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FACULTY OF CHEMICAL ENGINEERING

UniversitiTeknologi MARA (UiTM) Terengganu


Kampus Bukit Besi
23200 Dungun, TERENGGANU

TECHNICAL/EXECUTIVE REPORT : CHEMICAL ENGINEERING


Lab No. : 1 Subject : CHE 246- Separation Process
Principle
Experiment Title Distillation Column System ( Model : BP 681-
Mark
: 80) 100
Date
16 January 2017
:
Participant Course : EH 110 Semester : 4 Group: 4C
*Please No. Name Matrix No. Signature
cancel MUHAMMAD FAID SYAHMI B
1 2014696228
which is not ZULKIFLEE
necessary. 2 MOHD AIRIE FAZUWA MOHD RAFI 2015865928
NIK FADHULLAH SYAFIQ AIMAN BIN
3 2014817408
FAUZI
4 NURUL NAJIHAH BT FADZIN 2015861238
5 NUR SYIIRIIN BT SAHRI 2015861368

Instructor 1. MADAM SOPIAH BINTI AMBONG @ KHALID

Objective The objective of this experiment is to :


1) To operate the vapor in liquid separation process using a Bubble Cap Distillation
Unit.
2) To analyze the sample for the Top and Bottom product by Refractometer to
obtain the refractive index in order to determine their respective composition.
3) To calculate the number of stages by using McCabe Thiele method and therefore
the number of stages can be defined theoretically and almost accurately.
4) To determine the height equivalent theoretical plates (HETP) at total reflux
5) To determine the effect of liquid and vapor loading on the HETP at total reflux
Abstract :
The objectives of this experiment were to obtain an unknown solution by simple
distillation and to separate acetone-water by fractional distillation. The results that was
determined after simple distillation was the name of the unknown which was acetone. By
performing fractional distillation acetone and water were successfully separated. The
temperature per mL was collected or each distillation performed and a chart and table
were made for both. In conclusion, acetone was determined to be the unknown used in
the simple distillation and acetone- water was separated successfully by fractional
distillation.

Introduction: The SOLTEQ Distillation Column System (Model: BP 681-80) is developed primarily
for teaching, training and research purposes. It is used for the separation of
mixtures at atmospheric and vacuum pressure in a batch or a continuous operation.
The unit has the following special features :
 Direct heat input into the reboiler by natural circulation evaporation using
two electrical cartridge heaters.
 Silver coated and vacuum jacketed bubble cap column minimizes heat loss to
the surroundings.
 Sampling on each tray and on the bottom and top product to determine the
practical separation behavior of the particular mixture.
 A column packed with Raschig ring.

The method of distillation system unit for the separation of liquid mixtures are now
described. The vapor mixture rises from the reboiler , passes over the column trays
and is fully condensed in the condenser. The condensate runs down the column
counter-current to the vapor through the trays back into the reboiler. At each tray
,the rising vapor attempts to achieve equilibrium with the liquid condensate, thus
effecting both mass and heat transfer. In the ideal case, the rising vapor should be in
equilibrium with the liquid but in actual columns, complete exchange does not
always take place.
The efficiency of a bubble cap distillation column can be evaluated using the
number of theoretical plates required to achieve the same separation as the actual
column. As the purity of a distillate is dependent to a very large extent on the
number of plates, determination of the number of theoretical plates in a column is
very important in the design of a distillation unit.
Data/Results
/Calculation: Apendix A
Table 1 : Composition Table Based on Refractive Index
Purify of ethanol = 0.95
Density of ethanol = 0.7854g/mL
Density of water = 1.0 g/mL

Volume of Volume of Mole fraction Wt% ethanol Refractive


ethanol (mL) water (mL) ethanol index (RI)
0 10 0 0 1.3319
1.0 9.0 0.0331 0.0803 1.3349
2.0 8.0 0.0713 0.1641 1.3399
3.0 7.0 0.1163 0.2518 1.3453
4.0 6.0 0.1710 0.3437 1.3498
5.0 5.0 0.2340 0.4390 1.3549
6.0 4.0 0.3157 0.5766 1.3576
7.0 3.0 0.4175 0.6470 1.3587
8.0 2.0 0.5515 0.7585 1.3604
8.5 1.5 0.6353 0.8165 1.3605
9.0 1.0 0.7330 0.8761 1.3604
9.5 0.5 0.8537 0.9370 1.3602
10.0 0.0 1.0000 1.0000 1.3600
Mass Mass Mole Mole Water Mole Wt%
ethanol Water Ethanol Fraction ethanol
Ethanol
(g) (g)
0 10 0 o.56 0 0
0.7854 9 0.0171 0.5 0.0331 0.0803
1.5708 8 0.0341 0.444 0.0713 0.1641
2.3562 7 0.0512 0.389 0.1163 0.2518
3.1416 6 0.0683 0.333 0.1710 0.3437
3.9270 5 0.0850 0.278 0.2340 0.4390
4.7124 4 0.1024 0.222 0.3157 0.5766
5.4978 3 0.1195 0.167 0.4175 0.6470
6.2832 2 0.1366 0.111 0.5515 0.7585
6.6759 1.5 0.1451 0.083 0.6353 0.8165
7.0686 1 0.1537 0.056 0.7330 0.8761
7.4613 0.5 0.1622 0.028 0.8537 0.9370
7.854 0 0.1707 0 1 1
Calculation
Density of ethanol = 0.7854 g/mL
Density of Water = 1.0 g/mL

Volume of Ethanol (mL) = 1.0 mL Molecular mass of Ethanol = 46 g/mol


Volume of Water (mL) = 9.0 mL Molecular mass of Water = 18 g/mol

Mass of Ethanol
= 0.7854 g/mL x 1.0 mL
= 0.7854 g

Mole of Ethanol
= 0.7854 g / (46 g/mol)
= 0.0171 mole

Mass of Water
= 1.0 g/mL x 9.0 mL
=9g

Mole of Water
= 9 g / (18 g/mol)
= 0.5 mole

Mole Fraction of Ethanol


= (0.0171 mole) / (0.0171 + 0.5) mole
= 0.0331

Wt% Ethanol
= (0.7854 g) / (0.7854 g + 9 g)
= 0.0803

*For other values, the calculations are the same as above.


Refractive Index (RI)
1.365

1.36

1.355

1.35

1.345 Refractive Index (RI)

1.34

1.335

1.33 Mole Fraction Ethanol


0 0.5 1 1.5

Appendix B
Table 2: Result to Experiment 1
Heater W1a Distillate
and
W1b Power (%) Temp (⁰C) Refractive Index Mole Fraction

50 1.3420 0.1599

75 1.3419 0.0880

100 1.3432 0.0988

Heater W1a Bottom Product


and
W1b Power (%) Temp (⁰C) Refractive Index Mole Fraction

50 1.3320 0.0011

75 1.3348 0.0320

100 1.3333 0.0154

Heater W1a
and
W1b Power (%) HETP (mm)

50
75
100
Discussion:

Conclusion: During experimentation of the distillation column the group noticed distillate being
formed during the total reflux. This indicate that the problem with the reflux valve.
This could also explain the problem with the reboiler volume during distillation
experiments. The behavior of reflux valve should be monitored to determine
whether it is functioning well. The conclusion can be made is based on the
objective written. This experiment being analyze the sample for the Top and
Bottom product by Refractometer and the refractive index has been obtained
throughout the process.
A 50% heater power ethanol solution was to be distilled from water and
analyzed for purity. Solutions of differing concentrations of ethanol were analyzed
with a refractometer and a calibration curved shown in the results. The composition
of the product was not equal to 100% ethanol. As conclusion, ethanol present in the
column from previous experiments could be a source of impurity that may have
oxidized.Even though there were impurities present while conducting the
experiment, the separation of two components was observed applying the concept
of binary distillation.
References:
1) Lab manual separation (Distillation)
2) http://www.slideshare.net/mxr3/lab-report-continuous-distillation-column-uitm
3) http://www.che.ufl.edu/unit-ops-lab/experiments/Distillation/Distillation-theory.pdf
4) http://www.che.ufl.edu/unit-ops-lab/experiments/Distillation/BD-Overview.pdf
5) http://swc2.hccs.edu/pahlavan/2423L7.pdf

Authorize Person Initial Date Stamp

Approval of the
Technician
results.

Allocated Marks for Technical/Executive report

Criteria Full Marks

Abstract 20

Objective 10

Data/Results/Calculation 20

Discussion 20

Conclusion 10

References 10

Overall structure/organization and Quality 10

TOTAL 100