Design and Construction of a Lab-Scale System to Produce

Biodiesel from Waste Oil Using Immobilized Lipase

Team member ID Number

Mubarak Salyem Alsheraifi 200415260
Humaid Saeed Alshamsi 200417806
Nayef Mohammed Albraik 200416292
Abdelaziz Hassan Suwaidi 200215582
Saud Abdulaziz Aljahori 200440225
UAE University
College of Engineering
Industrial Training and Graduation Project Unit
Chemical & Petroleum Engineering Department


Advisor: Dr. Sulaiman Al-Zuhair
Contents
Introduction and Background
Summary of GPI
Detailed Design and Simulation
Lab Scale Experiment
Economics and Cost
HAZOP and Environmental Impact of the process
Conclusion and Way Forward
Introduction and Background
Biodiesel, defined as methyl (or ethyl) ester of long chain
fatty acids, is derived from vegetable oils or animal fats,
for use in compression-ignition (diesel) engine.

Enzymatic transesterification has been proposed recently
to overcome the problems facing conventional chemical
methods without compromising their advantages.
Introduction and Background
The objective of this project is to design and construct a lab-
scale system to continuously produce approximately 1000 g/hr
relatively pure biodiesel by using immobilized lipase as
catalyst.

The design objective of the project is to know how to design
the main equipments of the lab-scale system.

The main equipments in the-lab-scale system are heat
exchanger, liquid-liquid extraction, reactor, and distillation
column
Summary of GPI
In GPI, literature survey was conducted on biodiesel
production, physical, and chemical properties were
collected.

Different methodologies and processes for biodiesel
production from waste cooking oil have been studied to
choose the suitable process flow diagram.

Then, based on the estimated production capacity,
material and energy balances on the whole system as well
as each individual unit had been performed
Summary of GPI
Based on the estimated production capacity, material and
energy balances on the whole system as well as each individual
unit had been performed.

Material balance was done in GPI to know the amount of
materials needed for the reaction such as amount of the enzyme
catalyst, which was achieved using the mass and mole
conservation.

The search result from GPI has shown that activity of the
enzyme is highest at 45C.



Process Flow Diagram
Summary of GPI
The energy balance sheet designed in order to calculate
the temperatures in all streams and add heaters or coolers
as needed to make the temperature of the stream entering
the reactor equal to 45C also to operate the distillation at
95 .

Detailed Design
Heat Exchanger.

Liquid Liquid Extraction.

Reactor Design.

Distillation column.
Factors Involved in Reactor Design
Feedstock composition
Single feedstock
Reactant in a solvent
Multi-component feedstock
Scale of process
output of product
Process kinetics
Effect of composition
(concentration)
Effect of temperature
Catalyst
Thermodynamics
Reactor type
Batch / continuous
Semi batch / Semi
continuous
Isothermal, non-isothermal,
adiabatic
Single pass / recycle
Multiple reactors
Others
Materials of construction
instrumentation
safety
Reactor Design
The structure parameters mainly include:
1. Reactor diameter.
2. Reactor length.
3. The Volume of the reactor.
4. Weight of the catalyst used in the reactor.
5. Pressure drop inside the reactor.

Reactor Design
Physical Properties

1. Average Density

2. Average Viscosity

=
i i avg
x

=
i i avg
x
Reactor Design
Volume of the reactor :




The polymath software program was using to calculate
volume of reactor.



) ( reactants of Density
reactants of Mass
) ( reactants of rate flow Volumetric
average
o

v =
Reactor Design - Polymath
Reactor Design

Weight of catalyst

Cross section area

Length of reactor


The activity of lipase will be decreased with time





W
b
= V
( ) D
4

A
2
in C
=
C
A
V
L =
t
i
e E E
o
=
Reactor Design

Pressure drop inside the reactor
2
1
2
1
|
|
.
|

\
|
=
o
o
o
P
L
P
P |
(

+

= G
D D g
G
P P o c
o
75 . 1
) 1 ( 150 ) 1 (
3
|
|
|
|
C
A
m
G
-
=
Reactor Design Specifications
Unit Data Variable
Mole/hr 1
Molar flow of Substrate ( Waste Oil)
Mole/hr 6
Molar flow of alcohol (Methanol)
o
C 45
Temperature
LU/g 1000
Catalyst activity
g/m
3
7.98 * 10
5

Average Density
Kg/m.s 0.0005432
Average Viscosity
LU/m
3
450 *10
6

Bulk Density
m
3
/ min 3.77*10
-5

Volumetric flow rate
kg/m
2
.S 2.836
Superficial mass velocity (G)
- 0.38
Porosity
m 232.3 *10
-10

Catalyst diameter (Dp)
Novozym 435 (Candida Antarctica lipase
immobilized)
Type of Catalyst
Reactor Results
m
3

6 *10
-5

Rector volume
g
27
Weight of catalyst
atm
0.034
Pressure drop
m
0.0118
Reactor Diameter
m
0.54
Reactor length
Reactor Design
Classification of Homogeneous and Heterogeneous
Reactor Models

REACTION PHASE

REACTOR MODEL


Homogeneous


Plug Flow, CSTR, Batch


Heterogeneous:-

Catalytic
Two Phase
Gas-Catalyst or
Liquid-Catalyst

Three Phase
Gas-Liquid-Catalyst



Non-Catalytic

Gas-Liquid





Packed-Bed or Fluidized-Bed



Trickle-bed, Bubble Fixed-Bed
CSTR Slurry, Bubble Slurry,
3-Phase Fluidized



Gas-Liquid CSTR, Gas-Liquid
Bubble Column


Multi-phase Reactors- Advantages and
Disadvantages
A packed bed is a hollow tube, pipe, or other vessel that is
filled with a packing material. The packing can be randomly
filled with small objects it is name catalyst.

Packed Bed Reactor
Advantages Disadvantages
High conversion per unit mass of catalyst Undesired thermal gradients may exist
Low operating cost Poor temperature control
Continuous operation Unit may be difficult to service and clean
Concentric Tube Construction
Parallel Flow Counterflow Parallel Flow Counterflow
- : :
Parallel Flow Counterflow Parallel Flow Counterflow
Heat transfer Area calculations
) T - (T
) T - T (
ln
) T - (T - ) T - T (
T
c1 h2
c2 1 h
c1 h2 c2 1 h
m
= A
Th1
Tc2
Th2
Tc1
T m.Cp. Q A =
Heat transfer Area calculations
F . T U.A. Q
m
A =
F . T U.
Q
A
m
A
=
i i
o
i
o o
o
calculated
h r
r
r
r
k
r
h
U
1
) ( ) ln(
1
1
+ +
=
0.33
h
f
i i
.Re.Pr j
K
.d h
Nu = =
1/3 0.55
shell
e
h
o
Pr R
D
0.36.k
h =
Design Data
E-101 E-102
Data Tube shell Tube shell Unit
Fluid Steam Stream5 Steam Stream8 -----
Fluid flow 16434.32 15579.77 28297.80 7060.60 kg/yr
Temperature in 140 28 140 43.9
o
C
Temperature out 120 45 120 95
o
C
Density 1.5 919 1.5 978 kg/m
3

Duty 21.13 37.12 W
T
lm
93.5 59.19
o
C
U 30.12 18.11 W/m
2
.
o
C
H.E Construction
Heat Transfer Area 0.0081 0.0364 m
2

No. of tubes 1 5 Tubes
Tube length 0.24 1.114 m
Tube inside diameter 0.0068 0.0068 m
Shell diameter 0.0166 0.0165 m
Shell material of construction Carbon steel
Tube material of construction Carbon steel
Shell and Tube Advantages
The configuration gives a large surface area in a small
volume.
Good mechanical layout: a good shape for pressure
operation.
Uses well-established fabrication techniques.
Can be constructed from a wide range of materials.
Easily cleaned.
Well-established design procedures.

Modified McCabe Thiele
Assumptions:
Ternary components of Glycerol, Biodiesel and Water
Biodiesel & Glycerol are partially miscible
The two-phase region is inside the envelope.
The one-phase region is outside the envelope.
Right Angle Triangle
Equilibrium line
Equilibrium Plot
0.00
0.10
0.20
0.30
0.40
0.50
0.60
0.70
0.80
0.90
1.00
0.00 0.02 0.04 0.06 0.08 0.10 0.12 0.14 0.16 0.18 0.20
Xg Biodiesel Phase
Y
g

W
a
t
e
r

P
h
a
s
e
0.00
0.10
0.20
0.30
0.40
0.50
0.60
0.70
0.80
0.90
1.00
Equation Used
3 . 0 Spacing Tray Trays of Number Height + =
Height
30
1
Diameter Tower =
L D Area Tower t =
Extraction Column Specifications
Equipment Name: (T-101).
Type of Equipment : Liquid Liquid Extraction Column
Data Value Unit
Height 1.4 m
Area 0.22 m
2

Diameter 0.05 m
Tube Material Of Construction Carbon steel
Volume 0.003 m
3

Number Of Actual Stages 2 Stages
Simulation
Comparison Using HYSYS simulator was not
possible since this equipment runs on a very slow
flow rate which can not be solved or simulated by
HYSYS.

ChemCAD simulator was unable to solve the system
effectively which also lacks the ability to calculated
design variables for a liquid liquid extraction unit
Design Alternatives
Mixer settlers
Centrifugal
Packed Column

Plate liquid liquid extraction column was chosen the efficiency
of the plate tower is much higher

Plate tower can easily operate with more than one feed and
inside cooling is easier

The presence of solid does not prevent the plate tower
performance.
Assumption
Binary mixture of Tert butanol and water
Total Condenser
Partial Boiler
Number of Trays Using McCabe Thiele method
Equation used in Distillation Design
q
=
stage Theortical
stage actual
N
N
u
V
Area
gas
=
m 6 . 0 N * Spacing Plate Height
stage actual
+ =
stages N
stage actual
6 =
Distillation Column Specification
Equipment Name: (T-102).
Type of Equipment : Distillation column
Data Value Unit
Max Vapor Velocity 0.6 m/s
Height 1.2 m
Cross Sectional Area 5.5 * 10
-4
m
2

Inside Diameter 0.0263 m
Tube Material Of Construction Carbon steel
Volume 6.5*10^
-4
m
3

Number Of Actual Stages 6 stages
HYSYS Simulation Results
For a Packed Tower
D = 0.30 m
H = 1.50 m

Design Alternative
Packed Tower

The Design of Plate Column is More Equation Reliable.

Trays have Higher Efficacy

Plate Tower is Easier to Operate With More Than One Feed
And Inside Cooling is Easier

The Presence of Solid Does not Prevent the Plate Tower
Performance.
Process of biodiesel experiment
Flow rate: 2.8x10
-3
ml/s and RPM 1, Dynamic viscosity = 5.3031 mpa.s,
Kinematic viscosity = 6.1131mm
2
/sec and Density = 0.8675 g/cm.
Cost Analysis
The Purchased cost of the main equipments (heat
exchanger, packed bed reactor, liquid-liquid extraction and
distillation).
) F F B B ( C F C C
P M 2 1
0
P BM
0
P BM
+ = =
2
10 3 10 2 1
0
P 10
)] A ( [log K ) A ( log K K C log + + =
2
10 10
0
) (log 3473 . 0 log 08516 . 0 4771 . 0 N N F
F F N C C
q
q BM P BM
+ =
=
BM P BM
F C C
0
=
Bare Module cost (Cbm)
Equipment type Cbm
Heat Exchanger (E-101 & E-102) $429+$1,621= $2050
Packed bed reactor (R-101) $49227
Liquid-liquid Extraction (T-101)
(Tower + Trays)
$6,610.81+ $6,398.39 = $13,009
Distillation column (T-102)
(Column + Trays)
$8548+$19052= $27600
Total $91512
Annual cost for utilities
Utilities Price Cost ($/yr)
Steam 1.268*10
-5
$/g 1011
Catalyst 1500 $/kg 120
Duty of condenser 72 GJ/yr 112.8
Duty of reboiler 1.08 GJ/yr 18.14
Total 1262
Cost of catalyst = price of catalyst *weight of catalyst* time change of catalyst
Price of electrical $16.8/GJ
Gross Profit
Tert-Butanol Biodiesel Oil Glycerol Methanol
Feed (kg/year) 1197.32 9022.8 8760 714.82 873.37
Density (kg/L) 0.7809 0.88 0.913 1.261 0.7913
price ($/L) $0.70 $0.78 $0.08 $0.44 $0.20
Cost ($/year) $654.49 $7,997.48 $767.58 $249.42 $137.26
Gross Profit $6,688
Cash Flow Diagram
Cash Flow Diagram
($100,000)
($80,000)
($60,000)
($40,000)
($20,000)
$0
$20,000
$40,000
$60,000
$80,000
$100,000
$120,000
0 5 10 15 20 25 30 35 40
Years
$
HAZOP (Hazard and Operability Study)
Systematic method for stimulating peoples imagination to
identify, evaluate hazards for the processing units.
Aim: identifying potential hazards and operability
problems caused by deviations from the design intent
HAZOP technique requires a detailed source of
information concerning the design and operation of the
process.

HAZOP Procedure
Hazard Cause Deviation Consequence Impact
Material/energy
contained and
controlled
during normal
operation

Toxicity
Flammability
Reactivity
Elevated
pressure
Initiating event
of process
upset; start of
accident event
sequence

Mechanical
failure
Procedural
error
External force
Fouling
Excursion
beyond design/
operating limits

No flow
High
temperature
Low level
Impurities
Wrong material
Step omitted
Loss of
containment of
process
material/ energy

Fire
Explosion
Hazardous
material release
Severity of
consequences;
loss

Casualties
Property
damage
Business
interruption
Environmental
damage
Process piping and Insemination Diagram
Equipment Name : R-101
Equipment Type : Packed Bed Reactor
Deviation Causes
Potential
Consequence
Safeguards
Recommendation
s
Low Flow
(Stream 6)

Valve Or Pump
Failure

Low Production
Rate, Not Serious
Problem
Auxiliary Pump
Input A Low Flow
Alarm
High Flow
(Stream 6)
Valve Stuck
Open
Sudden Decrease In
Temperature Of The
Column, Low
Conversion
Proportional
Valve
Pressure Alarm

No Flow
(Stream 6)
Pump Failure
Not Serious
Problems
Auxiliary Pump Flow Alarm
Packed Bed Reactor
Packed Bed Reactor
No Flow
(Stream 7)
Blockage Inside
Packed Bed Reactor
Low Production Rate,
High Pressure Drop,
Building Up Pressure
Up Stream.
Clean With Tert-
Butanol To Dissolve
What Even Blocks
The PBR, Back Flow
For Cleaning
Regular Maintenance,
Regular Check Of
7hr/Day
High Pressure
(Stream 6)
Oil Or Glycerol
Freezing Inside
Reactor
Flow, Damage Pump,
Reduction Of Enzyme
Activity
Temperature Alarm
Relief Valve In The
Vent
Low Temperature
(Stream 5 & 6)
Control Temperature
Failure
Reduction Of Enzyme
Activity, Low
Conversion
Input And Output
Temperature (High
And Low)
Alarm
Hot Water Cycle
(Temperature Control)
High Temperature
(Stream 5 & 6)
Valve Stuck
Reduction Of Enzyme
Activity, Low
Conversion
Input And Output
Temperature (High
And Low)
Alarm
Cooling Water Cycle
(Temperature Control)
Equipment Name: T-101
Equipment Description: Biodiesel Extraction Column
Deviation Causes
Potential
Consequence
Safeguards Recommendations
No Flow
(Stream 7)
Pump Failure /
Controller Malfunction
No Biodiesel
Separation

System Cleaning Flow Alarm
Low Flow
(Stream 7)
Reactor Blocked
Product Purity
Decrease
Flow Controller Low Flow Alarm
High Flow
(Stream 7)
Valve Stuck Open
Extraction Column
Flood And No
Separation
Flow Controller
High Flow Alarm / High
Level Alarm
Reveres Flow
(Stream 7)
Back Pressure /
Pressure Drop
Reactor Flooding No Return Valve Flow Alarm
No Flow
(Water Stream)
Valve / Controller
Malfunction / Pump
Failure
No Biodiesel
Separation
Flow Controller /
Auxiliary Pump
Flow Alarm
Extraction Column
Extraction Column
Low Flow
(Water Stream)
Valve Stuck Close /
Pipe Blocked / Leaking
Product Purity
Decrease
Low Flow Alarm Flow Controller
High Flow
(Water Stream)
Valve Stuck Open
Extraction Column
Fluid And No
Separation
Bleeding Valve /
Flow Controller
High Flow Alarm / High
Level Alarm
Reveres Flow
(Water Stream)
Back Pressure
No Biodiesel
Separation
No Return Valve Flow Alarm
No Flow
(Stream 9)
High Flow in
Stream 10
Back Pressure / No
Separation
Auxiliary Pump Flow Alarm
Low Flow
(Stream 9)
Valve Stuck Close /
Pipe Blocked / Leaking
No Product Flow Controller Low Flow Alarm
High Flow
(Stream 9)
Valve Stuck Open No Separation Flow Controller High Flow Alarm
Reveres Flow
(Stream 9)
Back Pressure Column Flooding No Return Valve Flow Alarm
Equipment Name: T-102
Equipment Type: Distillation Column

Deviation Causes
Potential
Consequence
Safeguards Recommendations
Low Flow
(Stream 11)
Valve Failure
Reboiler Overheat


Controlling Of
Flow Rate Inlet
Level Alarm
High Flow
(Stream 11)
Valve Failure
The Separation
Process Will
Decrease
Bleeding Valve Level Alarm
High Level
(Stream 11)
Failure Of Level
Controller
Flooding In The
Column
Close The Input Stream
High Level Alarm
High Pressure
Drop In The
Column
Blocking Of
The Trays
Less Product

Pressure Controller
Pressure Alarm
Distillation Column
Distillation Column
High
Temperature
(Stream 11)
Valve Failure
Of He
Higher Loading In
The Condenser,
Lower Reflux, And
Less Purity Of Top
Product
Need Of
Temperature Alarm
Low Flow
(Stream 11)
Large Reflux
Less Product In
Stream 9
Low Level Tert-Butanol
Make Up
Low Flow Alarm
Need Of Low Flow
Alarm
High Flow
( Stream11)
Failure Of
Reflux Pump
Less Separation
Process
Flow Controller
Shutting Down
Need Of
High Flow Alarm
Low Flow
(Stream13)
Pump Failure
Less Product In
Stream 10
Using Of
Auxiliary Pump
Need Of
Low Flow Alarm
High Flow
(Stream 13)
Large Recycle
Stream
Less Separation
Process
Need Of
High Flow Alarm
Potential Ethical and Environmental Issues
Using waste oil is important for environmental issue such as
1. Alternative feed stocks that either improves the
environmental performance of a process or that do not
deplete non-renewable resources

2. Minimization the generation of waste and recycling

3. Separation systems have maximum recovery and minimum
energy
Potential Ethical and Environmental Issues
1. Lipase enzyme enhance selectivity in the reactions

2. Reaction Have High conversion (Minimize the Reactor
Waste)


Conducting experiments to determine the rate of
enzymatic production of biodiesel.

Detailed design of main units and equipments.

Construction of lab-scale system for continuous
production.

Testing of the produced biodiesel (physical, chemical and
mechanical properties)

Conclusion
Conclusion
Biodiesel formed from enzymatic transesterification of
waste vegetable oils with methanol and produced
approximately 1000 g/hr.

The specification of biodiesel production found by using
gas chromatography was a Dynamic viscosity of 5.3031
mpa.s, Kinematic viscosity of 6.1131mm
2
/sec and Density
of 0.8675 g/cm.

These design results led to a capital cost of 91,500 $, an
annual cost of 1,262 $/yr and a gross profit of 6,688 $/yr.


Thanks for Listening