EQUIPMENT DESIGN

PRODUCTION OF
PHTHALIC ANHYDRIDE VIA
VAPOR-PHASE CATALYTIC OXIDATION OF O-XYLENE

PRODUCTION OF PHTHALIC ANHYDRIDE VIA VAPOR-PHASE CATALYTIC OXIDATION OF O-XYLENE

T-01 DESIGN
DISTILLATION COLUMN
SPECIFICATION SHEET
Item
Item Number
Number of Item
Operation
Type

Distillation Column
T-01
1
Continuous
Plate Distillation Column

Design Data
Area
Diameter
Active Area
Downcomer Area
Height of Column
Number of Plates
Tray Spacing
Hole Diameter
Plate Thickness
Hole Area
Weir height
Weir length
Area of one hole
Number of holes
Number of holes per tray
Dry plate pressure drop

0.35 m2
0.66 m
0.28 m2
0.0345 m2
5.1 m
17
0.122 m
4.0 mm
50 mm
0.0317 m2
50 mm
0.48 m
1.26 105 m2
2638
156
605.09 Pa

Mechanical Design
Material of Construction
Shell thickness
Head type
Head height
Head Thickness

Stainless Steel
4 mm
Ellipsoidal Head
4 mm
4 mm

Nozzle Sizing
Feed Inlet
Diameter
Thickness

13 m
3.50 m

Top Vapour
Outlet
13 mm
3.5 mm

Reflux
Inlet
25 mm
3.5 mm

Bottom Liquid
Outlet
13 mm
3.5 mm

Bottom Vapour Outlet

DISTILLING COLUMN

18 mm
3.5 mm

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PRODUCTION OF PHTHALIC ANHYDRIDE VIA VAPOR-PHASE CATALYTIC OXIDATION OF O-XYLENE

Stream 14: Distillate

2 = 199C

Stream 13: Liquid Feed

mass in = 11080.41

1 = 180C

Stream 15: Bottoms

2 = 287C

Distillation is a unit operation most widely used to separate liquid mixture into more or less pure
components. In distillation, separation of constituents is based upon differences in boiling points.

Supplementary Data
Chemical Formula

Chemical Name

Molecular weight

Boiling Point

H2O

Water

18.02

100

C8H4O3

Phthalic Anhydride

148.00

286.8

C4H2O3

Maleic Anhydride

98.00

199.6

Light Key: MAN

Heavy Key: PAN

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From energy balance:

CALCULATION OF BUBBLE POINT AND DEW POINT TEMPERATURE
DISTILLATE

Mass (kg)

kmoles

Xi

PAN

105.98

0.7161

0.0704

MAN

373.61

3.8123

0.3749

Water

101.62

5.6393

0.5547

Total

1197.720

10.1677

1.0000

Pressure
COMPONENT
PAN
MAN
Water

A
15.9984
16.2747
18.3036

COMPONENT
PAN
MAN
Water

Ki = Pi/P
0.119712
0.982312
15.01076

DEW POINT
760 mmHg
B
C
4467.01
-83.15
3765.65
-82.15
3816.44
-46.13
Yi
0.0704
0.3749
0.5547
1.000

DEW POINT TEMP

BOTTOMS
PAN
MAN
Total

xi=yi/Ki
0.58808
0.38165
0.03695
1.001306

T(C)
199
199
199

Pi(mmHg)
90.98131
746.55709
11408.18002

1
8.20563
125.39060

Mass (kg)
10492.34
6.85
10502.84

kmoles
70.8942
0.0699
70.9641

Xi
0.999
0.001
1

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BUBBLE POINT
Pressure
COMPONENT
PAN
MAN

A
15.9984
16.2747

B
4467.01
3765.65

COMPONENT
PAN
MAN

Ki = Pi/P
0.997338
5.818135

Xi
0.999
0.001
1

BUBBLE POINT TEMP

120 kPa
C
-83.15
-82.15
yi = KiXi
0.99634
0.00582
1.002

T(C)
287
287

Pi(mmHg)
1.05277
5.11287

1
5.83366

10.32784

5.83366

8.08075

5.3253

999.0

4.1059

Where alpha ()= [1]

Determination of Minimum Number of Stages Nm

log[( )( )]

[2]

log(, )

log[(5.3253)(999.0)]
log(8.08075)

= 4.1059 5

1
2

Equation 19.5, Unit Operations of Chemical Engineering, 5th ed., p.589

Fenske equation (Equation 11.7-12) Geankoplis, 1978

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Determination of Minimum Reflux Ratio Rmin

[3]
1 =

q = 1.93215 (for cold liquid feed, from energy balance)

Distillate
PAN
MAN
Water
Total

Flow rate
105.98
373.61
101.62
581.22

mole
0.7161
3.8123
5.6393
10.1677

Xi
0.0704
0.3749
0.5547
1.0000

Xi
0.0704
3.21199
75.1485

3.4155
3.4155
3.4155

(.Xif)/(-)
-0.0291
0.6234
0.5690
1.1633

Using trial and error, =5.39

[4]
+ 1 =

= 1.5725 1 = 0.5725
= 1.2( ) = 1.2(0.5725)
= 0.6870
From Fig. 11.7-3.Geankoplis (1978),

= 0.4072
+1

= 0.3641
+ 1

= .

Therefore:
=

4.1059
=
= 10
0.45
0.45

( ) = 9

Underwood Equation: Units Operation of Chemical Engineering, 5th ed., p.602

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Determination of Overall Plate Efficiency

= 51 32.5[log( . , )]5
= 0.103
= 51 32.5[log((0.103 )(6.56704))]
= 56.52%

Number Actual of Trays

, =

9
=
= 16.14

0.5652

, =
Determination of feed plate number
Using Kirkbridge method to get the feed location;

, 2

log [ ] = 0.206 [() ( , ) ( ,) ] [6]

From Material Balance in kmol and mol. fractions:

5
6

xf, hk

xf, lk

xb, lk

xd, hk

70.96

10.17

0.9565

0.0343

0.0010

0.0823

OConnells Correlation [Towler, G. &Sinnot, R.(2002)]

11.7-1, Principles of Transport Processes, Geankoplis

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70.96 0.8826 0.0010 2

log [ ] = 0.206 [(
)(
)(
) ]

10.17 0.0478 0.0704

log [

] = 0.3265

= 0.4715

+ = 17
0.4715 + = 17
= 11.55
= 12; = 5
=
Thus, feed is entering at the 5th stage from the bottom.
Physical Properties of the mixture at the top and bottom of the column
TOP

BOTTOM

472.15 K

560.15 K

Density of the Vapour (kg/m3)7

1.26

38.95

Density of the Liquid (kg/m3)7

907.44

875.69

Average Molecular Weight (kg / kmol)

57.16

147.95

Surface Tension

0.0285

0.0201

Temperature (K)

Table A.2-9, Principles of Transport Processes, Geankoplis, pg. 857

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COLUMN DIAMETER
From Energy Balance in kg
11080.4100 kg

11049.9059 kg

Distillate (D)

581.22 kg

579.2686 kg

Vapour to Condenser-(Vn)

980.53

2113.9249

Liquid Reflux-(Ln)

399.31 kg

1534.6563 kg

10052.8400 kg

10042.9700 kg

976.88 kg

2041.4583 kg

11479.72 kg

14564.7053 kg

Feed-(F)

Bottoms Product-(B)
()
()
Determination of Liquid-Vapor flow Factor, FLV
Top:
=

399.31
980.53

[8]

1.26 3

907.44 3

= 0.0152
Bottoms:
=

11479.72 38.95 3

976.88
875.69 3
= 2.4784

Fair Correlation Equation 14-89, Perrys Chemical Engineering Handbook, 8th ed.,pg.14-37

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Select Plate Spacing: 0.5m [9]

From Fig. 11.27 Pg. 568 from Coulson and Richardsons Chemical Engineering Vol. 6, R.K Sinnott,
(2005)
= 0.082
= 0.065
Correction of Surface Tension
Top:
0.02851000 0.2
= (
) (0.082) = 0.0880
20
Bottoms:
0.02011000 0.2
= (
) (0.065) = 0.0698
20

Determination of Flooding Velocity

10
= 1

Top:

= 0.0880

907.44 3 1.26 3

1.26 3

Perrys Chemical Engineering Handbook, 8th Ed., p.14-29

Eqn. 11.81 Sinnott, R. K. Coulson and Richardsons Chemical Engineering, pg. 568

10

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= .

Bottoms:

= 0.065

875.69 3 38.95 3

38.95 3

= .

Maximum flow rate (gas velocity), Uf

Assume 80% flooding11,
= 0.80 (2.36

) = 1.888

= 0.80 (0.3013

) = 0.2410

Maximum Vapor Volumetric Flow Rate

Top:
= (581.22

3
1
3
)(
)(
) = 0.1281
1.26 3600

Bottoms:

3
1
3
= (10052.84 ) (
)(
) = 0.0749

38.95 3600

11

Sinnott, R. K. Coulson and Richardsons Chemical Engineering, pg. 585

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Net Area Required

=

0.1281

1.8880

= 0.0678 2

0.0749

0.2410

= 0.3108 2

As first trial, take downcomer area as 10% of total, therefore bubbling area = 90%
Column-Cross Sectional Area
0.06782
=
= 0.07542
0.90
=

0.29742
= 0.34532
0.90

Column Diameter
0.07542 (4)

=
= 0.3099

0.34532 (4)
= 0.6631

Therefore our Column Diameter

= .

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PRODUCTION OF PHTHALIC ANHYDRIDE VIA VAPOR-PHASE CATALYTIC OXIDATION OF O-XYLENE

PROVISIONAL PLATE DESIGN

DC =0.66 m
Ac = 0.3453 m2

Downcomer Area, Ad
= 0.10(0.34532 ) = 0.03452
= 0.10(0.07542 ) = 0.0075 2

. . = (11479.72

3
1
)(
)(
)

875.69 3600

3
. . = 0.0036

Plate Diameter:
, =
= 0.31082 0.0345
2 = 0.31082
, = 2
= 0.3108 2 2(0.03452 ) = 0.2762 2
0.2762 2 (4)
=
= 0.5931

Hole Area, Ah:

Take 12 percent of Aa
= 0.12 = (0.12)(0.27622 ) = 0.0331 2

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Weir Length, lw:

0.0345 2
100% =
= 10

0.34531 2
From Figure 11.31 (Coulson, 2005)

= 0.725

= (0.725)(0.66 ) = 0.4807
Take Weir Height = 50mm
Hole Diameter

= 4.0mm

Plate thickness = 5mm

Check Weeping
= (11479.72

1
1

)(
)(
) = 0.1329
24 3600

Minimum liquid flow rate,

At 70% turn down
= (0.1329

3
) (0.7) = 0.0930

Weir crest,
212

3
= 750 [
]

3
0.093
= 750 [
]
875.69(0.4713)

= 2.78

12

Eqn. 11.85

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At minimum rate
+ = 2.78 + 50
+ = 52.77
From Figure 11.30, (Coulson, 2005)
2 = 30.1

Determination of Minimum Design Vapour Velocity

=
=

2 0.90(25.4 )
( )1/2

30.1 0.90(25.4 4)

(38.95 3 )1/2

= 1.74

. 0.1281
^ =
=

0.03312
^ = 3.87

> ; .
PLATE PRESSURE DROP

For Dry Plate Drop:

0.0331 2
100% =
100% = 12

0.2762 2
5
=
= 1.25

4

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From Figure 11.34 [Coulson, 2005]

Co = 0.90
Dry Plate Pressure Drop, hd
Maximum vapor velocity through holes, h max
3

0.1281

=
=
=
3.87
0.0331 2

2
= 51 (
) ( )

4.03 2 1.26
= 51[
] [
] = 1.42
0.90 907.44

Residual head
12.5103 12.5103
=
=
= 13.78

907.44
Total plate drop:
= + + +
= (1.42 + 13.78 + 2.77 + 50)
= .

= 9.81103
= 9.81103 (67.97 )(907.44)
= .

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PRODUCTION OF PHTHALIC ANHYDRIDE VIA VAPOR-PHASE CATALYTIC OXIDATION OF O-XYLENE

Downcomer Liquid Back Up

Apron Sizing
= 10 = (50 10) = 40
= = (

40
) (0.4807 ) = 0.01922
1000

Since Ad>Aap, use Aap in eqn.

2
0.1686

= 166 [
] = 166 [
]

(907.44 3 )(0.01922 )

= 0.0162
Back-up in downcomer, hb
= + + +
= (2.78 + 50 + 67.97 + 0.0096)
= 120.76 = 0.12076

Check Plate Spacing

<

1
( + )
2

1
50
0.12172 < (0.25 +
)
2
1000
. < . ; Plate Spacing is acceptable
Check Residence Time
=

(0.03452 )(0.12076) (875.691

0.1329

= 27.4829

> 3 ;

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Check Entrainment
3

0.1281

=
=
=
0.4123
0.31082

( ) 0.4123
% =
=
= 0.80

0.5154

% = %
From Fig. 11.29 Pg. 570 from R.K Sinnott, 2005
= .
Number of Holes
=

= (0.004)2 = 1.26 105 2

4
4

=
=

0.0331
= 2637.97
1.26 105 2

= 2638
=

2638
= 155.18
17

= 156
Plate Layout
0.4807
=
= 0.728

0.66
From Fig. 11.32 Pg. 574 from R.K Sinnott, 2005
= 830
= 1800 830 = 970
Assumptions:
Use cartridge type construction
Allow 50 mm unperforated strip round tape edge
50 mm wide calming zone

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970
= (0.70 0.05) (
) = 1.10
180
= 0.05(1.10) = 0.0552

= +
= 0.5075 + 0.05
= 0.5575
= 2(0.5575)(0.05 ) = 0.05575 2

,
=
, = (0.276 0.055 0.05575)2

= .

0.03312
=
= 0.2006

0.165 2

From Fig. 11.33 Pg. 575 from R.K Sinnott, 2005

= 2.2

The hole pitch should not be less than 2.0 and not greater than 4.0
Therefore Hole Pitch is satisfactory

= 2.2 = 2.2(4.0) = 10

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MECHANICAL DESIGN
Column Height
= ( 1) + + ( )
Where H = 1m (for Vapour disengagement and liquid hold up)
Top clearance = 0.5 m
Bottom clearance = 0.5 m
= (17 1)0.25 + 1 + 17 (

5
)
1000

= 5.085
= .
Volume of Column
= ( )( )
= (5.1 )(0.34532 ) = .

Shell Thickness
=

+
2

Take Pi (Design Pressure) as 1.1 times the Atmospheric Pressure

= 1.1(101325) = 111457.5 = 0.11

Take f (Carbon Steel) = 105 N/mm2

Take J (Joint efficiency) = 0.8
Take C (Corrosion Allowance) = 3.175 mm

(0.11 2 ) (663)

2 (105 2 ) (0.8) 0.11 2

+ 3.175 = 3.61

= .

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Head Thickness
For Ellipsoidal head:
Equation from Chapter 2.3.2 NPTEL Chemical Engineering Design - II
=

+
2 0.2

For Ellipsoidal head ( = 4 )

2

1
0.586
(2 + ( ) ) = (2 + ( 0.586 ) ) = 1
6
2
6
2(
)
4

(0.11 2 ) (700)(1)

2(0.8) (105 2 ) 0.2 (0.11 2 )

+ 3.175 = 3.63

= .
Nozzle Sizing
General Guidelines: [Process Engineering and Design Using Visual Basic. (2008).]
For Inlet Fluids (Liquid or Gas): v2<= 1000
For Outlet Gas: v2<= 3600
For Outlet Liquids: v= 1m/s
Take J (Joint efficiency) = 0.8
Take C (Corrosion Allowance) = 3.175mm
Feed Inlet Nozzle
Density(kg/m3)

954.63

V2(kg/ms2)

1000

1000 .2

954.63 3

= 1.023

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= (11080.41

1
1

)(
)(
) = 0.128
3600 24

0.128

=
=
= 0.000132
(954.63 ) (1.023 )
3

4
4(0.000132 )

=
= 0.0129 = 12.9

Feed Inlet Nozzle Thickness

Take f (Carbon Steel) = 125 N/mm2 (Fig. 11.33, Coulson 2005)
=

(0.11
(2) (125

+
2

)(22)

) (0.8) (0.11 2 )
2

+ 3.175 = 3.18

= .
Top Vapour Outlet
Density(kg/m3)

2.245

V2(kg/ms2)

3600

3600 .2

2.245 3

= (980.53

= 40.04

1
1

)(
)(
) = 0.0113
24 3600

0.0113

=
=
= 0.00012
(2.245 ) (40.04 )
3

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4
4(0.00012 )

=
=
= 0.01268 = 12.68

=
Top Outlet Nozzle Thickness
Take f (Carbon Steel) = 120N/mm2 (Fig. 11.33, Coulson 2005)
=

(0.11
(2) (120

+
2

)(13 )

2 ) (0.8) (0.11

2)

+ 3.175 = 3.18

= .
Top Reflux Inlet

Density(kg/m3)

820.321

V2(kg/ms2)

1000

1000 .2

820.321 3

= (399.31

= 1.104

1
1

)(
)(
) = 0.0046
24 3600

0.0046

=
=
= 5.08 106 2

(820.321 ) (1.104 )
3

4
4(5.08 106 2 )

=
=
= 0.0025 = 25

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Top Reflux Nozzle Thickness

Take f (Carbon Steel) = 120 N/mm2
=

(0.11
(2) (120

+
2

)(67)

+ 3.175 = 3.21

) (0.8) (0.11 2 )
2
= .

Bottom Liquid Outlet

Density(kg/m3)

991.52

=1
= (11479.72

1
1

)(
)(
) = 0.1329
24 3600

0.1329

=
=
= 0.0001342
(991.52 ) (1.0 )
3

4
4(0.0001342 )

=
=
= 0.0131 = 13.1

=
Bottom Liquid Nozzle Thickness
Take f (Carbon Steel) = 95 N/mm2 (Fig. 11.33, Coulson 2005)
=

(0.11
(2) (95

+
2

) (23 )

) (0.8) (0.11 2 )

+ 3.175 = 3.19

= .

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Bottom Vapour Inlet

Density(kg/m3)

2.245

V2(kg/ms2)

1000

1000 .2

= 21.11

2.245 3

= (976.88

1
1

)(
)(
) = 0.0113

24 3600

0.0113

=
=
= 0.000242
(2.245 ) (21.11 )
3

4
4(0.000242 )

=
= 0.0174 = 17.4

Bottom Vapour Inlet Nozzle Thickness

Take f (Carbon Steel) = 95
=

(0.11
(2) (95

+
2

) (100)

) (0.9) (0.11 2 )

+ 3.175 = 3.239

= .

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