FACULTY OF CHEMICAL ENGINEERING

Universiti Teknologi MARA (UiTM) Terengganu

Kampus Bukit Besi,
Bukit Besi, Dungun, TERENGGANU

TECHNICAL/EXECUTIVE REPORT : CHEMICAL ENGINEERING

Lab No : 1 Subject : CHE 246 - SEPARATION

PROCESS

BATCH DISTILLATION AT TOTAL

100
Topic : Mark :
REFLUX
Date : 17th April 2018
Participant : Course : EH 110 4A Semester : 4 Group: 5
No. Name Matrix No. Signature
1 Arif Hanafi Bin Md Zaki 2016800892
2 Muhammad Firdaus Bin Rusli 2016697802
3 Mohd Taufiq Bin Rosmizi 2015810618
4 Muhammad Ameruddin Daniel Bin Sulong 2016800832
5 Muhamad Kamal Bin Muhammad Fahimuddin 2016800654
Instructor : 1. Miss Norkamruzita Binti Saadon

Abstract : The purpose of the experiment is to determine the number of theoretical plates at
total reflux. Distillation column provided to us to run the experiment. The re-boiler was heat
until the temperature of the tray become constant. This is to allow the distillation column
become stable before the sample was taken from the bottom product and distillate product.
The temperature was different for each tray. The temperature of the tray decrease from
bottom tray to distillate tray. The bottom product and distillate product was took and both
product are allowed to cool down before proceed to other process.

The experiment started off by ensuring that all valves were closed. Then only we
can turn on the power on for the control panel. A 25 L mixture containing ethanol and
filtered water is prepared to the unit as so; the charge port cap at the re-boiler E-301 is
opened and the re-boiler is filled with 25 L of the mixture. Then through the feed charge
port, the leftover from the ethanol-water mixture is poured into the feed vessel V-101.

Then, the reflux divider KS-401 is set to total reflux. The intention of doing so is to
prevent any distillate from escaping once the distillation column is started. Cooling water
was allowed to flow into the condenser E-302 and product coolers E-303 and E-304 by
opening valves V25, V26 and V27. After that, set the setpoint value to 85°C in the AUTO
mode and ensure that the setpoint of re-boiler is higher than boiling point.

After 10 minutes, take the distillate and bottom sampling. Before that set the reflux
divider to total reflux for 1 minute and set back to its original position. Collect the enough
 sampling for the analysis. From the sampling, put the refractive index (RI) data inside the
table.

Objective : 1. To determine the theoretical stages at total reflux.

2. To determine the effect of liquid and vapor loading on the theoretical stages at total
reflux.
3. To operate a batch distillation unit at total reflux.
4. To carry out mass balance calculations on the distillation unit.

Density of water, ρwater 1 g/mL

Data/Results
/Calculation : Density of ethanol, ρethanol 0.789 g/mL

Molecular Weight of water 18.02 g/mole

Molecular Weight of ethanol 46.07 g/mole

Volume of Volume Mole of

Ethanol Refractive
ethanol of water ethanol
Wt.% index (RI)
(mL) (mL) (mole)
0 10.0 0 0.0000 1.3368
1.0 9.0 0.0171 0.0789 1.3409
2.0 8.0 0.0342 0.1578 1.3473
3.0 7.0 0.0513 0.2367 1.3525
4.0 6.0 0.0685 0.3156 1.3539
5.0 5.0 0.0856 0.3945 1.3577
6.0 4.0 0.1027 0.4734 1.3589
7.0 3.0 0.1198 0.5523 1.3593
8.0 2.0 0.1370 0.6312 1.3660
8.5 1.5 0.1456 0.6707 1.3668
9.0 1.0 0.1541 0.7101 1.3674
9.5 0.5 0.1627 0.7496 1.3678
10.0 0.0 0.1713 0.7890 1.3686

Table 1: Composition data based on Refractive Index.

Sample Calculation :
Mass fraction ethanol = Volume (%) ethanol × Density ethanol
Mole of ethanol = Mass of ethanol / Molecular weight ethanol
CALIBRATION CURVE

Refractive Index vs Mole Fraction

1.365

1.36

1.355

1.35

1.345

1.34

1.335

1.33

1.325

1.32

1.315
0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 0.16 0.18

Graph 1 : Refractive index vs mole fraction graph

BATCH DISTILLATION AT TOTAL REFLUX

TIM DISTILLATE BOTTOM PRODUCT

E MOLE MOLE
(MIN TEMP REFRAC TEMP REFRAC
FRACTI FRACTIO
) (OC) T INDEX (OC) T INDEX
ON N
0 67.6 1.3456 0.0297 42 1.343 0.0227
5 64.3 1.3483 0.0375 29.9 1.3426 0.0216
10 63.9 1.3518 0.0490 30.1 1.3426 0.0216
15 63.8 1.3579 0.0885 30.2 1.3426 0.0216
20 63.7 1.358 0.0899 30.4 1.3426 0.0216

Interpolation for mole fraction

Ethanol mole fraction distillate, XD
Refractive index
(XD)
1.3409 0.0171
1.3456 X
1.3473 0.0342
X = 0.0297

Interpolation mole fraction bottom, XB

Ethanol mole fraction

Refractive index
(XB)

1.3409 0.0171
1.343 X
1.3473 0.0342

X= 0.0227

MCCABE-THIELE METHOD (TOTAL REFLUX)

XD = 0.0899
XB = 0.0216

Theoretical number of plates = 4 stages

Discussion : Top D
XDA= 0.0899

Feed F
XFA
XFB

Bottom B
XBA = 0.0216

The diagram shown the illustrated to give more understanding about distillation
process. The feed enters in the middle column, the vapor went up to the stage as top product
and the liquid down the stage as bottom product. The distillate of product X DA is 0.0899,
while XBA is 0.0216. During the experiment, the vapor flows up the tray and contacted with
the liquid down flowing. This is experiment are going to separate ethanol and water. While
the equipment stabilize, we conducted the boiler with the constant value of heater power
75%.

We collected the sample every 5minutes for the top and bottom final product. Then
we test the concentration of the liquid by recorded the refractive index for each sample. We
also observed the temperature drop in the re-boiler TT102.

The graph plotted based on the calculation of refractive index and mole fraction from table
1. The product recorded are from top and bottom to get the straight line. Calibration curve
get from the refractive index in organic distillation experiment. To determine the theoretical
number of plates in the distillation unit using the McCabe-Thiele method by doing the
graph. First draw the scale on the graph and label the XFA, XBA, XDA. Then draw the straight
line as the mole fraction of top and bottom product. Draw the calibration curve from the
relationship of (RI) and the mole fraction. Lastly plot the total reflux, and calculated the
 stages. We get the theoretical number of plates is 4 stages.

Conclusion : From the experiment that we have conducted for batch distillation at total reflux,
we were able to achieve the objectives that we have aimed which is to determine the
theoretical stages at total reflux to determine the effect of liquid and vapor loading on the
theoretical stages at total reflux, to operate a batch distillation unit at total reflux and to
carry out the mass balance calculations on the distillation unit. We managed plotting the
McCabe-Thiele graphical method because we have enough information to plot the graph.
So, we managed to achieve the theoretical stages over time in a batch distillation and able to
calculate the theoretical stages. We got 4 numbers of stages with re-boiler and the number
theoretical stages is 3. We did manage to plot the refractive index vs mole fraction graph
and Ethanol-Water equilibrium graph. This was done by the data recorded and some
calculations. Based on the first graph, we can see that when the refractive index increases,
the mole fraction of ethanol increases too. Same goes for the second graph. As the mole
fraction Ethanol in liquid increases, the mole fraction Ethanol in vapor will increase too. So,
by plotting these two graphs, we were able to plot the McCabe-Thiele graphical method to
know the number of theoretical stages of the distillation column unit.

References : 1) Experimental manual

2) McGabe, Smith & Harriot, “Unit Operations of Chemical Engineering”, McGraw
Hill, (Singapore), 2001.
3) Geankoplis C.J., “Transport Processes and Unit Operations”, Prentice Hall,
(Singapore), 1995.
4) http://www.separationprocesses.com/Distillation/DT_Chp05b.htm

Authorize Person Initial Date Stamp

Approval Technician

Instructor
 Allocated Marks for Technical/Executive report

Criteria Full Marks

Abstract 10
Objective 10
Data/Results/Calculation 20
Discussion 30
Conclusion 10
References 10
Overall structure/organization and Quality 10
TOTAL 100

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