BACHELOR OF CHEMICAL ENGINEERING (HONS)

LAB REPORT SUBMISSION FORM

EKC 2131 CHEMICAL ENGINEERING LAB III
NAME Nisha Fareena Khan ID 1102171011
EXPERIMENT NO. & TITLE SIEVE PLATE DISTILLATION COLUMN
EXP 5
WEEK OF EXPERIMENT 3
DATE OF EXPERIMENT 12/11/2019
DATE OF SUBMISSION 19/11/2019

NAME OF GROUP MEMBERS ID

Nisha fareena Khan 1102171011
Mathaneshan Rajagopal 1103173003

MARKING SIGNATURES
DETAILS TOTAL MARKS
AWARDED
Attitude 5
Participation 5
CHEMICAL ENGINEERING LAB III
Lab Report 40 INCHARGE
(DR. PADMESH/MS. MADIHAH MISKAN)
Total 50

On-time submission Late submission

Table of Content

1. Abstract ………………………………………………………. 2
2. Objective ………………………………………………………. 3
3. Introduction …………………………………………………….. 3-6
4. Procedure …………………………………………………….7-10
5. Result and Discussion …………………………………………..11-13
6. Conclusion and Recommendation ………………………………14
7. References …………………………………………………..15
8. Appendix …………………………………………………..16-20

1
1.0.Abstract

Distillation is the dominant separation technology in chemical industries despite its huge
energy consumption. Distillation consumes about 3% of the total energy consumed globally.
In this experiment we discuss Sieve plates distillation columns. The main objectives of this
experiment is to study the operation of packed bed distillation column, and to operate the
column under total reflux of 4:15 and 10:15, desired reflux condition using Rayleigh’s,
Fenske’s and Mc-Cabe Thiele’s methods. Different compositions of the top, bottom and the
feed distillates are obtained during the experiment for the different reflux ratios and total reflux
condition. For the total reflux the number of stages obtained are 2.14, following up with the
4:15 reflux having 6.23 stages and 10:15 having 3.5 number of stages. This results directly
shows that the greater the reflux ratio the lesser will be the number of stages. Using Frenske’s
equation the number of stages are 1.784 which are approximately equal to the total reflux
condition. The refractive index for the feed is 1.326 that gives the composition of 0.23. For the
molar feed F through Rayleigh’s equation is 0.0495kmol, B is 0.023kmol and D is 0.027kmol.
The value of q obtain is calculated to be 1.108 and the ROL for both the desired reflux are to
be 0.57 and 0.35 respectively. The actual number of stages in the equipment are 7 that give us
the efficiency of 30.57 with the total reflux condition.

2
2.0.Objective:
1. To study the operation of a packed bed distillation column.
2. To verify the rayleigh equation.
3. To obtain the T-x data under total reflux condition at steady state and compare it
with theoretical value.
4. To operate the column under total reflux condition and calculate the minimum
number of theoretical stages using fenske’s equation.
5. To operate the column under any desired reflux condition and calculate theoretical
number of stages using Mc-Cabe Thiele’s method.
6. To calculate the overall efficiency of the sieve plate distillation column.

3.0.Introduction:
1. Principles:

Distillation is a method of separating the components of a solution which depends upon

the distribution of the substances between a gas and a liquid phase. It is called as ‘the workhorse
of chemical industries’. This process separates mixture into two or more products that consist
of different boiling points. This is done through vaporization when the two or more products
have different boiling points. Therefore the liquid phase is richer in less volatile components
that has high boiling point and the vapour phase is richer is high volatile components that has
low boing boiling point. Distillation is the most common process in an industry as it has an
efficiency of 90% in separation processes.

Transport of more volatile component occurs from liquid to vapour phase while
transport of less volatile component occurs from vapour to liquid phase. Thus, distillation
column involves counter-diffusion of components not necessarily to be equimolar. A typical
distillation column consist of five sections that will break down to enriching section, stripping
section, feed entry, reflux and recycle. A distillation column may consist of different type of
packing material whereby in this experiment sieve tray are discussed.

Sieve trays are used in gas absorption and in distillation. A typical example of Sieve
tray is shown in figure 3.1. In the sieve tray, vapour bubbles up through simple holes in the
tray through the flowing liquid. The opening hole sizes in the plates range from 3 to 12 mm in
diameter, with 5 mm a common size. The vapour area of the holes varies between 5 to 15% of
the tray area. The liquid is maintained on the tray’s surface and prevented from flowing down

3
through the holes by the kinetic energy of the gas or vapour. The depth of liquid on the tray is
maintained by an overflow, outlet weir. The overflow liquid flows into the downspout to the
next tray below (Geankoplis, C. J, 1993, p611)

Figure 3.1: Sieve Tray used in distillation column.

Sieve trays are shown in the figure 3.2 where they are the least expensive tray option.
In sieve trays, vapour flowing up through the tower contacts the liquid by passing through
small perforations in the tray floor. Sieve trays rely on vapour velocity to exclude liquid from
falling through the perforations in the tray floor. If the vapour velocity is much lower than
design, liquid will begin to flow through the perforations rather than into the down-comer. This
condition is known as weeping. Where weeping is severe, the equilibrium efficiency will be
very low. For this reason, sieve trays have a very small turndown ratio (Sciencedirect, 2014,
Sieve-tray).

Figure 3.2: Vapor flow through trays. Vapor flow through (a) bubble cap, (b) perforations,
and (c) valves.

4
 The figure 3.3 shows a Sieve plate in normal operation. The down-comers are the
segment shaped region between the curved wall of the column and the straight chord of weir.
Each column usually occupies 10-15 percent of the column cross section leaving 70-80 percent
of the column are for bubbling or contacting. For small columns the down-comers might be
welded to the plate and projecting up above the plate to form a circular weir. For very large
columns the additional down-comers might be in the middle of the plate to decrease the length
of the liquid flow path. In some cases a underflow weir or a tray inlet weir is installed as shown
in figure 3.3 to improve liquid distribution and to improve vapour bubble from entering the
down-comers (McCabe_W.L._Smith_J.C._Harriott_P, 1993, p561).

Figure 3.3: Operation of Sieve plate.

5
2. Application:

1. The sieve tray has been in the distillation market place for many decades. It has
been used extensively in distillation columns worldwide as a highly efficient
vapour-liquid-contacting device.
2. Distillation plants supply water to areas that have scarcity of water by purification.
3. Liquor, wine and beer are produced by means of distillation.
4. Cosmetic product, pharmaceutical product, and chemical products if on a small
scale are produced using packed bed distillation.

3. Advantages and Disadvantages:

Advantages Disadvantages
1. Sieve plates are the least expensive 1. Higher pressure drops than packed
tray options. columns
2. The liquid-vapour contact in the cross- 2. Foaming can occur because the liquid
flow operation is more effective than is agitated by the vapour flowing up
cross-flow operations in packed through it.
columns. 3. Sieve trays are not suitable for
3. Cooling coils can be easily added to fouling service.
the plate column. 4. Low pressure drop as compare to
4. Sieve plates can handle high liquid other tray columns.
flow rates. (Trayus, 2009 ,Sieve-Bubblecap-trays)

6
4.0.Procedure
4.1.Opening Procedure
1. A standard curve of x vs R.I at methanol water ratio from 0 – 1 was prepared.
2. The volume of water and methanol was noted down.
3. All the valve V1-V16 were kept in closed position.
4. Switches on the panel were at OFF position.
5. Water was filled in the cold water tank.
6. The reboiler was filled with methanol-water solution with 2L of methanol and 13L
of water, valve V1 and air vent valve V2 were opened.
7. After on valve V1 and V2 were closed.
8. Electric supply was connected to set up.
9. The process temperature was set at 95°C.
10. The heater and cooling water pump were started.
11. The cold water flow rate valve V3 was adjusted to a moderate value.
12. Cyclic timer for total reflux was set.
13. Waiting time was 25-30 minute for the system to achieve steady state.
14. The samples were taken from the bottom & distillate stream.
15. Samples were cooled down to room temperature in order to measure the refractive
indices.
16. Refractive indices of samples at different temperatures were measured.
17. The temperature and refractive indices were noted.
18. The cyclic timer was adjusted to a desired reflux ration and for 3-5 min.
19. The samples from both distillate and bottom product were taken out.
20. Samples were cooled down to room temperature and refractive indices were
measured.
21. Refractive indices of samples at different temperatures were measured.
22. The refractive indices were measured.
23. The experiment for different set point temperatures and reflux ratios was repeated.
4.2.Closing Procedure:
1. When the experiment was over water supply was shut down.
2. The pump, heater, and main power supply were Switch OFF.
3. The column, reflux drum and receiving tank were drained.

7
 Figure 4.1 shows the block diagram of Sieve plate distillation column. The set-up
consists of a column, which is has sieve plates inside with holes diameter ranging from 3-
12mm. Valve V2-V9 are provided for each tray segment. An electric heater is installed at
the bottom of the column. A tank is provided to collect the bottom product. Shell and tube
type condenser is provided to condensate the vapour. A tank with pump and rota-meter is
provided for circulation of cooling water. Reflux drum is provided to collect the
condensate. Receiving tank is for collecting the distillate. Drain valves are provided for
drainage purposes.

Figure 4.1: Block diagram of Sieve plate distillation column.

8
 4.3.Formulas Used:

Rayleigh’s Equation

It is used to find the Feed composition or composition of the bottom distillate. For batch
distillation process where a fixed quantity of feed is charged to the distillation column and
separation of volatile products is done by supplying heat through the still or reboiler. As the
boiling point of liquid is reached a portion of liquid starts to vaporize to the top of the column
and directed to the condenser, the vapor leaving the column is always in equilibrium with the
liquid in the bottom of the column, thus a material balance equation is produced by Rayleigh
called Rayleigh Equation which provides standard equilibrium data (Neutrium, 2016,
Distillation).

Fenske’s Equation

The Fenske equation in continuous fractional distillation is an equation used for calculating the
minimum number of theoretical plates required for the separation of a binary feed stream by
a fractionation column that is being operated at total reflux (i.e., which means that no overhead
product distillate is being withdrawn from the column).

9
Mc-Cabe Thiele’s method

To calculate the slope of the feed line.

Fraction of liquid in the feed.

y = ( q/ q − 1 ) x – (xF /(q – 1)) To calculate the q-line.

ROL=xd/R+1 Rectifying operating line(y-intercept).

Efficiency:

For the composition of total reflux values:

𝑁𝑡ℎ𝑒𝑜
ή=𝑁𝑎𝑐𝑡𝑢𝑎𝑙 𝑥100

10
 5. Result and Discussion

The McCabe-Thiele method uses the equilibrium curve diagram to determine the number
of theoretical stages require to achieve a desired degree of separation. The main information
required are the feed conditions, distillate, feed composition, and the bottom composition and
reflux ratio (Neutrium, 2016, Distillation). If a column is designed to follow the MaCabe-
Thiele’s method for separation of a binary mixture where the feed has concentration of xf, the
bottom distillate has a concentration of xw, and the top distillate has a composition of xd. The
method involves plotting the diagram into 3 sections the rectifying section operating line
(ROL), the feed line and the stripping section line (SOL). The number of theoretical stages can
be determine from the number of triangles that can be drawn between the operating lines.
Following the relation of R is inversely proportional to the number of stages, which means that
the greater the Reflux ratio the lesser will be the no of stages involved.

In this experiment 3 different reflux ratio were tested out one was the total reflux, following
by the 4:15 reflux and 10:15 reflux. The graph 5.4 shows the total reflux whereby the
composition of the feed xf obtained is 0.23, composition of the distillate xd obtained is 0.63,
and the composition of bottom reflux xw is 0.07. With the following composition line are
plotted on the equilibrium curve where the number of stages are plotted using McCabe-Thiele’s
method. The composition of the following date were obtained from the calibration data plotted
on graph 5.1. The table 5.2 shows the calibration data obtained by taking down the RI values
of different mixtures of methanol and water. From the calibration graph the values of different
compositions can be obtain. The deviations in the curve or the calibration chart is due to error
in measurement and error in equipment therefore the readings consist of instrumental and
graphical error.

Tthe 100 96.4 93.5 91.2 89.3 87.7 84.4 81.7 78.0 75.3 73.1 71.2 69.3 67.5 66.0 65.0 64.5

Xthe 0 0.02 0.04 0.06 0.08 0.1 0.15 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 0.95 1.0

Ythe 0 0.134 0.23 0.304 0.365 0.418 0.517 0.579 0.665 0.729 0.779 0.825 0.87 0.915 0.958 0.979 1.0

Table 5.2: T-x-y date for ethanol water system.

11
 The number of stages obtained from the total reflux graph are 2.14 stages for the total
reflux. Furthermore in the second experiment the reflux ratio taken was 4:15 and after 15
minutes the distillate from the top and bottom obtain had a composition of xd 0.73 and xw 0.07
respectively. The compositions were taken from the graph 5.1. From the graph 5.5 the
compositions are marked on the diagonal of the equilibrium curve. From the graph 5.3 the
boiling point with respect to the composition of the feed is obtain that comes out to be 80.5⁰C,
from the boiling point the average temperature is obtain that comes out to be 52.75⁰C. From
the boiling point the latent heat of methanol and water is obtained. However, from the average
temperature the heat capacity is obtained. The value of q is obtain from the latent heat and the
heat capacity. The value of q is obtain is 1.108 where the q line is obtain to be y = 10.25x –
2.12, the slope is positive. The ROL obtain is 0.57 where the point xd cuts the y-intercept at
0.57. The slope obtain is a positive slope and passes through a point 0.958 when the x-intercept
is 0.3. At the reflux 4:15 the number of stages obtain are 6.23 stages.

In the graph 5.6 the reflux is 10:15 has a feed composition xf of 0.23, top distillate xd
is 0.58 and bottom distillate xw is 0.04. The points are marked on the diagonal of the
equilibrium curve. From point xf the point q is drawn till it cuts the equilibrium line at 0.958
with the x-intercept at 0.3. The point q obtain is 1.108 and the value of reflux R is 0.667.
Therefore the y-intercept obtain is 0.35. The q line is obtain to be y = 10.25x – 2.12 with a
positive slope. The number of stages obtain with the reflux 10:15 are 3.5 stages that are much
lesser then the 4:15 reflux which are 6.23 stages which shows that the reflux R is inversely
proportional to the number of stages. The lesser the reflux, the greater the number of stages
obtain.

The basic steps that are involved in McCabe-Thiele’s method are break down to:

1. Points 𝑥𝐹 , 𝑥𝐷 and 𝑥𝐹 were marked on the diagonal of the equilibrium curve.

2. From 𝑥𝐹 , the q line was drawn till it cut the equilibrium at A.
3. Points 𝑥𝐷 and A were joined and extended till the y-axis.
4. The value of q obtain was 1.108. And the y line is 10.26x-2.12.
5. On putting value of 𝑥𝐷, we get, R=0.2667
6. Intercept of rectifying section operating line (ROL) on y-axis =Xd/R+1= 0.57
7. The above intercept was marked on the y-axis and joined with point XD which gave
the ROL. The point where it cut the q line (say B) was marked.
8. The points B and XB were joined to get the stripping section operating line (SOL).

12
 The minimum number of stages obtained from Fenske’s equation for practical and
experimental calculations are 1.784 under total reflux. That is quite close to the number of
stages obtain from the graph. This implies that our equipment is working fine. If we look into
the value of F which is the molar composition of feed that comes out to be 0.0495kmol the
value of B molar composition of bottom distillate is 0.023kmol and the value of D molar
composition of top distillate is 0.027kmol. The efficiency of the total reflux against the actual
number of stages that are 7 obtain from the equipment is 30.57 which shows that the theoretical
calculations give us an efficiency of 30.57 that might involve errors in calculations are
precision in graph readings.

13
 6. Conclusion and Recommendation

As per the observations the current setup is made of 7 actual tray column. The total reflux
graph give us 2.14 stages with an efficiency of 30.57. The reflux of 4:15 gives us stages amount
of 6.23. Whereas the 10:15 reflux ratio give us 3.5 stages. Which means the lesser reflux ratio
the greater the number of stages. Further calculations taking into account the diameter, height
and other parameters of the distillation column which will give us more insight to the column
internals and hence the problem are being done. The minimum number of stages obtained from
Fenske equation under total reflux are 1.784. This implies that our equipment is working fine.
The molar composition of the feed and the bottom reflux is obtained by Rayleigh’s equation.
As per recommendation the top reflux drum should be isolated of any kind of leakage
to avoid damage or loss of steam to atmosphere. The feed drum should be kept clean in order
to prevent accumulation inside the drum and effect the boiling value. The reflux ratio should
be observed several times for different refluxes to give the greatest efficiency.

14
 7. References

Sciencedirect, 2014, “Sieve-Trays”. [online].[Accessed 15th November,2019]. Available from

World Wide Web:

https://www.sciencedirect.com/topics/engineering/sieve-tray

McCabe_W.L._Smith_J.C._Harriott_P, 1993, “Unit Operation of Chemical Engineering”

(5th Edition). McGraw-Hill, Inc.: Distillation. P561..

Geankoplis, C. J. (1993). Types of Separation Processes and Methods, “In Transport

Processes and Unit Operations” (3rd Edition ed., p. 585). Minnesota: Prentice Hall P-611.

Neutrium, 2016, “Unit Operations and Distillations”. [online].[Accessed 10th

November,2019]. Available from World Wide Web:

https://neutrium.net/unit-operations/distillation/mccabe-thiele-plot/

Traysrus, 2009, “Sieve-Bubble-Cap-Trays”. [online].[Accessed 17th November,2019].

Available from World Wide Web:

http://www.traysrus.co.uk/sieve-bubble-cap-trays.php

15
 8. Appendix
Data

Relative volatility α 3.32

Molecular weight of methanol MM 32 g/mole
Molecular weight of Water MW 18 g/mole
Enthalpy of feed HF 0 kJ/kmole
Packed height Z 0.90 m

N Volume Volum Mass of Mass Moles of Moles Mole Refrectiv

o of e of Methano of Methano of fraction e Index
Methano Water l Wate l Wate of
l (ml) (0.79*V) r (mol) r Methano
(ml) (g) (1*V) (mol) l
(g) X
1 0 10 0 10 0 0 0 1.3185
2 1 9 0.79 9 0.025 0.056 0.048 1.3215
3 2 8 1.58 8 0.049 0.111 0.099 1.323
4 3 7 2.37 7 0.074 0.167 0.160 1.3255
5 4 6 3.16 6 0.099 0.222 0.229 1.326
6 5 5 3.96 5 0.123 0.278 0.308 1.326
7 6 4 4.75 4 0.149 0.333 0.401 1.3278
8 7 3 5.54 3 0.173 0.389 0.510 1.3255
9 8 2 6.34 2 0.198 0.444 0.641 1.3245
10 9 1 7.13 1 0.223 0.500 0.801 1.321
11 10 0 7.92 0 0.248 0.556 1 1.315
Table 1: Observation table for calibration Chart.

16
 Time Top Reflux Bottom reflux
Total Reflux 1.324 1.322
4:15 1.323 1.322
10:15 1.325 1.32
Table 2: Refractive Index of distillates.

Refractive Index Xd Xw Xf
Refractive
Bottom
Index Top

1.324 1.322 0.68 0.07 0.23

1.323 1.322 0.73 0.07 0.23

1.325 1.32 0.58 0.04 0.23

Table 3: Refractive Index with composition.

McCabe-Thiele method:

Boiling point temperature = 80.5⁰C (From Graph)

80.5+25
Average temperature tBP = = 52.75⁰C.
2

To Calculate the value of q:

Calculation of q value: q = λF + CPF(tBP − tF ) λF

Where, tBP – Bubble point of feed

tavg – Average temperature

λF – Latent heat of methanol-water feed mixture at tBP

CPF – Heat capacity of methanol-water feed mixture at tavg

From Perry’s handbook,

Latent heat of water at 80.5°C (tBP), λW = 4.16 x 104 J/mol

17
Latent heat of methanol at 80.5°C, λM = 3.43 x 104 J/mol

Heat capacity of water at 52.75°C (tavg), CPW = 75.34 J/mol-K

Heat capacity of methanol at 52.75°C, CPM = 87.46 J/mol-K

Therefore,

λF = (xF*λM) + ((1-xF)*λW)

= ((0.23)*(3.43 x 104 )) + ((0.77)*(4.16 x 104 ))

λF = 39990.00 J/mol.

After putting values, q = λF + CPF(tBP − tF ) λF

we get,

q = 1.108

Equation of q line:

y = ( q/ q − 1 ) x – (xF /(q – 1))

After putting values of xF and q, we get:

y = 10.25x – 2.12. (Slope is positive).

4:15 reflux ratio:

R=L/D=0.2667

ROL=xd/R+1 =0.57

10:15 reflux ratio:

R=L/D=0.667

ROL=xd/R+1 =0.35

18
Rayleigh’s Method

For the composition of total reflux values:

ρ𝑽
𝑭 = 𝑴𝑾 𝑿𝟏𝟎𝟎𝟎 = 𝟎. 𝟎𝟒𝟗𝟓𝒌𝒎𝒐𝒍

Putting values into Rayleigh’s equation to find B which is the outlet moles of the bottom
product.

0.0495(1−0.23) 0.0495𝑥0.23
3.32ln[ ]=𝑙𝑛
𝐵(1−0.07) 𝐵𝑥0.07

B = 0.023 kmol

D = F-B

D = 0.0495-0.023 = 0.027 kmol.

Fenske’s Equation

For the composition of total reflux values:

Nm =(log [ 0.68(1-0.07)/0.07(1-0.68)]/log3.32)-1

Nm = 1.784 no of stages.

19
Efficiency:

For the composition of total reflux values:

𝑁𝑡ℎ𝑒𝑜
ή=𝑁𝑎𝑐𝑡𝑢𝑎𝑙 𝑥100

2.14
ή= 𝑥100 = 30.57
7

20