DESIGN OF A PACKED DISTILLATION COLUMN

NAME INDEX NO

: Sandaruwan R.A.N. : 090466M

DATE OF SUB: 01 / 08 / 2013

Task identification
According to the determination of packed column height through the number of ideal stages and the HETP value, first the conditions and the objective of the column have to be clarrified using the data provided by the customer. So the required data has been provided as follows.

System: carbon disulphide carbon tetrachloride Feed rate: 45kmol/hr Feed composition: 40mol% carbon disulphide Distillate composition: 90mol% carbon disulphide Bottom product composition: 4mol% carbon disulphide Feed condition: saturated liquid

Selection of packing material Principal requirements of a packing are, Provide a large surface area for high interfacial area between the gas and liquid Have an open structure, so low resistance to gas flow Promote uniform liquid distribution on the packing surface Promote uniform vapour gas flow across the column cross section To satisfy these requirements many diverse types and shapes have been developed. In this distillation column design, berl saddles types rings are used as packing material. Berl saddles were developed to give improved liquid distribution compared to rasching rings. These are the original type of saddle packing. They have a smaller free gas space but their aerodynamic shape is better giving a lower pressure drop and higher capacity. They are usually made up by ceramic or metal or carbon or plastic. The choice of material will depend on the nature of the fluids and the operating temperature. Ceramic packing will be the first choice for corrosive liquids and low cost. Metal packing are usually selected for non corrosive service. They have higher capacity and efficiency. Plastic are normally polypropylene. It is inexpensive and most popular when temperature does not exceed 250F. In the process industries, random packings re more commonly used. So for this design plastic berl saddles are selected and random packing is used. Packing size In general the largest size of packing should be used upto 50mm. small sizes are more expensive than the larger sizes. The size of packing used influences the height and diameter of a column, the pressure drop and cost of packing. When packing size is increased, the cost per unit volume of packing and the pressure drop per unit height of packing are reduced, but in other side which will reduce the mass transfer efficiency. Reduced mass transfer efficiency results in a taller column. Also use of too large a size in a smaller column can cause poor liquid distribution.

In this design packing size is selected as 25mm to maintain the column diameter below 0.3m. Pressure drop across packing Recommended design values, mm water per m packing

According to this, 60mm water per m of packing is selected as pressure drop.

Calculating equilibrium data Equilibrium data calculation for Carbon disulphide Carbon tetrachloride vapour Liquid system According to antion equation = /( + ) Where, A, B, C Vp T - Constants in the antion equation - Vapour pressure (mmHg) - Temperature (K)

Antion constants for Chloroform and Benzene Carbon disulphide (A) 15.9844 2690.85 -31.62 = 46C =77C Carbon tetrachloride (B) 15.8742 2808.19 -45.99

A B C Boling point of Carbon disulphide

Boling point of Carbon tetrachloride From Raouls law, P = Pox Where,

P - Partial pressure

Po Vapour pressure X Molar fraction in the liquid phase Applying Raoults law for A and B; PA = P0AxA PB = PoBxB From Daltons Law; p A + pB = P T Where, PT Total pressure pA + pB = PT = pOAxA + poBxB PT = 750 mm Hg (1bar) xA + xB = 1 pA + pB = PT = p0AxA + poB (1 - xA) P T - p0 B ---------p0A - poB

xA = From Daltons law;

PA = yAPT

yA = (pOA/PT) xA

Sample calculation At 46 C = /( + ) = 15.9844-2690.85/(319-31.62) = 6.621 = 750.695Hgmm = /( + ) =15.8742-28.08.19/(319-45.99) = 5.588 =267.2Hgmm xA = = P T - p0 B ---------p0A - poB 0.998 yA = (pOA/PT) xA =0.999

Equilibrium data

Temperature (C)
46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77

PA
750.71 775.48 800.89 826.95 853.68 881.07 909.15 937.92 967.40 997.59 1028.52 1060.19 1092.61 1125.80 1159.76 1194.52 1230.08 1266.45 1303.64 1341.68 1380.57 1420.32 1460.95 1502.47 1544.89 1588.22 1632.49 1677.69 1723.84 1770.96 1819.06 1868.16

PB
267.25 277.47 288.00 298.86 310.04 321.55 333.41 345.61 358.17 371.09 384.37 398.04 412.09 426.54 441.38 456.63 472.30 488.39 504.92 521.88 539.29 557.16 575.50 594.30 613.59 633.37 653.65 674.44 695.74 717.57 739.93 762.83

XA 1.00 0.95 0.90 0.85 0.81 0.77 0.72 0.68 0.64 0.60 0.57 0.53 0.50 0.46 0.43 0.40 0.37 0.34 0.31 0.28 0.25 0.22 0.20 0.17 0.15 0.12 0.10 0.08 0.05 0.03 0.01 -0.01

YA 1.00 0.98 0.96 0.94 0.92 0.90 0.88 0.85 0.83 0.80 0.78 0.75 0.72 0.69 0.66 0.63 0.60 0.57 0.53 0.50 0.46 0.42 0.38 0.34 0.30 0.26 0.21 0.17 0.12 0.07 0.02 -0.03

Equilibrium curve

Reflux ratio Determination of minimum reflux ratio (Rm) q line equation

yq

q 1 . xq . xf q 1 q 1

Heat required to vapourise 1 mole of feed Molar latent heat of the feed

In this case feed is a saturated liquid so feed is at its boiling point If Feed at boiling point q = 1 and q line is passing through the point of (Xf , Xf) = 0.4

Top operating line equation

y n 1 R 1 .x n .x 1 R 1 R D

But, at minimum reflux ratio we can rewrite top operating line equation as follows,
y n 1 Rm 1 .x n .x 1 Rm 1 Rm D

Top operating line is passing through the point of (XD , XD) XD = 0.9 In minimum reflux ratio intersection of the top operating line and Q line should be at the curve.

According to the graph, Intercept of the top operating line = 0.414 Gradient of the top operating line = 0.54

Therefore

Rm 1 Rm

= 0.54

Minimum reflux ratio, Operating reflux ratio

Rm = 1.174

When we operate high reflux ratio our plates are less than high reflux ratio. Then construction cost is less. But we have to spend lot of money on operating cost and steams. So in industry reflux ratio is between 1.2-1.5 of minimum reflux ratio. Here distill concentration is high so I think operating reflux ratio should be 1.3Rm R = 1.3Rm

Then operating reflux ratio

= 1.3 * 1.174 R = 1.5262

HETP Value For the design of packed distillation columns it is simpler to treat the separation as a stage process and use the concept of the height of an equivalent equilibrium stage to convert the number of ideal stage required to a height of packing. The height of an equivalent equilibrium stage, called height of a theoretical plate (HETP), is the height of packing that will give the same separation as an equilibrium stage. The HETP for a given type and size of packing is essentially constant and independent of the system physical properties.

HETP value for a packing size of 25 mm can be assumed as a 0.46 m.

Number of ideal stages required Then top operating line equation, +1 = 0.6041 + 0.3563 q = 0.4

No of ideal stage required = 12-1 = 11 Feed tray location is above the 5th tray from the top of the tower Column height Column height = number of stages * HETP = 11* 0.46 m = 5.06 m Column height = 5.1m

Column diameter Material balance F=D+W Material balance for carbon disulphide

F. = D + W F. = D + (F-D) D=

( )
45(0.40.04) 0.90.04

D=

kmol/hr

D = 18.837 kmol/hr Then, W = (45 18.837)kmol/hr = 26.163 kmol/hr Material balance for rectifying section

L+D=G

R=

18.837

1.5262 =

L = 28.75 kmol/hr So, 28.75 + 18.375 = G G = 47.125kmol/hr Distillate (D) = 18.837 kmol/hr Down ward liquid flow rate (L) = 28.75 kmol/hr Upward vapour flow rate (G) = 47.125 kmol/hr Material balance for stripping section W + = According to BOL,

+1 =

Gradient = 1.55 and W = 26.163kmol/hr

= 1.55

= 73.732kmol/hr = 73.732 26.163 = 47.569kmol/hr Bottom product (W) = 26.163kmol/hr Upwardvapour flow rate in stripping section ( ) = 47.569kmol/hr section Downward liquid flow rate in stripping ( ) = 73.732kmol/hr

Vapour liquid equilibrium mixture for carbon disulphide and carbon tetrachloride

For rectifying section Composition of the 4th tray (above plate to the feed) 5 = 0.62 4 = 0.43 So, temperature of the 4th tray = 333K Composition of the 1st tray (top plate to the feed) 1 = 0.9 0 = 0.9 Temperature of the 1st tray = 324K Average temperature of the striping section =
333+324 2

= 328.5K Average carbon disulphide composition of vapour (y) = 0.760 Average carbon disulphide composition of liquid (x) = 0.665

Density

Molecular weight of C2 = 0.0761kg/mol Molecular weight of C4 = 0.1538kg/mol For rectifying section, Density of C2 at 328.5K = 1207.566kg/3 Density of C4 at 328.5K = 1526.596 kg/3 For liquid Weight fraction of C2 =
0.6650.0761 0.6650.0761+0.3350.1538

= 0.4955 Basis 1000kg,

0.49551000 Volume of C2 = 1207.566

= 0.413 Volume of C4 =
0.50451000 1526.596

= 0.333 Density of liquid mixture =

1000 0.41+0.33

= 1351.35kg/3 For vapour mixer According to, PV = nRT

Average molecular weight of the vapour stream = 0.760.0761+0.240.1538 = 0.09475kg/mol

110 5 94.75 8.314328.5

Density of vapour mixture = 3.47kg/3 For stripping section Composition of 6th plate (below plate to the feed tray) 6 = 0.58

5 = 0.38 Temperature of the 5th tray = 334 K Composition of 11th plate (lowest plate of tower) 12 = 0.07 11 = 0.06 Temperature of the 11th plate = 347 K Average temperature for stripping section =
334+347 2

= 340.5 K Average carbon disulphide composition of vapour (y) = 0.325 Average carbon disulphide composition of liquid (x) = 0.22 Density of C2 at 340.5K = 1187.885 kg/3 Density of C4 at 340.5K = 1503.208kg/3 Similar to above calculation, For liquid mixer Weight fraction of the C2 = 0.1225 Density of liquid mixture = 1455.8kg/3 For vapour mixer Average molecular weight of the mixer = 0.12855kg/mol Density of vapour mixer = 4.541kg/3

Column diameter for rectifying section Gas flow rate = 47.125 kmol/hr =
47.1250.09475103 3600

kg/s

= 1.24 kg/s Average molecular weight of liquid mixer = 0.6650.0761+ 0.3350.1538 = 0.1021kg/mol Liquid flow rate = 28.75kmol/hr =
28.750.102110 3 3600

kg/s

= 0.8154kg/s Gas density at 328.5K = 3.47kg/3 Liquid density at 328.5K = 1351.35kg/3

= =

3.47 1351.35

0.8154 1.24

= 0.033 Pressure drop correlation graph

Pressure drop = 60mm water per m of packing According to the graph, 4 = 2.2 At flooding, 4 = 5.6 Percentage flooding =
2.2 5.6

= 0 .627

62.7% satisfactory Viscosity calculation

1 Log [viscosity] = [VISA] [

For carbon disulphide VISA = 274.08 VISB = 200.22 T = 328.5k

1 Log [viscosity] = [274.08] [ 328.5

1 200.22

1 = 0.292 mNs/2
For carbon tetrachloride VISA = 540.15 VISB = 290.84 T = 328.5k
1 Log [viscosity] = [540.15] [ 328.5

1 290.84

2 = 0.6125 mNs/2
Average viscosity of mixer

= ( 3 )3 = (0.665 0.2923 + 0.335 0.61253 )3 = 0.3821 mNs/2

1 1

= [

4 ( ) 13.1F ( / )0.1

For this type packing material (plastic), = 170

 = [

2.23.47(1351.35 3.47) 13.1170(0.3821/1351.35)0.1

= 10.46kg/2 Column area required =

1.24 10.46

= 0.11852
4

Diameter =

0.1185

Diameter of the rectifying section= 0.388m

Column diameter for stripping section Gas flow rate = 47.569kmol/hr =

47.5690.1285510 3 3600

kg/s

= 1.7 kg/s Average molecular weight of liquid mixer = 0.220.0761+ 0.780.1538 = 0.1367kg/mol Liquid flow rate = 73.732kmol/hr =
73.7320.136710 3 3600

kg/s

= 2.8kg/s Gas density at 340.5K = 4.541kg/3 Liquid density at 340.5K = 1455.8kg/3

= =

2.8 1.7

4.541 1455.8

= 0.092 From the graph, 4 = 1.6 At flooding, 4 = 3.8 Percentage flooding =

1.6 3.8

= 0 .6488

64.88% satisfactory

Viscosity calculation Similar to above calculation, T = 340.5K For carbon disulphide

1 = 0.273mNs/2
For carbon tetrachloride

2 = 0.536mNs/2
Average viscosity of mixer,

= (0.22 0.2733 + 0.78 0.5363 )3 = 0.468 mNs/2

= [

3.84.541(1455.84.541) 13.1170(0.468/1455.8)0.1

= 24.635kg/2 Column area required =

1.7 24.635

= 0.0692
4

Diameter =

0.069

Diameter of the stripping section= 0.296m

Feed tray location Feed is given to the 7th tray from the bottom, So, it can be assumed as feed is fed into column at 7.5th stage. Height of the feed location from the bottom of column = 7.5*HETP = 3.45 m

Condenser heat load Latent heat calculation

Latent heat of C2 = 351kJ/kg Latent heat of C4 = 194kJ/kg , C2 C4 For top products Temperature of top plate = 322K Carbon disulphide,
552 322 0.38 = 26711.1 [ ] 552 319.3

319.3 349.8 552 556.35

26711.1 29837.2

= 26593kJ/kmol Carbon tetrachloride,

556.35 322 0.38 = 29837.2 [ ] 556.35 349.8

= 31303.8kJ/kmol Latent heat of mixtures

For rectifying section, , = 265930.9 + 31303.80.1 = 27064.08 kJ/kmol Therefore condenser heat load = G , = 47.12527064.08 = 1275.4MJ/hr

= 354.3kW Boiler heat load calculation Using equation, , + W = 1 , 1 + = + =

2 (1 1

+ 2 + 3 2 + 4 3 ) 4 -0.001452 0.034455

1 2 3 85600 -122 0.5605 C2 -752700 8966.1 -30.394 C4 Average temperature of stripping section, T = 340.5K Calculating the latent heat of mixture For stripping section Temperature of bottom plate = 348K

For Carbon disulphide, = =

2 (1 1

+ 2 + 3 2 + 4 3 ) 122T + 0.5605 2 0.001452 3 )

340 .5 (85600 298

= 2397.325kJ/kmol

552 340.5 0.38 = 26711.1 [ ] 552 319.3

= 25758.8kJ/kmol

Carbon tetrachloride, =
340 .5 (752700 + 298

8966.1T 30.394 2 + 0.034455 3 )

= 5671.523kJ/kmol

556.35 340.5 0.38 = 29837.2 [ ] 556.35 349.8

= 30340.7kJ/kmol

For stripping section, , = 25758.80.22 +30340.70.78 Latent heat of mixture = 29332.7 kJ/kmol Enthalpy of liquid mixture( , ) = 2397.3250.22 + 5671.5230.78 = 4951.2 kJ/kmol Enthalpy of carbon disulphide, = 2397.325 + 29332.7 = 31730kJ/kmol Enthalpy of carbon disulphide, = 5671.523 + 29332.7 = 35004.2kJ/kmol Enthalpy of vapour mixture ( , ) = 317300.325 + 35004.20.675 = 33940.1 kJ/kmol

For bottom product (residue), Temperature = 348K For Carbon disulphide, =

348 (85600 298

122T + 0.5605 2 0.001452 3 )

= 2778.2kJ/kmol Carbon tetrachloride, =

348 (752700 + 298

8966.1T 30.394 2 + 0.034455 3 )

= 6703.6kJ/kmol

Enthalpy of liquid mixture of residue( ) = 2778.2 0.04 + 6703.60.96 = 6546 kJ/kmol

Substituting to equation, , + W = 1 , 1 + 47.56933940.1 + 26.1636546 = 73.7324951.2 + = 1420.7MJ/hr = 394.6kW Heat load of the reboiler = 394.6kW

Final data Packing material Packing size Pressure drop Reflux ratio Number of ideal stages Column height Diameter of rectifying Diameter of stripping Feed tray location Condenser heat load Reboiler heat load plastic 25mm 62water mm/ m of packing 1.5262 11 5.1m 0.388m 0.296m 3.45m from bottom 354.3kW 394.6kW

Referencess http://www.engineeringtoolbox.com/fluids-evaporation-latent-heat-d_147.html http://www.britannica.com/EBchecked/topic/94993/carbon-disulfide-CS2 http://encyclopedia2.thefreedictionary.com/Carbon+Tetrachloride CULSON & RICHARDSONS, CHEMICAL ENGINEERING, Volume 6, 3 rd edition, R K Sinnott CULSON & RICHARDSONS, CHEMICAL ENGINEERING, Volume 2, 5 th edition PERRYS CHEMICAL ENGINEERS HAND BOOK, 8th edition, DON W. GREEN, ROBERT H. PERRY DISTILLATION DESIGN, HENRY Z. KISTER