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INTRODUCTION
Distillation is one of the separation method used in the chemical industry to separate the
mixtures of a liquid and gaseous solution. The separation process is depends on the
differences in the volatilities in a boiling liquid mixture. Distillation is only takes part in the
physical separation process and does not involve any chemical reaction.
A design consists of chemical and mechanical evaluation to calculate for total stages,
height, thickness, support, as well as the insulation. A key in distillation process is relative
volatility, α.
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:
4. Determine the stage and reflux requirements: the number of equilibrium stages
CHEMICAL DESIGN
The purpose of this distillation column is to separate the component mixture. Basically,
components which are methanol, water and Formaldehyde are to be separated to the
bottom stream. These components will go through another seperation process. The feed is
fed to the distillation column at 350 kPa and 365.78K. The products at the top column leave
the column at 250 kPa and 366.58K. The products at the bottom column leave the column at
300 kPa and 412.95K. Methanol and Formaldehyde were chosen as the key components
being Methanol as the light key component while Formaldehyde 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.
COMPLETE DIAGRAM
The composition of the inlet and outlet streams for distillation column is shown in table 3.1:
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.
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
COMPONENT a b C d E
𝐵
ln 𝑃0 = 𝐴 − + 𝐶𝑥 ln 𝑇 + 𝐷𝑥𝑇^𝐸 (3.3)
𝑇
𝑃0
𝐾𝑖 = (3.4)
𝑃𝑟
TBubble(guess) = 367 K
PT = 350 kPa
Psat yi Psat yi
Notes: The satisfactory Tbubble is obtained using Goal Seek operation in Microsoft Excel
TBubble(guess) = 369 K
PT = 250 kPa
Psat yi Psat yi
Notes: The satisfactory Tbubble is obtained using Goal Seek operation in Microsoft Excel
TBubble(guess) = 412.95 K
PT = 300 kPa
Psat yi Psat yi
Notes: The satisfactory Tbubble is obtained using Goal Seek operation in Microsoft Excel
𝑦𝑖 𝑃𝑠𝑎𝑡,𝐼
𝐾𝑖 = =
𝑥𝑖 𝑃𝑟
Where Psat,I = saturated pressure of component, i
PT = total pressure
At feed, stream 16
COMPONENT xi,f yi Ki
At top, stream 19
COMPONENT xi,f yi Ki
Formaldehyde - - 0
At bottom, stream 18
COMPONENT xi,f yi Ki
Methanol 0.0050 0.0005 0.1000
0.6250 0.1747
Water 0.1092
𝐾
∝𝑖𝑗 = 𝐾𝑖 (3.6)
𝑗
𝑃𝑖 = 𝑃𝑖 𝑋𝑖 (3.7)
The relative volatility of two components can be expressed as the ratio of their K value,
𝐾
∝𝑖𝑗 = 𝐾 𝐿𝐾
𝐻𝐾
Component Ki 𝜶𝑳𝑲,𝑯𝑲
Component Ki 𝜶𝑳𝑲,𝑯𝑲
Formaldehyde 2.4068 1
The following approximation may be used to calculate the average relative volatility
𝛼𝑎𝑣𝑔 = 3√𝛼𝑓 𝛼𝑡 𝛼𝑏
Therefore
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:
𝛼𝑖 𝑥𝑖,𝑓
∑ = 𝑅𝑚 + 1 (3.10)
𝛼𝑖 −𝜃
Where,
αi = the relative volatility of component i with respect to some reference component,
usually the heavy key
Rm = the minimum reflux ratio
Xi,d = concentration of component i in the tops at minimum reflux
and θ is the root of the equation:
𝛼𝑖 𝑥𝑖,𝑓
∑ =1−𝑞 (3.11)
𝛼𝑖 −𝜃
where,
The value of θ must satisfy the relation αHK < θ < αLK. By assuming the feed is enter at its
boiling where q = 1, the value of θ is determined using goal seek in excel application.
𝛼𝑥
By using goal seek, θ = 1.8456 when ∑ 𝛼𝑖 −𝜃
𝑖,𝑓
=0
𝑖
Formaldehyde
1.0000 0.3221 0.3221 0.3950
Water
0.0701 0.5723 0.0401 -0.3505
∑[αxr /α-θ]
0.000143
The value of θ is then substitute in to the equation as below
𝛼𝑖 𝑥𝑖,𝑓
∑ = 𝑅𝑚 + 1
𝛼𝑖 − 𝜃
Formaldehyde
1.0 0.0001 0.0001 0.0001
Water
1.9795 0.3000 0.59385 1.3305
Therefore,
𝑅𝑚 + 1 = 3.3553
𝑅𝑚 = 2.3554
Therefore, by Goal seek operation in Microsoft Office Execl, the minimum reflux ratio is
determined to be 2.3554.
Minimum number of stages by Winn’s method
𝑛+2
3.5 69.6826 2.007 188.314 1−2.007
1.5828 =( )( ) ( )
0.9417 1.5 5
𝑛 + 2 = 9.678 = 10 𝑠𝑡𝑎𝑔𝑒𝑠
Therefore the minimum number of theoretical stages is determined to be 10 stages
using Winn’s methods.
Column Efficiency
The prediction of overall column efficiency can be obtained from the correlation given by
O’Connell below:
𝐸𝑜 = 51 − 32.5 log(𝜇𝑎 𝛼𝑎 )
Where μa = the molar average of liquid viscosity, mNs/m2
αa = average relative volatilities of the light key
Physical Properties
= 23.3682 kg/kmole
= 27.8342 kg/kmole
= 22.5230 kg/kmole
Calculation of Density
At top,
Liquid Density, ρL = ∑ xi ρi
ρL =596.9082 kg/m3
𝑅𝑀𝑀 𝑇𝑆𝑇𝑃 𝑃
Vapor Density, ρV = 𝑉 × 𝑇
×𝑃
𝑆𝑇𝑃 𝑆𝑇𝑃
ρV =2.2832 kg/m3
At bottom,
Liquid Density, ρL = ∑ xi ρi
ρL =927.425 kg/m3
𝑅𝑀𝑀 𝑇𝑆𝑇𝑃 𝑃
Vapor Density, ρV = × ×
𝑉𝑆𝑇𝑃 𝑇 𝑃𝑆𝑇𝑃
ρV =1.9681 kg/m3
Liquid and Vapor Flowrates
Liquid Rate:
𝑉𝑛 = 𝐿𝑛 + 𝐷
𝐿𝑛 = 𝑉𝑛 − 𝐷
=16.777-5
=11.777 kmole/h
Liquid Rate:
𝐿𝑚 = 𝐿𝑛 + 𝐹
=11.777+216,3314
=228.1084 kmole/h
Vapor Rate:
𝑉𝑚 = 𝐿𝑚 − 𝑊
=228.1084 − 188.3314
=39.777 kmole/h
Column Diameter
There are several approaches to column diameter design. In general, a better approximation
is based on flooding considerations. The flooding velocity can be determined using the
correlation given by Fair in 1961
𝜌𝐿 − 𝜌𝑉
𝑢𝑓 = 𝐾1 √
𝜌𝑉
𝐿𝑊 𝜌𝑉
𝐹𝐿𝑉 = √
𝑉𝑊 𝜌𝐿
𝐿𝑚 𝜌𝑉 228.1084 1.9681
𝐵𝑜𝑡𝑡𝑜𝑚 𝐹𝐿𝑉 = √ = √
𝑉𝑚 𝜌𝐿 39.777 927.425
𝐿𝑛 𝜌𝑉 11.77 2,2832
𝑇𝑜𝑝 𝐹𝐿𝑉 = √ = √
𝑉𝑛 𝜌𝐿 16.77 596.9082
Therefore
927.425-1.9681
Bottom, uf = 0.20√ = 4.3369 m/s
1.9681
596.9082-2.2832
Top, uf = 0.21√ = 3.3889 m/s
2.2832
For design, assumption of 85 per cent of the flooding velocity is used
Bottom 𝑢̂𝑣 = 4.3369 × 0.85 =3.1334 m/s
Top 𝑢̂𝑣 = 3.3889 × 0.85 =2.8805 m/s
Maximum volumetric flow rate
Vm RMM
𝐵𝑜𝑡𝑡𝑜𝑚 =
ρV
39.77×22.5329
=
1.9681
= 12.6487 𝑚3 /𝑠
Vn RMM
𝑇𝑜𝑝 =
ρV
16.77×27.8342
=
2.2832
= 8.5184 𝑚3 /𝑠
As a first trial take the downcomer area as 12 per cent of the total
4.0367
𝐵𝑜𝑡𝑡𝑜𝑚𝐴𝑑 = = 4.5872 𝑚2
0.88
2.9573
𝑇𝑜𝑝𝐴𝑑 = = 3.3606 𝑚2
0.88
4𝐴𝑑
𝐷=√
𝜋
4 × 4.5872
𝐵𝑜𝑡𝑡𝑜𝑚 𝐷 = √ = 2.4167 𝑚
𝜋
4 × 3.3606
𝑇𝑜𝑝 𝐷 = √ = 2.0685 𝑚
𝜋
An initial selection of plate type either reverse, single pass or multiple pass can be
determined using the theory proposed by Huang and Hodson (1958). The selection will
depend on the liquid flow rate and column diameter.
Based on the graph by Huang and Hodson (1958), at liquid flow rate = 0.02188 m3/s
and Dc = 2.5 m a single pass (cross flow) can be used.
Provisional Plate Design
Net Area, An = AC - Ad
= 4.9087 – 0.5890
= 4.3196 m2
Hole area Ah
Take as 10 per cent of Aa = 0.10 × 3.7307
= 0.3730 m2
Weir Dimension
Weir Length
By referring to the figure in Appendix, the relationship between weir length and newcomer
could be seen.
The y-axis
𝐴𝑑 0.5890
× 100 = × 100 = 11.99
𝐴𝑥 4.9087
From the Appendix, the weir length can be determine as below
𝐼𝑤
= 0.74
𝐷𝑐
𝐼𝑤
= 0.74
2.5
𝐼𝑤 = 1.85 𝑚
Weir Height
Hole Diameter
The holes are made by drilling or punching. Punching would be cheaper than drilling,
however the minimum size of hole that can be punched will depend on the plate thickness.
The preferred hole diameter is 5mm. Typical plate thicknesses used for design are 5 mm for
carbon steel and 3 mm for stainless steel.
The height of weir liquid crest can be determined using the Francis weir formula as below
2
𝐿𝑤 3
ℎ𝑜𝑤 = 750 ( )
𝜌𝐿 𝐼𝑤
Where ℎ𝑜𝑤 = weir crest, mm liquid
𝐿𝑤 = liquid flow rate, kg/s
𝐼𝑤 = weir length, m
228.1084 × 22.5329
𝑀𝑎𝑥𝑖𝑚𝑢𝑚 𝐿𝑤 = = 1.4277 𝑘𝑔/𝑠
3600
Minimum 𝐿𝑤 at 70 per cent turn down = 0.70 × 1.4277 = 0.9994 kg/s
Therefore
2
1.4277 3
𝑀𝑎𝑥𝑖𝑚𝑢𝑚 ℎ𝑜𝑤 = 750 ( ) = 6.6352 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
927.425 × 1.85
2
0.9994 3
𝑀𝑎𝑥𝑖𝑚𝑢𝑚 ℎ𝑜𝑤 = 750 ( ) = 5.2310 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
927.425 × 1.85
Check Weeping
The weep point is considered to be the minimum vapor velocity that will provide a stable tray
operation, preventing liquid from passing through the holes and bypassing the overflow weir
and downcomer. The minimum vapor velocity can be estimated using correlation given by
Eduljee in 1959
(𝐾2 − 0.90)(25.4 − 𝑑ℎ )
𝑢̂ℎ =
𝜌𝑣 1/2
Where 𝑢̂ℎ = minimum vapor velocity through the holes, m/s
𝑑ℎ = hole diameter, mm
𝐾2 = constant, dependent on the depth of clear liquid on the plate
At minimum rate
ℎ𝑤 + ℎ𝑜𝑤 = 45 + 5.2310 = 50.2310 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
From appendix,
𝐾2 = 30.25
Therefore,
(30.25 − 0.90)(25.4 − 5)
𝑢̂ℎ (min) = 1 = 8.8259 𝑚/𝑠
1.96812
Actual minimum vapor velocity
𝑚𝑖𝑛𝑖𝑚𝑢𝑚 𝑣𝑎𝑝𝑜𝑟 𝑟𝑎𝑡𝑒
𝑢̂ℎ =
𝐴ℎ
12.6487 × 0.7
𝑢̂ℎ =
0.3730
𝑢̂ℎ = 23.7375 𝑚/𝑠
Therefore, the actual minimum vapor velocity is calculated to be 23.7375 m/s which is above
the minimum vapor velocity pf 8.8259 m/s. This indicates that the minimum operating rate
will be well above weep point.
Plate Pressure Drop
The total pressure drop is taken as the sum of the dry plate drop (hd) the head of clear liquid
on the plate (hw + how and residual head hr)
The pressure drop calculated for the flow of vapor through the dry plate can be calculated as
below
𝑢̂ℎ 2 𝜌𝑣
ℎ𝑑 = 51 ( )
𝐶0 𝜌𝐿
Where
hd = dry plate drop, mm liquid
û h = velocity through the holes, m/s
C0 = orifice coefficient
Maximum vapor velocity through holes
12.6487
𝑢̂ℎ = = 33.9107 𝑚/𝑠
0.3730
The value of C0 can be obtained from Appendix
𝐴ℎ 0.3730
× 100 = × 100 = 9.9981
𝐴𝑎 3.7307
𝑃𝑙𝑎𝑡𝑒 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠, 𝑡𝑝 5
= =1
𝐻𝑜𝑙𝑒 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟, 𝑑ℎ 5
Therefore
𝐶0 = 0.84
33.9107 2 1.9681
ℎ𝑑 = 51 ( ) = 176.381 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
0.84 927.425
Residual Head
The residual head can be estimated the simple equation proposed by Hunt (1955). The
equation is defined the residual drop as a fixed value of 12.5 mm of water.
The downcomer from a tray must be adequate to carry the liquid flow plus entrained foam
and froth. The area of the downcomer and plate spacing must be such that the level of the
liquid and froth in the downcomer is kept below the top of the outlet weir on the plate above
otherwise the column will flood. In terms of clear liquid the downcomer backup can
expressed as below
ℎ𝑏 = (ℎ𝑤 + ℎ𝑜𝑤 ) + ℎ𝑡 + ℎ𝑑𝑐
Where
hb = downcomer back-up, measured from plate surface, mm
hdc = head loss in the downcomer, mm
The head loss in the downcomer is given by
𝑙𝑤𝑑 2
ℎ𝑑𝑐 = 166 ( )
𝜌𝐿 𝐴𝑚
Where
lwd = liquid flow rate in downcomer, kg/s
Am = either the downcomer area Ad or the clearance area under the downcomer
Aap, whichever is the smaller, m2
The clearance area is given by
𝐴𝑎𝑝 = ℎ𝑎𝑝 𝐼𝑤
Where
hap = height of the bottom edge of the apron above the plate
= hw – (5 to 10) mm
Take
ℎ𝑎𝑝 = ℎ𝑤 − 10
ℎ𝑎𝑝 = 45 − 10 = 35 𝑚𝑚
Area under apron
𝐴𝑎𝑝 = 35 × 103 × 1.85 = 0.0647 𝑚𝑚2
Since Aap is smaller than Ad the value of Aap = 0.0647 m2 is used to calculate hdc
2
1.4277
ℎ𝑑𝑐 = 166 ( ) = 93.9757 𝑚𝑚
927.425 × 0.0647
Backup in downcomer
ℎ𝑏 = (50.2310) + 240.09 + 0.0939 = 0.290 𝑚
Check residence time
0.0647 × 3.7307 × 927.425
𝑡𝑟 = = 380 𝑠
0.5890
Since it falls under recommended value which is more than 3 seconds, the residence time of
380 s sufficient for the entrained vapor to disengage from the liquid in order to prevent
heavily aerated liquid being carried under the downcomer.
Check Entrainment
Actual velocity
12.6487 𝑚
𝑢𝑛 = = 2.9282
4.3196 𝑠
From Appendix, at percent flooding 86.41% and FLV = 0.043 the fractional flooding, Ψ =
0.089 which is well below 0.1. It must be below 0.1 because below this figure the effect
on efficiency will be small.
Perforated Area
86
Mean length, unperforated edge strips = (2.5 − 50 × 10−3 )𝜋 × 180 = 3.5919 𝑚
94
Mean length of calming zone = (2.5 − 50 × 10−3 ) × sin 2
= 1.7918 𝑚
Generally, T-101 is a 10 stages tray column with valve trays as plate contactor and employs
stainless steel as a material of construction. T-101 is determined to be 2.5 in diameter and 6
m in height. Others calculated design values can be summarized into Table