EH2248A

DESIGN PROJECT 2
SEP 2019-JAN 2020
PRODUCTION OF 100,000 MTPA OF PHTHALIC ANHYDRIDE VIA
OXIDATION OF O-XYLENE WITH EFFICIENT WASTE TREATMENT
PROCESSES

CHAPTER 8A: CHEMICAL DESIGN OF MAJOR

EQUIPMENT
(DISTILLATION COLUMN)

GROUP MEMBERS

MUHAMMAD AFIQ BIN ABD MASAHURIN 2016522983

SUPERVISOR:
CHANG SIU HUA

FACULTY OF CHEMICAL ENGINEERING

UNIVERSITI TEKNOLOGI MARA
CAWANGAN PULAU PINANG
 DECLARATION

“Thereby declare that this report is the result of my own work except for quotation and
summaries which have been duly acknowledge”

MUHAMMAD AFIQ BIN ABD

MASAHURIN

2016522983

i
 SUPERVISOR’S CERTIFICATION

“Thereby declare that I have read this thesis and in my opinion this

project report is sufficient in terms of scope and quality for the award

of the Bachelor in Chemical Engineering (Hons).”

Signature : ………………………………………

Name : CHANG SIU HUA

Date : ………………………………………

ii
 Table of Contents

DECLARATION i
SUPERVISOR’S CERTIFICATION ii
List of Tables iv
List of Figures v
Chemical Design of Distillation Column 1
8.1 Process background 1
8.2 Assumption of Design Process 3
8.2.1 Selection of key component 5
8.2.2 Bubble and Dew Point Temperature. 5
8.2.3 Relative Volatility 8
8.2.4 Minimum Reflux Ratio 10
8.2.5 Optimum Reflux Ratio 11
8.2.6 Minimum Number of Stages By using Fenske Equation. 12
8.2.8 Efficiency of Plate in Column 15
8.2.9 Location of feed tray 16
8.3 Column Tray Selection 17
8.3.1 Type of Plate Selection 18
8.4 Relative Molecular Weight 18
8.4.1 Density of Mixture. 19
8.4.2 Maximum Allowable Vapor Density 20
8.4.3 Flooding Velocity 21
8.5 Column Diameter And Area 23
8.6 Pressure Drop 24
8.6.1 Column Size 24
CONCLUSION 25
REFERENCES 26

iii
 List of Tables

Table 8. 1Boiling point of liquid component...................................................................... 3

Table 8. 2: Mole flowrate and mole fraction in distillation column, T-101.......................... 4
Table 8. 3: Mole flowrate,fraction and split fraction in distillation column, T-101 .............. 4
Table 8. 4: Heavy and light key component in distillation column, T-101 ......................... 5
Table 8. 5: Antoinne Constant of component in distillation column,T-101 ........................ 6
Table 8. 6 : Vapor pressure of component at Feed, Top and Bottom in distillation colum 6
Table 8. 7: Bubble Point Data calculation at 240 °C ,1 atm. ............................................. 7
Table 8. 8: Dew Point Data calculation at 180°C,1 atm. ................................................... 8
Table 8. 9: Relative Volatility of component in distillation column, T-101 ......................... 9
Table 8. 10: Summary Data for Ɵ Determination. .......................................................... 11
Table 8. 11: Summary Data for Rmin Determination. ..................................................... 11
Table 8. 12: Summary for Nm determination. ................................................................ 13
Table 8. 13: Description of Plate tower and Packed Tower ............................................ 17
Table 8. 14: MW, Mole Fraction and density of component each stream ....................... 18
Table 8. 15: Relative Molecular Weight of each stream ................................................. 19
Table 8. 16: Liquid and vapor density at feed stream..................................................... 19
Table 8. 17: Liquid and vapor density at bottom stream ................................................. 20
Table 8. 18: Liquid and vapor density at top stream....................................................... 20
Table 8. 19 : Dimension of the Column .......................................................................... 24

iv
 List of Figures

Figure 8. 1: Gilliland correlation ..................................................................................... 14

Figure 8. 2 : Flooding Velocity, Sieve Plate.................................................................... 22

v
Chemical Design of Distillation Column

8.1 Process background

The main objective of this proposed project is to produce 81.377 kmol/hr of Phthalic
Anhydride (PA) which is equivalent to 100,000 tonnes per annum by using oxidation
method. The following chemical reaction shows the oxidation of o-xylene in producing
phthalic anhydride.

𝐶6 𝐻4 (𝐶𝐻3 )2 (𝑙) + 3𝑂2 (𝑔) → 𝐶6 𝐻4 (𝐶𝑂)2 𝑂(𝑙) + 3𝐻2 𝑂(𝑙) (desired reaction)
(8.1)
O-xylene Phthalic Anhydride

𝐶6 𝐻4 (𝐶𝐻3 )2 (𝑙) + 7.5𝑂2 (𝑔) → 𝐶2 𝐻2 (𝐶𝑂)2 𝑂(𝑙) + 4𝐶𝑂2 (𝑔) + 3𝐻2 𝑂(𝑙) (undesired reaction)
(8.2)
O-xylene Maleic Anhydride

There are 4 main chemical reaction occurred in the reactor based on the Figure
1.2. The reaction of O-Xylene and air will develop 4 reactions in the reactor. The first
reaction is the production of phthalic anhydride and water from the oxidation of O-Xylene.
The second reaction will produce maleic anhydride, carbon dioxide and water from
oxidation of O-Xylene. Next, the third reaction is the formation of carbon dioxide and water
by Oxidation of O-Xylene. Finally, the oxidation of O-Xylene will produce carbon monoxide
and water.

The feedstock which is O-Xylene is reacted completely in the reaction resulting the
air as unreacted compound [24]. The remaining air flow out of the reactor is in huge
amount. The recycle process is considered to be done to the utilization of the remaining
air in the reactor from the condenser but there are few problems to analyse before
constructing the recycling system. The main problem is the construction cost for the
recycles system is expensive and the air can get easily from environment. The outlet air
from the reactor is mix with others compound such as carbon dioxide, carbon monoxide,
maleic anhydride, water and small amount of phthalic anhydride classified as vent gas at
the vapor outlet of switch condenser.
 In the process there are two major equipment for separation which is stripping
column and distillation column. Before entering the stripping column and distillation
column, preparation of separation is needed. The outlet product from reactor is in form of
vapor and high temperature. The temperature and phase need to adjust before entering
the separation process. The crude product temperature will be adjusted with waste heat
boiler. It is an equipment to utilize the heat from the crude product to generate steam for
plant usage.

Distillation is used to separate components in a feed mixture based upon their

relative boiling points. A simple, continuous column can make the separation between two
components into two product streams. In multi-component systems, the two main
components to be separated are designated as the light and heavy keys. The light key is
the more volatile component in greater purity in the top product stream, and the heavy key
is the less volatile component in greater purity in the bottom product stream. In this process
the chemical design of distillation column is shown.

Furthermore, distillation is by far the most important separation process in the

petroleum and chemical industries. It is the separation of key components in a mixture by
the difference in their relative volatility, or boiling points. It is also known as fractional
distillation or fractionation. In most cases, distillation is the most economical separating
method for liquid mixtures. However, it can be energy intensive. Distillation can consume
more than 50% of a plant’s operating energy cost. There are alternatives to distillation
process such as solvent extraction, membrane separation or adsorption process. On the
other hand, these processes often have higher investment costs. Therefore, distillation
remains the main choice in the industry, especially in large-scale applications. Distillation
column T-101 was designed to separate main product, PA from MA, water, carbon dioxide
and oxygen. The separation is mainly based on the volatility of the component based on
its boiling temperature.

2
8.2 Assumption of Design Process

Table 8. 1Boiling point of liquid component.[1]

Component Normal Boiling Point (oC)

Phthalic Anhydride 284
Maleic Anhydride 202
Carbon Dioxide -56.6
Water 100
Oxygen -182.96
Nitrogen -195.80

The following steps should be considered in order to develop reliable design of distillation
column [2];
1. Degree of separation such as products specification being specified.
2. Selecting suitable operating condition: temperature and pressure.
3. Determining number of stage and reflux requirement: number of equilibrium stage.
4. Selecting appropriate contacting device either plate or packing. Determining size
of the column: diameter, number of real stages.
5. Designing the internal of the column: plates, distributors, packing support.
6. Conduct mechanical design: vessels, internal fitting.

Since the distillation process for this PA plant involved multicomponent distillation,
the process in determining the number of stages and reflux requirement much more
complex than separation process for binary mixture. The complexity of multicomponent
distillation calculation can be reduced by neglecting the component that exist in a small
amount at feed stream.

3
Table 8. 2: Mole flowrate and mole fraction in distillation column, T-101

Component Mole flowrate in (kmol/hr) Mole Fraction

Oxygen 0.021 0.0009788
PA 74.252 0.85
MA 3.767 0.044
Carbon dioxide 0.02 0.01323
Water 8.346 0.097
Nitrogen 0.031 0.003021
TOTAL 378 1

Based on Table above, there are very small amount of oxygen, carbon dioxide and
nitrogen entering T-101, therefore these components can be considered as trace and will
be neglected during calculations. Considering only Phthalic anhydride, Maleic anhydride
and water entering T-101, the new mole flow used in the calculation and targeted split
fraction for each component at the top and bottom of the column being specified as in
Table below.

Table 8. 3: Mole flowrate,fraction and split fraction in distillation column, T-101

Component Mole flowrate Mole Split Split

in (kmol/hr) Fraction Fraction(Top) Fraction(Bottom)
PA 74.252 0.85 0 1
MA 3.767 0.044 0.931019 0.068981
Water 8.346 0.097 1 0
TOTAL 86.365 1

After excluding oxygen, carbon dioxide and nitrogen from entering the distillation
column (T-101), the percentage error between the final and initial total flowrate of mixture
calculated is 0.51% which is less than 1.0%. The percentage error obtained is relatively
small therefore the assumption by neglecting the components with small amount can be
accepted. This small amount of component is may known as a trace component inside the
system.

4
8.2.1 Selection of key component

Key component desired for separation process will be categorized into heavy key
and light key component. Heavy key component is a component that has high boiling point
and it will be out from top product and being enriched at bottom product. While light
component is the component with low boiling point that is desired to keep out from bottom
product and being enriched at top product [3].

Table 8. 4: Heavy and light key component in distillation column, T-101

Heavy Component (Boiling Point) Light Component (Boiling point)

Phthalic anhydride (284˚C) Water (100˚C)
Maleic anhydride (202 ˚C)

8.2.2 Bubble and Dew Point Temperature.

Operating pressure for each stream will be used to determine the bubble and dew
point. Bubble point is the point whereby any rise in the temperature of saturated liquid that
will cause the formation of vapor and it can be determined from the pressure of feed and
bottom stream[4]. Meanwhile dew point is a point whereby any drop in the temperature of
saturated vapor that will cause the formation of liquid droplet and this point can be
determined from the top stream operating pressure [5]. For multicomponent mixtures at
given pressure with the relation of equilibrium constant (K), bubble and dew point can be
calculated as follow,

Bubble point : ∑ 𝑌𝑖 = ∑ 𝑋𝑖. 𝐾𝑖 (8.3)

𝑌𝑖
Dew point : ∑ 𝑋𝑖 = ∑ (8.4)
𝐾𝑖

Where:
Ki = equilibrium constant for component i
xi = liquid mol fraction for component i
yi = vapour mol fraction for component i
Equilibrium constant, K:

5
 𝑃𝑠𝑎𝑡
K= (8.5)
𝑃

Whereby Psat is vapor pressure and P is the operating pressure both in Pa. Psat will be
calculated by using Antoine Equation as follows :

𝐵
log(𝑃𝑠𝑎𝑡 ) = 𝐴 − (𝑇+𝐶 ) (8.6)

Table 8. 5: Antoinne Constant of component in distillation column,T-101 [1]

Component A B C
H2O 8.14019 1810.94 244.485
MAog 16.2747 3765.65 82.15
PA 15.9984 4467.01 59.46

Where; Antoine constant=A, B and C. is used to find out vapor pressure in every stream.

Table 8. 6 : Vapor pressure of component at Feed, Top and Bottom in distillation column,
T-101

feed Top Bottom

sat sat sat sat
Component log P P (mmhg) log P P (mmhg) log Psat Psat (mmhg)
H2O -2.004 0.0099 3.8508 7092.51 4.3849 24260.51
MA -3.9397 0.00011 1.8011 63.25 4.505 31988.95
PA -10.3852 0.00000 -2.8315 0.0015 0.9706 9.35

From Table above the value of k can be determine,

Sample Calculation
𝐵
log(𝑃𝑠𝑎𝑡 ) = 𝐴 − ( )
𝑇+𝐶

1810.94
(𝐹𝑜𝑟 𝑤𝑎𝑡𝑒𝑟 𝑎𝑡 𝑏𝑜𝑡𝑡𝑜𝑚) log (𝑃𝑠𝑎𝑡 ) = 8.14019 − ( ) = 4.3849
423 − 244.485

𝑃𝑠𝑎𝑡 = 24260.51mmHg

6
Find K,
𝑃𝑠𝑎𝑡
𝐾=
𝑃𝑂𝑝𝑒𝑟𝑎𝑡𝑖𝑜𝑛

24260.51 𝑚𝑚𝐻𝑔
𝐾= = 31.92
760𝑚𝑚𝐻𝑔
Bubble Point Calculation:
The temperature required for the formation of bubble point is at 240°C and the bottom
stream of distillation column operate at pressure of 1atm (760mmHg). Data required for
the bubble point calculation at bottom stream is tabulated in the Table.

Table 8. 7: Bubble Point Data calculation at 240 °C ,1 atm.

Bottom
Component X Ki Yi=XiKi
H2O 0.0000001222 31.92 0.0000039
MA 0.0235 42.09 0.989
PA 0.9705 0.012 0.011
1.0000 1.0000

Dew Point calculation:

The temperature required for the formation of dew point is at 180°C and the top
stream of distillation column operate at pressure 1 atm (760mmHg). Data required for the
dew point calculation at top stream is tabulated in the Table 8.8 Vapor pressure of ethanol,
and carbon dioxide are calculated by using Equation 8.5.

7
Table 8. 8: Dew Point Data calculation at 180°C,1 atm.

Top
Component Y Ki X=Y/ki
H2O 0.9275 9.3323 0.0992
MA 0.0733 0.0832 0.8811
PA 0.000000038183 0.000001974 0.0197
1.0000 1.0033

8.2.3 Relative Volatility

Relative volatility is widely being used in designing large industrial distillation

process that involve the contacting of vapor and liquid phases in a series of equilibrium
stages. It is a measure of the differences between vapor pressure of liquid mixture
component which is more volatile and the vapor pressure of less volatile components of
the mixture. It denotes the ease or difficulty in using distillation to separate high volatile
components from less volatile components in a mixture. It is easier to separate the mixture
components in distillation column when the relative volatility of a liquid mixture is higher
[6]. Furthermore, this measure is not applied to separation process that involve component
that chemically react to each other. For distilling a multicomponent mixture feed into the
separation column, it should be design to produce an overhead fraction containing
predominantly more volatile components and a bottom fraction which containing
predominantly less volatile components. Therefore, the column is design involving key
components that governing the separation design for both Light Key (LK) component and
High Key (HK) component. The lighter components referred to components with lower
boiling point and higher vapor pressure while the heavier components is the component
with higher boiling point and lower vapor pressure[7]. By convention, the relative volatility
represent as α and the distillation of ay multicomponent mixture can be expressed as the
ratio of their K value as shown in the Equation shown below,

𝛼= (𝑦𝐿𝐾 / 𝑥𝐿𝐾 )(𝑦𝐻𝐾 / 𝑥𝐻𝐾 )= 𝐾𝐿𝐾/𝐾𝐻𝐾 (8.7)

Where:

8
yLK, yHK is the vapor-liquid concentration of LK and HK component in vapor phase.
xLK, xHK is the vapor-liquid concentration of LK and HK component in liquid phase.
KLK is the equilibrium constant of light key (LK) component.
KHK is the equilibrium constant for heavy key (HK) component.

Average volatility can be calculated as follows:

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑣𝑜𝑙𝑎𝑡𝑖𝑙𝑖𝑡𝑦=𝛼𝑎𝑣𝑔= (𝛼𝑡𝑜p 𝑥 𝛼𝑏𝑜𝑡𝑡𝑜𝑚)1/2 (8.8)

Where:
αtop is the relative volatility at the distillate.
αbottom is the relative volatility at the bottom.
Take an assumption MA as the heavy key. As H2O and PA known as Light than light key
and heavy than heavy key.
Sample Calculation,(water)
K lk 9.3323
(Top) α= = = 112.17
K hk 0.0832
K lk 31.92
(Bottom) α= =
K hk 42.09
= 0.75837
1
(average) α = (αTop × αBottom )(2)
1
(average) α = (112.17 × 0.75837)(2) = 9.2231

Table 8. 9: Relative Volatility of component in distillation column, T-101

Relative Volatility(α)
Component Top Bottom Average
H2O 112.17 0.75837 9.2231
MA 1 1 1
PA 2.3725E-05 0.0002851 8.224E-05

9
8.2.4 Minimum Reflux Ratio

Minimum Reflux Ratio (Rmin) is the lowest value of reflux at which separation can
be achieved even with an infinite number of plates. Furthermore, it is possible to achieve
a separation at any reflux ratio above the minimum reflux ratio because the number of
plates required to be decreases when reflux ratio increase [8]. Otherwise, the distance
between the operating line and equilibrium curve will becomes smaller as the reflux ratio
is being reduced. In other words, Rmin also defined as the minimum amount of liquid flow
that returned back to the column. The value of Rmin for separation column can be
identified through Equation of reflux ratio which have been derived by Underwood and
Colburn[5]. These Equation can be used to estimate the value of minimum reflux ratio for
multicomponent distillations process. Besides that, the value of θ which usually lies
between the relative volatility of light component and heavy component can be sloved by
using the Underwood Equation. The Equation is stated in the following form:

αiXi,d
∑ = R m+ 1 (8.9)
αi −θ

Where:
αi is the relative volatility of component i with respect to some reference component
(usually heavy key)
Rm is the minimum reflux ratio Xi,d is the concentration of component i in the top at
minimum reflux.
Then, θ is the root of equation as follows:

𝑋𝑖,𝑓
∑ =1−𝑞 (8.10)
(𝛼𝑖 −𝜃)/𝛼

Where:
Xi,f is the concentration of component i in the feed q is depends on the condition of the
feed.
The value of 𝜃 is obtain from trial and error method :
By using solver in Microsoft excel 𝜃 value obtain is 0.086996.

10
Table 8. 10: Summary Data for Ɵ Determination.

Component α α-Ɵ/α Xf Xf/[(α-Ɵ)/α]

H2O 9.2231 0.99057 0.097 0.09792
MA 1 0.913004 0.044 0.04819
PA 8.224E-05 -1056.83 0.85 -0.000804
0.14530

The value of Xf/[(α-Ɵ)/α] is satisfied as the fraction is approach to 0.14530 which

is the value of actual vapor fraction in feed. Therefore, 𝜃=0.086996 is used in the following
table:

Table 8. 11: Summary Data for Rmin Determination.

Component α α-Ɵ/α xd Xd/[(α-Ɵ)/α]

H2O 9.2231 0.99057 0.0992 0.1001446
MA 1 0.913004 0.8811 0.9650556
PA 8.224E-05 -1056.83 0.0197 -1.86406E-05
1.06518155

The average value Xd/[(α-Ɵ)/α] gives the Rmin+1 that is minimum reflux
ratio=1.06518155.
Where, Rmin=0.0651816.

8.2.5 Optimum Reflux Ratio

It is important in selecting practical reflux ratio where it specified separation is

achieved at minimum cost. Optimum reflux ratio will lead to lowest operating cost since it
reduce number of stages required, hence reduce the capital cost. There is no rule in
selection of design reflux ratio[3]. However, many systems the optimum lies between 1.2
and 1.5 times the minimum reflux ratio. For this systems, can be solve by using this
equation.

11
Optimum reflux ratio, R = 1.5Rm (0.0651816)
= 1.5 (0.0651816)
= 0.0978.

8.2.6 Minimum Number of Stages By using Fenske Equation.

In order to estimate the minimum stages required at total reflux, Fenske equation
can be applied to multicomponent systems and can be written as stated in equation stated
[4].

𝑥𝑙𝑘 𝑥ℎ𝑘
log[ ] [ ]
𝑥ℎ𝑘 𝐷 𝑥𝑙𝑘 𝐵
𝑁𝑚 = log∝𝑙𝑘
(8.11)

Where;
d = ratio of the concentration of any component i to the concentration of a reference
component r, and the suffixes d and b where denote the distillate (d) and the bottoms (b)
Nm = Minimum number of stages at total reflux, including the reboiler
𝛼i = average relative volatility of the component i with respect to the reference component

Since the separation is specified in key of components where components are

denote according to heavy or light component, therefore, use of equation (8.11) are much
more easier to solve.

Where;
Nm = Minimum number of theoretical stages in column at total reflux
xLK,d = Mole fraction of light key at distillate
xHK,d = Mole fraction of heavy key at distillate
xLK,b = Mole fraction of light key at bottom
xHK,b = Mole fraction of heavy key at bottom
𝛼LK = Average relative volatility of the light key with the respect to the heavy key

12
 All data can be summary as follows;

Table 8. 12: Summary for Nm determination.

Description Value
Mole fraction of light key at distillate, xLK,d 0.0993
Mole fraction of heavy key at distillate, xHK,d 0.9008
Mole fraction of light key at bottom, xLK,b 0.0000039
Mole fraction of heavy key at bottom, xHK,b 0.989
Average relative volatility of the light key with the respect to the heavy key, 9.2231
𝛼LK

0.0993 1
log[ ][ ]
0.9008 0.0000039
𝑁𝑚 = log 9.2231
= 4.61

The minimum number of trays for this equipment is 4.61.

13
 Figure 8. 1: Gilliland correlation

From calculation have been done, Nm value obtained is 4.61. Thus, number of
theoretical stages can be determined by using Gilliland correlation as shown in Figure 8.1
[1]. From this figure a few calculations required as follows;

𝑅 − 𝑅𝑚𝑖𝑛 0.0978 − 0.0651816

=
𝑅+1 0.0978 + 1

= 0.03

From the x-value, the y-value can be determined. The value of y = 0.7

𝑁 − 4.61
= 0.7
𝑁+1

N =17.7 ≈ 18

14
8.2.8 Efficiency of Plate in Column

The overall column efficiency is correlated with the product of the relative volatility
of the light key component (relative to the heavy key) and the molar average viscosity of
the feed, estimated at the average column temperature. The correlation found to give
reliable estimates of the overall column efficiency for hydrocarbon systems and can be
used to make an approximate estimate of the efficiency for other systems. Based on
Harvenson et al, the range of efficiency of plate is 30% to 80%. So, the nominal value is
assumed as Eo=80% [7]

The no. of actual tray (Nact)

𝑁
𝑁𝑎𝑐𝑡 = 𝐸 (8.12)
𝑜

18
𝑁𝑎𝑐𝑡 = = 22.5 ≈ 23
0.8

The Column Height (Hc) :

Hc = (Nact − 1)(hTS ) + hDS (8.13)

hTS = height of tray spacing

hDS = height of disengagement space(top& bottom)

Hc = (23 − 1)(0.45) + 3 = 12.9 ≈ 13 m

HTS= 0.45m, as referred to guidelines selection of tray spacing. This value was
suitable for column operating in spray regime and required to avoid excessive entrainment
[7]. The height of disengagement space(top& bottom) hDS= 3m [7].

15
8.2.9 Location of feed tray

Feed point location can be estimate by using the Fenske equation in order to
calculate the number of stages in the rectifying and stripping sections separately, but this
requires an estimate of the feed-point temperature. Another alternative method is
application of empirical equation as stated in equation below [1],

 B x  xb,lk 
2

N   f ,hk
log r = 0.206 log     (8.14)
Ns  D  x f ,lk  x  
  d ,hk  

Where;
Nr = Number of stages above the feed, including any partial condenser
Ns = Number of stages below the feed, including the reboiler
B = Molar flow bottom product
D = Molar flow top products
xf,HK = Concentration of the heavy key in the feed
xf,LK = Concentration of the light key in the feed
xd,HK = Concentration of the heavy key in the top product
xb,LK = Concentration of the light key if in the bottom product

𝑁𝑟 60.507 0.0303 0.0235 2

log = 0.206 log[( )( )( ) ]
𝑁𝑠 25.931 0.0273 0.0368
𝑁𝑟
= 1.011
𝑁𝑠
𝑁𝑟 = 1.011𝑁𝑠
𝑁𝑟 + 𝑁𝑠 = 23
1.011𝑁𝑠 + 𝑁𝑠 = 23
𝑁𝑠 = 11.43 𝑠𝑡𝑎𝑔𝑒 ≈ 12 𝑠𝑡𝑎𝑔𝑒𝑠
𝑁𝑟 = 1.011(12) = 12.13 𝑠𝑡𝑎𝑔𝑒 ≈ 12 𝑠𝑡𝑎𝑔𝑒

16
8.3 Column Tray Selection

In the production of ethanol, the most suitable type of column for separation
process that being chosen is the plate tower distillation column rather than packed tower
column. Tray column is the most selected type of distillation column that usually being
used in petrochemical industry as it utilizes temperature and pressure differential to
separate the desired products. For most tray column, the weir holds the liquid flow in each
tray inside the column. Therefore, the vapor should able to overcome this liquid to move
up the column. Then, liquid and vapor will be contacted above the tray and they will be
separated. Besides that, tray column also performs well in high liquid and vapor loading.
There are several conditions which more favor to plate column instead of packed column
as described below:

Table 8. 13: Description of Plate tower and Packed Tower [9]

Plate Tower Distillation Column Packed Tower Distillation Column

1. Design of tray column more reliable 1. Liquid dispersion difficulties
2. Can be designed to handle wide ranges 2. Packing must be removed before
of liquid rates without flooding. cleaning.
3. Plates are more accessible for cleaning 3. Weight of packed column is more than
(easy if handling liquids that contain plate column (for large column heights).
dispersed solids). 4. Packing may damage when there are
4. Design information for plate column temperature changed.
more readily available and reliable. 5. Not suitable for very low liquid flow rates.
5. Inter stage cooling can be provided to 6. The liquid hold-up is lower in a packed
remove heat of reaction or solution in plate. column (important when the hold-up of
6. Better at handling solids or other toxic or flammable liquids must be kept as
sources of fouling. small as possible for safety reasons).
7. Offer better predictability than packed
towers.

17
8.3.1 Type of Plate Selection

There are many types of flow depends on the plate that are being used in the
distillation column to separate the liquid vapor to obtain the final products. Cross flow plate
is the most commonly used plate contactor in separation process. These plate flow allow
the liquid to move downwards while the vapor flow upwards. The liquid moves from one
plate to another via down comer and certain level of liquid usually maintained by the weirs
on the plate inside the distillation column. The most suitable cross flow trays to be used in
obtaining phthalic anhydride as the final products is Sieve Plate which also known as
Perforated Plate. These types of plates are preferred to be used due to the following
reason [9]:

1. Their fundamentals are well established, entailing low risk.

2. The trays are low in cost relative to many other types of trays.
3. Easily handle wide variations in flow rates.
4. Lighter in weight, easier and cheaper to install.
5. Pressure drop is low as compared to bubble cap trays.
6. Peak efficiency is generally high.
7. Maintenance cost is reduced due to the ease of cleaning.
.
8.4 Relative Molecular Weight

Relative Molecular Weight (RMW) is the average molecular weight of the mixture
for each stream and this parameter can be identified through Equation 8.21. This section
is calculated using Excel sheets.

Table 8. 14: MW, Mole Fraction and density of component each stream

Component MW(Kg/Kmol) Xf Xb Xd
H2O 18.0150 0.097 0.0000 0.0992
MA 98.0580 0.044 0.0235 0.8811
PA 148.1180 0.85 0.9705 0.0197

18
𝑅𝑀𝑊=Σ𝑋𝑖𝑀𝑊
Table 8. 15: Relative Molecular Weight of each stream

Component RMW feed RMW bottom RMW top

H2O 1.7475 0.0000 1.7871
MA 4.3146 2.3044 86.398
PA 125.90 143.75 2.9179
Total 130.96 146.05 91.103

8.4.1 Density of Mixture.

𝐿𝑖𝑞𝑢𝑖𝑑 𝐷𝑒𝑛𝑠𝑖𝑡𝑦= Σ𝜌𝑖=Σ𝑋𝑖𝜌𝑖 (8.30)

𝑉𝑎𝑝𝑜𝑟 𝐷𝑒𝑛𝑠𝑖𝑡𝑦=Σ𝜌𝑣=Σ𝑀𝑊𝑉𝑠𝑡𝑑/2(8.31)
Where:
ρl is the density of liquid (kg/m3)
ρv is the density of vapor (kg/m3)
Tstd is the temperature standard (273K)
Toprt is the operating temperature
Pstd is the pressure standard (1 bar)
Poprt is the operating pressure
Vstd= 22.414 liters

Table 8. 16: Liquid and vapor density at feed stream

Feed stream (To=423 K ,Po=1.013 bar)

Component Density(kg/m3) ρl(kg/m3) ρv(kg/m3)
H2O 1000.0000 97.00 0.8738
MA 1480.0000 65.12 2.1573
PA 1530.0000 1300.5 6.625
1462.62 9.6561

19
Table 8. 17: Liquid and vapor density at bottom stream

bottom stream (To=513 K ,Po=1.013 bar)

Component Density(kg/m3) ρl(kg/m3) ρv(kg/m3)
H2O 1000.0000 0.0000 0.00
MA 1480.0000 34.7800 1.1522
PA 1530.0000 1494.0450 7.188
1528.8251 8.3402

Table 8. 18: Liquid and vapor density at top stream

Top stream (To=453 K ,Po=1.013 bar)

Component Density(kg/m3) ρl(kg/m3) ρv(kg/m3)
H2O 1000.0000 1.7871 0.8934
MA 1480.0000 44.8223 4.320
PA 1530.0000 2.9179 1.459
94.8823 6.6724

8.4.2 Maximum Allowable Vapor Density

𝜌𝑙−𝜌𝑣 1/2
𝑈𝑣 = (−0.171(𝐿𝑡)2 + 0.27𝐿𝑡 − 0.047)[ ] (8.15)
𝜌𝑣

Uv is the maximum allowable vapor velocity based on the total column cross sectional
area (m/s).
Lt is the plate spacing (m)

1528.8251 − 9.6561 1
𝑈𝑣 = (−0.171(0.45)2 + 0.27(0.45) − 0.047)[ ]2 = 0.5001𝑚/𝑠
9.6561

20
8.4.3 Flooding Velocity

The upper limit of vapor velocity can be determined through flooding condition.
High vapor velocity is needed for column with high efficiency which normally lies between
70% to 90% because flooding might occur. Value of Uf are assumed to be between 80%
to 85% of flooding in designing a distillation column. The value of Uf also can be estimated
from the correlation by Fair as being stated in the equation below:

𝜌𝑙−𝜌𝑣
𝑈𝑓 = 𝐾1√ (8.16)
𝜌𝑣

Where:
Uf is the flooding vapor velocity (m/s) based on net column cross sectional area.
AnK1 is a constant which obtain from the Flooding Velocity, Sieve Plates figure.

In determining the value of K1, liquid vapor flow factor (FLV) must be calculated by using
equation below:
𝐿𝑤 𝜌𝑣
𝐹𝑙𝑣 = 𝑉𝑤 √ 𝜌𝑙 (8.17)

Where:
LW is the liquid mass flow rate, kg/s
VW is the vapor mass flowrate, kg/s
Liquid Vapor Flow Factor, FLV

2.0963 9.6561
𝐹𝑙𝑣 = √ = 0.048
3.4488 1528.8251

Based on Figure 8.2 (Flooding Velocity, Sieve Plates figure), the value of K1 at FLV =0.5001
and plate spacing of 0.45m can be obtained [7].

21
 Figure 8. 2 : Flooding Velocity, Sieve Plate

K1=0.08
The value of Uf then can be calculated based on the K1=0.08 obtained from the Flooding
Velocity, Sieve Plates:

1528.8231 − 9.6561
𝑈𝑓 = 0.08√ = 0.9898𝑚/𝑠
9.6561

Then,

𝑚 𝑚
𝑈𝑛 = 0.85 × 𝐹𝑙𝑜𝑜𝑑𝑖𝑛𝑔 𝑉𝑒𝑙𝑜𝑐𝑖𝑡𝑦 = 0.85 × 0.2679 = 0.841
𝑠 𝑠

22
8.5 Column Diameter And Area

In obtaining the diameter of distillation column, the vapor flowrate plays as an

important parameter. The vapor velocity should be lower from a condition which may cause
an excessive liquid entrainment (high pressure drop). From the previous maximum vapor
velocity obtained, the diameter of the column can be calculated using equation below:

4(Vw)
𝐷𝑐 = √ (8.18)
(π)(ρv)(Uv)

Where:
VW is the maximum vapor rate in kg/s
Therefore,

6650.280𝑘𝑚𝑜𝑙 73080𝑘𝑔 1 ℎ𝑟 𝑘𝑔
𝑉𝑤 = = × = 20.3
94.8823𝑘𝑔 ℎ𝑟 3600 𝑠 𝑠
ℎ𝑟 ( )
𝑘𝑚𝑜𝑙

Solve for Dc,

4(20.3)
𝐷𝑐 = √ = 2.31 𝑚
(𝜋)(9.6561)(0.5001)

As the diameter of column obtained is 1.3011 m, the area of the column can be determined
using Equation 8.18:

𝜋𝐷𝑐 2 𝜋(2.31)2
𝐴𝑐 = = = 4.19 𝑚2
4 4

23
8.6 Pressure Drop

∆p ≈ 0.1psi/tray ( 0.5-0.7 kpa/tray) – atmospheric and superatmospheric pressure

operation

∆p ≈ 0.05 psi/tray (0.25-0.35 kpa/tray) – vacuum column operation

Assuming 100 mm water pressure drop per plate.

Column pressure drop = ΔP per plate × 𝜌water × g × number of stages

= 0.5 × 1000 × 9.81 × 23

= 206.01 kpa

Top pressure = 101.3 kPa (1 atm)

Estimated bottom pressure = 206.01 + 101.3 = 307.31 kPa

8.6.1 Column Size

Table 8. 19 : Dimension of the Column

Column diameter, dc 2.31 m

Column Area, Ac 4.19 m2

Number of trays 23

Column height 13 m

Length/diameter ratio 5.63

24
 CONCLUSION

In conclusion, all the dimension for the distillation column have been calculated.
The height of the column is about 13 m and the diameter is 2.31 m. Besides that, the
number of tray been calculated is about 23 trays. Therefore, the feasibility of the design
can be accepted because apply the standard of the size column for the chemical design.

25
 REFERENCES

[1] C. Reid, T. K. Sherwood, and J. M. Prausnitz, “Physical property data bank

(Appendix C),” The Properties of Gases and Liquids 3rd ed.

[2] R. K. Sinnott, “Chemical Engineering Design,” Coulson and Richardson’s Chemical

Engineering, no. 6, p. 1279, 2005.

[3] U. M. Diwekar and K. P. Madhavan, “Multicomponent Batch Distillation Column

Design,” Industrial and Engineering Chemistry Research, vol. 30, no. 4, pp. 713–
721, 1991.

[4] W. Smith, “Multicomponent distillation,” International Journal of Heat and Mass

Transfer, vol. 7, no. 2, p. 279, 1964.

[5] R. S. Hassan, G. A. Gasmelseed, B. A. Karama, and A. E. Musa, “A short-Cut

Method for Designing Multi-Component Fractionation Column,” Journal of Applied
and Industrial Sciences, vol. 1, no. 3, pp. 44–48, 2013.

[6] I. T. De Aguascalientes and D. D. I. Química, “a Short Method for the Design of

Reactive Distillation Column,” pp. 978–981, 2010.

[7] I. J. Halvorsen and S. Skogestad, “Distillation theory,” Encyclopedia of separation

science,Volume 2, Chapter 2, no. August, p. 4954, 2000.

[8] R. Vooradi and S. Anne, “Design of Control Structure for Binary Distillation Column,”
Iieng.Org, pp. 133–137, 2015.

[9] A. Górak and Z. Olujic, Distillation : equipment and processes. .

26