PRODUCTION OF

GLYCEROL
‘A. INCORPORATED’
 1. PROCESS
INTRODUCTION
1.0 PROCESS DESCRIPTION
■ Fatty acid production industries use vegetable oil as one of the main source
■ In splitting vegetable oil process, glycerol is produced as a co-product while
the main product is fatty acid
■ In a single process cycle, the process is divided into two: separation process
(fat splitting) and glycerol refining
■ Water with high-pressure steam contacted counter flow of oil in separating
column
Bottom: Glycerol(10%) Top: Fatty acids
■ Next, sweet water contains 12% of glycerol passed through from flash
chamber to decrease the temperature of flow
■ To increase concentration of glycerol (12%-75%-80%) – sweet water is
passed along triple effect evaporator (without additional heat)
■ After that, the crude was settled for 48hr at elevated temperature – to reduce
fatty impurities that could interfere with process
■ Settled crude contains 78% glycerol, 0.2% total fatty acids and 22% water
■ Caustic is added: - To saponify fatty impurities
- To reduce possibility of co-distillation with glycerol
■ Then, stream heated in heat exchanger and entered column where distillation of
settled crude was carried out (200oC, 8kPa)
■ Distilled glycerine condensed in three stages: -
i. First stage – purest glycerine (99% glycerol)
ii. Second and third stage – lower grades of glycerine
■ Final purification, glycerol is treated with activated charcoal
■ Lastly, the charcoal is removed by filtration or ion exchange filter method
1.1 PROCESS SELECTION
■ Process selected: Fat splitting process
■ Most efficient and cheap method for big scale production
■ Full counter-current flow of oil and water produces a high degree of
splitting without the need of catalyst
■ Degree of splitting: More than 99%
■ Reaction time: 2 to 3 hours
1.2 OBJECTIVES
■ The purification techniques involved in producing high-purity glycerol.
■ To identify the equipment needed and flow process to produce glycerol
production.
■ Converting the triglyceride in vegetable oil using H2O molecule to
produce glycerol and fatty acids.
■ To deliver design and basic engineering using HYSYS software.
■ Using a HYSYS software for plant design shows how easy to use it in
production.
■ Mass and energy balance to produce 1 000 tonne of glycerol per year.
2. PROCESS FLOW
DIAGRAM
 10

9
14
3
2
11
Condenser
4 6

7 8 8 15
13

1
12
Fat 17
Storage

18
16
Glycerol Purity
99.5%

Glycerol Storage Tank

3. HYSYS
 Process Flow Diagram Using HYSYS

Equipment ID Equipment Name Equipment ID Equipment Name Equipment ID Equipment Name

X-100 Splitting tank V-103 + E-102 Separator + Heater = E-104 Cooler

Evaporator 3
VLV-100 Valve P-100 Pump V-105 Tank
V-100 Separator V-100 Tank P-101 Pump
V-101 + E-100 Separator + Heater = Evaporator 1 E-103 Heater CRV-100 Conversion Tank

V-102 + E-101 Separator + Heater = Evaporator 2 T-100 Shorcut Column V-106 Separator
 Splitting Tower (up1) Fatty Acids

■ The value of Hysys mass balance is 522970.51 kg/hr compared to manual mass balance is
522975.88 kg/hr
■ The different value between hysys and manual mass balance is 5.37 kg/hr
 Splitting Tower (down1) Glycerol

■ The value of Hysys mass balance 48067.18 kg/hr compared to manual mass balance is 48067.67
kg/hr
■ The different value between hysys and manual mass balance is 0.49 kg/hr
■ The value of Hysys with manual mass balance is different because factor of the oil that use.
■ Manual mass balance the oil that use is palm oil while in the Hysys is Soybean oil.
 Evaporator 3 (l8) – Last Evaporator

 The value of Hysys mass balance is 17549.57 kg/hr compared to manual mass balance is
15021.09 kg/hr
 The different value between hysys and manual mass balance is 2528.48 kg/hr
 Distillation Column (l13)

■ The value of Hysys mass balance is 16424 kg/hr compared to manual mass balance is
12077.26 kg/hr.
■ The different mass balance value between Hysys and manual mass balance is 4346.91
kg/hr.
 Separator Tank (l21) – Glycerol Purify

■ The value of Hysys mass balance is 16424.17 kg/hr compared to manual mass balance is
12076.995 kg/hr.
■ The different mass balance value between Hysys and manual mass balance is 4347.175
kg/hr.
4. MASS BALANCE
 Calculation

Water = 28,840.58 kg/hr Fatty acid = 48,067.67 kg/hr

Water = 522,975.88 kg/hr

Water = 90,367.17 kg/hr Splitting

Tower
Oil/Fat = 451,835.75 kg/hr

water = 36,050.71 kg/hr

Glycerol = 12,016.88 kg/hr
 water = 36,050.71 kg/hr
Glycerol = 12,016.88 kg/hr

water = 363,046.5 kg/hr

Evaporators

water = 3,004.21 kg/hr

Glycerol = 12,016.88 kg/hr
 water = 3,004.21 kg/hr
Glycerol = 12,016.88 kg/hr

water = 883.58 kg/hr

Settling Tank

water = 2,120.63 kg/hr

Glycerol = 12,016.88 kg/hr
 water = 2120.63 kg/hr
Glycerol = 12,016.88 kg/hr

water = 2,060.25 kg/hr

Distillation Tank

water = 60.38 kg/hr

Glycerol = 12,016.88 kg/hr
 water = 60.38 kg/hr
Glycerol = 12,016.88 kg/hr

Activated carbon = 2,403,376 kg/hr

Bleaching Tank

water = 60.38 kg/hr

Glycerol = 12,016.88 kg/hr
Activated carbon = 2,403,376 kg/hr
 water = 60.38 kg/hr
Glycerol = 12,016.88 kg/hr
Activated carbon = 2,403,376 kg/hr

Ion Exchange
Filter
water = 57.97 kg/hr
Glycerol = 12,016.88 kg/hr Activated carbon = 2,403,375.59 kg/hr
Activated carbon = 2.145 kg/hr

Method Used
■ The mass balance achieved was
calculated backward, from the
quantity of product desired to the
number of raw material needed.
Assumption and
Relation
Fat splitter
• The Degree of splitting was assumed to be
at 100% without any contamination from
fatty acids. The actual degree of splitting
between fatty acid and glycerol form
triglycerides is >99%.
• The percentage of fatty from oil is 90% and
glycerol is 10% from the process.
• From a literature obtained the amount of
steam used for the process are 200kg/ton
of oil.
• The amount of water to hydrolysed 100g of
oil was 6ml. Hence from that it is assumed
that the percentage of water used for the
process is 6%
 Still Feed Tank.
Evaporators Still feed tank is where the fatty acid
The based on various source the triple impurities will undergoes
stage evaporator was design to saponification process react with
increase the concentration of the caustic soda. There are not inlet of
glycerine from 15% to 80%. Based on caustic soda as the condition to used
the literature, the amount of water is when the Sweet water came from
expelled was able to determined. saponification process which consist
impurities from fatty acids.

Ion Exchange Filter

Settling Tank Distillation Still There are some water
The crude glycerol obtained will To further increase the purity of that are expelled during
settled in the tank to remove any glycerol. The distillation still is used this process. This
impurities and some water. With which eliminate soap and any other process causes some
assumption there are no impurities impurities. impurities which range
from fatty acids, there are no outlet of The efficiency of the distillation from 0.02% to
fatty acid with little outlet of water. 0.0002%. Assumption
made that there are
only 0.0002% of
Bleach Tank impurity happen.
Activated Charcoal are inserted at
200g/Litre glycerol
5. ENERGY BALANCE
1. Fat Splitting Process (Splitter)
2. Heat exchanger
3. Condenser
 1. Fat Splitting Process (Splitter)
Substances min ΔHin mout ΔHout min ΔHin mout ΔHout

H2O (v) 90 367.17 157 605.56 119 207.75 2 687.72 1.424 x 1010 320.40 x 106

H2O (l) 28 840.58 0 - - 0 0

Oil (l) 451 835.75 523 949 - - 2.367 x 1011 0

Glycerol (l) - - 12 016.88 1 641.75 0 19.729 x 106

Fatty acid - - 432 608.71 3 477.23 0 1.504 x 109

(l)
2.504 x 1011 1.844 x 1011

Qout – Qin = -2.485 x 1011

 2. Heat Exchanger
Substances min ΔHin mout ΔHout min ΔHin mout ΔHout
Water (v) 2120.63 2 687.72 2 120.63 2 765 5.699 x 106 5.864 x 106

Glycerol (l) 12 016.88 1 641.75 12 016.88 2 128.22 19.73 x 106 25.575 x

106
23.429 x 106 31.439 x 106

Qout – Qin = 6.01 x 106

 3. Condenser
Substances min Hin mout Hout minΔHin moutΔHout

Water (v) 60.38 2 765 - 0 166.95 x -

103
Glycerol (l) 12 016.88 2 128.22 12 016.88 668.86 25.57 x 106 13.91 x 103

Water (l) - - 60.38 230.39 - 8.04 x 106

25.74 x 106 8.05 x 106

Qout – Qin = -17.69 x 106