
F = V + L
90.19 = V + L
The overall mol fraction (Zi) of entering stream is as follows:
CH3COOCH3 = 0.02
CH3I = 0.03
CO = 0.02
H2 = 0.65
CH3CHO = 0.13
CH3COOH = 0.13
The vapor pressures (KPa) of pure species at 94°C are as follows;
PsatCH3COOCH3 = 314.9
PsatCH3I = 468.4
PsatCO = 289
PsatH2 = 289
PsatCH3CHO = 931.2
PsatCH3COOH = 46.13
First, we do Bubble P calculation with (Zi) = (Xi) to determine Pbubl
Pbubl = ∑ (XI Pisat )
= 341KPa
Second, we do dew P calculation with (Zi) = (Yi) to determine Pdew
Pdew = 1/∑ (YI Pisat )
= 185KPa
Since the given pressure lies between Pbubl and Pdew , the system is in two phase region and a flash
calculation can be made.
As Ki = Pisat/P
K CH3COOCH3 = 1.0896
K CH3I = 1.62
KCO = 1
K H2 = 1
KCH3CHO = 3.222
KCH3COOH = 0.1596
Now using the relation
∑ Zi Ki/[1+V(Ki-1)] = 1
Solution for V by trial yields:
V = 83.33Kgmol/h
L = 6.86Khmol/h
To determine the mol fraction of top and bottom stream following relations are followed.
Yi = Zi Ki /[1+V(Ki-1)]
Xi = Yi / Ki
The amounts and the fractions of components are represented below in tabulated form
Stream Inlet Stream Outlet Streams
Stream Name Feed Top Bottom
Flowrate Kg/h Xmol Kgmol/h Kg/h Xmol Kgmol/h Kg/h Xmol Kgmol/h
CH3COOCH3 159.58 0.02 2.15 124.48 0.02 1.68 35.10 0.07 0.47
CH3I 402.30 0.03 2.83 340.00 0.03 2.40 62.29 0.06 0.44
CO 60.32 0.02 2.15 60.32 0.03 2.15 0.00 0 0.00
H2 117.91 0.65 58.95 117.91 0.71 58.95 0.00 0 0.00
CH3CHO 530.61 0.13 12.05 487.62 0.0.13 11.07 42.99 0.14 0.98
CH3COOH 723.34 0.13 12.05 425.03 0.08 7.08 298.31 0.0.72 4.97
Total 1994.05 1.00 90.19 1555.36 1.000 83.33 438.69 1.000 6.86
4.3 MATERIAL BALANCE ACROSS ABSORBER C-100
In absorption, absorption factor L/KV for a relatively dilute component in the gas phase
determines how readily that component will absorb in the liquid phase. Here L and V are the
liquid and gas flow rate respectively and K is the vapor liquid equilibrium value for that
component. When the absorption factor for the given component is large, its absorptivity in the
liquid is increased. When the absorption factor is increased by increasing the liquid flow rate, the
number of trays in the column required to achieve specified separation decreases. However at
high values of absorption factor, an increase in liquid flow rate achieves diminishing returns.
Accordingly, an optimum for process design has been established, namely, 1.2<L/KV<2.0.
In the material balance across absorber we are using here L/KV=1.22. From this we will
determine the flow rate of liquid entering.
Assumption: Exit gas is saturated with liquid (water).
The column is operating at 261.29 KPa. Water is entering at 25°C.
Feed Flow rate = 83.33 Kgmol/h
CH3CHO in Feed = 11.07 Kg mol/h
Mol fraction = 0.13
Feed inlet pressure = 288.8 KPa
Operating Pressure = 261.29 KPa
Partial Pressure of CH3CHO in Feed
= 0.13 x 288.8 = 38.36KPa
99% recovery of CH3CHO is required so
Partial Pressure of CH3CHO in exit gas
= 38.36 x 0.01 = 0.38 KPa
CH3CHO in Exit gas = 11.07 x 0.01 = 0.1107 Kg mol/h
CO in exit gas = 2.15 Kg mol/h
H2 in exit gas = 58.95 Kg mol/h
Total gaseous component in exit gas
= 0.1107 +2.15 + 58.95
= 61.22 Kg mol/h
Partial pressure of H2O = 1.70 KPa
Y H2O in exit gas = 1.70/261.29 = 0.0065
Ygas = 1 – 0.0065 = 0.9935
Exit gas flow rate = 61.22/0.9935 = 61.618 Kg mol/h
H2O in exit gas = 61.618 – 61.22 = 0.40 Kg mol/h
Liquid Flow rate
As partial pressure of CH3CHO in exit gas is 38.36 KPa so from equilibrium data of
acetaldehyde and water system w/w% corresponding to 39.9 KPa (which is close enough to
38.36 KPa) is 2.5%.
Kg mol of CH3CHO = 2.5/44.05 = 0.0567
Kg mol of H2O = (100-2.5)/18 = 5.416
Total Kg mol = 0.0567 + 5.416 = 5.473
Vapor fraction of CH3CHO
y = 39.9/261.29 = 0.1527
Liquid fraction of CH3CHO
x = 0.0567/5.473 = 0.0104
K = y/x = 14.727
Let
L/KV = 1.22
L = 14.727 x 83.33 x 1.22
= 1497.19 Kg mol/h
= 26949.46 Kg/h
The flow rates and compositions of inlet and outlet streams are shown below in tabulated form
Stream Inlet Streams Outlet streams
Name Feed Inlet Liquid Inlet Exit Gas Exit Liquid
Flow rate Kg/h Kgmol/h Kg/h Kgmol/h Kg/h Kgmol/h Kg/h Kgmol/h
CH3COOCH3 124.48 1.68 0.00 0.00 0.00 0.00 124.48 1.68
CH3I 340.00 2.40 0.00 0.00 0.00 0.00 340.00 2.40
CO 60.32 2.15 0.00 0.00 60.32 2.15 0.00 0.00
H2 117.91 58.95 0.00 0.00 117.91 58.95 0.00 0.00
CH3CHO 487.62 11.07 0.00 0.00 4.88 0.11 482.74 10.96
CH3COOH 425.03 7.08 0.00 0.00 0.00 0.00 425.03 7.08
H2O 0.00 0.00 26949.46 1497.19 7.21 0.40 26942.25 1496.79
Total 1555.36 83.33 26949.46 1497.19 190.31 61.62 28314.51 1518.90
4.4 MATERIAL BALANCE ACROSS DISTILLATION COLUMN C-101
C-101 is water recovery column.99% acetic acid of purity 2.58% is recovered in this column
because of high relative volatility difference
Assumption: 3.28% CH3CHO does not recover in C-101
F = D + W
28753.20 = D + W
Acetic acid at top = 0 Kg mol/h
Acetic acid at bottom = 12.05 Kg mol/h
= 723.34 Kg/h
Bottom flow rate = 723.34/0.0258
= 28048.694 Kg/h
Top Flow rate = 28753.20 – 28048.694
= 704.57 Kg/h
The top and bottom compositions are determined using HYSYS simulator and are represented
here in tabulated form
Name Feed Top Bottom
Flow rate Kg/h Kgmol/h Kg/h Kg mol/h Kg/h Kgmol/h
CH3COOCH3 159.58 2.15 159.02 2.15 0.56 2.15
CH3I 402.30 2.83 34.27 0.24 368.03 2.83
CH3CHO 525.74 11.93 508.59 11.55 17.15 0.39
CH3COOH 723.34 12.05 0.00 0.00 723.34 12.05
H2O 26942.25 1496.79 2.67 0.15 26939.58 1496.64
Total 28753.20 1525.76 704.57 14.08 28048.64 1514.07
4.5 MATERIAL BALANCE ACROSS DISTILLATION COLUMN C-102
C-102 is acetaldehyde (which is main product) recovery column.99.95% acetaldehyde of purity

97.88% is recovered in this column because of high relative volatility difference of acetaldehyde
and other components.
Assumption: 1.05 % CH3CHO does not recover in C-102
F = D + W
704.57 = D + W
Acetaldehyde at top = 11.42 Kg mol/h = 503.247 Kg/h
Acetaldehyde at bottom = 0.12 Kg mol/h = 5.34 Kg/h
Top flow rate = 503.247/0.9788
= 514.1469 Kg/h
Bottom Flow rate = 704.57 – 514.1469
= 190.42 Kg/h
The top and bottom compositions are determined using HYSYS simulator and are represented
here in tabulated form
Name Feed Top Bottom
Flow rate Kg/h Kg mol/h Kg/h Kg mol/h Kg/h Kg mol/h
CH3COOCH3 159.02 2.15 0.13 0.001714 158.89 2.14
CH3I 34.27 0.24 10.78 0.075941 23.49 0.17
CH3CHO 508.59 11.55 503.24 11.42431 5.35 0.12
H2O 2.67 0.15 0 0 2.67 0.15
Total 704.57 14.08 514.1469 11.50196 190.40 2.58
4.6 OVERALL MATERIAL BALANCE
Inlet Stream Mass Flow (Kg/h)
Liquid inlet stream of reactor R-100 1454.22
Gas inlet stream of reactor R-100 538.80
Water inlet stream of absorber C-100 26949.46
Total Mass input to plant 28943
Outlet Stream Mass Flow (Kg/h)
Gas outlet stream of absorber C-100 190.31
Bottom Product stream of distillation column C-101 28048.64
Bottom Product stream of distillation column C-102 190.40
Top Product stream of distillation column C-102 514.15
Top mass output from plant 28943
Chapter 5
ENERGY BALANCE

5.1 ENERGY BALANCE ACROSS REACTOR R-100
Heat of Reaction
Reaction completes in two steps which are as follows
(1) CH3COOCH3+CO (CH3CO)2O H= -56000KJ/mol
(2) (CH3CO)2O+H2 CH3CHO+CH3COOH H = -23000KJ/mol
Reaction temperature 160°C
Reaction Pressure 310.2 KPa
Reference temperature 25°C
Reference Pressure 101.3 KPa
Reaction (1)
The following schematic shows the procedure for calculating heat of reaction for first reaction
(160°C) CH3COOCH3 + CO (CH3CO)2O (160°C)
(25°C) CH3COOCH3 + CO (CH3CO)2O (25°C)
H CH3COOCH3 = 160 m CpdT

25
= 12.05 x (-45000)
= -542250 KJ/h
H CO = 160 m CpdT
25
= 12.05 x (-4000)
= -48200 KJ/h
H°25 = 12.05 x (-56000)
= -674800 KJ/h
H(CH3CO)2O = 25
160
m CpdT
= 12.05 x (28400)
= 342220 KJ/h
HRex1 = H CH3COOCH3 + H CO + H°25 + H(CH3CO)2O

= -542250 + (-48200) + (-674800) + 342220
= -923030 KJ/h
Reaction (2)
The following schematic shows the procedure for calculating heat of reaction for first reaction
(160°C) (CH3CO)2O + H2 CH3CHO + CH3COOH (160°C)
(25°C) (CH3CO)2O + H2 CH3CHO + CH3COOH (25°C)
H(CH3CO)2O = 160 m CpdT

25
= 12.05 x (28400)
= -342220 KJ/h
H H2 = 160 m CpdT
25
= 12.05 x (-3959)
= -47706KJ/h
H°25 = 12.05 x (-23000)
= -277150 KJ/h
H CH3COOH = 25
160
m CpdT
= 12.05 x (35900)
= 432595 KJ/h
H CH3CHO = 25
160
m CpdT
= 12.05 x (8400)
= 101220 KJ/h
H Rex2 = H(CH3CO)2O + H H2 + H25 + H CH3COOH + H CH3CHO
= -342220 + (-47706) + (-277150) + (432595) + (101220)
= -133261 KJ/h
H Reaction = H Rex1 + H Rex2
= (-923030) + (-133261)
= -1056291 KJ/h
= -1.06 x 106 KJ/h
Heat duty of Reactor(R-100)
Q = H Products - (H Reactants + H Reaction)
Reactants
Component Temperature(C) Pressure (KPa)
CH3COOCH3 25 312
CH3I 25 312
CO 160 368
H2 160 368

25
= 14.2 x 136.7
= 1941.14 KJ/h
H CH3I = 25 m CpdT

25
= 2.8 x 152.9
= 428.12
25
= 14.2 x 198.6
= 2820.12 KJ/h
H H2 = 160 m CpdT
25
= 71 x 3859
= 273989 KJ/h
H Reactants = 279179.6 KJ/h
Products
Component Temperature(C) Pressure (KPa)
CH3COOCH3 160 310.2
CO 160 310.2
H2 160 310.2
CH3CHO 160 310.2
CH3COOH 160 310.2
H Products = H CH3COOCH3 + H CO + H H2 + H CH3CHO + H CH3COOCH3
H CH3COOCH3 = 160
25
m CpdT
= 2.15 x (-397000)
= -855181.28 KJ/h
H CH3I = 160
25
m CpdT
= 2.83 x 206300
= 584711.8 KJ/h
25
= 2.15 x (-106600)
= -229628.2 kJ/h
H H2 = 160 m CpdT
25
= 58.95 x 3859
= 227500.75 KJ/h
H CH3CHO = 160 m CpdT

25
= 12.05 x (-156000)
= -1879127.1 KJ/h
H CH3COOH = 160
25
m CpdT
= 12.05 x (-424700)
= -5115803.2 KJ/h
H Products = -7267527 KJ/h
Q = H Products - (H Reactants + H Reaction )
= -7297527 - (279179.6 - 7267527)
= -6490416 KJ/h
= -6.5 x 106KJ/h
This heat must be removed to maintain the reaction temperature 160°C.For removing heat
process water at 10°C is used here. Let ∆T for water is 8 so the outlet temperature of water will
be 18°C.
The flow rate of cooling water can be determined assuming
Heat lost by hot fluid = Heat gained by cold fluid
Q = m Cp ∆T
m = -6.5 x 106 /(8 x 76.41)
= 11484.1 Kg/h
5.2 ENERGY BALANCE ACROSS CONDENSER E-100
Main purpose of condenser E-100 is the separation of condensable components from non
condensable components (CO and H2).The vapour stream enters the condenser at 160°C and
leaves at temperature 94°C.
Assumption: Pressure drop across condenser is 11.2KPa
The conditions of inlet and outlet streams are as follows;
Stream Temperature(C) Pressure

(KPa)
Inlet 160 310.2
Outlet 94 299
Inlet Stream
As the inlet stream of condenser E-100 is the outlet stream of reactor so there is no need to
calculate the enthalpy of this stream. Its enthalpy is same as that the enthalpy of outlet vapor
stream of reactor R-100.
HInlet = -7267527 KJ/h
Outlet Stream

25
= 2.15 x (-402100)
= -866167.2 KJ/h
HCH3I = 94 m CpdT

25
= 2.83 x 17950
= 50875.3KJ/h
HCO = 94 m CpdT

25
= 2.15 x (-108000)
= -232643.8KJ/h
HH2 = 94 m CpdT
25
= 58.95 x 2589
= 152630.1KJ/h
HCH3CHO = 94 m CpdT

25
= 12.05 x (-159300)
= -1918878KJ/h
HCH3COOH = 94 m CpdT

25
= 12.05 x (-466900)
= -5624131.1KJ/h
HOutlet = H CH3COOCH3 + HCH3I + HCO + HH2 + HCH3CHO + HCH3COOH
= -8438314.65 KJ/h
Heat duty
Q = Houtlet - HInlet
= (-8438314.65) - (-7267527)
= -1170788KJ/h
= -1.17 x 106 KJ/h
The process water is used as cooling media for condensation. Process water is entering at 10°C
and leaving at 18°C.∆T for water stream is taken 8°C for economical reasons. The flow rate of
water require to condense vapors can be determined assuming
Q = m Cp ∆T
m = 1170788/ (8 x 76.41) = 1915.3 Kg/h
5.3 ENERGY BALANCE ACROSS 2-PAHSE SEPARATOR V-102
Two phase separator operates at constant pressure and constant temperature conditions. Here
gaseous phase contain all carbon monoxide and hydrogen along with other components becomes
separates from liquid phase. The amounts of components in gaseous and liquid phases are
mentioned in material balance across 2-phase separator.
Enthalpy of Inlet Stream

25
= 2.15 x (-404200)
= -870690.86KJ//h

25
= 2.83 x 16830
= 47701KJ/h

25
= 2.15 x (-180600)
= -233936.24KJ/h

25
= 58.95 x 1968
= 116020.1KJ/h

25
= 12.05 x (-160700)
= -1935742KJ/h

25
= 12.05 x (-469600)
= -5656655KJ/h
Hinlet = H CH3COOCH3 + HCH3I + HCO + HH2 + HCH3CHO + HCH3COOH
= -8533302.4KJ/h
= -8.53 x 106KJ/h
Top Stream

25
= 1.68 x (-404200)
= -679201.61KJ//h

25
= 2.40 x 16830
= 40314.62KJ/h

25
= 2.15 x (-180600)
= -233936.24KJ/h

25
= 58.95 x 4968
= 116020.08KJ/h

25
= 11.07 x (-160700)
= -1778902.48KJ/h

25
= 7.08 x (-469600)
= -3323824.63KJ/h
HTop = H CH3COOCH3 + HCH3I + HCO + HH2 + HCH3CHO + HCH3COOH
= -5.86 x 106 KJ/h
Bottom Stream

25
= 0.47 x (-404200)
= -191489KJ//h

25
= 0.44 x 16830
= 7386.296KJ/h

25
= 0.98 x (-160700)
= -156839KJ/h

25
= 4.97 x (-469600)
= -2332830KJ/h
HBottom = H CH3COOCH3 + HCH3I + HCH3CHO + HCH3COOH
= -2.67 x 106 KJ/h
Enthalpy balance
Hinlet = Htop + HBottom
-8.53 x 106 = -5.86 x 106 + -2.67 x 106
-8.53 x 106 = -8.53 x 106
5.4 ENERGY BALANCE ACROSS ABSORBER C-100
In absorber(C-102) water is being used as solvent because acetaldehyde is infinitely soluble in

this solvent. Moreover it is cheaper one. Process water stream is coming from cooling tower at
25C°.
Assumption: (1) Leaving Gas is saturated with water
(2) P in the absorber is 21KPa
The conditions of inlet and outlet streams of absorber are as follows;

(KPa)
Feed inlet 94 289
Water inlet 25 268
Gas outlet 25 266
Liquid outlet 32 287
Feed inlet Stream
The enthalpy of inlet stream of absorber is same as that of top stream of separator V-100 i.e.
HFeed = -5.86 x 106 KJ/h
Water inlet Stream
HH2O = 25 m CpdT

25
= 1497.19 x (-2.849 x 105)
= -4.27 x 108KJ/h
Gas outlet Stream

25
= 2.15 x (-1.06 x 105)
= -6.67 x 106 KJ/h
25
= 58.95 x 0
= 0 KJ/h

25
= 0.11 x (1.0899 x 105)
= -9.27 x 105KJ/h

25
= 0.40 x (-2.848 x 105)
= -114068.39KJ/h
Hgas = -354468.42 KJ/h
= -3.54 x 105KJ/h
Liquid outlet Stream
We assume the temperature of liquid outlet stream and make energy balance across absorber. If
energy streams are balance then our assumed temperature is correct. Let the temperature of
liquid outlet stream be 32°C.
HCH3COOCH3 = 32 m CpdT

25
= 1.68 x (-4.407 x 105)
= -740534.76 KJ/h

25
= 2.4 x (-1.454 x 104)
= -34829.2 KJ/h

25
= 10.96 x (-1.893 x 105)
= -2074541.2 KJ/h
25
= 7.08 x (-4.06 x 105)
= -2873664.4KJ/h
HH2O = 32 m CpDt

25
= 1496.79 x (-2.844 x 105)
= -425687524KJ/h
HLiquid = -4.31 x 108 KJ/h
Enthalpy Balance
HFeed +Hwater = Hgas + Hliquid
-5.86 x 106+(-4.27x108) = -3.54 x 105 + (-4.31 x 108)
4.32 x 108 KJ/h = 4.32 x 108 KJ/h
5.5 ENERGY BALANCE ACROSS MIXER M-100
In mixer the bottom stream of absorber (C-100) and bottom stream of separator are mixed
together. The basic purpose of mixer here the mixing of these streams so that maximum product
can be recovered in next equipments.
Assumption: The outlet stream leaves the mixer at lowest inlet conditions i.e.32°C and 287KPa
The conditions of outlet and inlet streams are shown below

(KPa)
Separator bottom stream 94 289
Absorber bottom Stream 32 287
Outlet Liquid 32 287
There is no need to calculate again the enthalpies of separator bottom stream and absorber
bottom stream because these are already calculated. At this step only enthalpy calculation of
outlet stream of mixer are done and then the difference of outlet and inlet streams gives the
amount of energy require for mixing.
Separator bottom Stream
HBottom = -2.67 x 106 KJ/h
Absorber bottom stream
HLiquid = -4.31 x 108 KJ/h
Hinlet = (-2.67 x 106) + (-4.31 x 108)
= -4.34 x x108KJ/h
Mixer outlet Stream
HCH3COOCH3 = 32 m CpdT

25
= 2.15 x (-4.407 x 105)
= -9.49 x 105KJ/h

25
= 2.83 x (-1.454 x 104)
= -4.12 x 104KJ/h

25
= 11.93 x (-1.893 x 105)
= -2.26 x 106KJ/h

25
= 12.05 x (-4.06 x 105)
= -5.58 x 106KJ/h
25
= 1496.79 x (-2.844 x 105)
= -4.3 x 108KJ/h
Houtlet = (-9.49 x 105)-(4.12 x 104)-(2.26 x 106)–(5.58 x 106)– (4.3 x 108)
= -4.35 x 108KJ/h
Energy require for mixing
Q = (-4.35 x 108) - (-4.34 x 108)
= -1.0 x 108KJ/h
5.6 ENERGY BALNCE ACROSS HEAT EXCHANGER E-101
The outlet stream of mixture is the inlet stream of heat exchanger E-101.This exchanger brings
the process stream to its saturation temperature 115.7°C. The heating media used to fulfill this
purpose is saturated steam at 170°C.The conditions of inlet and outlet streams of E-101 are as
follows;

(KPa)
Process stream Inlet 32 287
Process stream outlet 115.7 241.3
Steam inlet 170 792.02
Steam outlet 170 778.2
Process inlet stream
Hinlet = -4.35 x 108KJ/h
Process outlet stream
HCH3COOCH3 = 115.7 m CpdT

25
= 2.15 x (-4.02 x 105)
= -8.66 x 105KJ/h
HCH3I = 115.7 m CpdT
25
= 2.83 x (1.802 x 104)
= 5.11 x 104KJ/h
HCH3CHO = 115.7 m CpdT

25
= 11.93 x (-1.59 x 105)
= -1.90 x 106KJ/h
HCH3COOH = 115.7 m CpdT

25
= 12.05 x (-4.67 x 105)
= -5.62 x 106KJ/h
HH2O = 115.7 m CpdT

25
= 1496.79 x (-2.78 x 105)
= -4.16 x 108KJ/h
Houtlet = -4.25 x 108KJ/h
Heat duty of E-101
Q = (-4.25 x 108) - (-4.35 x 108)
= 9.92 x 106KJ/h
Flow ate of steam
Assumption
QH = QC
m = QH/λ
= 9.92 x 106/37450
= 265Kgmol/h
= 4770Kg/h
5.7 ENERGY BALANCE ACROSS DISTILLATION COLUMN C-101
C-101 is acetic acid recovery column which is byproduct of the process. The first step in the
energy balance of distillation column is the estimation of top and bottom temperatures. The feed
is saturated liquid at 115.7°C and 241.3KPa.
Assumptions:
1. Reboiler is operating at 230KPa

2. Condenser is operating at 210KPa
3. ∆P in column is 20KPa
Estimation of top temperature Td
By dew point calculation ∑(Xd/K)=1
Component Xd K at 52.6°C Xd/K
Methyl acetate 0.15 0.4275 0.36
Methyl iodide 0.02 0.6705 0.03
Acetaldehyde 0.82 1.432 0.57
Water 0.01 0.2361 0.04
∑Xd = 1.00 ∑(Xd/K )= 1.00
So the top stage temperature is 52.6°C.
Estimation of bottom temperature Tw
By a boiling point calculation ∑(Xd/K)=1
Component Xw K at 124.2°C Xw * K
Methyl acetate 5 x 10-6 47.71 0.000237
Methyl iodide 0.002 3.939 0.006756
Acetaldehyde 0.00026 38.12 0.009817
Acetic acid 0.0079 1.126 0.008972
Water 0.99 0.9844 0.974608
∑Xw = 1.00 ∑(Xw * K ) = 1.00
So the bottom stage temperature is 124.2°C.
Condenser outlet temperature
Assume that the outlet stream of condenser is saturated liquid. So temperature of this saturated
stream can be determined by boiling point calculations at condenser pressure i.e.210KPa
By a bubble point calculation ∑(Xd * K) = 1
Component Xd K at 45.14°C Xd *K
Methyl acetate 0.15 0.3171 0.0483
Methyl iodide 0.02 0.5537 0.00949
Water 0.01 0.1454 0.00153
∑Xd = 1.00 ∑(Xd * K )= 1.00
So the condenser outlet temperature is 45.14°C.
Enthalpy of Feed Stream
The conditions of feed stream of C-101 column as same as that of the outlet stream of heat
exchanger E-101.So there is no need again to calculate the enthalpy of this stream.
∆H Feed = -4.25 x 108KJ/h
Condenser inlet stream

25
= 2.15 x (-4.38 x 105)
= - 9.4 x 105KJ/h

25
= 0.24 x (-1.27 x 104)
= -3.07 x 103KJ/h

25
= 11.55 x (-1.63 x 105)
= -1.88 x 106KJ/h
HH2O = 52.6 m CpdT

25
= 0.15 x (-2.83 x 105)
= -4.19 x 104KJ/h
Hinlett = -2865547.2KJ/h
Condenser outlet stream (Top stream Enthalpy)

25
= 2.15 x (-4.39 x 105)
= - 9.42 x 105KJ/h

25
= 0.24 x (-1.34 x 104)
= -3.23 x 103KJ/h

25
= 11.55 x (-1.63 x 105)
= -1.89 x 106KJ/h
HH2O = 45.14 m CpdT

25
= 0.15 x (-2.83 x 105)
= -4.20 x 104KJ/h
Houtlet = -2872557.9KJ/h
HTop = -2872557.9KJ/h
Condenser Duty
QC = (-2872557.9) - (-2865547.2)
= -7011KJ/h
Enthalpy of Bottom stream
Bottom stream is leaving at 124.2°C and 230KPa
124.2 m CpdT
25
.HCH3COOCH3 =
= 0.01 x (-4.01 x 105)
= -3.01 x 103KJ/h

25
= 2.59 x (1.87 x 104)
= 4.86 x 104KJ/h

25
= 0.39 x (-1.58 x 105)
= -6.17 x 104KJ/h
HCH3COOH = 124.2 m CpdT
25
= 12.05 x (-4.51 x 105)
= -5.53 x 106KJ/h
HH2O = 124.2 m CpdT

25
= 1496.64 x (-2.77 x 105)
= -4.15 x 108KJ/h
HBottom = -4.21 x 108KJ/h
Reboiler Duty
Applying overall energy balance across column C-101
HFeed + QR = QC + Htop + HBottom
QR = 1102054 KJ/h
5.8 ENERGY BALANCE ACROSS HEAT EXCHANGER E-104
The top product of C-101 passes through pump. This pump increases its pressure from 210KPa
to 282KPa. The outlet stream of pup enters the heat exchanger E-101.This exchanger brings the
process stream to its saturation temperature 52.12°C. The heating media used to fulfill this
purpose is saturated steam at 100°C.The conditions of inlet and outlet streams of E-101 are as
follows;

(KPa)
Process stream Inlet 45.13 282
Process stream outlet 52.12 262
Steam inlet 100 101.3
Steam outlet 100 101.3
Process inlet stream

25
= 2.15 x (-4.39 x 105)
= - 9.42 x 105KJ/h

25
= 0.24 x (-1.34 x 104)
= -3.23 x 103KJ/h

25
= 11.55 x (-1.88 x 105)
= -2.17 x 106KJ/h
HH2O = 45.14 m CpdT

25
= 0.15 x (-2.83 x 105)
= -4.20 x 104KJ/h
Hinlet = -3156581.6KJ/h
Process outlet stream

25
= 2.15 x (-4.38 x 105)
= - 9.40 x 105KJ/h

25
= 0.24 x (-1.28 x 104)
= -3.08 x 103KJ/h

25
= 11.55 x (-1.63 x 105)
= -1.88 x 106KJ/h
HH2O = 52.12 m CpdT
25
= 0.15 x (-2.83 x 105)
= -4.19 x 104KJ/h
Houtlet = -2865556.85KJ/h
Heat Duty
QC = (-2865556.85) - (-3156581.6K)
= 291025KJ/h
Steam Flow rate
Assumption
QH = QC
m = QC/λ
= 291025/40780
= 7.136Kgmol/h
= 128.45Kg/h
5.9 ENERGY BALANCE ACROSS DISTILLATION COLUMN C-102
C-102 is acetaldehyde recovery column which is main product of the process. The first step in
the energy balance of distillation column is the estimation of top and bottom temperatures. The
feed is saturated liquid at 52.12°C and 262KPa.
Assumptions:
1. Reboiler is operating at 240KPa

2. Condenser is operating at 220KPa
3. ∆P in column is 20KPa
Estimation of top temperature Td
By a dew point calculation ∑(Xd/K)=1
Component Xd K at 42.51°C Xd/K
Methyl acetate 0.00015 0.2717 0.00055
Methyl iodide 0.0066 0.4901 0.0135
∑Xd = 1.00 ∑(Xd/K )= 1.00
So the top stage temperature is 42.51°C.
Estimation of bottom temperature Tw
By a boiling point calculation ∑(Xd/K)=1
Component Xw K at 79.65°C Xw * K
Methyl acetate 0.83 0.8943 0.7435
Methyl iodide 0.06 1.191 0.0764
Water 0.06 1.077 0.06184
∑Xw = 1.00 ∑(Xw * K ) = 1.00
So the bottom stage temperature is 79.65°C.
Enthalpy of Feed Stream
The conditions of feed stream of C-102 column as same as that of the outlet stream of heat
exchanger E-102.So there is no need again to calculate the enthalpy of this stream.
∆H Feed = -2865556.85KJ/h
Condenser inlet stream
HCH3COOCH3 = 42.51 25 m CpdT
= 0.0017 x (-4.39 x 105)
= - 7.53 x 102KJ/h
HCH3I = 42.51 25 m CpdT
= 0.076 x (-1.36 x 104)
= -1.03 x 103KJ/h
HCH3CHO = 42.51 25 m CpdT
= 11.424 x (-1.63 x 105)
= -1.87 x 106KJ/h
Hinlet = -1868518.5KJ/h
Condenser outlet stream (Top stream Enthalpy)
HCH3COOCH3 = 20 25 m CpdT
= 0.0017 x (-4.42 x 105)
= - 7.58 x 102KJ/h
HCH3I = 20 25 m CpdT
= 0.076 x (-1.55 x 104)
= -1.18 x 103KJ/h
HCH3CHO = 20 25 m CpdT
= 11.424 x (-1.90 x 105)
= -2.18 x 106KJ/h
Houtlet = -2177125.8KJ/h
Condenser Duty
QC = (-2177125.8) - (-1868518.5)
= -308607.28KJ/h
Enthalpy of Bottom stream
Bottom stream is leaving at 79.65°C and 240KPa.
25
= 2.14 x (-4.34 x 105)
= -9.31 x 105KJ/h

25
= 0.17 x (1.65 x 104)
= 2.73 x 103KJ/h

25
= 0.12 x (-1.61 x 105)
= -1.96 x 104KJ/h
HH2O = 79.65 m CpdT

25
= 0.15 x (-2.81 x 105)
= -4.16 x 104KJ/h
HBottom = -989117.25KJ/h
Reboiler Duty
Applying overall energy balance across column C-101
HFeed + QR = QC + Htop + HBottom
QR = -609283.43 KJ/h
5.10 OVEALL ENERGY BALANCE
Inlet Stream Enthalpy (KJ/h)
Liquid inlet stream of R-100 2.37 x 103
Gas inlet stream of R-100 2.77 x 105
Water inlet stream of absorber C-100 4.27 x 108
Mixing energy of mixer M-100 2.62 x 104
Heat Exchanger E-101 duty 9.92 x 106
Heat Exchanger E-102 duty 2.91 x 105
Reboiler duty of distillation column C-101 1.10 x 106
Reboiler duty of distillation column C-102 6.09 x 105
Total energy input to plant 4.39 x 108
Outlet Stream Enthalpy (KJ/h)
Heat duty of reactor R-100 6.49 x 106
Heat duty of Condenser E-100 1.17 x 106
Gas exit stream of Absorber C-100 3.54 x 105
Condenser duty of distillation column C-101 7.01 x 103
Condenser duty of distillation column C-102 3.05 x 105
Enthalpy of bottom stream of distillation column C-101 4.21 x 108
Enthalpy of bottom stream of distillation column C-102 9.89 x 105
Enthalpy of top stream of distillation column C-102 2.18 x 106
Total energy output of the plant 4.32 x 108
Chapter 6
REACTOR DESIGN

6.1 SELECTION OF REACTOR
The production of acetaldehyde from methyl acetate involves gas-liquid reaction. Gas-liquid
reactors are basically used for two purposes.
 For making a particular product such as chlorobenzene by the reaction of gaseous

chlorine with liquid benzene.
 For separation of a constituent such as the separation of CO2 from a gaseous mixture
using either water, caustic soda or potassium carbonate
The reactors used for carrying out gas-liquid reactions are as follows;
 Packed Column
 Spray column
 Tray column
 Simple Bubble column
 Packed bubble column
 Agitated tank
6.1.2 PACKED COLUMN
Packed column is conventionally used when the purpose is to absorb a constituent from a gas. The liquid
is distributed over the packing, and the gas forms the continuous phase. The pressure drop for the gas is
relatively low and the packed column is therefore very suitable for treating large volume flows of gas
mixtures.
6.1.3 SPRAY COLUMN

This is similar to packed column but in the packed column liquid hold-up is comparatively low. Here gas
is in continuous phase while liquid is in dispersed phase.
6.1.4 TRAY COLUMN
In the sieve tray column gas is dispersed in the liquid passing over the tray. Because the tray is
relatively shallow, the pressure drop in the gas phase is fairly low, and liquid hold-up, although a
little larger than for a packed column, is still relatively small. Tray column is useful when
stepwise operation and relatively large volumetric flow rate of gas is to be treated.
6.1.5 SIMPLE BUBBLE COLUMN
The bubble column is simply a vessel filled with liquid, with a sparger ring at the base for
dispersing the gas. In some cases the draft tube is used to direct recirculation of the liquid and to

influence the bubble motion. One of the disadvantages of the simple bubble column is that
coalescence of the bubble tends to occur with the formation of large slugs whose upper surfaces
are in the form of spherical caps.
6.1.6 PACKED BUBBLE COLUMN
To avoid the formation of very large bubbles the column is packed with some type of packing
such as Rasching rings. The reactor thus becomes an ordinary packed column operated in a
flooded condition and with a sparger to disperse the gas; naturally maximum superficial gas
velocity is much less than in the unflooded packed column.
6.1.7 AGITATED TANK

An agitated tank is used to disperse the gas into the liquid contained in a tank. A vaned-disc impeller is
normally used. An agitated tank provides small bubbles and thus high surface area of contact between
gas and liquid phases, but its greater mechanical complication compared with a simple bubble column is
a disadvantage with corrosive materials and at high pressures and temperatures. If necessary, stagewise
operation can be achieved by having several compartments in a vertical column, with impellers
mounted on a common shaft.
6.2 BASIS OF SELECTION
For the selection of right kind of reactor we have to see whether the diffusion or chemical
reaction is the dominating phenomenon. Hatta number will dictate whether the reaction is slow,
instantaneous or fast. Then we makes a comparison between rate of diffusion and rate of
chemical reaction and select the slower one (rate determining) for the design of reactor. For
liquid-gas reaction most commonly used reactor is CSTR in countercurrent manner as shown by
the following table.

6.3 SELECTION OF CSTR
The Hatta number is defined as
=(k1DA)1/2 /kL
(Ref: Chemical engineering Design by Coulson and Richardson Vol:3)
where
 Hatta number
k1 Rate constant (m3Kmol-1s-1)
DA Diffusion coefficient (m2/s)
kL Mass transfer coefficient of liquid (m/s)

The reaction we are dealing with as follows;
CH3COOCH3 + CO (CH3CO)2O
(CH3CO)2O + H2 CH3COOCH + CH3CHO
The first step is the rate determing step.
Reaction conditions are as follows;
Reaction temperature 160C
Reaction pressure 310.2KPa
Rate constant k1 0.112 m3Kmol-1s-1
Let A refers to carbon monoxide (gas) and B refers to methyl acetate (liquid).The reaction is
exothermic and taking place in the liquid phase.
Mass flow rate of A = 396.8Kg/h
Density of A = 2.41Kg/ m3
Volumetric flow rate of B = 396.8/2.41
= 164.65m3/h
Molar flow rate of B = 14.2Kgmol/h
Conc. of B = 14.2/164.88
= 0.0861Kgmol/m3
Diffusivity of CO in Methyl acetate solution can be determined from the following correlation
DA = 167.1 x 10-9 e-1027.6/T [3]
Where
D Rate of diffusion in m2/s
T Temperature in Kelvin
DA = 167.1 x 10-9 e-1027.6/433.15
= 1.56 x 10-8 m2/s
For bubble dispersion (plate column, bubble column, agitated vessel)
kL ranges from 2 x10-4m/s to 4x10-4m/s

and for packed column
kL ranges from 0.5 x10-4m/s to 1x10-4m/s [2]
For Bubble dispersion 2 x10-4 < kL < 2 x10-4 so
 = (k1CBDA)1/2 /kL\  = (k1CBDA)1/2 /kL\
 = 0.061  = 0.122
For Packed column 0.5 x10-4 < kL < 1 x10-4 so
 = (k1DA)1/2 /kL\  = (k1DA)1/2 /kL\
 = 0.246  = 0.42
All the values of  lies in the II region of the graph shown above. The value of reaction factor f A
is unity for  >0.1 in regionII.It shows that the reaction is moderate and talking place in the bulk
of liquid where CAL=0.So both interfacial area and hold-up should be high. A packed column in

any case therefore would be unsuitable. We therefore conclude from above consideration that an
agitated tank, a simple bubble column or packed bubble column should be chosen.Now among
the bubble dispersed reactors the agitated tank (CSTR) is the best because of following reasons;
 Very less chances of coalescence

 High liquid hold up
 High interfacial area
 Less resistance in gas diffusion
Bubble column is not suitable because there is great chances of coalescence and in the case of
packed bubble column there will be high pressure drop which will require a reactor of large wall
thickness and hence cost will be high. [2]
6.4 DESIGN OF CSTR
The volume of CSTR is calculated from well known expression which is as follows;
V/FBO = XB/rB (1)
Where
V volume of CSTR
FBO molar flow of methyl acetate
XB molar conversion of methyl acetate
rB rate of reaction of methyl acetate
The reaction completes in two steps which are as follows;
CH3COOCH3(l) + CO(g) (CH3CO)2O(g)
(CH3CO)2O(g) + H2(g) CH3COOCH3(g) + CH3CHO(g)
CH3COOPd is used as catalyst along with CH3I.Plladium acetate forms a complex [Pd(CO)2I2]-
The reaction mechanism is as follows;
[Pd(CO)2I2]- + CH3I [CH3Pd(CO)2I3]-
[CH3Pd(CO)2I3]- + CO [CH3COPd(CO)2I3]-
[CH3COPd(CO)2I3]- + CH3COOCH3 [Pd(CO)2I2]- + (CH3CO)2O + CH3I

(CH3CO)2O + H2 CH3CHO + CH3COOH
The rate of reaction on the basis of methyl acetate is a as follows;
rB = k11K11K12PBWA*/(1+K11P+K11K12PA*) (2)
Where
A* = Equilibrium dissolved conc. of CO
E* = Equilibrium dissolved conc. of H2
P = Con. of Methyl iodide. Kg mol/m3
B = Conc. of methyl acetate Kgmol/m3
W = Conc. of catalyst Kgmol/m3
At 310.2KPa and 160°C the values of above parameter are as follows;
k11 = 0.112 m3Kgmol-1s-1
K11 = 1.75 m3/Kg mol
K12 = 2.86 m3/Kg mol
Values of Henry constant at these conditions for gaseous component are
He for CO 11.80 Kg mol/m3MPa-1
He for H2 5.980 Kg mol/m3MPa-1
[20]
Total pressure of the system is 310.2KPa or 0.3102MPa
Mole of CO = 14.2
Mol of H2 = 70
Total moles = 85.2
Mole fraction of CO = 0.17
Mole fraction of H2 = 0.83
Partial pressure of CO = 0.17 x 0.3102
= 0.0527MPa

Partial Pressure of H2 = 0.83 x 0.3102
= 0.257
Equilibrium Conc. of CO = 0.0527/11.80
= 0.0045 Kg mol/m3
Equilibrium Conc. of H2 = 0.257/5.980
` = 0.042 Kg mol/m3
Putting all these values in equation (2)
rB = 0.00016Kg mol/m3.s
= 0.000161mol/lit.s
= 0.57mol/lit.hr
Hence the required reaction volume of CSTR using equation (1)
Vr = 21.2 m3
= 5593.28gal (rated capacity)
For all CSTR having capacity less than 500gal the allowable head space is taken as 15% while
for reactors having capacity greater than 500gal allowable head space is taken as 10% .As in our
case the capacity of CSTR is 5593.28gal so allowable head space is 839gal.
Total volume of CSTR
V = 5593+839
= 6432 gal
= 23.32 m3 (actual capacity)
Now, we have a number of options available. One option is not to fill the standard reactor up to
the rated volume but only up to the calculated reaction volume of 5593.28 gal (21.2 m3) and
maintain the volumetric flow rate. This means that the conversion will be 0.85 as specified.
CSTRs have a minimum operating reaction volume to avoid imperfect mixing. Mixing depends
on the properties of the reaction mixture, the impeller design and speed, and the internal design
of the CSTR. The minimum operating reaction volume for good mixing should be determined by

consulting with the manufacturer of the CSTR.. A second option is to again fill the reactor up to
maximum capacity, and maintain the volumetric flow rate. In this case, the residence time
increases because of the increased reaction volume, increasing the conversion. This design will
give some flexibility. If the demand for product increases, the feed rate can be increased, but the
conversion will decrease. The original required conversion is 0.85 [5]
The L/D ratio of CSTR is taken unity because of two reasons
1. It is more economical
2. Availability of well developed correlations for this ratio
L/D = 1
D Diameter of CSTR
L Length of CSTR
As volume of reactor related to its diameter is
V = (D2/4) x L
Solving these equations for L and D
D = 5.20m
L = 5.20m
6.5 DESIGN PRESSURE
A vessel must be designed to withstand the maximum pressure to which it is likely to be

subjected in operation. For vessels under internal pressure, the design pressure is normally taken
as the pressure at which the relief device is set. This will normally be 5 to 10 per cent above the
normal working pressure, to avoid spurious operation during minor process upsets. When
deciding the design pressure, the hydrostatic pressure in the base of the column should be added
to the operating pressure, if significant.[1]
The height of liquid in the CSTR corresponding to reaction volume is 2.88ft or 0.27m.The
hydrostatic pressure of liquid reaction mixture will be
PHyd = gh
= 1104 x 9.8 x 5.20

= 56225.63 Pa
= 56.3KPa
So hydrostatic has significant effect.
Pworking = 310.2 + 56.3
= 366.5KPa
Pdesign = 366.5 + 18.33
= 384.8KPa (5% more than working pressure)
6.6 DESIGN TEMPERATURE
The strength of metals decreases with increasing temperature so the maximum allowable design
stress will depend on the material temperature. The design temperature at which the design stress
is evaluated should be taken as the maximum working temperature of the material, with due
allowance for any uncertainty involved in predicting vessel wall temperatures. [1].
We chose austenitic stainless steel for the fabrication of CSTR for which the design stress is
evaluated at 200C. So the Design temperature of the CSTR is 200C.
6.7 MATERIAL OF CONSTRUCTION
The most important characteristics to be considered when selecting a material of construction

are:
1. Mechanical properties
(a) Strength-tensile strength
(b) Stiffness-elastic modulus (Young's modulus)
(c) Toughness-fracture resistance
(d) Hardness-wear resistance
(e) Fatigue resistance
(f) Creep resistance
2. The effect of high and low temperatures on the mechanical properties
3. Corrosion resistance

4. Any special properties required; such as, thermal conductivity, electrical resistance, magnetic
properties
5. Ease of fabrication-forming, welding, casting
6. Availability in standard sizes-plates, sections, tubes
7. Cost
Keeping in view all above factors we chose austenitic steel as material of construction for the
fabrication of CSTR. Although it has high cost as compared to carbon steel and low alloy steel
but it has high corrosion resistance. Moreover it has high tensile strength.Integranular corrosion
is one of the problems associated with the use of austenitic steel but this problem arises due to
the presence of chloride ions. As there is no chloride ion present in the reaction mixture so there
is negligible chance of intergranular stress corrosion [1].
6.8 WALL THICKNESS
The shape of most of the chemical process equipment is either cylindrical or spherical or some
composite of these. The main purpose of process equipment is to contain a media under desired
pressure and temperature. In doing so it is also subjected to the action of steady and dynamic
support loadings, piping reactions, and thermal shocks which require an overall knowledge of
stresses imposed by these conditions. The final thickness of process vessel, therefore, is chosen
so that it is not only adequate against the induced stresses caused by internal pressure, but also
ensures safety against stresses caused by extraneous agencies.
The thickness of wall depends on the operating pressure and temperature. For low pressure thin
walls are used. The following relation is used to calculate wall thickness with assumption t/Di
not exceeding 0.25.
t = PDi/(2fJ-P)
Where
t wall thickness
P design pressure
Di inner diameter of vessel
f allowable design stress for material specified
J joint efficiency factor

For stainless steel and non-ferrous pressure parts, generally no corrosion allowance is required.
As we selected stainless steel so corrosion allowance is zero this case. In the design of chemical
process equipment joint efficiency factor 1.0 or 0.85 is commonly used. Design stress value is
determined by dividing the appropriate properties of the material (i.e. the ultimate stress or the
stress at elastic limit at the design temperature and taking the lowest value.[Battacharyyia,2001]
P = 384680 N/m2
Di = 5.20
J = 1
f = 1.13 x 108/2.5=4.52 x 107 N/m2
Putting these values in the above expression, the thickness of the wall comes
t = 8.86 x 10-3m
= 8.86mm
Standard thickness available is 9mm.Therefore, to fabricate this CSTR steel plate of 9mm thick
is to be used.
6.9 DESIGN OF AGITATOR
Agitator in CSTR is provided for gas-liquid mixing. Turbulent mixing is important in operations
involving mass and heat transfer. Such processes involving mass and heat transfer are also called
shear controlled processes.
The most suitable agitator for a particular application will depend on the type of mixing required,
the capacity of the vessel, and the fluid properties, mainly the viscosity. The three basic types of
impeller are used at high Reynolds numbers (low viscosity). They can be classified according to
the predominant direction of flow leaving the impeller. The flat-bladed (Rushton) turbines are
essentially radial-flow devices, suitable for processes controlled by turbulent mixing (shear
controlled processes). The propeller and pitched bladed turbines are essentially axial-flow
devices, suitable for bulk fluid mixing. Paddle, anchor and helical ribbon agitators and other
special shapes, are used for more viscous fluids. [1]
For shear controlled processes disc turbine is commonly used which creates a high shear rate. It
is especially useful for dispersing a gas into a liquid. In CSTR our purpose is to disperse H2 and

CO into Methyl acetate and as well as the process under consideration is shear controlled
(involving mass and heat transfer), so we selected disc turbine with 4 baffles.[4].
The shaft power required to drive an agitator can be estimated using the following generalized
dimensionless equation.
Np = K Reb Frc
Where
Np = P/DN
Re = Reynolds number = D2N/
Fr = Froude number = DN2/g
P = Shaft power, W,
K = a constant, depend on the agitator type, size , and the agitator tank geometry y
 = fluid density, Kg/m3
 = Fluid viscosity, NS/m2
N = agitator speed, s-1 (rps)
D = agitator diameter, m,
g = gravitational acceleration, 9.8m/s2
For turbine agitator
D/DT = 1/3
DT = 5.20m
D = 1.73m
 = 3.84 x 10-4 Ns/m2
N = 0.87 s-1 (rps)
 = 1104Kg/m3
Putting these values in the relation for Reynolds number
Re = 7.51 x 106

As Reynold number is very high which may result in developed flow but we are required
developing flow for efficient contact between gas and liquid. To avoid developed flow, swirling
and vortex formation we use baffles in CSTR.Usually number of baffles used is 4, so we are
using 4 baffles. For turbine agitators the width of baffle need be no more than one twelfth of the
vessel diameter.
Corresponding to Re=106
Np = Kt = 6.30
And power consumption
P = NpD5N3
= 6.30 x (1.73)5 x (0.87)3 x 1104
= 7290W
= 9.77hp
For turbine agitator
D/DT = 1/3 L/DT = 1
J/DT = 1/12 E/DT = 1/3
W/D = 1/5 L/D = 1/4
Putting the values in above relations
D = impeller diameter = 1.73m
J = Width of baffles = 0.43m
E = Height of impeller above vessel floor = 1.73m
W = impeller width = 0.35m
L = length of impeller blades = 0.43m
6.10 DESIGN OF HEAD
The ends of cylindrical process vessel are to be closed before putting into operation. This is done
by means of heads and enclosures, which are of different shapes. The vessels are usually
provided with the following types of heads.

a. Flat Head
b. Standard dished or torispherical head
c. Ellipsoidal
d. Hemispherical
e. Conical or toriconical head
The selection of particular type of head depends on the factor like process temperature and
pressure, nature of the materials to be handled, position of the vessel(Horizontal or vertical),
nature of the support and above all economy.
6.10.1 TORISPHERICAL HEAD
For production of acetaldehyde from methyl acetate using CSTR we selected flanged and
standard dished (Torispherical) head .Torispherical head finds its application in the construction
of vertical process vessels for low pressure, horizontal cylindrical tanks for volatile fluids such as
naphtha, gasoline and kerosene and for large diameter storage tanks in which the vapor pressure
and hydrostatic pressure are too great for the flanged only heads.
We didn’t recommend heads other than torisherical because of following reasons;
6.10.2 FLATE HEADS
The discontinuity stresses at the junction of head and shell are high. For a given diameter and
operating condition, material cost for flat head is maximum.
6.10.3 ELLIPSOIDAL HEADS
These types of heads are generally recommended in the pressure range of 0.7MN/m 2 and
preferably for the vessels designed to operate above 1.5MN/m2.
6.10.4 HEMISPHERICAL HEADS
These types of heads are perhaps the most expensive and widely used in heavy duty high
pressure vessels due to the fact that the most efficient use of material is achieved.
6.10.5 CONICAL HEADS
These types of heads are used as bottoms for the process equipments like evaporators, spray
driers, crystallizers, settling tanks, silos etc.The particular advantage is the accumulation and
removal of solids from such equipments. They are commonly used as reducers. [12]
6.11PLATE THICKNESS FOR DISHED HEAD
In order to determine the thickness of the dished head and plate required for fabricating dished
head for CSTR we assume that there will be no uncompensated opening in the
head..Specifications of head are as follows;
Ri = Do
ri = 0.06Do
Sf = 40mm
P = 384.68KPa = 0.38468MN/m2
f = 45.2 MN/m2
Do = Di + t = 5.20 + 0.009 = 5.21m = 5210mm
Where
Ri = Crown inside radius
ri = Knuckle inside radius
Sf = Shape factor
P = Design pressure
f = Allowable design stress
Do = Vessel outside diameter
Di = Vessel inside diameter
Thickness of the head is determined from the following relation
t = P Do C/2fJ (1)
Solution of equation (1) will require iteration because ‘C’ is a function of‘t’.As the first
approximation we assume
Ri = Ro = Do
Now using the relation
ho = Ro –[( Ro - Do /2) x (Ro + Do/2 – 2ro )]1/2 (2)
= 5.21 –[( 5.21 – 5.21 /2) x (5.21 + 5.21 /2 – 2x0.3126 )]1/2

= 0.88m
Now
D2o/4Ro = (5.21)2/(4x5.21)
= 1.30m
(Do ro/2)1/2 = (5.21x 0.3126/2)1/2
= 0.90
Out of these quantities calculated above ‘ho’ is least. Therefore effective external height of the
head is equal to ho i.e. hE = 0.88 so
hE /Do = 0.88/5.21 = 0.17
As diameter of the vessel is not very large so head can be fabricated from a single plate and
therefore J=1
Now putting these values in equation (1)
t/Do = PC/2fJ
= 0.38468C/(2x45.2x1)
= 1.70 x 10-3 C (3)
With the help of table given below various values of t/Do are to be tried for hE /Do = 0.17 to
match the relation (3). It is found that for t/D o= 0.002 and corresponding value of C=1.32 gives
t/DoC = 1.52 x 10-3 which is close to approximation.
From the above findings, the corroded head thickness is obtained as follows;
t/Do = 0.002
= 0.01m
= 10mm
Compared to 5.21 m, 10mm is very small hence first approximation of Ri = Ro does not introduce
any considerable error in the result.
6.12 DETERMINATION OF HEAT TRANSFER AREA
To transfer heat, size either a STR with a jacket or one with internal coils. Try the jacketed
reactor first because it is the least costly. The available heat-transfer area consists of the

cylindrical surface of the reactor and the dished bottom. Only 80% of the total surface area of an
STR is available for heat transfer. The upper head contains nozzles, a port for the mixer, lugs for
support, and usually a sight glass.
As the reaction is exothermic so we are using cooling water at Tin =10°C to maintain the
temperature at 160°C(320◦F).∆T is selected 8.The selected heat transfer area must provide an
amount of heat equal to 6.5x106 KJ/h to keep the temperature at 160°C.
First we calculate the amount of heat which can be removed by using a simple jacket. For this we
require jacket temperature which is simply the average of jacket inlet and outlet temperature.
Tj = (10+18)/2 = 14°C(57.2°F)
The area of jacket when bottom head is flat can be determined from the following relation;
Aj = ∏DiL + ∏Di2/4
= (3.14x 5.2 x 5.2) + (3.14 x 5.2/4)
= 106.13m2
Now we choose an approximate overall heat transfer coefficient for standard CSTR [H.Silla,
2003].When cooling media is water and agitated liquid is organic liquid then approximate heat
transfer coefficient for jacket lies in the range 60-110Btu/h. ◦F.ft2.
Let Uj = 100 Btu/h.°F.ft2
Aj = ∏DiL + ∏Di2/4
= 106.132m2
= 1142ft2
Heat removed by jacket area can be determiner from following relation
Qj = Uj Aj (Tj – TR) (1)
Where
Qj = heat transfer by jacket
Aj = jacket area
Uj = jacket heat transfer coefficient
Tj = jacket temperature

TR = Reaction temperature
Putting values in relation (1)
Qj = Uj Aj (Tj – TR)
= 70 x 1142 x (57.2 - 320)
= 3 x 107Btu/h
= 3.16 x 107KJ/h
This value of Qj shows that a simple jacket is sufficient for providing the required amount of heat
i.e. 6.5x106 KJ/h.
6.13 SELECTION OF SUPPORT
Design of process vessel cannot be complete without the selection and design of a suitable
support for it, and also without examining the effect of support on shell. A process vessel is
usually supported either in vertical or horizontal position depending on the process requirement.
For example, a distillation column, an absorption column, an evaporator or a CSTR will always
be supported in vertical position. On the other hand a heat exchanger or condenser or a storage
vessel can be supported either in vertical or horizontal position depending upon the floor area
and the head room available.For vertical vessels the common supports are;
a. Skirt support
b. Bracket or lug support
c. Leg support
d. Ring support
We are using here Bracket or Lug support because it is widely used for all types of vessels. It is
used to support vessels of smaller height (subjected to minor wind load).Lugs are welded to the
vessel and rest on columns or beams.
The advantages of bracket support are:
a. They are easily constructed with a minimum length of weld seam
b. They can absorb diametrical expansions(provided they are equipped with a device for
sliding)
c. They can be easily leveled.

SPECIFICATION SHEET
Item CSTR
Number of Item 1
Item Code R-100
3
Capacity 23.32m
Operating Temperature 160◦C
Operating Pressure 366.5KPa
Length 5.20m
Diameter 5.20m
Impeller Diameter 1.73m
-3
Wall thickness 9 x 10 m
Material of Construction Austenitic Stainless Steel
Head type Torispherical
Support Bracket
-3
Head thickness 12 x 10 m
2
Jacket area 106.13m

Chapter 7
DESIGN OF 2-PHASE SEPARATOR

7.1 TWO PHASE VAPOR LIQUID SEPARATOR
The separation of liquid droplets and mists from gas or vapor streams is analogous to the
separation of solid particles and, with the possible exception of filtration, the same techniques
and equipment can be used.
Where the carryover of some fine droplets can be tolerated it is often sufficient to rely on gravity
settling in a vertical or horizontal separating vessel (knockout pot).
Knitted mesh demisting pads are frequently used to improve the performance of separating
vessels where the droplets are likely to be small, down to 1mm, and where high separating
efficiencies are required. Proprietary demister pads are available in a wide range of materials,
metals and plastics, thickness and pad densities. For liquid separators, stainless steel pads around
100 mm thick and with a nominal density of 150 kg/m3 would generally be used.
Use of a mister pad allows a smaller vessel to be used. Separating efficiencies above 99% can be
obtained with low pressure drop. The design and specification of demister pads for gas liquid
separators is discussed by Pryce Bailey and Davies (1973). The design methods for horizontal
separators given below are based on a procedure given by Gerunda (1981).
Cyclone separators are also frequently used for gas liquid separation. They can be designed using
the same methods for gas solids cyclones. The inlet velocity should be kept below 30 m/s to
avoid pick-up of liquid form the cyclone surfaces.
7.2 TYPES OF SEPARATOR
7.2.1 HORIZOTAL VAPOR LIQUID SEPARATOR

7.2.2 VERICAL VAPOR LIQUID SEPARATOR
7.2.3 CYCLON VAPOR LIQUID SEPARATOR

7.3 SELECTION OF SEPARATOR
Based on the configuration, the most common types of separators are horizontal, vertical and
spherical. A concise comparison of their attributes is presented in the following table
Vertical Horizontal Spherical

Function configuration
configuration configuration
For small leases

For High gas For low gas
Usage at moderate
liquid ratio liquid ratio
pressure
Large fluid Low fluid Capacity rated

Capacity
capacity capacity low
Handling foreign
Rated no 1 Rated no 2 Rated no 3
materials
Separation
Rated no 1 Rated no 2 Rated no 3
efficiency
Maintenance and
Very difficult Accessible Average
inspection
Coast/ unit & Average & Least &

Highest & easy
installation most difficult average
Overall ranking Rated no2 Rated no 1 Rated no3
For the selection of a particular separator, preliminary survey of the conditions and factors
prevailing on the location from where the feed is origination must be done. The main factors
underlying this survey as well as the basic steps included in the selection of a separator are
1- Operating temperature
2- Operating pressure
3- No of stages (i.e. no of individual separators employed
4- The feed composition

The choice of a separator for the processing of a gas-liquid mixture under given operating
conditions and for a specific application normally takes place guided by the general classification
illustrated below:
No of Operating
Configuration Function phase Application
pressure
separators
Medium
2-phases 3-phases Low temp High temp
temp
Low Medium High

20-200psi 200-700psi 700-500psi
Using the comparison or various configurations and keeping in mind that our feed has a high gas
to liquid ratio i.e. of 3.5 with the operating condition being 80˚c temperature and a pressure of 42
psi. We come to the conclusion that the most suitable separator for use is the vertical
configuration.
Advantages of using a vertical separator
1. Vertical configurations are most suitable for handling foreign materials which is very
necessary since our feed contains a reasonable amount of solid residues from the reaction.
2. Vertical separators are good for use with low highest gas-liquid ratios and hence are ideal
for use with our feed conditions having a gas-liquid ratio of only 3.5.
3. Vertical separators have adequate gas capacities.
4. Vertical separators have the best separation efficiency of the three types.
5. Vertical separators have intermediate cost per unit capacity.
6. The cost of installation is not prohibitively high even though it lies between the other two
types.
7. However the overall all ranking of the horizontal separators is number 2 in relations to
maintenance and inspection.

7.4 MATERIAL BALANCE ACROSS SEPARATOR
Flow rate=1555.36
kg/hr
This includes:
CH3COOCH3=124.48
kg/hr
CH3I=340.00 kg/hr
CO=60.32 kg/hr
Vapor outlet H2=117.91 kg/hr
CH3CHO=487.62 kg/hr
CH3COOH=425.03
kg/hr
Mixture
Inlet Two Phase separator
Flow rate=1994.05kg/hr
Flow rate=438.69
This includes:
kg/hr
CH3COOCH3=159.58
This includes:
kg/hr
CH3COOCH3=35.10
CH3I=402.30 kg/hr
kg/hr
CO=60.32 kg/hr
Liquid outlet CH3I=62.29 kg/hr
H2=117.91 kg/hr
CH3CHO=42.99 kg/hr
CH3CHO=530.61 kg/hr
CH3COOH=298.31
CH3COOH=723.34 kg/hr
kg/hr
7.5 SELECTION CRETERIA [21]
1. A vessel handling large amounts of liquid or a large Liquid surge volume will usually be
horizontal. Also,
2. Where water must be separated from hydrocarbon liquid, The vessel will be horizontal. A
vessel with small surge volume would be a vertical.
3. If L/D (length to diameter ratio) lies between 3 and 5, then vertical separator is designed.
And if L/D is greater than 5 then try with horizontal vessel.
4. The inlet velocity should be kept below 30 m/s to avoid pick-up of liquid form the
cyclone surfaces in the cyclone separators.

7.6 DESIGN OF VERTICAL 2-PHASE SEPARATOR
7.6.1 INPUTS
Operating operation: P = 289KPa
Vapor mass flow rate: Wv = 1555.36 kg/hr
Vapor density: ρv = 2.10 kg/m3
Liquid mass flow rate: WL = 438.69 kg/hr
Liquid density: ρL = 941.90 kg/m3
Mixture mass flow rate: ρmix = 1994.05 kg/hr
Mixture density: ρmix = 2.70 kg/m3
Hold up Time: Ѳ = 15 minimum (Assumption by choice)
7.6.2 VESSEL DIAMETER CALCULATIONS
The vessel diameter is based on the settling velocity, Us of liquid droplets.
Us = 0.15*Ut
Ut = 0.07[{(ρL – ρv)/ ρv}]
Ut = 0.07[{(941.90 – 2.10)/2.10}]1/2
= 1.48 m/sec
So;
Us = 0.20 m/sec
Vapor volumetric flow rate:
Qv = [Wv/( 3600*ρv)]
Qv = 0.21 m3/sec
Minimum Vessel Diameter:
Dv = [(4*Qv)/(∏*Us)]1/2

= 1.16 m (use standard diameter: 1.20m)
so;
Dv = 1.20m
m
7.6.3 VESSEL HEIGHT CALCULATIONS
Liquid volumetric flow rate:
QL = [WL/( 3600*ρL)]
QL = 1.30*10-04m3/sec
Volume held in vessel:
Vv = QL* Ѳ
= 1.30*10-04(15*60)
Vv = 0.12 m3
Liquid depth required:
hv = (volume held-up)/(vessel cross-sectional Area)
hv = (0.12)/{∏*(1.16)2/4}
hv = 0.14 m
Increase 0.4 m to allow space for positioning the level controller.
So;
hv = 0.54 m

This is vertical two phase separator with standard dimensions;
H = hv + Dv/2 + Dv + 1.2
H = 3.54 m
Using Standard Height; 3600 m
H= 3.60 m
While;
L/D ratio = 3.60/1.20 = 3
7.6.4 L/D VERIFICATION [1]
The most economical length to diameter ratio will depend on the operating pressure. As a general
guide the following values can be used:

Operating pressure, bar Length: diameter, Lv/Dv
0 -20 3
20 -35 4
>35 5
As the operating pressure lies between 0 to 20 bar, ( 2.08 bar, 42 psi) for which satisfactory L/D
is 3.
7.6.5 NOZZEL SIZING
Nozzle diameter:
d = [(4*Q)/(3600*∏*Vmax)]1/2
Where, Vmax is maximum velocity;
Vmax = 100/(ρ)1/2
Inlet nozzle
Nozzle diameter:
d = [(4*Qmix)/(3600*∏*Vmax)]1/2
Inlet Nozzle diameter = 0.15 m
Vapor outlet nozzle
Nozzle diameter:
d = [(4*Qv)/(3600*∏*Vmax)]1/2
Vapor outlet Nozzle diameter = 0.15 m

Liquid Outlet nozzle
Nozzle diameter:
d = [(4*QL)/(3600*∏*Vmax)]1/2
Liquid outlet nozzle diameter = 0.05 m
SPECIFICATION SHEET
Vapor liquid separator
Item
1
Number of Item
V-100
Item Code
94°C
Operating Temperature
389KPa
Operating Pressure
3.60m
height
1.20m
Diameter
0.15m
Inlet nozzle Diameter
0.15m
Outlet vapor nozzle
Diameter
0.05m
Outlet liquid nozzle
diameter

Chapter 8
DESIGN OF ABSORBER

8.1 ABSORPTION
The removal of one or more component from the mixture of gases by using a suitable solvent is
second major operation of Chemical Engineering that based on mass transfer. In gas absorption a
soluble vapor is absorbed from its mixture with an inert gas by means of a liquid in which the
solute is more or less soluble.
The purpose of such gas scrubbing operations may be any of the following;
1. For Separation of component having the economic value.
2. As a stage in the preparation of some compound.
3. For removing of undesired component (pollution).
8.2 TYPES OF ABSORPTION
8.2.1 PHYICAL ABSORPTION
In this type of absorption we will consider a pure physical solvent in which there is a low heat of
solution of solute. This small heat release plus high liquid-to-solute ratio means that the liquid
temperature changes very little in the absorber. In physical absorption mass transfer take place
purely by diffusion
.8.2.2 CHEMICAL ABSORPTION
In this type of absorption as soon as a particular component comes in contact with the absorbing
liquid a chemical reaction take place, thereby reducing the concentration of component in the
liquid phase, which enhances the rate of diffusion.
In chemical stripping, the liquid solvent reacts with the gas stream but in physical stripping, gas
and liquid streams does not react with each other.
Changing the conditions of the stripping column can influence the effectiveness and efficiency of
stripping. Some important controllable conditions are as follows:
1. Pressure of the column.

2. Temperature of the column.
3. Ratio of liquid and gas stream rates

Reducing the total pressure of the column may increase the total efficiency of the stripping
column. Increasing the temperature of the stripping column may increase the efficiency of the
column.
The stripping factor (S) is defined as
S = KV/L
Where;
V is the vapor flow rate.
L is the liquid flow rate.
The stripping medium may be steam or a dry or inert gas (nitrogen, carbon oxides, hydrogen.)
Use of inert gas has a disadvantage that after stripping operation, solute still has to be recovered
from a gas stream. For this reason, inert gas mostly steam is used. The steam + stripped solute
effluent from stripper then condensed and the water and solute separated by decantation. Steam
cannot be used when water and condensed solute are miscible.
8.3 FACTORS AFFECTING ABSORPTION
8.3.1 PRESSURE DROP AND LIMITING FLOW RATES
Increasing L/V increasing the driving force everywhere in the column except at the very top and
the absorption column does not need to be as tall, However using a larger amount of liquid gives
a more dilute liquid product which makes it more difficult to recover in stripper. The optimum
liquid rate for absorption is found by balancing the operating cost for both equipments. In
general the liquid rate for the absorber should be between 1.1 to 1.5 times he minimum rates
8.3.2 PACKING SIZE AND LIQUID REDISTRIBUTION
In the case of random packing the packing density i.e. the number of packing pieces per cubic
foot, is ordinarily less in the immediate vicinity of the tower walls, and this leads to a tendency
of the liquid to segregate toward the walls and the gas to flow in the center of the tower
(channeling). This tendency is much less pronounced provided the diameter of the individual
packing pieces is smaller than at least one eighth the tower diameter, but it is recommended that,
if possible, the ratio dp/d not exceed 1:15. Even so it is customary to provide for redistribution of
the liquid at intervals varying from three to ten times the tower diameter, but at least every 20 ft.

With proper attention to liquid distribution, packed towers are successfully built to diameters of
20 ft or more.
8.3.3 WETTING RATE
Packing, in packed column, must be wetted to an extent above the minimum level recommended
by the packing manufacture to get the desired efficiency for a given gas liquid mass transfer
operation. As such packing wetting should be checked to make sure it is wetted above the
prescribed minimum level, particularly under circumstances where very low liquid rates have to
be used.
8.3.4 ENTRAINMENT ELIMINATE
Especially at high gas velocities, the gas leaving the top of the packing may carry off droplets of
liquid as a mist. This may be removed by mist eliminators, through which the gas must pass,
installed above the liquid inlet. A layer of wire meshes several inches thick or 2 or 3 ft of dry
random packing are very effective.
8.3.5 LIQUID HOLD UP
The amount of liquid retained by the packing is known as liquid hold up of packing or simply
holdup of packing. The efficiency of packed columns is closely related to the liquid holdup of
the packing.
8.4 TYPES OF ABSORPTION COLUMN
There are two major types of absorbers which are used for absorption purposes:
1. Packed column
2. Plate column
8.5 COMPARISON BETWEEN PACKED AND PLATE COLUMN
8.5.1 CONTACT
The packed column provides continuous contact between vapor and liquid phases while the
plate column brings the two phases into contact on stage wise basis.

8.5.2 SCALE
For column having diameter of less than approximately 3 ft. It is more usual to employ packed
towers because of high fabrication cost of small trays. But if the column is very large then the
liquid distribution is problem and large volume of packing and its weight is problem.
8.5.3 PRESSURE DROP
Pressure drop in packed column is less than the plate column. In plate column there is additional
friction generated as the vapors pass through the liquid on each tray. If there are large No. of
Plates in the tower, this pressure drop may be quite high and the use of packed column could
affect considerable saving.
8.5.4 LIQUID HOLDUP
Because of the liquid on each plate there may be a Urge quantity of the liquid in plate column,
whereas in a packed tower the liquid flows as a thin film over the packing.
8.5.5 SIZE AND COST
For diameters of less than 3 ft. packed tower require lower fabrication and material costs than
plate tower with regard to height, a packed column is usually shorter than the equivalent plate
column.
8.6 DESIGN OF ABSORPTION COLUMN
Following steps are followed for designing of absorption column:
1. Selection of column.
2. Selection of packing material
3. Selection of solvent
4. Finding the number of transfer units (NOG)
5. Calculating the actual diameter of column
6. Determining the height of packing
7. Determining the height of the column
8. Determining the pressure drop.
9. Determining the thickness of shell

8.6.1 SELECTION OF COLUMN
From the above consideration packed column is selected as the absorber, because in our case the
diameter of the column is less than 3 ft. As the solubility is infinity so the liquid will absorb as
much gases as it remain in contact with gases so packed tower provide more contact. It is easy to
operate.
8.6.2 SELECTION OF PACKING, MATERIAL
The largest size of packing that is suitable for the size of column should be used; up to 50 mm.
Small sizes are appreciably more expensive than the larger sizes. Above 50 mm the lower cost
per cubic meter does not normally compensate for the mass transfer efficiency. Use of too large a
size in a small column can cause poor liquid distribution.
The principal requirements of a packing are that it should:
1. Provide a large surface area: a high interfacial area between the liquid and the gas.
2. Have an open structure: low resistance to gas flow.
3. Promote uniform liquid distribution on the packing surface.
4. Promote uniform vapor gas flow across the column cross-section.
5. Be chemically non reactive to fluids admitted into the system.
6. Possess sufficient structural strength to offer ease in handling and installation.
7. Economic from commercial point of view.
Many diverse types and shapes of packing have been developed to satisfy these requirements;
they can be divided into following broad classes:
Packing with regular geometry
The advantage of structured packing over random packing is their low HETP (Typically less than
0.5 m) .The regular packing offers the advantages of lower pressure drop and greater possible
throughput of fluids, usually at the expense at least of more costly installation than random
packing.
These are used in the following applications:-
 For difficult separations, requiring many stages such as the operation of isotopes
 High vacuum distillations
 For column revamps: to increase capacity and reduce reflux ratio requirements

Regular packing comes in a wide range of variety. The simplest types of such packing are the
counter flow trays or plates are the counter flow trays used in fractionating columns. Besides
there are:
Stacked Rashing rings
The larger sizes of rashing rings (3 inch or larger) may be carefully stacked one upon the other to
provide continuous passage for the gas.
Woven wire Screens
These are made up of wire mesh or perforated metal sheets. The material is folded and arranged
with a regular geometry to give a high surface area with a void high fraction.
Spray pack and Pan pack
The spray pack and pan pack, is made of sheets of several layers of expended metal lath which
have been formed into the wave-shape surfaces.
Wood grids
Wood grids or hurdles are inexpensive, and both the arrangements shown and many variants
shown are used in filling water-cooling towers. Drip-point ceramic grid tiles are large and easily
stacked; they provide very effective contact at low gas pressure drop.
Packing with irregular geometry (Dumped Packing)
It is dumped into the column and take up a random arrangement.
Some principal types of packing are given as under:
Rings:
1. Rashing rings
2. Lessing rings
3. Partition rings
4. Pall ring
Saddles:
1. Berl saddle
2. Intalox saddle

8.6.3 SELECTION OF SOLVENT
For the purpose to remove constituents from the gas, the following properties are important.
Gas solubility
The gas solubility should be high, thus increasing the rate of absorption and decreasing the
quantity of solvent required, generally solvents of a chemical nature similar to that of the solute
to be absorbed will provide good solubility.
Chemical reaction of solvent with the solute will frequently result in very high gas solubility, but
if the solvent is to be used to recover for reuse, the reaction must be reversible. For example,
hydrogen sulfide may be removed from gas mixtures using ethanolamine solutions since the
sulfide is readily absorbed at low temperatures and easily stripped at high temperatures. Caustic
soda absorbs hydrogen sulfide excellently but will not release it in a stripping operation.
Volatility
The solvent should have a low vapor pressure.
Cost
The solvent should be inexpensive, so that losses are not costly, and should be readily available.
Viscosity
Low viscosity is preferred for reasons of rapid absorption rates, improved flooding
characteristics in absorption towers, low pressure drops on pumping, and good heat transfer
characteristics.
Miscellaneous
The solvent if possible should be nontoxic, nonflammable, and chemically stable and should
have a low freezing point.
8.6.4 FINDING THE NUMBER OF TRANFER UNITS

Material Balance across Absorber
Partial pressure of CH3CHO in feed = 13.4/100 x 42 = 5.6 psia
= 287.65 mmHg
Partial pressure of CH3CHO in exit gas = 5.6 x 0.01 = 0.66psi
= 2.8 mm Hg

Table 8.1 Equilibrium data for acetaldehyde –water system
%w/w of CH3CHO P.P mmHg Kpa Psia
0.1 252.6 33.60 4.87
0.3 472.8 62.88 9.12
0.5 622.3 82.77 12.00
0.7 743.7 98.91 14.34
0.9 852.7 113.41 16.44
From equilibrium data (Table 8.1)
Partial pressure at 2.5 % v/v CH3CHO = 300mmHg
Operating pressure = 38 psia
= 1964/6 mmHg
Mole fraction of CH3CHO in vapor
yi = 300/1946.6
= 0.1527
Mole fraction of CH3CHO in liquid
xi = 0.0103
Slope
m = yi / xi
= 0.152/ 0.013
= 14.8
y1/y2 = 287.65 / 2.82
= 100

Optimum value lies b/w 0.4and 0.6 .Choosing high concentration will favour efficient separation,
mGm/Lm = 0.6
From graph [1]
NOG = 10
8.6.5 CALCULATING THE ACTUAL DIAMETER OF COLUMN
Required data
Column used Packed bed absorber
Absorber efficiency: 98%
Absorbent fluid: Water
Molecular wt. of Absorbent 18
Packing used 1in ceramic Intalox saddles
Packing factor, Fp 300 m-1
Characterization factor of packing Cf 98.4
Surface area of the packing material, a 253
Temp 25oC
Pressure 2.6 atm
Gas flow rate 0.432 Kg/hr
liquid flow rate 10.71 Kg/hr
Density of gas, dg 2.01 Kg/m3
Density of liquid, dL 997 Kg/m3
Flow factor = 0.432/10.71[2.01/997]0.5
= 0.77

Now for diameter the required data is
Packing size Dp = 25mm = 1in
Pressure drop taken 35 mm of water (it should b/w 15-50)
Now using flow factor value & assumed pressure drop read the value of K4 [1]
K4 = 0.35
And at flooding 80 %
K4 = 0.8
%age flooding = 0.35/0.8 =63.2%
Vw* = gas mass flow rate per unit cross sectional area,
It can be calculated from following relation [1]
Vw* = 0.75 kg/m2.s
Now area of column
Ac = V*w / G b
= 0.65 m2
Diameter of Column
D = 0.92m ≈ 1
Corrected area
A = 0.65 m2
% flooding at selected diameter is 62 %.
8.6.6 DETERMINING THE HEIGHT OF PACKING
The height of tower can be calculated by the formula
Z = HOG * NOG
Where
HOG is height of overall gas phase transfer unit
NOG is no. of overall gas phase transfer unit

According to Cornell method
HG = 0.011h (Sc)n 0.5 (Dc/0.305)1.11 (Z/3.05) 0.33 / ( L*w f1f2f3) 0.5
HL = 0.305 fh (Sc)L 0.5 K3 (Z/3.05)0.15
Where
HG = height of gas phase transfer unit
HL = Height of liquid phase transfer unit
(Sc)g = Gas Schmidt number = (mn /dnDn)
(Sc)L = Liquid Schmidt number = (mL /dLDL)
D = Column diameter
Z = Column height in m
K3 = Percentage flooding correction factor (figure 11.41)
Yh = HG factor from (figure 11.42)
fh = HL factor from (figure 11.43)
L*w = Liquid mass flow rate per unit area column cross-sectional area
f1 = Liquid velocity correction factor (from fig 11. = (mL / mW) 0.16
f2 = Liquid density correction factor = (rW /rL) 1.25
f3 = Surface tension correction factor = sW / sL)
Dg = Diffusion coefficient for mixture of gases
HG Calculation
For multi component gas phase diffusivity is calculated by Blank’s law,
Di,mix = 1 / [ Σ (xj / Dij)]
Where
Xj = mol fraction of component j in inert gases
Dij = Diffusivity of component i w.r.t j

Now for our case
Dg mix = 0.129 cm2/s
= 0.502 ft2/hr
(Sc)g = 0.609
h = 58
At 25 oC, liquid is water so,
f1 = f2 = f3 = 1
L*w = L/A
= 16.5/0.65
= 16.4 kg/m2s
Putting all the above values in the given equations we get
HG = 0.577 m
HL Calculation
HL = 0.305 fh (Sc)L0.5 K3 (Z/3.05)
(Sc)L = 590
K3 at 62 % flooding is 0.83
fh at given value of L*w = 0.1
HL = 0.704 m
Height of overall gas phase transfer unit HOG
The height of overall gas phase transfer unit can be calculated
HOG = HG + m Gm / Lm* HL
= 0.577 + (0.6)(0.704)
= 0.99m
As
Z = HOG * NOG

= 10 * 0.99
= 9.9 m
= 10m
8.6.7 DETERMINING HEIGHT OF COLUMN
Now effective height of column = 8.4 m
Hold up and distribution height = 0.25 * (D+1)
= 1.23m
Total Height of column = 12.36 m
8.6.8 DETERMINING THE PRESSURE DROP
Wetting rate
Wetting rate can be calculated by the relation
Lw = MWR / (Aρa)
Volumetric flow rate = L/ dL
= 27.03 m3/hr
Velocity = vol. flow rate / area of column
= 41.58 m/hr
MWR = 0.96 m3 / hr
Satisfied .it should be greater than 0 .8
Pressure drop [1]
Flow factor = Gb / Lt (dg / dL )0.5
= 0.77
K4 = 0.35
From graph (11.44)
∆P/Z = 20 in of water/ft of packing
= 20mm Hg /m of packing

So ∆P/Z is allow able and within limit.
8.6.9 DETERMINING THE THICKNESS OF SHELL
Material used for making the shell is carbon steel.
Thickness of shell
ts = [(p D) / (2f J – p)] + c
Where,
Working Pressure = 2.6 atm
Design Pressure, p = 1.05 x 2 = 2.73 atm
Permissible Stress, f = 1007 N/m2
Joint Efficiency, J = 0.85
Corrosion allowance, c = 2mm
Hence,
ts = 7.47 mm
= 7.47x 10 -3 m

SPECIFICATION SHEET
Item Packed Absorption Column
No. required 1
Column type Packed
Item code C-100
FUNCTION
separation of acetaldehyde from gases , CO and H2
DESIGN DATA
Inside diameter 0.92m
2
Area of column 0.65 m
Type of packing Ceramic intalox saddles
Size of packing 0.025 m
Packing arrangement Dumped
NTU 10
HOG 0.99 m
Height of packing 10 m
Pressure drop 20mmHg/m of packing
Type of liquid distributor Trough type liquid distributor
Type of gas distributor Trough type gas distributor
Type of packing support Gas injection support
Height of column 12.36 m
-3
Thickness of shell 7.4x10 m

Chapter 9
DESIGNOF HAT EXCHANGER

9.1 INTRODUCTION
Heat exchanger is the equipment used to exchange heat between two fluids with different
temperature. A heat exchanger is a heat-transfer devise that is used for transfer of internal
thermal energy between two or more fluids available at different temperatures. In most heat
exchangers, the fluids are separated by a heat-transfer surface, and ideally they do not mix. Heat
exchangers are used in the process, power, petroleum, transportation, air conditioning,
refrigeration, cryogenic, heat recovery, alternate fuels, and other industries. Common examples
of heat exchangers familiar to us in day-to-day use are automobile radiators, condensers,
evaporators, air pre-heaters, and oil coolers.
9.2 TYPES OF HEAT EXCHANGER
 Double pipe exchangers

 Shell and tube exchangers
 Plate and frame exchangers
 Plate- Fin exchangers
 Spiral heat exchangers
9.3 SELECTION CRITERIA FOR HEAT EXCHANGER
Following things must be undertaken while selecting a heat exchanger for a given duty.
 Maintenance, inspection, cleaning, extension, and repair possibilities

 Overall economy
 Fabrication technique
 Intended application
 Flow rates
 Operating pressure and temperature
 Flow arrangements
9.4 SHELL AND TUBE HEAT EXCHANGER
A shell and tube heat exchanger is a class of heat exchanger designs. It is the most common type
of heat exchanger in oil refineries and other large chemical processes, and is suited for higher-
pressure applications. As its name implies, this type of heat exchanger consists of a shell (a large
pressure vessel) with a bundle of tubes inside it. One fluid runs through the tubes, and another
fluid flows over the tubes (through the shell) to transfer heat between the two fluids. The set of
tubes is called a tube bundle, and may be composed by several types of tubes: plain,
longitudinally finned etc.
9.5 CLASSIFICATION OF SHELL AND TUBE HEAT EXCHANGER
They are classified on the basis of following things;
 Consideration for differential thermal expansion of tubes and shell.

 Means of directing fluid through the tubes.
 Means of controlling fluid flow through the shell.
 Consideration for ease of maintenance and servicing.
 Types
Following are the main types of shell and tube heat exchanger
 Straight tube
 Fixed tube-sheet exchangers
 U-tube exchangers and
 Floating head exchangers—satisfy these design requirements.

9.6 ADVANTAGES OF SHELL AND TUBE HEAT EXCHANGER
It is used for high heat transfer duties.
 It occupies less space.

 Occupies not too much space
 Its maintenance is easy.
It can be fabricated with wide variety of materials depending upon fluid properties.
9.7 WORKING PRINCIPLE
Heat exchangers work because heat naturally flows from higher temperature to lower
temperatures. Therefore if a hot fluid and a cold fluid are separated by a heat conducting surface
heat can be transferred from the hot fluid to the cold fluid. It also accommodates following
things as well.
 Fixed -tube construction

 Units designed for liquid to liquid (PW) applications.
 Available in two pass construction.
 Fixed tube bundles for convenience in cleaning and inspection.
Strong, durable construction with mild steel tubes and rugged cast-iron or steel head in standard
units. (Optional materials are available).
Baffle arrangements designed to maximize heat transfer performance. Tubes expanded into
stationary tube sheet allow for tube expansions and contractions, due to thermal fluctuations,
without causing stresses on the joints. Welding tubes to the tube sheet is optional.
In many of the cases heat transfer involved in heat exchangers the heat is transferred from one
fluid to the other one through retaining wall. Heat transferred through warmer fluid to cold fluid
through several thermal resistances in series. By analogy with electric conduction, we may relate
the heat flux q to the temperature gradient Th – Tc, by introducing a total resistance to heat
transfer Rtot, defined as
Rtot = (Th-Tc)/q
The total resistance is comprised of the resistances due to convective heat transfer in the two
fluids, the resistance due to fouling that occurred with the wall with the passage of time and the
resistance to the transfer of heat through the retaining wall.

9.8 TEMA DESIGNATION
Because of the number of variations in mechanical designs for front and rear heads and shells,
and for commercial reasons, TEMA has designated a system of notations that correspond to each
major type of front head, shell type and rear head. The first letter identifies the front head, the
second letter identifies the shell type and the third letter identifies the rear head type. The TEMA
standard notation system is shown on the next page. Selecting the best TEMA type for a given
application is beyond the scope of this discussion. Refer to the API Training Manual section
entitled Selecting TEMA Heat Exchangers.
9.9 DESIGN OF SHELL AND TUBE HEAT EXCHANGER
Following steps are involved:
1. Collect physical properties i.e heat capacity, viscosity, density and thermal conductivity.
2. Specifications define, calculate heat duty and make energy balance if needed to calculate
unspecified flow rate and temperature.
3. Calculation of LMTD
4. LMTD Correction factor. Decide number of shell and tube passes.
5. Assume Overall Heat Transfer Coefficient.
6. Area Calculation: A=Q/(U ∆ To,m)
7. Decide type, tube size and material layout. Assign fluids to shell and tube side.
8. Determine number of Tubes
9. Determine tube side heat transfer coefficient.
10. Shell side configuration. Determine shell inside diameter on the basis of tube outside
diameter, number of tubes, tube passes and pitch.
11. Determine shell side heat transfer coefficient.
12. Correct overall heat transfer coefficient. If the error is less than 30% then proceed to next
step. Otherwise go back to step 6 and redo the calculations on the basis of calculated
value of overall heat transfer coefficient.
13. Estimate tube and shell side pressure drops. Pressure drop must be within the
specifications. If not within the limits then go back to step 8 and do a re-estimation.

9.9.1 COLLECTION OF PHYSICAL DATA
Heat capacity of process stream at 350 C = 4.069KJ/Kg0C
Viscosity of process stream at 350 C = 1.195x10-2Cp = 1.195x10-5Pa.s
Thermal conductivity = 0.6715 W/mK
Density of process stream = 937.2 kg/m3
Enthalpy of steam = 1730 KJ/kg
Viscosity of steam at 2000C = 0.016cp
Mass flow rate of process stream = 28753.15Kg/hr = 7.986 Kg/s
9.9.2 CALCULATION OF HEAT DUTY
Cold Fluid process stream
Hot Fluid Steam
For Cold Fluid:
Qc = mc ( Cp )( ∆ T)c
Qc = 7.986 x 4.069 x (115-35)
Qc = 2622.64 KJ/s
For Hot Fluid:
Qh = λ*mh
mh = 1.516 Kg/s
9.9.3 CALCULATION OF LMTD
Inlet temperature of the steam = Th,in = 2000C
Outlet temperature of the steam = Th,out = 2000C
Inlet temperature of the process stream Tc,in = 35°C
Outlet temperature of process stream Tc,out = 115°C
LMTD = [(Th,in-Tc,out)-(Th,out-Tc,in)]/ln[(Th,in-Tc,out)/(Th,out-Tc,in)]
= 88.24°C
Production of Acetaldehyde | 9.9.1 COLLECTION OF PHYSICAL DATA 115
9.9.4 LMTD CORRECTION FACTOR
R = (Th,in-Th,out)/(Tc,out-Tc,in )
R = (200-200)/(115-35)
R = 0
S = (Tc,out-Tc,in)/(Th,in-Tc,in)
Using relation 14.9 from Plant Design & Economics for Chemical Engineers by Timmerhaus
F=(R+1)0.5 ln[(1-P)/(1-RP)] /(R-1)ln[2-P[(R+1)-(R2+1)0.5]/[2-P[(R+1)+(R2+1)0.5]
Putting R=0 and S=0.865 in the above relation
F=0.97
For the condensing steam mostly 1-2 Shell and tube heat exchanger is used. Steam flows through
the tube side since the condensate may be corrosive. Steam is passed through the tubes also to
avoid heat losses. When steam passes through tube side there is no need more than two passes.
Corrected LMTD
∆To,m = F*LMTD
∆To,m = 0.97x88.24 °C
= 85.6 0C
Where
∆To,m = Overall mean temperature difference
9.9.5 ASSUME OVERALL HEAT TRANSFER COEFFICIENT
When the hot fluid is steam and cold fluid is light organics we can assume overall heat transfer
coefficient in the range 500 to 1000 [18].
Let
U = 750 W/m2.K
9.9.6 AREA CALCULATION
A = Q/(U ∆ To,m)
A = 30.58 m2
9.9.7 TUBE LAYOUT AND SIZE
Tube outside diameter = do =1 in = 0.0254m
Length of tube = Lt = 4.87m
BWG=16
Inside diameter = di = 0.0211m
Wall thickness = tw = 0.00021m
Flow area per tube = at‘= 0.0003m2
Effective tube length = tEL= L-2(Tube sheet thickness) = 4.826m
Tube pitch = Pt = 0.03175m
9.9.8 CALCULATION OF NUMBER OF TUBES
Number of tubes = Heat transfer area/Tube side area
Nt = A/πdo Lt
Nt = 30.58/(3.14*0.0254*4.87)
Nt = 82
Nearest tube count = Nt = 86
Total flow area
Total flow area = number of tubes *flow area per tube /number of tube passes
at = Nt * at‘/nt
at = 86 (0.0003/2)
at = 0.129 m2
Mass Velocity
Mass velocity = mass flow rate /total flow area
Gt = mh/at
Gt = 1.516/0.0129
Gt = 117.519Kg/sec.m2

Reynolds Number
Reynolds numbers = tube inside dia mass velocity/viscosity
Ret = di *Gt/μ
Ret = (117.52)(0.0211)/1.745x10-5
Ret = 142101
As Ret>2100 so flow inside the tubes is turbulent
9.9. 9 TUBE SIDE FILM COEFFICIENT
The heat transfer coefficients associated with condensation of steam are very high. It is
customary to adopt conventional and conservative value for the film coefficient, since it is not
the controlling film, rather than obtain by calculation
hi = 1.5 x 104 W/m2.K
hd = 6 x 10-4 K m2/W
9.9.10 SHELL SIDE CONFIGRATION
Tube bundle diameter = Db = d0 (Nt/K1)1/n1
K1 = 0.249
n1 = 2.207
Db = 0.35m
[Coulson etal]
Now, from the graph using split ring floating head heat exchanger
Shell clearance = 53 mm
Diameter of shell = Ds
Ds = 0.35 + 0.053
Ds = 0.403 m
Shell area
Shell flow area
As = [(Pt - do)Ds LB]/Pt

= [(0.3175-0.0254)0.403 x 0.10075]/0.03175
= 0.00812 m2
Mass Velocity
Mass velocity = mass flow rate /total flow area
Gs = ms/as
Gs = 7.986/0.00812
Gs = 983.61Kg/sec.m2
Equivalent Diameter of shell
Equivalent diameter = 4shell flow area/wetted perimeter
De = 4(0.86Pt2 – 0.25пdo2)/пdo
De = 4[0.86(0.31750)2 – 0.25x3.14 (0.0254)2]/3.14x0.02
De = 0.01806 m
Reynolds Number
Viscosity of shell side fluid
μ = 0.1775 x 10-3 Pa.s
Reynolds numbers = (shell inside dia)(mass velocity)/viscosity
Res = De Gs/μ
Res = 983.608 x 0.01806/0.1775 x 10-3
Res = 100079
As Res>2100 so flow in the shell side is turbulent.
9.9.11 SHELL SIDE FILM COEFFICIENT
The following relation is used for the determination of shell side film coefficient
Hs = 0.36k/De(De Gs/μ)0.55(μCp/k)0.33(μ/μw)0.14

K = 0.6715 W/m.k
μ = 0.1175 x 10-3 Pa.s
μw = 1.195 x 10-5 Pa.s
Cp = 4.096
Wall temperature
Average temperature of steam = 2500C
Average temperature of feed = 75.350C
∆Tavg = 250-75.35
∆Tavg = 174.650C
Let ∆T across steam = 20 %
= 0.2 x 174.65
= 350C
Let ∆T across feed = 70%
= 0.7 x 174.65
= 122.2550C
Wall temperature = 122.255+75.35
= 195.6050C
Hence putting these values gives,
Hs = 1148.88W/m2.K
9.9.12 CORRECTED OVERALL HEAT TRANSFER COEFFICIENT
Clean coefficient:
1/U0 = 1/h0 + 1/hd + [d0ln(d0/di)]/2kw + d0/dihi
Where
ho = 1.5 x 104 W/m2.K
hd = 6 x 10-4 K m2/W

kw for stainless steel = 16 W/m.K
Putting values gives
Ud = 606.21 W/m2.K
Clean coefficient:
1/U0 = 1/h0 + [d0ln(d0/di)]/2kw + d0/dihi
Uc = 878.72 W/m2.k
Actual heat transfer required
A0req = Q/UDcalc ∆TLMTD
A = 27.47 m2
Hence
%age over design = 15.54%
%age error in heat transfer area
%age difference
[(Udcalculated – Udassumed) / Udassumed] x 100 = 23.71%
Dirt Factor:
Rd = (Uc –Ud )/Uc Ud

= (378-282)/378*282
= 0.000511 m2.K/W
9.9.13 PRESSURE DROP
Tube side pressure drop
Tube side pressure drop is calculated from following relation
∆PtCal = fGt2Ln/5.22 x 1010 Dets Ѳt
Where
f = 0.000611
∆PtCal = [0.0006119(86651.23)216 x 2]/95.22 x 1010(0.069)(0.0207)
∆PtCal = 1.972 psi

∆PtCal/2 = ∆Ptoriginal
∆Pt = 0.986 psi = 1 psi
Shell side pressure drop
To determine shell side pressure we have to determine equivalent diameter for shell side pressure
drop i.e.
De = 4 flow area/frictional perimeter
De = 4(0.86Pt2 – 0.25пdo2)/пdo
= 0.01806m
Reynolds number based on equivalent diameter for pressure drop
Res = De Gs/μ
Res = 100079
The following relation is used to determine the shell side pressure drop
∆Ps = 8jf(Ds/De)(L/LB)(р μs2/2)(μ/μw) -0.14
jf = 1.89 x10-2
∆Ps = 62129.64N/m2
= 9.011Psia
= 62Kpa
9.10 MECHANICAL DESIGN
Mechanical design involves the design of pressure-retaining and non-pressure-retaining

components and equipments to withstand the design loads and the deterioration in service so that
the equipment will function satisfactorily and reliably throughout its life.
9.10.1 SELECTION OF HEAT EXCHANGER TYPE
There are many types design available in TEMA standard. These designs differ in their head type
at front end, head type at rear end and shell type. Selection is made on the basis of specific
requirements. In our case we have selected AEL exchanger because
1.It is cheap

2. Its design is simple
3.It can be easily manufactured
4.Most suitable for one phase fluid
5.Provides long flow path
A→ Channel with removable cover
E→ One shell pass
L→ Fixed tube sheet like a stationary head
9.10.2 SHELL MATERIAL
Carbon steel is chosen as fabricating material for shell side because of following reasons
1. It is cheap 300£/tonn
2. It is easily available
3. It can be easily worked
4. Have good tensile strength
9.10.3 NOZZEL DIAMETER
Material used = carbon steel
Feed nozzle for Shell Fluid
Mass flow rate of shell side fluid = 2622.64Kg/sec
Density of fluid = 937Kg/m3
Velocity of fluid = mass velocity/density
= 1.049m/sec
So,
A = m/ρv
= 2622.64 /937 x 1.049
= 0.008m2
Diameter of the nozzle = [Ax 4 / Π] 0.5
= [(0.008)4/3.14]0.5
= 0.1m
9.10.4 BAFFLE DETAILS
Baffle cut
25% cut (the length of the baffle from the shell to the flat edge of the baffle is 75% of the
diameter of the shell)
Baffle diameter
For shell diameter of 6in to 25in Baffle diameter is given by the relation,
Db = Ds- 1.66mm
= 401.4mm
Baffle spacing
Not all 1-2 exchangers have 25% cut segmental baffles. When it is desire that a fluid pass
through shell with extremely small pressure drop, it is possible to depart from the use of 25% cut
segmental baffles and use only support plates. These will usually be half circules, 50%cut plates
which provide rigidity and prevent tubes from sagging. If 25%cut baffles are used then according
to Perry’s Chemical Engineering Handbook
Minimum baffle spacing
PD = Di/5
PD = 0.0806m
Number of baffles
NB = (L/baffle spacing) -1
= 59
Height of baffle
Height of baffle = 0.75 * Ds
= 0.3022m
9.10.5 TUBE SIDE CALCULATIONS
Material used = Stainless steel304

Composition: C=0.08% Mn=2% Cr=17-20% Ni=8-11%

Stainless steel is selected because
1. It has high tensile strength (108N/mm2 ) as compared to mild steel (77 N/mm2)
2. Stainless steel304 has low cost (1600£/ton) as compared to other types of stainless steel
(Ferritic, Austentic, Martenstic)
3.It has high corrosion resistance due to high Cr content(17%-20%)
No. of tube passes = 2
Number of tubes = 86
Outside diameter = 0.0254m
Inside diameter = 0.0211m
Wall thickness of tubes = 0.021m
Length of tubes = 4.876m
Tube Pitch
The center to center distance between two adjacent tubes is known as tube pitch. According to
TEMA standards the minimum pitch must be 1.25 times the outside diameter of the tube
Pt = 1.25*Do
Pt = 0.03175m
9.10.6 CHANNEL DESIGN
Channel Length
Lc = 1.3 x (cross sectional area of tube/pass)/Ds
= 1.3(3.14x0.0833/2)/0.667
= 0.25ft

SPECIFICATION SHEET
Item name Shell and tube heat exchanger
Item required 1
Type 1-2 pass shell and tube
Shell diameter 0.403m
Tube diameter 0.0254m
Number of tubes 86
Tube length 4.87m
Tube thickness BWG 16
Number of baffles 59
Material of construction Stainless steel304

Chapter 10
DESIGN OF DISTILLATION COLUMN

10.1 DISTILLATION
In industry it is common practice to separate a liquid mixture by distilling the components, which
have lower boiling points when they are in pure condition from those having higher boiling
points. This process is accomplished by partial vaporization and subsequent condensation.
“It is a process in which a liquid or vapor mixture of two or more substances is separated
into its component fractions of desired purity, by the application and removal of heat”.
The creation or addition of another phase in distillation is obtained by the repeated vaporization
and condensation of the fluid. The separation process exploits the differences in vapor pressure
of key components in the mixture initiate the separation.
The advantages of distillation are its simple flow sheet, low capital investment and low risk. The
separation process is able to handle wide ranges of feed concentrations and throughputs while
producing a high purity product.
10.2 TYPES OF DISTILLATION COLUMNS
There are many types of distillation columns, each designed to perform specific types of
separations, and each design differs in terms of complexity.
 Batch columns
 Continuous columns
10.2.1 Batch Columns
In batch operation, the feed to the column is introduced batch-wise. That is, the column is
charged with a 'batch' and then the distillation process is carried out. When the desired
purification of product is achieved, a next batch of feed is introduced.
10.2.2 Continuous Columns
In contrast, continuous columns process a continuous feed stream. No interruptions occur unless
there is a problem with the column or surrounding process units. They are capable of handling
high throughputs and are the more common of the two types. We shall concentrate only on this
class of columns.

10.3 SELECTION BETWEEN PLATE AND PACKED COLUMN
Vapor liquid mass transfer operation may be carried either in plate column or packed column.
These two types of operations are quite different. A selection scheme considering the factors
under four headings,
i) Factors that depend on the system i.e. scale, foaming, fouling factors, corrosive
systems, heat evolution, pressure drop, liquid holdup.
ii) Factors that depend on the fluid flow moment.
iii) Factors that depends upon the physical characteristics of the column and its internals
i.e. maintenance, weight, side stream, size and cost.
iv) Factors that depend upon mode of operation i.e. batch distillation, continuous
distillation, turndown, and intermittent distillation.
10.4 SELECTION OF THE PLATE TYPE
There are four main tray types, the bubble cap, sieve tray, ballast or valve trays and the counter
flow trays.
I have selected sieve tray because:
i) They are lighter in weight and less expensive. It is easier and cheaper to install.
ii) Pressure drop is low as compared to bubble cap trays.
iii) Peak efficiency is generally high.
iv) Maintenance cost is reduced due to the ease of cleaning.
10.4.1 Selection Criteria of Trays
Cost
Cost of plate depends upon material of construction used.
For mild steel, the ratio of cost between plates is
Sieve plate : valve plate : bubble-cap plate
3 : 1.5 : 1.0.

Capacity
Sieve tray > valve tray > bubble-cap tray
Operating Range
It is the range of liquid and vapor flow rates which must be above the weeping conditions and
below the flooding conditions. Operating range flexibility comparison is
Bubble cape tray > Valve tray > Sieve tray
For good design, sieve plate gives satisfactory operating range.
Pressure drop
Bubble-cap tray > valve tray > sieve tray
Choice of Tray Type (Sieve Tray)
 Sieve plates are lighter in weight and less expensive. It is easier and cheaper to install.
 Pressure drop is low as compared to bubble cap trays.
 Maintenance cost is reduced due to ease of cleaning.
 If properly designed, sieve tray gives desired separation
10.5 MAIN COMPONENTS OF DISTILLATION COLUMN
Column internals such as trays/plates and/or packing which are used to enhance component
separations.
 A reboiler to provide the necessary vaporization for the distillation process. The liquid
removed from the reboiler is known as the bottoms product or simply, bottoms.
 A condenser to cool and condense the vapor leaving the top of the column. The
condensed liquid that is removed from the system is known as the distillate or top
product.
 A reflux drums to hold the condensed vapor from the top of the column so that liquid
(reflux) can be recycled back to the column. The condensed liquid is stored in a holding
vessel known as the reflux drum. Some of this liquid is recycled back to the top of the
column and this is called the reflux.

A schematic of a typical distillation unit with a single feed and two product streams is shown
above.
10.6 FACTORS AFFECTING OPERATION OF DISTILLATION COLUMN
10.6.1 Vapor Flow Conditions
Adverse vapor flow conditions can cause:
10.6.2 Foaming
Foaming refers to the expansion of liquid due to passage of vapor or gas. Although it provides
high interfacial liquid-vapor contact, excessive foaming often leads to liquid buildup on trays. In
some cases, foaming may be so bad that the foam mixes with liquid on the tray above. Whether
foaming will occur depends primarily on physical properties of the liquid mixtures, but is
sometimes due to tray designs and condition. Whatever the cause, separation efficiency is always
reduced.
10.6.3 Entrainment
Entrainment refers to the liquid carried by vapor up to the tray above and is again caused by high
vapor flow rates. It is detrimental because tray efficiency is reduced: lower volatile material is
carried to a plate holding liquid of higher volatility. It could also contaminate high purity
distillate. Excessive entrainment can lead to flooding.

10.6.4 Weeping/Dumping
This phenomenon is caused by low vapor flow. The pressure exerted by the vapor is insufficient
to hold up the liquid on the tray. Therefore, liquid starts to leak through perforations. Excessive
weeping will lead to dumping. That is the liquid on all trays will crash (dump) through to the
base of the column (via a domino effect) and the column will have to be re-started. Weeping is
indicated by a sharp pressure drop in the column and reduced separation efficiency. 10.6.5
Flooding
Flooding is brought about by excessive vapor flow, causing liquid to be entrained in the vapor up
the column. The increased pressure from excessive vapor also backs up the liquid in the down
comer, causing an increase in liquid holdup on the plate above. Depending on the degree of
flooding, the maximum capacity of the column may be severely reduced. Flooding is detected by
sharp increases in column differential pressure and significant decrease in separation efficiency.
10.6.6 Reflux Conditions
Minimum trays are required under total reflux conditions, i.e. there is no withdrawal of distillate.
On the other hand, as reflux is decreased, more and more trays are required.
10.6.7 Feed Conditions
The state of the feed mixture and feed composition affects the operating lines and hence the
number of stages required for separation. It also affects the location of feed tray.
10.6.8 State of Trays and Packings
Remember that the actual number of trays required for a particular separation duty is determined
by the efficiency of the plate. Thus, any factors that cause a decrease in tray efficiency will also
change the performance of the column. Tray efficiencies are affected by fouling, wear and tear
and corrosion, and the rates at which these occur depends on the properties of the liquids being
processed. Thus appropriate materials should be specified for tray construction.
10.6.9 Column Diameter
Vapor flow velocity is dependent on column diameter. Weeping determines the minimum vapor
flow required while flooding determines the maximum vapor flow allowed, hence column
capacity. Thus, if the column diameter is not sized properly, the column will not perform well.

10.7 DESIGN OF PLATE DISTILLATION COLUMN
1. Calculation of Minimum Reflux Ratio Rm.
2. Calculation of optimum reflux ratio.
3. Calculation of minimum no of Plates
4. Calculation of theoretical number of Plates.
5. Determining the location of feed Plate
6. Calculation of actual number of Plates.
7. Calculation of diameter of the column.
8. Determination of weeping point.
9. Calculation of pressure drop.
10. Determination of number of holes
11. Calculation of the height of the column
Temperature of feed = 52.15o C
Temperature of top product = 42.40o C
Temperature of bottom product = 79.2o C
P = 262 KPa
Compositions
Component Feed ( Xf ) Top ( Xd ) Bottom (Xb)
Acetaldehyde 0.82 0.993249 0.047044
Methyl Iodide 0.02 0.006602 0.064146
Methyl Acetate 0.15 0.000149 0.831384
Water 0.01 - 0.057426

Heavy Key Component = Methyl Acetate
Light Key Component = Methyl Iodide
Relative volatility
Methyl Acetate (heavy) = 1
Methyl Iodide (light) = 2.51
10.7.1 CALCULATION OF MINIMUM REFLUX RATIO
Using Underwood equation
α A xfA α x
 B fB  1  q
αA  θ αB  θ
As feed is entering at its B.P. so, q = 1
By trial (estimation),  = 2.2516
Using equation of minimum reflux ratio
α A xfA α x
 B fB  R m  1
αA  θ αB  θ
putting all values Rm = 0.476
10.7.2 ACTUAL REFLUX RATIO
The rule of thumb is:
R = (1.2 ------- 1.5) Rmi
R = 1.5 Rmin
R = 0.716
10.7.3 CALCULATION OF MINIMUM NUMBER OF PLATES
The minimum no. of stages Nmin is obtained from Fenske relation which is
N min 
log     
X LK
X HK D
X HK
X LK B
log α AB ave

Nmin = 8.83
Nmin = 9
10.7.4 CALCULATION OF THEORATICAL NUMBER OF PLATES
Gilliland related the number of equilibrium stages and the minimum reflux ratio and the number
of equilibrium stages with a plot that was transformed by Eduljee into the relation;
N  N min   R  Rmin 
0.566

 .751   
N 1 R  1 
  
From which the theoretical number of stages to be,
N = 19
10.7.5 DETERMINING THE LOCATION OF FEED PLATE
The Kirkbridge method is used to determine the ratio of trays above and below the feed point.
 
  .206 log  B  x HK   x LK B  
2
log  N D
 N B   D
 x LK 
 x HK D  

From which,
NB + 2.91 ND = 19
Number of Plates above the feed tray = NB = 5
Number of Plates below the feed tray = ND = 14
10.7.6 ACTUAL NUMBER OF PLATES
Tray Efficiency
40.42  79.2
Average temperature of column = = 60.8oC
2
Feed viscosity at average temperature = ave = 0.100 Cp
(Relative volatility of key component)  ave = 1.69
Eo = 0.492 * (L * (αlk/αhk) av) – 0.245)

Overall efficiency of column = 75.28%
19
So, No. of actual trays = = 25
0.7523
Location of feed point = 20
10.7.7 CALULATION OF THE COLUMN DIAMETER
TOP CONDITIONS BOTTOM CONDITIONS
Ln = D* Rmin Lm = Ln + F
Ln = 0.102 kg/s Lm = 0.297 kg/s
Vn = Ln + D V m = Lm – B
Vn =0.2442 kg/s Vm =0.2442 kg/s
T = 40.42o C T = 79.2 oC
ρV = 3.747 Kg/m3 ρV = 5.910 Kg/m3
ρL = 753 Kg/m3 ρL = 922.8 Kg/m3
Maximum volumetric flow rate of Vapor
Top  0.2442  0.06517 m3/sec

3.747
0.2442
Bottom   0.04132 m3/sec
5.910
Maximum Volumetric flow rate of liquid
0.102
  .000135 3
Top 753 m /sec
0.297
Bottom   .000322 m3/sec
922
Calculate FLV = liquid vapor flow factor

LW V
FW 
VW L
LW = liquid flow rate
VW = vapor flow rate
 V = vapor density (kg / m3)
 L = liquid density (kg/ m3)
0.102 3.747
FW Top 
0.2442 753
= 0.0297
Bottom Calculation
0.297 5.91
FLV Bottom 
0.2442 922
= 0.0973
And for a tray spacing of Ts=600 mm.
Flooding parameter
Csb, flood = 0.1 m/s
σ = liquid surface tension, mN/m (dyne/cm.)
σ = 18.4 dynes/cm
Vnf = gas velocity through the net area at flood, m/s
Vnf = Csb * (σ/20) 0.2 * [(ρL – ρV)/ ρv] 0.5
Vnf = 1.306 m/sec
Flooding = 85 %
Let
Actual velocity, Vn = 0.85 × Vnf
i.e., Vn = 1.1101 m/s

Ac = 0.04132/1.1101
Ac = 0.037
So area of column at bottom, Ac = 0.037
Diameter of the column at the bottom
D = √(4 * Ac/)
= √(4 * 0.037)/(3.14)
= 0.217 m
Calculation at the TOP
0.102 3.747
FW Top 
0.2442 753.1
= 0.0297
And for a tray spacing of Ts=600 mm.
Flooding parameter
Csb, flood = 0.12 m/s.
σ = liquid surface tension,
σ = 21.04 dynes/cm
Vnf = gas velocity through the net area at flood,
Vnf = Csb * (σ/20) 0.2 * [(ρL – ρV)/ ρv] 0.5
Vnf = 1.71 m/sec
Flooding = 80 %
Let
Actual velocity, Vn = 0.85 × Vnf
i.e., Vn = 1.4535 m/s
Ac = 0.06517 /1.4535

Ac = 0.044
So area of column at top, Ac = 0.044
Diameter of the column at the bottom
D = √(4 * Ac/)
= √(4 * 0.044)/(3.14)
= 0.238 m
10.7.8 DETERMINATION OF THE WEEPING POINT
Column diameter (base) = 0.024 m

Column Area Ac  d2
4
Ac = 0.044 m2
Down comer area Ad  0.12  0.044 = 0.0053 m2
Net area An = Ac – Ad
= 0.0387 m2
Active area Aa =Ac – 2Ad = 0.0334 m2
Hole area Ah
take 10% Aa = 0.1 × 0.0334 = 0.00334 m2
Weir length
Ad / Ac = 0.12
Lw / dc = 0.76
Lw  0.76  0.24 = 0.181 m
(Recommended = 40 to 50mm)
Take weir height, hw = 50 mm
Hole diameter, dh = 5 mm
Plate thickness = 5 mm
Check Weeping
Maximum liquid rate= .297 kg/sec
Minimum liquid rate at 70% turn down  0.7  0.297 = 0.209kg/sec
Height of liquid crest over segmental weir
how = weir crust
for segmental down comer

2/3
 Lw 
Maximum how  750 
  l  Ad 
2/3
 0.297 
how  750 
 922  0.181 
= 11.007 mm liquid
2/3
 0.2090 
Minimum how  750  = 0.033 mm liquid
 930  0.729 
at minimum hw + how = 50 + 11.007= 61.007 mm liquid
Min design vapor velocity
K2 = 30.4
 K  0.925.4  an 
U min   2
v1 / 2
 30.4  0.925.4  5
U min   = 4.78 m/s
5.911 / 2
10.7.9 CALCULATION OF PRESSURE DROP
Dry Plate pressure drop
Maximum vapor velocity through holes
Uh = Max vapor volumetric flow Rate/Hole Area
Uh = .06517/0.00334 = 19.511 m/sec
Plate thickness / hole dia = 5 / 5 = 1.0

And let the hole pitch = 3
Ah/Ap = 0.07
Co = 0.83
2
Uˆ  
hd  51 h  V
 C o   L
2
19.511 5.91
hd  51  = 180.48 mm liquid
 0.83  922
Residual Head
12.5  10 3
hr   13.545 mm liquid
922
Total Pressure Drop
ht = hd + (hw + how) + hr
Total pressure drop = 180.48 + (50 + 11.007) + 13.545
ht = 255 mm liquidDown comer Liquid Backup
Take hap = hw – 10 = 40 mm
Area under apron = hap* Lw
= .04 *0.181 = 0.00724 m2

2
 l 
hdc  166 wd 
  L An 
2
 0.297 
hdc  166  = 0.32 mm liq.
 922  0.00724 
Backup in down comer
hb= (hw + how) + ht + hdc = 50 + 11.007 + 255 + 0.32
= 316 mm liquid = 0.316 mm liquid
½ (Tray spacing + weir height) = [½ * (600 + 50)] = 0.3195m

0.316 < ½ (Tray spacing + weir height)
So tray spacing is acceptable
10.7.10 DETERMINATION OF NUMBER OF HOLES
Diameter of one hole = 5 mm =0.005 m
Area of one hole = 22/7*(0.005 /2)2 = 1.9635 *10-6
Total Hole Area =0.00344 m2
No of Holes =0.02394 m2 / 1.9635 * 10-6 = 1701
10.7.11 CALCULATION OF HEIGHT OF COLUMN
Number of plates = 25
Spacing between each plate = 600 mm
Space for disengagement of vapor and liquid on top = 600 mm
Space for disengagement of vapor and liquid in bottom = 600 mm
Height of column = [(#of plates - 1) × (space between each plate)] + (space for
disengagement on top and bottom) = [((25-1)×600) + 1000)/1000] = 15.6 m
So height of column = 15.6 m

SPECIFICATION SHEET
Identification:
Item Distillation column
Item No. DC 1
No. required 1
Tray type Sieve tray
Function : Separation of Acetaldehyde
Operation: Continuous
Design Data
No. of trays = 25 No Weeping
Pressure = 262 KPa Weir Height = 0.05 m
Height of Column = 15.6 m Weir Length = 0.181 m
Diameter of Column =0.24 m Reflux Ratio = 0.716
Hole Size = 5 mm Tray Spacing = 0.6 m
Tray Pressure Drop = 0.093 m Efficiency = 75.6%
Hole Area = 0.003344 m2

Chapter 11
COST ESTIMATION

11.1 ECONOMIC ANALYSIS OF ACETALDEHYDE PLANT
The capital needed to supply the necessary manufacturing and plant facilities is called the fixed
capital investment while that necessary for the operation of the plant is termed as working capital
investment. The fixed capital portion may be further subdivided into:
Manufacturing fixed capital
Non-manufacturing fixed capital investment.
11.2 FIXED CAPITAL INVESTMENT
Manufacturing fixed capital investment represents the capital necessary for the installed process
equipment. With all auxiliaries that are needed for the complete process operation. Expenses for
piping, instruments, installation, and foundation and site preparation are typical examples of cost
included in the manufacturing fixed capital investment. Fixed capital required for the
construction overhead and for all plant components that are not directly related to the process
operation is designed as the non-manufacturing fixed capital investment.
11.3 WORKING CAPITAL
The working capital for an industrial plant consists of the total amount of the money invested in:
Raw material and supplies carried in stock.
Finished products in stock and semi finished products in the process of being manufactured.
Accounts receivable.
Cash kept on hand for monthly payments of operating expenses, such as salaries, wages and raw
material purchases.
Accounts payable
Taxes payable.
The ratio of the capital to total investment varies with different companies, but most chemical
plants use an initial working capital amounting to 10 to 20 % of the total capital investment

11.4 ESTIMATION OF PURCHASE EQUIPMENT COST
11.4.1 Cost of Feed storage tank V-100
Capacity of feed storage tank is 100 m3.The tank is made up of carbon steel tank and spherical in
shape. The tank is at pressure 310KPa. The purchased cost of liquid feed storage tank of this
specification can be estimated using fig.12-52 [18] the purchased cost of feed storage tank =
$500000
11.4.2 Cost of gas storage tank V-101
The capacity of gas storage tank is 1000 m3.The tank is made of carbon steel and is at
atmospheric pressure. Using fig.12-57 [18]
Cost of gas storage tank of above specifications is $90,000.
11.4.3 Cost of byproduct storage tank V-103
The capacity of byproduct storage tank is 50m3. Using fig.12-52 of [18] the cost of storage tank
for this capacity is $ 70,000.
11.4.4 Cost of product storage tank V-104
The capacity of product storage tank is 50m3. Using fig.12-52 [18] the cost of storage tank for
this capacity is $70,000.
11.4.5 Cost of CSTR R-100
Capacity of CSTR is 21.2m3. The material of construction of CSTR is stainless steel. For this
capacity and material the purchased cost of jacked CSTR is 12,000$ according to figure 13-15
[18].The pressure correction factor is 0.899(310.2/345) and agitator speed correction factor is
0.42(52.2/125).Applying these factors the cost of R-100 becomes $45310.
11.4.6 Cost of Condenser E-100
The available heat transfer are of the condenser is 9.81m2..The condenser is operating at 310KPa
and cooling water is used for condensation. Tubes are made of stainless steel 316 and shell is
made of carbon steel. Using fig.14-18 [18]
Purchased cost = $4800
Pressure adjustment factor is 0.98 so purchased cost after pressure adjustment

Purchased cost = 4800 x 0.98 = $4707
11.4.7 Cost of Separator V-102
Separator is operating at 389KPa pressure. It is made of stainless steel. Diameter and height are
1.2m and 3.6m respectively. The thickness of the separator is 10.54mm.
Shell weight = ∏ Di L t ρsteel
= 3.142 x 1.20 x 3.6 x 0.001054 x 7840
= 112.15Kg
The head of separator is torispherical and its weight can be calculated using following relation
[18]
Weight of head = 2∏ [(di/2)2 t ρ r]2
= 2 x 3.14 x [(1.2/2)2 x 0.001054 x 7840 x 0.6]2
= 22.43Kg
Total weight of the shell including 15% increase for nozzles, manholes and saddles
Total weight = (112.15 + 22.43) x 1.15
= 154.76Kg
Purchased cost = (Cost per unit Kg) x (Total weight)
= 73 x (154.76)-0.34 x (154.76)
= $2035
11.4.8 Cost of Absorber C-100
Absorber is made of stainless steel 316.The diameter of the column is 0.92m and height is
12.36m. Using fig.15-16 [18] purchased cost including installation and auxiliaries is $18000 per
meter of height.
Purchased cost = 18000 x 12.36
= $222480

11.4.9 Cost of Mixer M-100
It is static mixer. It is made of carbon steel. The diameter of the mixer is 0.1m. Using fig.12-
41[18] purchased cost of static mixer is $1200.
11.4.10 Cost of Heat Exchanger E-101
It is fixed tube shell and tube heat exchanger. Shell is made of carbon steel and tubes are made
of stainless steel. Shell side pressure is 287KPa and tube side pressure is 1035KPa.Satureated
steam is used is heating media. Using fig.14-18 [18] purchased cost of heat exchanger is
$9000.The pressure adjustment factor is 0.96.
Purchased cost = 9000 x 0.96
= $8640
11.4.11 Cost of Distillation Column C-101
Height of the column is 16.32m and diameter is 0.238m.Purchasedd cost for these specifications
is $ 29000.
Diameter correction factor = 0.238/0.5 = 0.476
Pressure corre4ction factor = 1
Material (Stainless steel 316) correction factor = 3
Purchased cost without internals and channels = 29000 x 3 x 0.476
= $41412
Steel connection cost
Column wall thickness = 6mm
Cost of coupling = $800 per meter of connection
= 800 x 16.32
= $13056
Cost of Trays
The trays used in the column are sieve trays and made up of stainless steel
Cost of trays = $700 per tray

= 700 x 25
= $17500
Purchased cost of column = 41412 + 13056 + 17500 = $71968
11.4.12 Cost of Pump P-100
Flow rate of the fluid 1454Kg/h. The density of the fluid is 1104Kg/m3.
Volumetric flow rate = 1454/114074
= 1.317m3/h
= 3.7 x 10-4m3/sec
Capacity = 3.7 x 10-4m3/sec
Using fig.12-13 [18] purchased cost of centrifugal pump
Purchased cost = $ 1100
11.4.13 Cost of Pump P-101
Capacity = 1.193m3/h
= 3.3 x 10-3m3/sec
The pump is made up of cast iron. Using fig.12-13 [18] purchased cost of centrifugal pump
11.4.14 Cost of Heat Exchanger E-102
It is double heat exchanger. It is made of carbon steel and stainless steel. Shell side pressure is
287KPa .Saturated steam is used is heating media. Steam pressure is 100KPa. Using fig.14-18
[18] purchased cost of heat exchanger is 9000$.

ESTIMATION OF TOTAL PURCHASE EQUIPMENT COST
S.No Equipment Quantity Cost ($)
1 Storage tank 3 7300
2 Reactor 1 45310
3 Heat Exchanger 3 15440
4 Distillation Column 2 143936
5 Absorber 1 222480
6 Separator 1 2035
7 Pump 2 2300
Total 13 438801
11.5 COST OF OOLING UTILITY
Total water used = (water used in Reactor R-100) + (water used in condenser E-100) +
(water used in absorber C-100) + (water used in Distillation column C-101) + (Water used in
Distillation column C-102)
= 10618 + 1915.3 + 26949.46 + 11.8 + 518.4
= 4013Kg/h
Using table 6-14 [18] cost of utilities
Cost of cooling water = 0.08$/1000Kg/h
= (0.08/1000) x 40013
= $ 3.2/h

11.6 COST OF HOT UTILITY
Total steam used = (steam used in heat exchanger E-101) + (steam used in heat
Exchanger E-104) + (steam used in Reboiler E-103) + (steam used in Reboiler E-106)
= 4770 + 128.45 + 500 + 276
= 5674.45Kg/h
Using table 6-14 [18] cost of utilities
Steam Cost = $ 4.40per 1000Kg/h
= (4.40/1000) x 5674.45
= $2497
11.7 ESTIMATION OF FIXED CAPITAL INVESTMENT
Component Selected % of Normalized % of Estimated Cost

FCI FCI ($)
Direct Cost
Purchased equipment 25 22.9 438801
Purchased equipment installation 9 8.3 159041.4
Instrumentation(installed) 10 9.2 176286.9
Piping(installed) 8 7.3 139879.8
Electrical(installed) 5 4.6 88143.43
Building(including services) 5 4.6 88143.43
Yard improvements 2 1.8 34490.91
Service facilities(installed) 15 13.8 264430.3

Indirect Cost
Engineering 8 7.3 139879.8
Construction expense 10 9.2 176286.9
Legal expense 2 1.8 34490.91
Contractor’s fee 2 1.8 34490.91
Contingency 8 7.3 139879.8
Fixed Capital Investment 109 100 1916161.57
11.8 ESTIMATION OF TOTAL CAPITAL INVESTMENT
Direct Cost, D.C 1389217
Indirect Cost ,I.D 525028.3
Fixed Capital Investment, FCI 1916161.57
Working Capital (WC) 15% of TCI 338146.2
Total Capital Investment (TCI), FCI + WC 2254308
11.9 PRODUCT COST
The following product cost analysis has been done on the annual basis depreciating the entire
total capital investment by the method of straight line for a life of 10 years assuming 5% salvage
value at the end of useful life.
d = [V-Vs/n]
V = (FCI) = $1916161.57
Vs = 0.05* FCI = $95808.08

n = 10
d = $182035.34/yr
Total product cost, TPC = TCI – d = $2072272.66
Fixed charges @ 15%of TPC = $310841
Direct production cost @60% of TPC = $1243364
Plant over head cost @10% of TPC = $483183.00
General expanse @15% of TPC = $207227.26

Chapter 12
INSTRUMENTATION AND PROCESS

CONTROL

12.1 INSTRUMENTS
Instruments are provided to monitor the key process variables during plant operation. They may
be incorporated in automatic control loops or used for the manual monitoring of the process
operation. They may also be part of an automatic computer data logging system. Instruments
monitoring critical process variables will be fitted with automatic alarms to alert the operators to
critical and hazardous situations.
12.2 INSTRUMENTATION AND CONTROL OBJECTIVES
The primary objective of the designer when specifying instrumentation and control schemes are:
1. Safer Plant Operation

 To keep the process variables within known safe operating limits.
 To detect dangerous situations as they develop and to provide alarms and automatic
shut-down systems.
 To provide inter locks and alarms to prevent dangerous operating procedures.
2. To achieve the design product output.
3. To maintain the product composition within the specified quality standards.
4. To operate at the lowest production cost, commensurate with the other objectives.
In a typical chemical processing plant these objectives are achieved by a combination of
automatic control, manual monitoring and laboratory analysis.
12.3 COMPONENT OF THE CONTROL SYSTEM
12.3.1 PROCESS
Any operation or series of operations that produces a desired final result is a process. In this
discussion the process is the cracking of naphtha.
12.3.2 MEASURING ELEMENT
Of all the parts of the control system the measuring element is perhaps the most important. If
measurements are not made properly the remainder of the system cannot operate satisfactorily.

Variables to be controlled
 Pressure measurements
 Temperature measurements
 Flow Rate measurements
 Level measurements
Variables to be recorded
 Indicated temperature
 Composition
 Pressure, etc.
12.3.3 CONTROLLER
The controller is the mechanism that responds to any error indicated by the error detecting
mechanism. The output of the controller is some predetermined function of the error.
In the controller there is also an error-detecting mechanism which compares the measured
variables with the desired value of the measured variable, the difference being the error.
12.3.4 FINAL CONTROL ELEMENT

The final control element receives the signal from the controller and by some predetermined
relationships changes the energy input to the process.
12.4 SELECTION OF CONTROLLER
In general the process controllers can be classified as:
 Pneumatic controllers
 Electronic controllers
 Hydraulic controllers
In the acetaldehyde manufacturing from methyl acetate the controller and the final control
element may be pneumatically operated due to the following reasons:

 The pneumatic controller is very rugged and almost free of maintenance. The maintenance
men have not had sufficient training and background in electronics, so basically
pneumatic equipment is simple.
 The pneumatic controller appears to be safer in a potentially explosive atmosphere which

is often present in the petro-chemical industry.
 Transmission distances are short. Pneumatic and electronic transmission system is

generally equal upto about 250 to 300 feet. Above this distance, electronic systems begin
to offer savings.
12.5 MODES OF CONTROL
The various type of control is called "modes" and they determine the type of response obtained.
In other words these describe the action of the controller that is the relationship of output signal
to the input or error signal. It must be noted that it is error that actuates the controller. The four
basic modes of control are:
 On-off Control
 Integral Control
 Proportional Control
 Rate or Derivative Control
In industry purely integral, proportional or derivative modes seldom occur alone in the control
system.
The On-off controller is the controller with very high gain. In this case the error signal at once
off the valve or any other parameter upon which it sits or completely sets the system.
12.6 ALARMS, SAFETY TRIPS AND INTERLOCKS
12.6.1ALARMS
Alarms are used to alert operators of serious, and potentially hazardous, deviations in process
conditions. Key instruments are fitted with switches and relays to operate audible and visual
alarms on the control panels.

12.6.2 SAFETY TRIPS
The basic components of automatic trip systems are:
 A sensor to monitor the control variable and provide an output signal when a preset valve
is exceeded (the instrument).
 A link to transfer the signal to the actuator usually consisting of a system of pneumatic or
electric relays.
 An actuator to carry out the required action; close or open a valve, switch off a motor.
A safety trip can be incorporated in control loop. In this system the high-temperature alarm
operates a solenoid valve, releasing the air on the pneumatic activator closing the valve on high
temperature.
12.6.3 INTERLOCKS
Where it is necessary to follow the fixed sequence of operations for example, during a plant
start-up and shut-down, or in batch operations-inter-locks are included to prevent operators
departed from the required sequence.
12.7 TYPES OF CONTROLLERS
12.7.1 FLOW CONTROLLER
These are used to control feed rate into a process unit. Orifice plates are by far the most type of
flow rate sensor. Normally, orifice plates are designed to give pressure drops in the range of 20
to 200inch of water.
12.7.2 TEMPERTUIRE CONTROLLER
Thermocouples are the most commonly used temperature sensing devices. The two dissimilar
wires produce a mili volt emf that varies with the "hot-junction" temperature. Iron constrictant
thermocouples are commonly used over the 0 to 1300°F temperature range.
12.7.3 PRESSURE CONTROLLER
Bourdon tubes, bellows, and diaphragms are used to sense pressure and differential pressure. For
example, in a mechanical system the process pressure force is balanced by the movement of a
spring. The spring position can be related to process pressure.

12.7.4 LEVEL CONTROLER
Liquid levels are detected in a variety of ways. The three most common are:
 Following the position of a float, that is lighter them the fluid.
 Measuring the apparent weight of a heavy cylinder as it buoyed up more or less by the
liquid (these are called displacement meters).
 Measuring the difference in static pressure between two fixed elevations, one in the vapor
above the liquid and the other under the liquid surface. The differential pressure between the
two level taps is directly related to the liquid level in the vessel.
12.8 CONTROL SCHEME FOR 2-PHASE SEPARATOR (FLSH DRUM)
Feed of flash drum is composed of five components i.e. Methyl acetate, Methyl iodide, Carbon
monoxide, Hydrogen, Acetaldehyde, Acetic acid. As feed is flashed from high pressure 210KPa
to low pressure 289KPa, vapor is produced and reaches equilibrium with the remaining liquid.
Steam flowing through a coil supplies necessary heat for maintaining the desired temperature in
the drum, despite any variations in the operating conditions. For this purpose there is need to
 Identify controlled variables

 Identify the manipulated variables
 Generate all feasible loop configurations.
Total mass balance (assuming constant molar density and insignificant vapor hold up):
Aρ dh/dt = Ff - (Fv + FL)

Component balance
Aρ d(hxi)/dt = Ff zi - (Fv yi + FL xi) i=1,2,…5

Heat balance
Cp,L A d(hT)/dt = Cp,f FfTf – (Cp,vFvT + Cp,L FLT) + UAs (Ts –T)
Vapor -liquid equilibrium relationship
yi = Ki (T, P) xi

Consistency constraints
N
∑xi = 1 and
i=1
N
∑yi = 1
I=1
All the relations above constitute system of 13 equations with 34 variables. These variables are
classified as follows:
Constants (N+7) = 12
A, As, U, ρ, Cpf, Cpv, CpL, and Ki (T,P) for i=1,2,…5
Externally specified (N) = 5:

Tf, zi for i=1,2,…4
Unspecified (2N +7) = 17

Ff, Fv, FL, ρ, T , h, Ts or (Ws) and xi, yi for i=1,2,…5
Controlled Variables:
Number of controlled variables
NCV = (2N + 7) - (2N + 3)

But which four of the 17 unspecified variables will be selected as controlled outputs? The
operating requirements dictate that T and P should be kept constant to achieve the desired
separation. Furthermore, for constant production the flow rate of the liquid feed should be
maintained at the desired value. Finally, liquid level should remain within bounds. Thus T, P Ff
and h are the controlled variables.

Control Scheme for Flash Drum
V-3
Fv
FC
S-1
PC
P
Ff
V-1
T
P-21
TC
h P-41
P-22
P-40
Ts, Ws
V-2 LC
P-30
FL
V-4

Chapter 13
HAZOP STUDY

13.1 INTRODUCTION
A HAZOP survey is one of the most common and widely accepted methods of systematic
qualitative hazard analysis. It is used for both new or existing facilities and can be applied to a
whole plant, a production unit, or a piece of equipment It uses as its database the usual sort of
plant and process information and relies on the judgment of engineering and safety experts in the
areas with which they are most familiar. The end result is, therefore reliable in terms of
engineering and operational expectations, but it is not quantitative and may not consider the
consequences of complex sequences of human errors. The objectives of a HAZOP study can be
summarized as follows:
 To identify (areas of the design that may possess a significant hazard potential.
 To identify and study features of the design that influence the probability of a hazardous
incident occurring.
 To familiarize the study team with the design information available.

 To ensure that a systematic study is made of the areas of significant hazard potential.
 To identify pertinent design information not currently available to the team.

 To provide a mechanism for feedback to the client of the study teams detailed comments.
13.2 STEPS CONDUCTED IN HAZOP STUDY
1. Specify the purpose, objective, and scope of the study. The purpose may be the analysis of
a yet to be built plant or a review of the risk of no existing unit. Given the purpose and the
circumstances of the study, the objectives listed above can he made more specific. The
scope of the study is the boundaries of the physical unit, and also the range of events and
variables considered. For example, at one time HAZOP's were mainly focused on fire and
explosion endpoints, while now the scope usually includes toxic release, offensive odor,
and environmental end-points. The initial establishment of purpose, objectives, and scope
is very important and should be precisely set down so that it will be clear, now and in the
future, what was and was not included in the study. These decisions need to be made by
an appropriate level of responsible management.
2. Select the HAZOP study team. The team leader should be skilled in HAZOP and in
interpersonal techniques to facilitate successful group interaction. As many other experts

should be included in the team to cover all aspects of design, operation, process chemistry,
and safety. The team leader should instruct the team in the HAZOP procedure and should
emphasize that the end objective of a HAZOP survey is hazard identification; solutions to
problems are a separate effort.
3. Collect data. Theodore16 has listed the following materials that are usually needed.
 Process description.
 Process flow sheets.
 Data on the chemical, physical and toxicological properties of all raw materials,
intermediates, and products.
 Piping and instrument diagrams (P&IDs).
 Equipment, piping, and instrument specifications.
 Process control logic diagrams.
 Layout drawings.
 Operating procedures.
 Maintenance procedures.
 Emergency response procedures.
 Safety and training manuals.

Figure 13.1 Hazop Method Flow Diagram

Table 13.1: HAZOP Guide Words and Meanings
Guide Words Meaning
No Negation of design intent
Less Quantitative decrease
More Quantitative increase
Part of Qualitative decrease
As well as Qualitative Increase
Reverse Logical opposite of the intent
Other than Complete substitution
4. Conduct the study. Using the information collected, the unit is divided into study "nodes"
and the sequence diagrammed in Figure, is followed for each node. Nodes are points in
the process where process parameters (pressure, temperature change between nodes as a
result of the operation of various pieces of equipment' such as distillation columns, heat
exchanges, or pumps. Various forms and work sheets have been developed to help
organize the node process parameters and control logic information.
5. When the nodes are identified and the parameters are identified, each node is studied by
applying the specialized guidewords to each parameter. These guide words and their
meanings are key elements of the HAZOP procedure. They are listed in Table (8.1).
6. Repeated cycling through this process, which considers how and why each parameter
might vary from the intended and the consequence, is the substance of the HAZOP study.
7. Write the report. As much detail about events and their consequence as is uncovered by
the study should be recorded. Obviously, if the HAZOP identifies a not improbable
sequence of events that would result in a disaster, appropriate follow-up action is needed.
Thus, although risk reduction action is not a part of the HAZOP, the HAZOP may trigger
the need for such action.

8. The HAZOP studies are time consuming and expensive. Just getting the P & ID's up to
date on an older plant may be a major engineering effort. Still, for processes with
significant risk, they are cost effective when balanced against the potential loss of life,
property, business, and even the future of the enterprise that may result from a major
release.
13.3 HAZOP STUDY OF STORAGE TANK FOR METHYL ACETATE
A HAZOP study is to be conducted on Methyl acetate storage tank, as presented by the

piping and instrumentation diagram show in fig. 13.2.
In this scheme, methyl acetate is unloaded from tank trucks into a storage tank maintained
under a slight positive pressure until it is transferred to the process. Application of the
guidewords to the storage tank is shown in Table (13.2) along with a listing of
consequences that results from process deviation. Some of the consequences identified
with these process deviations have raised additional questions that need resolution to
determine whether or not a hazard exists.

Figure 13.2 Piping and instrumentation diagram

Table 13.2 Applications of storage tank
Deviations from
What event could Consequences of this deviation on item of
operating
cause this deviation equipment under consideration
conditions
Level:
Less Tank runs dry Pump cavitates
Rupture of discharge Reagent released

line
V-3 open or broken Reagent released

V-1 open or broken Reagent released
Tank rupture (busting of Reagent released
vessel)
Unload too much from

More Tank overfills
column
Reverse flow from

process Tank overfills
Temperature: Temperature of inlet is

colder than normal
Less Temperature of inlet is Possible vacuum

hotter than normal
External fire
More Region released
Tank fails

Chapter 14
ENVIRONMENTAL IMPACT ASSESSMENT

14.1 ACUTE EFFECTS
The primary acute (short—term) effect of inhalation exposure to acetaldehyde is irritation of the
eyes, skin,, and respiratory tract in humans. Asthma, coughing, pulmonary edema, and necrosis
may also occur and, at extremely high concentrations, respiratory paralysis and death.
Acute inhalation of acetaldehyde resulted in a depressed respiratory rate and elevated blood
pressure in experimental animals.
Tests involving acute exposure of animals, such as the LC50 and LD50 tests in rats, rabbits, and
hamsters, have demonstrated acetaldehyde to have low acute toxicity from inhalation and
moderate acute toxicity from oral or dermal exposure.
14.2 CHRONIC EFFECTS
In hamsters, chronic (long-term) inhalation exposure to acetaldehyde has produced changes in

the nasal mucosa and trachea, growth retardation, slight anemia, and increased kidney weight.
Symptoms of chronic intoxication• of acetaldehyde in humans resemble those of alcoholism.
The RfC for acetaldehyde is 0.009 mg/m3 based on degeneration of olfactory epithelium in rats.
EPA has medium confidence in the principal studies because appropriate histopathology was
performed on an adequate number of animals and a no-observed-adverse-effect level (NOAEL)
and a lowest-observed-adverse- effect level. (LOAEL) were identified, but the duration was short
and only one species was tested; low confidence in the database due to the lack of chronic data
establishing NOAELs and due to the lack of reproductive and developmental toxicity data; and,
consequently, low confidence in the RIO.
EPA has not established an RID for acetaldehyde
14.3 REPRODUCTIVE/DEVELOPMENT EFFECTS
No information is available on the reproductive or developmental effects of acetaldehyde in

humans. Acetaldehyde has been shown, in animals, to cross the placenta to the fetus.
Data from animal studies suggest that acetaldehyde may be a potential developmental toxin. In
one study, a high incidence of embryonic resorptions was observed in mice injected with
acetaldehyde. In rats exposed to acetaldehyde by injection, skeletal malformations, reduced birth
weight, and increased postnatal mortality have been reported.

14.4 CANCER RISK
Human data regarding the carcinogenic effects of acetaldehyde are inadequate. Only one
epidemiology study is available that several limitations including short duration, small number of
subjects, and concurrent exposure to other chemicals and cigarettes.An increased incidence of
nasal tumors in rats and laryngeal tumors in hamsters has been observed following inhalation
exposure to acetaldehyde.EPA has classified acetaldehyde as a Group B2, probable human
carcinogen.EPA uses mathematical models, based on human and animal studies, to estimate the
probability of a person developing cancer from breathing air containing a specified concentration
of a chemical. EPA calculated an inhalation unit risk estimate of 2.2 H 10-6 (m g/m3)-1. EPA
estimates that, if an individual were to breathe air containing acetaldehyde at 0.5 m g/m3* over
his or her entire lifetime, that person would theoretically have no more than a one-in-a-million
increased chance of developing cancer as a direct result of breathing air containing this chemical.
Similarly, EPA estimates that breathing air containing 5.0 m g/m3 would result in not greater
than a one-in-a-hundred thousand increased chance of developing cancer, and air containing 50.0
m g/m3 would result in not greater than a one-in-ten thousand increased chance of developing
cancer.EPA’s Office of Air Quality Planning and Standards, for a hazard ranking under Section
112(g) of the Clean Air Act Amendments; has ranked acetaldehyde in the nonthreshold category.
The 1/ED1O value is 0.033 per (mg/kg)/d and this would place it in the low category under
Superfund’s ranking for carcinogenic hazard.
14.5 ATMOSPHERIC PERSISTENCE
Acetaldehyde exists in the atmosphere in the gas phase. It also can be formed in the atmosphere
as a result of photochemical oxidation of organic pollutants in urban atmospheres. The dominant
atmospheric loss process for acetaldehyde is by reaction with the hydroxyl radical. Based on this
reaction, the atmospheric half-life and lifetime is estimated to be 15 hours and 22 hours,
respectively. The products of this reaction include formaldehyde and peroxyacetyl nitrate (PAN).

REFERENCES
1. Coulson, Richardson, Chemical Engineering, Butterworth-Heinemann, Vol: 6,
Edit: 3, (287-297,807-816), 2003.
2. Coulson, Richardson, Chemical Engineering, Butterworth-Heinemann, Vol: 3,
Edit: 3, (196-212), 1994.
3. Journal of Chemical Engineering Data Vol.41,No.3,1996
4. McCabe, Smith, Harriott, Unit Operations of Chemical Engineering, McGraw-
Hill, Edition: 6, (239-358), 2001.
5. Harry Silla, Chemical Engineering Design and Economics, Marcel Dekker,
(240,375-394), 2003.
6. D.Q. Kern, Process Heat Transfer, (716-720, 791-846)
7. George Stephanopoulos, Chemical Process Control,
8. O.A. Hougen, K.M. Waston, R.A. Ragatz, Chemical Process Principles, John
Wiley & sons, INC, New York, Edit:2
9. David M. Himmelblau, Baic Principles and Calculations in Chemical
Engineering, Printice Hall PTR, Edit: 6, 1974.
10.J.M. Smith, H.C. Van Ness, M.M. Abbott, Introduction to Chemical
Engineering Thermodynamics, Mc Graw Hill, Edit: 6.
11.Robert. H. Perry, Don W. Green, Chemical engineer’s Handbook, Mc Graw
Hill, Edit: 7, 2004.
12.Bhattacharyya, Chemical Equipment Design Mechanical Aspects, CBS, Edit: 1,
2001.
13.Robert .E .Trey ball, Mass transfer operation.
14.Ernest E. Ludwig, Applied Process Design, Gulf Professional Publishing, Vol:
6, Edit: 3, 1997
15.Journal of Chemical and Engineering Data, Vol. 15, No. 3, 1970
16.T.Kuppan, Heat Exchanger Design Handbook, Marcel Dakker, INC., 2000.
17.Carl Branan, Rules of Thumb for Chemical Engineers, Golf Professional
Publicashing, Edit: 3,2002.
18.Max. S. Peters, Klaus D. Timmerhaus, Plant Design and Economics for
Chemical Engineers, Mc Graw Hill, Edit: 5, 1999.

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Chapter 1

Production of Acetaldehyde | Chapter 1 1

Production of Acetaldehyde | Chapter 1 2

1.2 PHYSICAL PROPERTIES

Production of Acetaldehyde | Chapter 1 3

Formula weight 44.052

Melting point, °C -123.5

Boiling point at 760 mm, °C 20.16

Vapor density (air = 1) 1.52

Surface tension at 20 OC, dyne/cm 21.2

Absolute viscosity at 15°C (cgs units) 0.02456

Specific heat, cal/(°C)(g) at 0 ºC 0.522

Latent heat of fusion, cal/g 17.6

Latent heat of vaporization, cal/g 139.5

Heat of combustion of liquid at constant Pressure Kcal/mol 379.2

Heat of formation at 273 K 39.55

Free energy of formation at 273 K, Kcal/mole -32.60

Critical temp, ºC 181.5

Critical pressure, (atm.) 63.2

Dissociation constant, Ka, at 0ºC 0.7(10-14)

Flash point, closed cup, °C -38

Ignition temperature in air, ºC 135

Explosive limits of mixtures with air, % acetaldehyde by volume 4-57

Production of Acetaldehyde | Chapter 1 4

Temperature °C Vapor Pressure mmHg Temperature °C Vapor Pressure mmHg

-20 123 20.16 760

15 622 100 3607

Table-1.3: Vapor Pressure of Aqueous solutions of Acetaldehyde

Temperature °C Vapor Pressure mmHg Temperature °C Vapor Pressure mmHg

10 4.9 4.9 74.5

10 10.5 10.5 139.8

20 5.4 5.4 125.2

20 12.9 12.9 259.2

Production of Acetaldehyde | Chapter 1 5

Temperature °C Acetylene Carbon Dioxide Nitrogen

1.3 CHEMICAL PROPERTIES

Acetaldehyde reactivity of condensation, Conditions, the is a highly reactive compound

Acetaldehyde decomposes at temperatures above 4000C, forming principally methane and

1.3.2 The Hydrate and Enol Form

In aqueous solutions, acetaldehyde exists in equilibrium with the acetaldehyde hydrate,

Production of Acetaldehyde | Chapter 1 6

Acetaldehyde is readily reduced to ethanol. Suitable catalysts for vapor-phase hydrogenation of

Paraldehyde is a colorless liquid, boiling at 125.35°C at l0l kPa ( l atm).

1.4 CHEMICAL REACTIONS

Metaldehyde [9002-91-9], a cyclic tetramer of acetaldehyde, is formed at temperatures below 0C

1.4.1 Reactions with Aldehydes and Ketones

The base-catalyzed self-addition of acetaldehyde leads to formation of the dimmer, acetaldol,

Production of Acetaldehyde | Chapter 1 7

A hexyl alcohol, 2-ethyl-1 butanol is produced industrially by the condensation of acetaldehyde

Condensation of acetaldehyde in the presence o dimethyl amine hydrochloride yields polyenals

Ethyl acetate is produced commercially by the Tischenko condensation of acetaldehyde using an

1.4.2 Reaction with Ammonia and Amities

1.4.3 Reactions with Alcohols, Mercaptants, and Phenols

Production of Acetaldehyde | Chapter 1 8

1.5 SHIPPING, HANDLING AND STORAGE

Production of Acetaldehyde | Chapter 1 9

2) Safety goggles should be used.

4) Drums should be stored out of doors, avoiding direct exposure to sunlight.

1.5.2 Shipping and Storage

1.6 CAPACITY AND CONSUMPTION

1.7 ECONOMIC ASPECTS AND FUTURE TRENDS

Production of Acetaldehyde | Chapter 1 10