3-1

CHAPTER 3

DESIGN FOR DISTILLATION COLUMN

3.1

INTRODUCTION

Distillation is most probably is the widely used separation process in the chemical industries. The design of a distillation column can be divided into several procedures:

1. Specify the degree of separation required: set product specification 2. Select the operation conditions: batch or continuous: operating pressure 3. Select the type of contacting device: plate or packing 4. Determine the stage and reflux requirements: the number of equilibrium stages 5. Size the column: diameter, number or real stages 6. Design the column internals: plates, distributors, packing supports 7. Mechanical design: vessel and internal packing

The separation of liquid mixtures by distillation is depends on the differences in the volatility between the components. This is known as continuous distillation. Vapor flows up to column and liquid counter-currently down the column. The vapor and liquid are brought into contact on plates. Part of the condensate from the condenser is returned on the top of the column to provide liquid flow above the feed point (reflux), and part of the liquid from the base of the column is vaporized in the reboiler and returned to provide the flow.

3-2 3.2 Chemical Design

The purpose of this distillation column is to separate the component mixture. Basically, components which are Propanal, DPE, water, 1-Propanol, Ethylene, Carbon Monoxide, Hydrogen and Ethane are to be separated to the bottom stream. These components will go through another distillation process. The feed is fed to the distillation column at 1.82 bar and 293K. The products at the top column leave the column at 1 bar and 357.36K. The products at the bottom column leave the column at 1.6bar and 382.35K. 1-Propanol and DPE were chosen as the key components being 1-Propanol as the light key component while DPE as the heavy key component. Distillation column with perforated tray has been chosen. Basically, this is the simplest type. The vapour passes up through perforations in the plate, and the liquid is retained on the plate by the vapour flow. There is no positive vapour liquid seal, and at low flow rate liquid will weep through the holes reducing efficiency. The perforation is usually small holes.

3.2.1

Complete Diagram

The composition of the inlet and outlet streams for distillation column is shown in table 3.1: Table 3.1 Summary of the inlet and outlet composition

Feed

Top

Bottom

Component

Molar Flow Rate (kmole/h)

Mole Fraction

Molar Flow Rate (kmole/h)

Mole Fraction

Molar Flow Rate (kmole/h)

Mole Fraction

1-Propanol

257.94

0.9768

1.2283

0.4853

256.7

0.9815

Water

2.2373

0.0085

0.45993

0.1817

1.7774

0.0068

Propanal

1.4473

0.0055

0.7767

0.3068

0.6706

0.0026

3-3

Dipropyl Ether

2.3986

0.0092

0.0118

0.0047

2.3868

0.0091

3.2.2

Bubble and Dew Point Temperature

To estimate the stages, and the condenser and reboiler temperatures, procedures are required for calculating dew and bubble points. By definition, a saturated liquid is at its bubble point (any rise in temperature will cause a drop in a liquid form). It can be calculated in terms of equilibrium constant, K. Bubble Point : Dew Point : = = = 1.0 / = 1.0 (3.1) (3.2)

Table 4.2 below shows the constants of Antoine equation for each component. (RK Sinnot, 1999) where the constant value for each component is taken from HYSYS. Table 3.2: The Antoine Constant COMPONENT 1-Propanol Water Propanal Dipropyl Ether 96.7 -7.45103 0.00 -1.24 1.0810-5 2.00 a 79.5 65.9 80.9 b -8.29103 -7.23103 -6.51103 c 0.00 0.00 0.00 d -8.9096 -7.18 -9.82 e 1.8210-6 4.0310-6 6.7910-6 f 2.00 2.00 2.00

Antoine equation: ln = + ln + ^ + (3.3)

(3.4)

3-4 Estimation of feed temperature, = / = 1.0

By using the goal seek method in the excel program, with constant operating pressure at feed is 1.6 bar, the calculated temperature is 363K. The data shown in Table 3.3: Table 3.3: Calculation of Bubble Point at Feed Stream COMPONENT 1-Propanol Water Propanal Dipropyl Ether ln Pi 5.19 5.07 6.54 5.23 Pi (kPa) 179.42 159.48 692.20 186.62 Xi 0.9768 0.0085 0.0055 0.0092 O.P (kPa) 182 182 182 182 Ki 0.99 0.88 3.80 1.03 TOTAL Yi=KiXi 0.962939 0.007448 0.020918 0.009434 1.00000

Hence, the bubble point temperature is 386.36 K By using the goal seek method in the excel program, with constant operating pressure at top is 0.5 bar, the calculated temperature is 60K. The data shown in Table 3.4: Dew Point Temperature (top column) = / = 1.0

Table 3.4: Calculation of Dew Point at Top Column COMPONENT 1-Propanol Water Propanal Dipropyl Ether ln Pi 3.59 3.54 5.44 4.01 Pi (kPa) 36.41 34.59 231.56 55.25 Yi 0.4853 0.1817 0.3068 0.0047 O.P (kPa) 50 50 50 50 Ki 0.73 0.69 4.63 1.10 TOTAL Xi=Yi/Ki 0.67 0.26 0.07 0.004 1

3-5 Hence, the dew point temperature is 345.56 K By using the goal seek method in the excel program, with constant operating pressure at bottom is 1.6 bar, the calculated temperature is 376K. The data shown in Table 3.5: Bubble Point Temperature (bottom column) = = 1.0

Table 3.5: Calculation of Bubble Point at Bottom Column COMPONENT 1-Propanol Water Propanal Dipropyl Ether ln Pi 4.69 4.59 6.20 4.85 Pi (kPa) 108.95 98.45 490.93 127.18 Xi 0.9815 0.0068 0.0026 0.0091 O.P (kPa) 110 110 110 110 Ki 0.99 0.89 4.46 1.16 TOTAL Yi=KiXi 0.97 0.01 0.01 0.01 1

Hence, the bubble point temperature is 372.33 K

3.2.3

Determination of Relative Volatility

The equilibrium vaporization constant K is defined for a compound by = (3.5)

Where, Yi = mole fraction of component i in vapour phase Xi = mole fraction of component i in liquid phase The relative volatility, which is needed in the calculation is defined as = (3.6)

3-6 Where i and j represent the components to be separated From Ideal system, Raoults law,

Pi = PiXi The relative volatility of two components can be expressed as the ratio of their K value, = KHK = Heavy key components 3.2.3.1 Top Column

(3.7)

(3.8)

Where, KLK = Light key components

Table 3.6 COMPONENT 1-Propanol Water Propanal DPE K 0.7300 0.6900 4.6300 1.1000 =

0.6636 0.6273 4.2091 1.0000

3.2.3.2 Bottom Column

Table 3.7 COMPONENT 1-Propanol Water Propanal K 0.9900 0.8900 4.4600 =

0.8534 0.7672 3.8448

3-7 DPE 1.1600 1.0000

Average relative volatility of the light key to heavy key; Top (Bottom )

LK

0.6636 (0.8534)

= 0.753

3.2.4

Minimum Number of Stages Using Fenskes Equation

The Fenskes Equation (1932) can be used to estimate the minimum stages required at total reflux. The derivation of the equation for binary system and applies equally to multi-component system. The minimum number of stages will be obtained from this equation:

Nmin

X X Log[(X LK )]d [( XHK )]b

HK LK

Log LK

(3.9)

0.73 0.0091 Log[( 1.1 )]d [( )] 0.9815 b = Log 0.753 = 17.94

= 20 stages

3.2.5

Minimum Reflux Ratio

Colburn (1941) and Underwood (1948) have derived equations for estimating the minimum reflux ratio for multicomponent distillations. The equation can be stated in the form: , = + 1 (3.10)

3-8 Where, i = the relative volatility of component i with respect to some reference component, usually the heavy key Rm = Xi,d = the minimum reflux ratio concentration of component i in the tops at minimum reflux

and is the root of the equation:

, = 1 Where, Xi,f =

(3.11)

the concentration of component i in the feed, and q depends on the condition of the feed

The value of must lie between the values of relative volatility of the light and heavy keys and is found by trial and error. As the feed at its boiling point q = 1 , =0 Table 3.8 Component 1-Propanol Water Propanal DPE Xi,f 0.9768 0.0085 0.0055 0.0092 i 0.7600 0.7000 4.0300 1.0000 iXi,f 0.7424 0.0060 0.0222 0.0092 estimate 3.9 3.9 3.9 3.9 3.9 (iXi,f)/(i - ) -0.2364 -0.0019 0.1705 -0.0032 -0.07

Therefore, = 3.9

3-9 Table 3.9 Component 1-Propanol Water Propanal DPE Xi,d 0.4853 0.1817 0.3068 0.0047 i 0.76 0.7 4.03 1 iXi,d 0.3688 0.1272 1.2364 0.0047 estimate 3.9 3.9 3.9 3.9 3.9 (iXi,d)/(i - ) -0.1175 -0.0397 9.5108 -0.0016 9.35

Taking equation 3.10, Rm + 1 = 9.35 Rm = 8.35 = 0.8931 + 1 Specimen calculation, for R = 2.0 2 = = 0.66 ( + 1) 3 Using Erbar Maddox correlation (Erbar and Maddox, 1961) from figure 11.11 (Coulson and Richardson, Volume 6, page 524), = 0.74 N=
18 0.74

= 24.3 For other reflux ratios R N 2 24.3 3 21.43 4 20.69 5 20.22

3-10 The optimum reflux ratio will be near to 4. Therefore, the optimum reflux ratio will be taken as 4 while the actual stage is 21.

3.2.6

Feed Point Location

Feed point location can be found using Kirkbride (1944) equation: = 0.2606 log Where, Nr Ns B D Xf,HK Xf,LK Xd,HK Xb,HK = = = = = = = = no. of stages above the feed, including any partial condenser no. of stages below the feed, including the reboiler molar flow bottom product molar flow top product concentration of the heavy key in the feed concentration of the light key in the feed concentration of the heavy key in the top product concentration of the heavy key in the bottom product 2.531 261.5 0.0092 0.9768 0.395 0.00382
2

, ,

x , x ,

(3.10)

= 0.2606 log

= 0.993 Actual number of plates is 24 Nr + Ns = 24

0.993Ns + Ns = 24 1.993Ns =9

3-11 Nr = 15

So, feed inlet is at stage 9 from bottom.

3.2.7

Efficiency of Distillation Column

Overall column efficiency is given as: = 51 32.5 log ( ) Where, = the molar average liquid viscosity, mNs/m2 = average relative volatility of the light key To find the viscosity of the flow: = 1 1 Table 3.8 Viscosity of the mixture Viscosity Coefficient A 1-Propanol Water Propanal DPE 0.9768 0.0085 0.0055 0.0092 951.04 658.25 343.44 410.58 B 327.83 283.16 219.33 219.67 -0.32859 -0.54418 -0.63690 -0.75852 TOTAL 0.46926 0.28564 0.23073 0.17438 1.16 0.4584 0.0024 0.0013 0.0016 0.4637 (3.12) (3.11)

Component

Mole fraction feed, x

Log

Viscosity (mNs/m2)

Where,
= 51 32.5 log ( )

3-12 = = 51 32.5 log (0.463674405 x 0.787) 55.44 %

Plate and overall column efficiencies will normally be between 30% to 70%. (Coulson and Richardsons, volume 6, page 547) 3.2.8 Physical Properties

3.2.8.1 Relative Molar Mass (RMM) RMM = (component mole fraction x molecular weight) (3.13)

Table 3.9 Liquid Density Component 1-Propanol Water Propanal DPE Molecular Weight 60.1 18.015 58.08 102.18 Feed 0.9768 0.0085 0.0055 0.0092 Mole Fraction Distillate 0.4853 0.1817 0.3068 0.0047 Bottom 0.9815 0.0068 0.0026 0.0091 Liquid Density (kg/m3) 803.4 1000 810 725

Feed, F

= 0.9768 (60.1) + 0.0085 (18.015) + 0.0055 (58.08) + 0.0092 (102.18) = 60.118 kg/kmol

Distillate, D

= 0.4853 (60.1) + 0.1817 (18.015) + 0.3068 (58.08) + 0.0047 (102.18) = 50.739 kg/kmol

Bottom, B

= 0.9815 (60.1) + 0.0068 (18.015) + 0.0026 (58.08) + 0.0091 (102.18) = 60.191 kg/kmol

3-13 3.2.8.2 Density Top Product : L L = = = v v = , 0.4835(803.4) + 0.1817(100) + 0.3068(810) + 0.0047(725) 823.51 kg/m3

(3.14)

(3.15)

=
=

29.167 / 22.4 3 /

273 357.21

1 1

1.731 kg/m3

Bottom Product: L L = = = v v = , 0.9815(803.4) + 0.0068(100) +0.0026(810) + 0.0091(725) 804.04 kg/m3

(4.16)

273 382.2

(4.17)

=
=

58.988 / 22.4 3 /

1.6 1

3.071 kg/m3

3.2.8.3 Surface Tension, Using Sugden (1924), equation 8.23 (Coulson and Richardsons, volume 6, page 335)

( =

1012

(3.18)

3-14 Where, Pch v L M = = = = = surface tension, MJ/m2 or (dyne/cm) Sugdens parachor Vapor density, kg/m3 Liquid density, kg/m3 relative molecular weight

For mixture, m = 1x1 + 2x2 + .. Where, m = surface tension mixture surface tension for mixture component mole fraction Table 3.10 Pch Distribution Pch Distribution 148.3 31.3 165.4 299.5 Mole Fraction Distillate 0.4853 0.1817 0.3068 0.0047 Bottom 0.9815 0.0068 0.0026 0.0091

(3.19)

1 , 2 = x1 , x2 =

Component

1-Propanol Water Propanal DPE

Pch at top

= =

, 0.4853 (148.3) + 0.1817 (31.3) + 0.3068 (165.4) + 0.0047 (299.5)

3-15 = Pch at bottom = = = 177.28097 , 0.9815 (148.3) + 0.0068 (31.3) + 0.0026 (165.4) + 00.0091 (299.5) 148.30792

Calculation of surface tension: Top Column, =

65.01 969.64 4.928 4 21.98

1012

= 67.965683 N/m

Bottom Column, =

59.04 1019.01 0.325 20.04

1012

= 15.27159545 N/m

Above feed point: Vapor flow rate: Vn Where, D R Hence, Vn = = 261.5 (2.531 + 1) 923.36 kmole/hr = = Distillate molar flowrate Reflux ratio = D(R + 1) (3.20)

Liquid down flow: Ln = Vn D = 923.36 261.5

(3.21)

3-16 = 661.86 kmole/hr Below the feed point: Liquid flow rate: Lm Where, F = Feed molar flowrate = Ln + F (3.22)

Hence, Lm = = 661.86 + 264.1 925.96kmole/hr (3.23)

Vapour flow rate: Vm = Lm W Where, W Hence, Vm = = 925.96 261.5 664.46kmole/hr = Bottom molar flowrate

The equation for the operating lines below the feed plate: = + 1 261.5 () 664.46 () (3.24)

925.96 664.46

+ 1

= 2.058(Xm + 1)

261.5 664.46

The equation for the operating lines above the feed plate: = + 1 (3.25)

3-17 661.86 923.36 261.5 923.36

+ 1

= 0.72 (Xn + 1) 2.01 x 10-3

1.731 823.51

(3.26)

= 0.72

= 0.033 where 0.72 is the slope of the top operating line.

3.071 804.04

(3.27)

= 1.39

= 0.09 where 1.39 is the slope of the bottom operating line.

3.2.9

Determination of Plate Spacing

The overall height of the column will depend on the plate spacing. Plate spacing from 0.15m to 1.0m are normally used. The spacing chosen will depend on the column diameter and the operating condition. Close spacing is used with small - diameter columns, and where head room is restricted, as it will be when a column is installed in a building. In this distillation column, the plate spacing is 0.5m as it is normally taken as the initial estimate recommended by Coulson and Richardsons, Chemical Engineering, Volume 6.

3-18 The principal factor that determines the column diameter is the vapor flowrate. The vapor velocity must be below that which would cause excessive liquid entrainment or highpressure drop. The equation below which is based on the Souder and Brown equation, Lowenstein (1961), Coulson & Richarsons Chemical Engineering, Volume 6, page 556, can be used to estimate the maximum allowable superficial velocity, and hence the column area and diameter of the distillation column.

= 0.171 2 + 0.271 0.047

0.5

(3.28)
0.5

= 0.171(0.5)2 + 0.271(0.5) 0.047 = 2.8173 m/s

969.64 4.928 4.928

Where, Uv = maximum allowable vapor velocity based on the gross (total) column cross Sectional area, m/s lt = plate spacing, m (range: 0.5 1.5)

3.2.9.1 Diameter of the column 4

(3.29)

Where Vw is the maximum vapor rate, kg/s = 15870 1 3600

= 4.41 kg/s

3-19

4(4.41) 4.928 (0.64)

= 1.33 m

3.2.9.2 Column Area The column area can be calculated from the calculated internal column diameter = = 2 4 (1.33)2 4 (3.30)

= 1.39 m2

4.2.10 Liquid Flow Arrangement Before deciding liquid flow arrangement, maximum volumetric liquid rate were determined by the value of maximum volumetric rate = 15740 1 3600 4.372 3 804.04 (3.31)

= 5.38 x 10-3 Dc = 1.128 m

Based in the values of maximum volumetric flow rate and the column diameter to Figure 11.28 from Coulson and Richardson, Chemical Engineering, Volume 6, page 568, the types of liquid flow rate could be considered as single pass.

3-20 Perforated plate, which is famously known as sieve tray is the simplest type of cross-flow plate. Cross flow trays are the most common used and least expensive. Sieve tray is chosen because it is consider cheaper and simpler contacting devices. The perforated trays enable designs with confident prediction of performance. According, most new designs today specify some type of perforated tray (sieve tray) instead of the traditional bubble-cap tray. Sieve tray also gives the lowest pressure drop.

3.2.11 Plate Design Column diameter, Dc = 1.33 m Column area, Ac = 1.39 m2

As a first trial, take the downcomer area as 12% of the total Downcomer area, Ad = 0.12 Ac = 0.12 x 1.39 m2 = 0.1668 m2 Net area, An = Ac - Ad = 1.39 m2 - 0.1668 m2 = 1.2232 m2 Active area, Aa = Ac 2Ad = 1.39 m2 2(0.1668 m2) = 1.0564 m2 Assume that the hole-active area is 10% Hole area, Ah = 0.10 Aa = 0.10 x 1.0564 m2 = 0.10564m2 (3.35) (3.34) (3.33) (3.32)

3-21 3.2.11.1 Weir Length

With segmental downcomers the length of the weir fixes the area of the downcomer. The chord length will normally be between 0.6 to 0.85 of the column diameter. A good initial value to use is 0.77, equivalent to a downcomer area of 15%. Referring to Figure 11.31 from Coulson and Richardsons, Chemical Engineering, Volume 6, page 572, with (Ad/Ac) x 100 is 12 percents, thus, Iw/Dc is 0.76

Weir length, Iw = 0.76Dc = 0.76 x 1.33 m = 1.011 m

3.2.11.2

Weir Height

For column operating above atmospheric pressure, the weir-heights will normally be between 40 mm to 90 mm (1.5 to 3.5 in); 40 to 50 mm is recommended.

Take Weir height, hw = 50 mm Hole diameter, dh Plate thickness, t = 5 mm (preferred size) = 3 mm (stainless steel)

For hole diameter = 5 mm, area of one hole, = ( )2 4 (0.005)2 4 (3.36)

= 1.9635 x 10-5 m2

3-22 Number of holes per plate, = 1 0.10564 = 1.9635 105 = 5380.19 holes 5380 holes (3.37)

3.2.11.3

Weir Liquid Crest

Check weeping to ensure enough vapour to prevent liquid flow through hole. = 15740 1 3600

= 4.372 kg/s Minimum liquid rate, at 70% turndown = 0.7 x 4.372 kg/s = 3.06 kg/s

The weir liquid can be determine by using the equation below = 750
2 3

(3.38)

Where, Iw Lw L = weir length, m = liquid flow rate, kg/s = liquid density, kg/m3

3-23 how = weir crest, mm liquid

At maximum rate: 4.372 = 750 804.04 1.011 = 20.40 mm liquid

2 3

At minimum rate: 3.06 = 750 1019.01 0.85728 = 18.15 mm liquid

2 3

At minimum rate, clear liquid depth, how + hw = 18.15 + 50 = 68.15 mm liquid From Figure 11.30, in Coulson and Richardsons, Chemical Engineering, Volume 6, page 571, weep point correlation, K2 = 30.7

3.2.11.4

Weep Point

The purpose to calculate this weep point is to know the lower limit of the operating range ccurs when liquid leakage through the plate holes becomes excessive. During weeping, a minor fraction of liquid flows to the tray below through the tray perforations rather than the downcomer. This downward-flowing liquid typically has been exposed to rising vapor; so, weeping only leads to a small reduction in overall tray efficiency, to a level rarely worse than the tray point efficiency. Minimum vapor velocity through the holes based on the holes area.

3-24

(min) =

2 0.9(25.4 ) 2
1

(3.39)

Where, Uh dh K2 = minimum vapor velocity, m/s = hole diameter, mm = constant

30.7 0.9(25.4 5) (3.071)2

1

= 8.036 m/s

(3.40)

4.41 3 0.7 3.071 = 0.10564 = 9.51 m/s

So, minimum operating rate will be above weep point.

3.2.12 Plate Pressure Drop Maximum vapor velocity through holes: = (3.41)

3-25 4.41 3 3.071 = 0.10564 = 13.59 m/s

From Figure 11.34 in Coulson and Richardsons, Chemical Engineering, Volume 6, page 576, for discharge coefficient for sieve plate, , 3 = = 0.6 5 = 0.1

we get Co = 0.74 , = 51
2

(3.42) 3.071 804.04

13.59 = 51 0.74

= 65.697 mm liquid

, =

12.5 103 12.5 103 804.04

(3.43)

= 15.55 mm liquid

Pressure drop per plate, ht

= hd + (hw + how) + hr = 65.697 + (50 + 18.15) + 15.55 = 149.397 mm liquid

(3.44)

3-26 3.2.13 Downcomer Liquid Back-Up The downcomer area and plate spacing must be such that the level of the liquid and froth in the downcomer is well below the top of the outlet weir on the plate above. If the level rises above the outlet weir the column will flood. Take hap = hw 10 mm = 50 10 = 40 mm Where, hap = height of the bottom edge of the apron above the plate

= 166

(3.45)

Where, Lwd Am = liquid flowrate in downcomer, kg/s = either the downcomer area, Ad or the clearance area under the downcomer, Aap whichever is smaller, m2

Area under apron, Aap = hap x Iw = 0.04 m x 1.011 = 0.04044 m2 Where, Aap = the clearance area under downcomer (3.46)

As this less than Ad = 0.1668 m2, equation 11.92 (Coulson and Richardsons, Volume 6, page 577) used Aap = 0.04044 m2

3-27 4.372 804.04 0.04044

2

= 166

= 3.00 mm

3.2.14 Backup on Downcomer hb = (hw + how) + ht + hdc = (50 + 18.15) +149.397 +3.00 = 220.547 mm hb 0.2205 m 0.2205 m < (plate spacing + weir height) < (0.5 + 0.05) m <0.5 m (3.47)

So, tray spacing = 0.5 m is acceptable (to avoid flooding).

3.2.15 Residence Time Sufficient residence time must be allowed in the downcomer for the entrained vapor to disengage from the liquid stream, to prevent heavily aerated liquid being carried under the downcomer. A time at least 3 seconds is recommended. = (3.48)

Where, tr Lwd hbc = residence time, s = liquid flowrate in downcomer, kg/s = clear liquid back up in the downcomer, m

3-28 0.1668 0.2205 804.04 4.372

= 6.764 s tr is greater than 3.0 which is recommended so tr is satisfactory.

3.2.16 Perforated Area From Figure 11.32, Coulson and Richardsons, Chemical Engineering, Volume 6, page 527, for the relaxation between angle subtended by chord, chord height and chord length: Iw/Dc = 1.011/1.33 = 0.76 Ih/Dc = 98 = 0.18

Angle subtended at plate edge by unperforated strips = 180 - 98 = 82 Mean length, unperforated edge strips = (Dc weir height) x x /180 = (1.33 0.05) x x 82/180 = 1.832 m Areas of unperforated edge strips, As = mean length unperforated edge x weir height = 1.832 x 0.05 = 0.0916 m2

3-29 Mean length of calming zone = Weir length + Width of unperforated strip = 1.011 + 0.05 = 1.061 m

Area of calming zone = 2 x (weir height x mean length calming zone) = 2 x 0.05 x 1.061 = 0.1061 m2 Total area available for perforation, Ap : = Active area (area of unperforated edge + area of calming) = 1.0564 (0.0916 + 0.1061) = 0.8587 m2 Ah/Ap = 1.0564/0.8587 = 0.123

From Figure 11.33, Coulson and Richardsons, Chemical Engineering, Volume 6, page 528, the relation between hole area and pitch, Ip/dh = 2.7; satisfactory, which is within 2.5 to 4.0

3.2.17 Column Size The column height will be calculated based on the given below. The equation determines the height of the column without taking the skirt or any support into consideration. Its determination is based on the condition in the column. Column height = (No. of stages 1) x (Tray spacing ) + (Tray spacing x 2) + (No. of stages 1)

3-30 x (Plate thickness) = (24 1)(0.5) + (24 1)(0.003) = 11.57 m By adding 10% safety factor so the column height are 12.7 m 13 m

3.2.18 Plate Design Specification

Table 3.10 Summary of Plate Design Item Column Diameter, Dc No. of Plates Plate Spacing No. of Stage Feed from bottom, F1 No. of Stage Solvent from bottom, F2 Plate Thickness Total Column Height, Ht Plate Material Downcomer Area, Ad Column Area, Ac Net Area, An Active Area, Aa Hole Area, Ah No. of Holes Weir Length, Iw Weir Height (standard) Value 1.33 m 24 plates 0.5 m 9 24 0.003 m 13 m Stainless Steel 0.1668 m2 1.39 m2 1.2232 m2 0.10564 m2 0.010564 m2 5380 units 1.011 m 0.05 m

3-31 3.3 3.3.1 Mechanical Design Introduction

Several factors need to be considered in the mechanical design of distillation column such as 1. Design pressure 2. Design temperature 3. Material of construction 4. Design stress 5. Wall thickness 6. Welded joint efficiency 7. Analysis of stresses a. Dead weight load b. Wind load c. Pressure stress d. Bending stress 8. Vessel support 9. Insulation

3.3.2

Column Design Specification = (1.82 1) bar = 0.82 bar

Operating pressure

Take as 10% above operating pressure Design pressure = 0.82 x 1.1 =0.902 bar = 0.0902 N/mm2

Design temperature

= 113.36C

Take as 10% above operating temperature Operating temperature = 113.36 x 1.1 = 124.694C

3-32 3.3.3 Material of Constructions

Selection of suitable material must be taking onto account the suitability of material for fabrication (particularly welding) as well as the compatibility of the material with the process environment. In this case, the material used in the construction of the distillation column is carbon steel as the material as it is the most used material in industry. For this material, the design stress at 150C is obtained from Table 13.2 for the typical design stresses for plate. = 115 N/mm2 = 360 N/mm2 =1 = 1330 mm = 0.0902 N/mm2 = 75 mm thick

Design stress, f Tensile strength Join factor Diameter vessel, D Operating pressure Insulation, mineral wool

3.3.4

Vessel Thickness

The minimum thickness of column required and other designs are calculated based on equation below: 2

3.49

Where, e Pi Di f J = minimum thickness of the plate required = internal pressure, N/mm2 = internal diameter, m = design stress, N/mm2 = joint factor

Therefore, minimum thickness required, = 0.0902 1330 2 1 (115) 0.0902

= 0.522 mm 0.6 mm

3-33 A much thicker wall is needed at the column base to withstand the wind and dead weight loads. As a first trial, divide the column into five sections, with the thickness increasing by 2 mm per section. Try 1, 3, 5, 7 and 9 mm. The average wall thickness is 5 mm. Take the first trial as 5 mm.

3.3.5

Heads and Closure

Hemispherical, ellipsoidal and torispherical heads are collectively referred to as domed heads. They are formed by pressing or spinning, large diameters are fabricated from formed sections. Torispherical are often referred to as dished ends. After comparing the thickness of all heads, torispherical head had been chosen because of operating pressure for this below 10 bars and suitable for liquid vapor phase process in inconsistent high pressure. The thickness of torispherical head can be calculated below: 2 + ( 0.2)

3.50

Where, Rc Rk = Crown radius = Knuckle radius = Dc = 0.06 Rc = 0.06 x 1330 = 79.8 mm Cs = Stress concentration = =
1 4 1 4

3+ 3+

1330 79.8

= 1.77 0.0902 1330 1.77 2 1 (115) + 0.09(1.77 0.2)

3.51

= 0.923 mm

Round up to 2 mm

3-34 For welding purposes the thickness of head were taken as same thickness of the vessel, = 2 mm. Its matching to joint factor were taken as 1. 3.3.6 Weight Loads

The major sources of the dead weight loads are:

1.

The vessel shell

2. The vessel fittings: manhole, nozzles 3. Internal fitting: plates, heating cooling coils 4. External fittings: ladders, platforms, piping 5. Auxiliary equipment which is not self supported, condensers, agitators 6. Insulation 7. The weight of liquid to fill the vessel.

3.3.6.1 Dead Weight of Vessel Dead weight of vessel can be calculated by using equation below: Wv = 240 x Cv x Dm x (Hv + 0.8 Dm)t x 10-3 kN Where, Wv Cv Dm = total weight of shell, excluding internal fitting such as plates = a factor to account for the weight of nozzles, man ways and internal supports. (In this distillation column, take Cv as 1.15) = mean diameter of vessel = (Dc + t) m = (1.33 + 0.007) = 1.337 m Hv t = height or length between tangent lines, m = wall thickness, m (3.52)

Wv

= 240 x 1.15 x 1.337(13.0 + 0.8(1.337)) x 0.007 = 36.34 kN

3-35 3.3.6.2 Weight of Plate, Wp From Nelson Guide, page 833 Chemical Engineering Volume 6; take contacting plates, 1.2 kN/m2 (for typical liquid loading). The total of weight of plate determine by multiply the value with number of plate design. 2 4 3.142 1.33 4
2

= =

= 1.3895 2 = 1.2 x 1.3895 = 1.6674 kN Where, 1.2 is factor for contacting plates including typical liquid loading in kN/m2

Weight of plate

Thus, for 24 plates

= 24 x 1.6674 = 40.017 kN

3.3.6.3 Weight of Insulations The mineral wool was chosen as insulation material. By referring to Coulson & Richardson, Chemical Engineering Design, Volume 6, page 833, Density of mineral wool, Thickness = 130 kg/m3 = 75 mm = 0.075 m Volume of insulation, Vi = x Di x Hv x thickness of insulation = (3.142)(1.33)(13.0)(0.075) = 4.074 m3 Weight of insulation, Wi = Volume of insulation x x g = 4.074 x 130 x 9.81 = 5196.07 N = 5.196 kN Double this to allow for fittings, 10.392 kN

3-36 3.3.6.4 Total Weight The total weight is the summation of dead weight of vessel, weight of accessories and weight of insulation:

Total weight

= Wv + W + Wi = 36.34 + 40.017 + 10.392 = 86.749 kN

(4.53)

3.3.7

Wind Load

A wind loading must be designed to withstand the highest wind speed that is likely to encounter at the site during the life of the plant. From the British Standard Code of Practice BS CP 3: 1972 Basic Data for the Design of Buildings, Chapter V Loading: Part 2 Winds Load, (Sinnot, 1999), a wind speed of 160 km/h (100 mph) can be used for preliminary design. For cylindrical column, semi-empirical equation can be used to estimate the wind pressure: = 0.05 x uw2

Pw Where,

(3.54)

Pw uw Pw

= wind pressure, N/m2 = wind speed, km/h

= 0.05 (160)2 = 1280 N/m2

Mean diameter, including insulation = Di + 2(t + tins) = 1330 + 2(7 + 75) = 1494 mm = 1.494 m

Loading (per linear meter), Fw

= PwDeff = 1280 x 1.5 = 1920 N/m

3-37 2 2 1920 132 2

, =

= 162240 Nm = 162.24 kNm

3.3.8

Analysis of Stresses of Vessel

3.3.8.1 Pressure Stress Thickness is taken as 9 mm as maximum.

1. Longitudinal stresses due to pressure is given by: 4 0.0902 1330 = 4 9 = 3.332 N/mm2

(3.55)

2. Circumferential stresses due to pressure are given by: 2 0.0902 1330 = 2 9 = 6.665 N/mm2

(3.56)

3.3.8.2 Dead Weight Stress Dead weight stresses is significant for tall columns. This stress can be tensile for points below the column support or compressive for points above the support. Dead weight stresses are given by: +

(3.57)

3-38 86749 1330 + 9 9

= 2.29 N/mm2 (compressive) 3.3.8.3 Bending Stress The bending stress will be compressive or tensile, depending on location and are given by: + 2

(3.58)

Where, Mx Do = Total bending moment = Outside diameter = Di + 2t = 1330 + 2(9) = 1348 mm Iv = Second moment area = 4 4 64 = 13484 13304 64 = 1.358 x 1011 mm4 162240 1.358 x 1011 1330 + 9 2

(3.59)

= 8.052 x 10-4 N/mm2 3.3.8.4 The Resultant Longitudinal Stress The resultant of longitudinal stress is the summation of longitudinal stresses, dead weight stresses and bending stress. = + For upwind, = 3.332 + (2.29) + 8.052 x 10 = 1.031 N/mm2 (3.60)

3-39 For downwind, = 3.332 + 2.29 8.052 104 = 1.041 N/mm2

Therefore, the greatest difference between the principles stresses, = = 6.665 1.041 = 5.624 N/mm2 The value obtained is well below the maximum allowable design stress which is 115 N/mm2 3.3.8.5 The Resultant Bulking Stress Local bulking will normally occur at stress than that required buckling the complete. A column design must be checked to ensure that the maximum value of the resultant axial stress does not exceed the critical value at which buckling will occur. t Do 9 1348 (3.61)

Critical buckling stress, c = 2 x 104 = 2 x 104

(3.62)

= 133.531 N/mm2

The maximum compressive stress will occur when the vessel is not under pressure + = 2.29 + 8.052 x 10-4 = 2.291 N/mm2

Since the result of maximum compressive stress is below the critical buckling stress of 157.07 N/mm2. Thus, the design is satisfactory. 3.3.9 Vessel Support Design

The method used to support a vessel will depend on the size, shape and weight of the vessel; the design temperature and pressure, the vessel location and arrangement; and the internal and external fittings and attachment. Since the distillation column is a vertical vessel, skirt support is used in this design.

3-40 A skirt support consists of a cylindrical or conical shell welded to the base of the vessel. A flange at the bottom of the skirt transmits the load to the foundations. The skirt may be welded to the bottom, level of the vessel. Skirt supports are recommended for vertical vessels as they do not imposed concentrated loads on the vessel shells; they are particularly suitable for use with tall columns subject to wind loading.

Type of support s Material of construction Design stress, f Youngs modulus Skirt height, hs Skirt thickness, ts Joint factor

= Straight cylindrical skirt = 90 = Carbon Steel = 115 N/mm2 = 200,000 N/mm2 =4m = 9 mm = 0.85

3.3.9.1 Weight of the Skirt Approximate weight, W approx = (/4 x Di2 x Hv) x L x 9.81 = (/4 x 1.332 x 13) x 804.04 x 9.81 = 91 492 N = 91.492 kN

Weight of vessel, W

= 86.749 kN

Total weight

= 91 492 kN + 86.749 kN = 178.241 kN

3.3.9.2 Analysis of Stresses of Skirt

1. Bending moment of skirt, Ms Bending moment at base skirt, Ms = 0.5 x Fw(Hv + Hs)2 = 0.5 x 1.92(13 + 4) = 277.44 kNm
2

(3.63)

3-41 2. Bending stress of skirt, bs , = = 4 + 4 162.24 103 103 1330 + 9 1330 9 (3.64)

= 12.888 N/mm2 3. Dead weight stress in skirt, ws = = ( + ) 152092.43 9(1128 + 9) (3.65)

= 4.731 N/mm2 ( + ) 84749 9(1330 + 9)

= =

(3.66)

= 2.291 N/mm2 4. Resultant stress in skirt, s Maximum s (tensile) = bs + ws test = 12.888 + 2.416 = 15.304 N/mm2 Maximum s (compressive) = bs - ws operating = 12.888 2.291 = 15.179 N/mm2 5. Criteria for Design Take the joint factor, J as 0.85 Where s = 90 s (tensile) 15.304 N/mm2 < < fs J sin s 115 x 0.85 sin 90 (3.67)

(4.68)

3-42 15.304 N/mm2

2 2

<

97.75 N/mm2 0.125 E(ts/Ds) sin s 0.125 x 200000(9/1330) sin 90 169.17 N/mm2

s (compressive) < 15.179 N/mm 15.179 N/mm < <

Both criteria are satisfied, add 2 mm for corrosion; gives a design thickness, ts of 11 mm. The type of this equipment is assumed to be completely satisfactory thus the corrosion rate is 0.25 mm/y. Since the operation of this equipment is assumed to be operated for 20 years, thus the corrosion rate will be added:

0.25 mm/y x 20

= 5 mm

The design thickness must be added with the corrosion rate, gives actual design thickness, ts of 16 mm. 3.3.9.3 Base Ring and Anchor Bolts The loads carried by the skirt are transmitted to the foundation slab by the skirt base ring (bearing plate). The moment produced by wind and other lateral will tend to overturn vessel. A variety of base ring designs is used with skirt supports. The simplest types, suitable for small vessel, are rolled angle. The preliminary design of base ring is done by using Scheimans short cut method. Scheiman gives the following guide rules which can be used for the selection of the anchor bolts. Refer to Coulson and Richardsons, Chemical Engineering, Volume 6, page 848.

1. Bolts smaller than 25 mm diameter should not be used. 2. Minimum number of bolts = 8 3. Use multiple of 4 bolts 4. Bolts pitch should not be less than 600 mm

Pitch circle diameter, Db Closest multiple of 4, Nb

= 3.2 m

Circumference of bolt circle = 2200 = 16 bolts

3-43 Bolt design stress, fb Fw Ms = 125 N/mm2 (Scheiman, 1963) = 1920 N/m = 162.24 kNm

Number of bolts required, at minimum recommended bolt spacing = Circumference of bolt circle / 600 = 2200 / 600 = 11.52 12 bolts 3.2 103 = 773.32 () 13 1 4 1 4 162240 86749 13 125 3.2

, = =

(3.69)

= 71.416mm2 Use M24 bolts (BS 4190:1967) root area = 353 mm2

4 71.416 4

(3.70)

= 9.536 mm

Total compressive load on the base ring per unit length: = 4

2

(3.71)

Where, Fb Ds = the compressive load on the base ring, Newtons per linear metre = skirt diameter, m

3-44 4 162240 86749 + 2 3.0 3.0

= 32.157 kN/m

The minimum width of the base ring: = 1 103 (3.72)

Where, Lb fc = base ring width, mm = the maximum allowable bearing pressure in the concrete foundation pad, which will depend on the mix sed, and will typically range from 3.5 to 7 N/mm2 (500 to 1000 psi) 32157 1 5 103

= 6.4314 mm

This is the minimum width required; actual width will depend on the chair design. Actual width required (Coulson and Richardsons, Chemical Engineering, Volume 6, page 849, figure 13.30) = Lr + ts + 50 mm = 76 + 16 + 50 = 142 mm

Actual bearing pressure on concrete foundation, = 32157 142 103

= 0.226 N/mm2

The minimum thickness is given by, = 3 (3.73)

Where, Lr tb = the distance from the edge of the skirt to the outer edge of the ring, mm = base ring thickness, mm

3-45 fc fr = actual bearing pressure on base, N/mm2 = allowable design stress in the ring material, typically 140 N/mm2

= 76

3 0.226 140

= 5.29 mm

The chair dimensions from figure 13.30 for bolt size M24.

Skirt is to be welded flush with outer diameter of column shell. 3.3.10 Design of Nozzles There are three nozzles in the distillation column, which are nozzles in feed inlet, top product outlet and bottom product outlet. By assuming that the flow of the pipe is turbulent flow, therefore to determine the optimum duct diameter is: Optimum duct diameter, dopt = 293 G0.53-0.37 Where, G = flowrate, kg/s = density, kg/m3 (3.74)

The material construction used for nozzles is carbon steel pipe.

3.3.10.1 G mix dopt

Feed Stream

= 1.587 x 104 kg/h = 4.4083 kg/s = 778.66 kg/m3 = 293 (4.4083)0.53 (778.66)-0.37 = 54.77 mm 55 mm 20 +

, =

3.75

3-46 Where, Ps = operating pressure = design stress at working temperature 0.0902 54.77 20 125 + 0.0902

: =

= 0.002 mm

So, the thickness of nozzle

= corrosion allowance + 0.002 = 2 + 0.002 = 2.002 mm

3.3.10.2 G mix dopt

Top Stream

= 128.5 kg/h = 0.0357 kg/s = 1.709 kg/m3 = 293 (0.0357)0.53 (1.709)-0.37 = 41.08 mm 41 mm 20 + 0.0902 41.08 20 125 + 0.0902

, =

: =

= 0.00148 mm

So, the thickness of nozzle

= corrosion allowance + 0.00148 = 2 + 0.00148 = 2.00148 mm

3-47 3.3.10.3 G mix dopt Bottom Stream

= 1.574 x 104 kg/h = 4.372 kg/s = 695.2 kg/m3 = 293 (4.372)0.53 (695.2)-0.37 = 56.88 mm 60 mm 20 + 0.0902 56.88 20 125 + 0.0902

, =

: =

= 0.0021 mm

So, the thickness of nozzle

= corrosion allowance + 0.0021 = 2 + 0.0021 = 2.0021 mm

3.3.11 Flange Design The flange class number required for a particular duty will depend on the design pressure and temperature and the flange material. The flange design is from the typical standard flange design in Coulson and Richardsons, Chemical Engineering, Volume 6, page 863, figure 13.37.

Table 3.12 The Summary of Flange Design Feed Stream dopt 65 d1 76.1 Flange D 160 b 14 H 32 Raised face d4 110 f 3 Bolting M12 Drilling No 4 d2 14 k 130 Boss d3 100

3-48 Top Stream dopt 25 d1 33.7 Flange D 100 b 14 H 24 Raised face d4 60 f 2 Bolting M10 Drilling No 4 d2 11 k 75 Boss d3 50

Bottom Stream dopt 50 d1 60.3 Flange D 140 b 14 H 28 Raised face d4 90 f 3 Bolting M12 Drilling No 4 d2 14 k 110 Boss d3 80

3.3.12 Summary of Mechanical Design Summary of design distillation column are shown in table below:

Table 3.13 The Summary of Mechanical Design Pressure Vessel Operating Pressure, Po Design Pressure, P1 Operating Temperature Design Temperature Column Material Safety Factor Design Stress Head and Closure Types Crown Radius, Rc Knuckle Radius, Rk Joint Factor, J Cs Minimum thickness, e Column Weight Dead weight of Vessel, Wv Weight of Plates, W p 10.52 kN 32.384 kN Torispherical Head 1.128 m 0.0677 m 1 1.77 10 mm 0.11 N/mm2 0.19 N/mm2 90 oC 99 oC Carbon Steel 10% 115 N/mm2

3-49 Weight of Insulation, W i Total Weight, W t Wind Speed, Uw Bending Moment, Mx Insulation Material Insulation Thickness Skirt Support Type of Support Material of Construction Youngs Modulus Approximate Weight, W approx Total Weight Bending Moment, Mx Skirt Thickness, ts Skirt Height, Hs Stiffness Ring Critical Buckling Pressure for Ring, Pc 140 N/mm2 Straight Cylindrical Skirt Carbon Steel 200,000 N/mm2 152.092 kN 205.844 kN 328.2 kNm 9 mm 4m 5.424 kN 53.752 kN 160 km/h 210.0429 kN/m Mineral Wool 75 mm

3-50 3.4 Costing for Distillation Column

The purchased cost of the equipment is calculated using equation below (Turton et al., Analysis, Synthesis, and Design of Chemical Processess, 3rd Edition, page 906): log10 Cp = K1 + K2 log10 (A) + K3 [log10 (A)]2 where, A K1, K2, K3 = capacity or size parameter for the equipment = constants in Table A.1 (Appendix A) (1.0)

3.4.1

Process Vessels

Column height = 13 m; Column diameter = 1.33 m Material of construction Volume = carbon steel with stainless steel cladding = 2 = (3.142)(1.33)2(13) = 72.25m3

From Table A.1 (Appendix A), K1 = 3.4974, K2 = 0.4485, K3 = 0.1074 log10 Cp = 3.4974 + 0.4485 log10 (72.25) + 0.1074 [log10 (72.25)]2 = 4.73 Cp = $ 53 751.28

Pressure factors for process vessels: For pressure vessel, when t vessel 0.003m,

3-51

+ 1 + 0.00315 2[850 0.6 + 1 ] = 0.003

(2.0)

0.0902 + 1 (1.33) + 0.00315 2[850 0.6 0.0902 + 1 ] = 0.003

, = 8.96 104

The bare module factor for process vessel (Turton et al., Analysis, Synthesis, and Design of Chemical Processess, 3rd Edition, page 927): CBM = CpFBM = Cp(B1 + B2FMFp) (3.0)

From Table A.4 (Appendix A), B1 = 2.25, B2 = 1.82 From Table A.3 (Appendix A), the identification number for carbon steel vertical process vessels is 18.

Hence, from Figure A.18 (Appendix A), material factor, FM = 1.0 CBM = 53751.28 [2.25 + (1.82)(1.0)(8.9610-4)] = $ 121 028.03

Use correlation: CEPCI for year of 2009 is 645.5 CEPCI for year of 2001 is 397 Therefore,

3-52 645.5 297

= 121 028.03 = $ 263042.40

= RM 802 279.32

3.4.2

Sieve Tray

Column height = 13 m; Column diameter = 1.33 m, Area = 5.56 m2; Number of trays = 24 From Table A.1 (Appendix A), K1 = 2.9949, K2 = 0.4465, K3 = 0.3961 log10 Cp = 2.9949+ 0.4465 log10 (5.56) + 0.3961 [log10 (5.56)]2 = 3.92 Cp = $ 8 275.15

The bare module cost for sieve trays (Turton et al., Analysis, Synthesis, and Design of Chemical Processess, 3rd Edition, page 930, Table A.5): CBM = CpNFBMFq Where, N Fq = number of trays = quantity factor for trays (4.0)

For N 20, Fq = 1 From Table A.6 (Appendix A), the identification number for stainless steel sieve trays is 61 Hence, from Figure A.19 (Appendix A), bare module factor, FBM = 1.8

3-53 CBM = (8275.15)(24)(1.8)(1) = $ 208 533.79

Use correlation: CEPCI for year of 2010 is 645.5 CEPCI for year of 2001 is 397 Therefore, = 208 533.79 = $ 453 227.48 = RM 1 382 343.81 645.5 297

Thus, the total cost for distillation column = RM 802 279.32 + RM 1 382 343.81 = RM 2 184 623.13

3-54 REFERENCES

R. K. Sinnot. 2003. Chemical Engineering Design. Vol 6, 3rd Ed, Elsevier Butterworth Heinemann. Felder, R. M. & Rousseau, R. W. 2000. Elementary Principles of Chemical Processes. 3rd Ed, John Wiley & Sons, Inc. Levenspiel, O. 1999. Chemical Reaction Engineering. 3rd. Ed, John Wiley & Sons, Inc. Perry, R. H. & Green, D. W. 1998. Perrys Chemical Engineers Handbook. 7th Ed, McGraw-Hill International Edition.

Walas, S. M. 1988. Chemical Process Equipment. Butterworths Publishers. Ludwig, E. E. 1995. Applied Process Design. Vol.2, 3rd. Ed, Gulf Publishing Company.