Energy Balance

Around
Distillation Column

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 67

 Distillation Column
Components D (Kmoles/hr)

Components F (Kmoles/hr) P.A 1.48649

M.A 0.1267
P.A 29.7297
O.X 0.1925
M.A 1.3340
O.X 0.385

Components W (Kmoles/hr)

P.A 28.2432
M.A 1.2073
O.X 0.1925

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 2

 General Equation of the Energy Balance
Calculation of energy balance

the amount of the energy supplied

the amount of the steams

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 69

 Steps Involved in Calculating Energy Balance
1. Heat Flow of Feed
Temperature = 513K
Pressure = 0.7 bar
Total Feed Flow rate = 31.448725 kmoles/hr

Cp = A + BT + CT2/2+ DT3/3 at T(avg)=405.5 k

CPavg = ∑ xi* CPi = 244.098 kJ/kmole.K
∆HF= m*Cp*∆T
∆HF = 1650460 kJ/day
∆HF = 458.46098 kW

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 70

 2) Heat Flow at Top of Distillation Column
A) Enthalpy Change for Reflux
Temperature = 410K
Pressure = 0.255 bar
Total Amount of Distillate Flow rate = 2.8863 kmoles/hr
Cp = A + BT + CT2/2+ DT3/3
at respective Boiling Point Temperature
CPavg = ∑ xi* CPi = 197.9084 kJ/kmole.K
Enthalpy change up to boiling point temperature
∆H= mv * CPavg *∆T
∆H= 191931 kJ/hr

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 71

 2) Heat Flow at Top of Distillation Column
B) Enthalpy Change for Vapors
Molar flow rate of vapors mv= R*D+D= D(R+1)
mv =2.8863(2+1)
mv = 8.6589kmoles/hr
Latent Heat =mv *λ (avg)
λ (avg) = 49027.11 kJ/Kmole
∆Hv =424520.8kJ/hr

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 72

 Heat Flow at Top of Distillation Column

Heat Flow= ∆HL+∆HV

Heat Flow at Top of D.C = 616451.8 kJ/hr
∆H=171.2366kW
Condenser Duty=Q c= ∆Hv-(∆HR+∆HD)
Heat Flow of Reflux=∆HR= mL*Cp*∆T
∆HR= 165074.4kJ/hr
∆HD= mD*Cp*∆T = 82537.27 kJ/hr

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 73

 Condenser Duty

Condenser Duty=Q c= ∆Hv-(∆HR+∆HD)

Q c= 368840 kJ/hr
Q c= 102.4556 kW
Cooling Media Conditions:
Tin= 298K TOut =343K P= 1bar
Mass flow rate of water = 1960.8719 kg/hr

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 74

 3) Heat Flow at Bottom of Distillation Column
Temperature = 500K
Pressure = 0.6 bar
Total Feed Flow rate = 29.64299 kmoles/hr

Cp = A + BT + CT2/2+ DT3/3 at T(avg)= 399K

CPavg = ∑ xi* CPi = 242.763KJ/kmole.K
∆HB= m*Cp*∆T
∆HB = 1453634.03kJ/day
∆HB = 403.7872kW

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 75

 Reboiler Duty

QB =(QC + ∆HW +∆H D)-∆HF

QB = 254551.3031 KJ/hr
QB = 70.7087 kW

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 76

 Steam Flow Rate Calculation

Steam Conditions
P= 1 bar
T= 373 K
λ = 2256.9 kJ/kg
QB= mSteam* λSteam
QB = 254551.3031 kJ/hr
mSteam = 112.8 kg/hr

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 77

 Steam Flow Rate Calculation
Steam Conditions
P= 1 bar
T= 373 K
λ = 2256.9 kJ/Kg
QB= mSteam* λSteam
mSteam = 112.8 kg/hr

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 78

 Distillation Column Design Steps
1. Specify the degree of separation required; set product specifications
2. Select operating conditions
3. Select the type of contact device
4. Determine stage and reflux required
5. Determine column size
6. Design the column internals

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 79

 Cont…

• Determine minimum number of plates Fenske eq.

• Determine the Minimum Reflux Ratio, Underwood Equation
• Choose Theoretical Reflux Ratio
• Determine total Number of Trays
• Determine Feed-Stage Location using Kirkbride Empirical Equation
• Principal Dimensions of the Column (Diameter/Height)

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 80

 The Selection of Column Internals
The selection of column internals has a big impact on the column
performance and the maintenance cost of a distillation tower.
There are several choices of column internals and the two major categories
are trays and packing. The choice of which to utilize depends on the
1. Pressure
2. Fouling potential,
3. Liquid to vapor density ratio,
4. Liquid loading, and
5. Most importantly the life cycle cost.

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 81

 Packing Selection
Packing divisions include grid packing, random packing, conventional structured
packing, and high capacity structured packing.
The rules of thumb for selecting packing are
1. The compounds are temperature sensitive
2. Pressure drop is important (vacuum service)
3. Liquid loads are low
4. Towers are small in diameter
5. Highly corrosive service (use plastic or carbon)
6. The system is foaming
7. The ratio of tower diameter to random packing is greater than 10

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 82

 Tray Column Selection
Trays can be divided into many categories, such as trays, high capacity trays,
multiple down comer trays and system limit trays. According to some rules of
thumb, trays should be selected if:
1. The compounds contain solids or foulants
2. There are many internal transitions
3. Liquid loads are high
4. There is a lack of experience in the service
5. Vessel wall needs periodic inspection
6. There are multiple liquid phases

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 83

 Tray Selection
Parameter Sieve Tray Valve Tray Bubble Cap Tray
Cost Low 1.5 times Sieve tray 3 times Sieve tray
Operating Range 50-120% of Design Greater flexibility Operate Efficiently at very
Capacity Than sieve 25-30% low rate 10%

Efficiency High High Moderate High

Pressure Drop Lowest Greater than Sieve Plate Highest
Maintenance Low Moderate Relatively high
Fouling Tendency Low moderate High Tends to collect
solids
Table 8

Summary:
Sieve Plate are cheapest and satisfactory , Valve are preferred when specified turn down ratio can't be meet by
sieve , Bubble cap are used where low vapor rate have to be handled.

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 84

 Design Calculations
𝐷. 𝑥𝐻.𝐾,𝐷 × 𝑊. 𝑥𝐿.𝐾,𝑤
𝑙𝑜𝑔
𝐷. 𝑥𝐿.𝐾,𝐷 × 𝑊. 𝑥𝐻.𝐾,𝑤 ൙
𝑁𝑚𝑖𝑛 = 𝑙𝑜𝑔 ∝𝑚
∝
∝𝑚 = 𝑖ൗ∝𝑗
Nmin = 3.1184 Stages
where,
𝑁𝑚𝑖𝑛 = minimum number of stages
𝐷. 𝑥𝐻.𝐾,𝐷 = mole fraction of distillate w.r.t heavy key component
𝐷. 𝑥𝐿.𝐾,𝐷 = mole fraction of distillate w.r.t light key component
𝑊. 𝑥𝐿.𝐾,𝑤 = mole fraction of bottom w.r.t light key component
𝑊. 𝑥𝐻.𝐾,𝑤 = mole fraction of bottom w.r.t heavy key component
∝𝑚 = relative volatility , ∝𝑖 = volatility of light component, ∝𝑗 = volatility of heavy
component

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 85

 Cont…
• R min Calculations
∝𝑖,𝑗 × 𝑍𝑖
1−𝑞 =෍
∝𝑖,𝑗 −∅
𝑖

∝𝑖,𝑗 × 𝐷. 𝑥𝑖,𝐷
𝑅𝑚𝑖𝑛 + 1 = ෍
∝𝑖,𝑗 −∅

𝑞=1
𝑞 = feed condition
∝𝑖,𝑗 = volatility of each component w.r.t heavy component
𝑍𝑖 = fraction of each component
∅ = common root = 3.56

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 86

 Cont…

Vmin = R D,min + 1 D

𝑅𝐷,𝑚𝑖𝑛 = 1.6170
Where,
𝑅𝐷,𝑚𝑖𝑛 = Minimum Reflux ratio
𝐷 = distillate
actual reflex Rule of thumb
𝑅 = 1.2(𝑅𝑚𝑖𝑛 )
𝑅= 2

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 87

 Literature Review
• Actual Stages
𝑁 − 𝑁𝑚𝑖𝑛
𝑌=
𝑁+1

𝑅−𝑅𝑚𝑖𝑛
𝑋= = 0.1099
𝑅+1

• Fig 22.5 (McCabe, Smith, & Harriot)

N =7.95
𝑁 = 𝐼𝑑𝑒𝑎𝑙 𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑝𝑙𝑎𝑡

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 88

 Approximate Dia of D.C
Dia of D.C =((4∗𝑉𝑤)/(𝑃𝑖*𝜌𝑣*𝑈𝑣))^(1/2)= 0.6m
Ideal No. of Trays= 8
Height of D.C= (N-1)*Tray Spscing+ 0.15* (N-1)*Tray Spscing
Height of D.C= 2.415m
Height to Dia Ratio:
H/D= 4.023297362

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 89

 Literature Review
• Feed Plate
2 0.206
𝑁𝑅 𝑧𝐻𝐾,𝐹 𝑥𝐿𝐾,𝑊 𝑊
=
𝑁𝑠 𝑧𝐿𝐾,𝐹 𝑥𝐻𝐾,𝐷 𝐷
N = 𝑁𝑅 + 𝑁𝑠
𝑁𝑅 = 4th
𝑁𝑠 = 4th
where,
𝑁𝑅 = number of plates in rectifying section
𝑁𝑠 = number of plates in stripping section
Feed stage = 4

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 90

 Diameter of Column
Diameter of Column
𝐿𝑥 𝜌𝐿
𝐹𝑙𝑣 =
𝑉𝑥 𝜌𝑣
• Flv(top)= 0.04564 Flv(bottom)=0.0385
• Q L = mass flow rate of liquids Q v =mass flow rate of vapors
• Fig 11.27 (Sinnot, 2005)
• K1(top)= 0.06 K1(bottom)=0.024
𝑢𝑓(𝑇𝑜𝑝) = 1.427 𝑢𝑓 (bottom)=0.672
Un=Actual flooding velocity=0.75Uf
Op. Uf=1.6747 Op. Uf=0.8037

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 91

 Cont…
• Net Area: 𝐴𝑛 = 𝑉𝑛 Τ𝑈𝑛 , 𝑚2
𝐴𝑛 (T)=0.3408 𝐴𝑛 (𝐵)=0.3133
• Down comer Area 𝐴𝑑 = 0.15(𝐴𝑛 ), 𝑚2
𝐴𝑑 𝑇 = 0.04090𝑚2 𝐴𝑑 = 0.03760
• Cross Sectional Area 𝐴𝑐 = 𝐴𝑛 +𝐴𝑑 , 𝑚2
𝐴𝑐 = 0.38175 𝐴𝑐 =0.351
4𝐴𝑐
• 𝐷𝑖𝑎 = , m
𝜋
• Dia(t) = 0.06685m Dia(b) =0.6973 m

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 92

 Internal Design of DC
• Height Calculations
𝐻𝑡 = (N-1) 𝑙𝑡 + 0.15(N-1) 𝑙𝑡
𝐿𝑤 =0.4881
H/D=3.612
• Ht = total height of column=2.415m
• Lt= tray spacing =0.3
• Selection of flow arrangement
• Fig 11.28 (Sinnot, 2005)
• Cross flow arrangement single pass

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 93

 Provisional Plate Design
• Active area= 𝐴𝑎 = 𝐴𝑐 − 2𝐴𝑑 ,
• 𝐴𝑎 = 𝑜. 4725𝑚2
• Fig 11.31 (Sinnot, 2005)
• (𝐴𝑑 /𝐴𝑐 )𝑥100 = 10.71
• (𝑙𝑤 /𝐷𝑐 )=0.73
• 𝑙𝑤 = 𝑤𝑒𝑖𝑟 𝑙𝑒𝑛𝑡ℎ = 0.4881m
• 𝐴ℎ = 𝐻𝑜𝑙𝑒 𝐴𝑟𝑒𝑎 = 0.045(𝐴𝑎 ) = 0. 0.031𝑚
• 𝐻𝑤 = 𝑤𝑒𝑖𝑟 ℎ𝑒𝑖𝑔ℎ𝑡 = 12 𝑚𝑚
• 𝑑ℎ = ℎ𝑜𝑙𝑒 𝑑𝑖𝑎. = 3.5 𝑚𝑚
• Plate thickness = 5mm

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 94

 Weeping Check
• 𝐿𝑤 = max. liq flow rate = 0.26 kg/s
• Turndown ratio = 0.70
• 𝐿𝑤𝑚 = min liq flow rate = 0.7𝐿𝑤 = 0.182 kg/s
Weir crest
𝐿𝑤 2Τ
• ℎ𝑜𝑤 = 750( ) 3
𝜌𝑣 ×𝑙𝑤
• ℎ𝑜𝑤,𝑚𝑎𝑥 = 3.743 𝑚𝑚 𝑙𝑖𝑞.
• ℎ𝑜𝑤,𝑚𝑖𝑛 = 2.951 mm liq.
• Fig 11.30 (Sinnot)
• (ℎ𝑤 +ℎ𝑜𝑤 )𝑚𝑖𝑛. = 14.95𝑚𝑚 𝑙𝑖𝑞.
• K2 = 27.25

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 95

 Cont…
• Minimum design vap. Velocity
𝐾2 − 0.90(25.4 − 𝑑ℎ )
𝑢ℎ =
(𝜌𝑣 )0.5
𝑢ℎ = 5.178 m/s
𝑉𝑤 = Max. vapor flow rate = 0.2518 kg/s
• Actual vapor velocity
𝑢ℎ′ = 5.927 kg/s
𝑢ℎ <𝑢ℎ ′so, there will be no weeping

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 96

 Pressure Drop Calculations
Dry Plate Drop
𝑢 2 𝜌𝑣
ℎ𝑑 = 51 ( )
𝐶𝑜 𝜌𝐿 𝑢
u=max. vapor velocity through holes= 𝐴𝑛
ℎ
Co= orifice coefficient =0.92, fig. 11.34
ℎ𝑑 = 2.2488 𝑚𝑚 𝑙𝑖𝑞
Residual Head
−3
ℎ𝑟 = 12.5 × 10 ൗ𝜌𝐿 = 8.206 𝑚𝑚 𝑙𝑖𝑞.
Total Pressure Drop
ℎ𝑡 = ℎ𝑑 + ℎ𝑟 + (ℎ𝑤 +ℎ𝑜𝑤 )𝑚𝑖𝑛 = 25.406 𝑚𝑚 𝑙𝑖𝑞.

Δ𝑃 = 9.81 × 10−3 ℎ𝑡 𝜌𝐿 = 379.65 𝑃𝑎

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 97

 Down-Comer Liquid Back-Up
Head loss in down comer
2
𝐿𝑤
ℎ𝑑𝑐 = 166
𝜌𝐿 𝐴𝑎𝑝
𝐴𝑎𝑝 =Area under apron = 𝑙𝑤 ℎ𝑎𝑝 =0.0318 𝑚2
ℎ𝑎𝑝 =height of apron = ℎ𝑤 − 10 =30 mm
ℎ𝑑𝑐 = 4.29 mm liq. (approx. 5mm liq.)

Backup in down comer

ℎ𝑏𝑐 = (ℎ𝑤 +ℎ𝑜𝑤 ) + ℎ𝑡 + ℎ𝑑𝑐 = 149.83 𝑚𝑚 = 0.149 𝑚𝑚
ℎ𝑏𝑐 < 0.5 𝑝𝑙𝑎𝑡𝑒 𝑠𝑝𝑎𝑐𝑖𝑛𝑔 + 𝑤𝑒𝑖𝑟 ℎ𝑒𝑖𝑔ℎ𝑡 , so plate spacing is acceptable
ℎ𝑏𝑐 < 0.17

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 98

 Entrainment
• Fig 11.29 (Sinnot, 2005)
𝑈𝑛
• % 𝐹𝑙𝑜𝑜𝑑𝑖𝑛𝑔 = = 35.3837%
𝑈𝑓
𝑉𝑚
• 𝑈𝑛 = 𝑎𝑐𝑡𝑢𝑎𝑙 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦 = = 0.3791
𝐴𝑛
• 𝑈𝑓 = 𝑓𝑙𝑜𝑜𝑑𝑖𝑛𝑔 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦
• Entrainment = Ψ = 0.00475

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 99

 Number of Holes
• Total Hole Area Aℎ = 0.03071 𝑚2
2
𝜋 dℎ
• Area of 1 hole = = 9.6× 10−6 𝑚2
4
• Number of holes = total area/area of 1 hole = 3193 holes

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 100
 Efficiency
Column Efficiency

𝐸 = 0.5/(0.3 × 𝛼𝐿𝐾/ 𝛼𝐻𝐾 )^0.25

𝐸0 = 56 %

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 101
 Specification Sheet
IDENTIFICATION
Table 9

Item Distillation Column

Tray Type Sieve Tray
Operation Continuous
Function
Separation of Phthalic Anhydride from Maleic Anhydride and Ortho xylen
Material Handled
PARAMETERS FEED TOP BOTTOM
QUANTITY 25543.93 Kg/hr 25160.77 Kg/hr 383.1589 Kg/hr
COMPOSITION OF P.A 57.5% 99.6% 1.9%
TEMPERATURE 513K 410K 500K
DESIGN DATA
NO. OF TRAYS 8
Feed Plate 4
PRESSURE Drop 379.5 Pa
HEIGHT OF COLUMN 2.415m
DIAMETER OF COLUMN 0.6686 m
REFLEX RATIO 2
TRAY SPACING 0.30 m
Vapor VELOCITY 0.3791 m/s

6/12/2019 100 TPD Production of Phthalic Anhydride By Partial Oxidation of O-xylene 102