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

Topic : BATCH DISTILLATION AT TOTAL REFLUX Mark : 100

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
3
4
Instructor 1.Miss Norkamruzita Binti Saadon
The purpose of the experiment is to determine the number of theoretical plates at total
Abstract : reflux. Distillation column provided to us to run the experiment. The reboiler 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 reboiler E-301 is opened and the
reboiler 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.

Objective : 1. To determine the high equivalent theoretical plates (HETP) at total reflux
2. To determine the effect of liquid and vapor loading on the HETP at total reflux
3. To operate a batch distillation unit at total reflux.
4. To carry out mass balance calculations on the distillation unit.
Data/Results Density of water, ρ water 1 g/mL

/Calculation: Density of ethanol, ρ ethanol 0.789 g/mL

Molecular Weight of water 18.02 g/mole

Molecular Weight of ethanol 46.07 g/mole

Volume of Volume of Mole of

Ethanol Refractive index
ethanol water ethanol
Wt.% (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
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

DISTILLATE BOTTOM PRODUCT

TIME
(MIN) REFRACT MOLE REFRACT MOLE
TEMP (OC) TEMP (OC)
INDEX FRACTION INDEX FRACTION
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

Mole fraction Distillate - XD (INTERPOLATE)

Ethanol
Refractive mole
index fraction
(x D)

1.3409 0.0171
1.3456 X
1.3473 0.0342

X = 0.0297
Mole Fraction Bottom-XB (INTERPOLATE)

Ethanol
Refractive mole
index fraction
(x B )

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:

Conclusion:

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

Comments: