Renewable Energy Processes:

Biodiesel
LIPICO Bioenergy:
Recognizing the importance of renewable resources
Biodiesel can be produced from
various sources of fats and oils.
The majority of commercial
biodiesel manufacturing
processes rely on base-
catalyzed transesterification of
methanol with refined fats and
oils of low free fatty acids which
is typically <0.1%.
A good transesterification
reaction is important in the
biodiesel production. However,
effective pre-treatment and
product purification is equally
important for producing high
quality biodiesel consistently.
LIPICO Bioenergy has
developed its patented
continuous transesterification
process for producing high
quality biodiesel.
In 2009, LIPICO Bioenergy has
successfully commissioned a
350,000 TPY continuous
biodiesel plant – the world’s
largest single-line palm biodiesel
plant producing biodiesel
meeting the latest and most
stringent European quality
standards and US ASTM
standard specifications.
Feedstock is the key factor of
the profitability of a biodiesel
plant.
Besides using conventional
feedstock of vegetable oil, there
is a need to look for cheaper
and easily available feedstock
for biodiesel production.
Re-Esterification can convert
low-cost high fatty acid content
fats and oils of vegetable or
animal origin into low FFA re-
esterified oil. The re-esterified oil
can be used directly as biofuel
or used as a feedstock for
transesterification-route
biodiesel plant.
In today's green-energy market, Fully Integrated Biodiesel Process
quality and availability are the
foremost concerns for biodiesel
consumers and it's all about
making standards for biodiesel
that are upheld and made even
more stringent for the future
than today.

LIPICO Bioenergy specializes in

all aspects of pretreatment,
production and purification of the
biodiesel product. We
continuously improve and
develop new, cost-effective
systems that set the industry
standards for tomorrow and
keep your plant running at
maximum efficiency today.
Pretreatment:
Good feedstock to ensure trouble-free biodiesel production

Why Pretreatment is necessary LIPICO Pretreatment Process

Most of crude oils and fats A specially designed pretreatment c) Deacidification
contain impurities that must be process is required to remove the
The de-gummed oil is then
removed before they can be used unwanted impurities. heated to high temperature of
for biodiesel production. 240 ~ 265 °C.
LIPICO Pretreatment process
A good pretreatment process will consists of: The oil is then stripped by live
ensure that quality of biodiesel o Degumming steam under high vacuum in the
can be produced consistently, o Adsorption deacidification column. Steam
high yield and in a most o Deacidification allows the evaporation of free
economical way. fatty acid so as to separate it
from the oil.
a) Degumming
Type of Impurities Fatty acid vapor is condensed
In the degumming section,
Impurities in crude oils and fats phosphoric acid or citric acid is as top distillate known as fatty
that will affect the yield and used to remove the non- acid distillate.
quality of biodiesel include: hydratable gums and trace metals The degummed, pretreated
in oil by converting them into non- (degummed, deacidified) oil will
• Free fatty acid soluble complexes.
• Moisture have a FFA content of less than
• Gums 0.1%.
b) Adsorption
• Solid particles
• Trace metals Adsorption clay (commonly
known as bleaching earth) or
Fats and oils may contain certain silica is used to adsorb the
amount of phospholipids (gums). insoluble precipitates formed in
If not properly removed, it can the degumming reaction. The
cause emulsions which in turn used clay will be filtered out using
resulted in significant product pressure leaf filters.
losses in the biodiesel production
process.

Free fatty acid will react with

alkaline catalyst used in the
biodiesel process to form soaps.
Therefore, it needs to be removed
to ensure minimum catalyst
consumption.

Feedstock for biodiesel

production usually does not
require the removal of color
bodies.

Deacidification plant with heating and cooling under vacuum for good
product oxidative stability and for FFA removal
 LIPICO Process Features:

o Effective removal of gums

ensure minimum
chemical consumption

o Effective removal of free

fatty acid to level suitable
for biodiesel production

o Continuous process

o Optimized heat recovery

system

o Consistent pre-treated oil

product quality - ensure
continuous production

o Fully automated for ease

Bleaching plant designed for removal of impurities such as gums, polar of operation
compounds and other metallic compounds in crude oil.

Pretreatment Process
Biodiesel Production:
Transesterification of oils and fats

What is Biodiesel?
Biodiesel is Fatty Acid Methyl
Esters (FAME) of vegetable oils
and fats or animal fats.

It can be mixed with any

proportion of fossil diesel and
distributed as commercial diesel
for transportation.

Reaction Chemistry
Biodiesel is produced by mixing
oils and fats with methanol in the
presence of catalyst.

The catalyst promotes the

exchange of fatty acids in
triglyceride molecules with
methanol to form methyl esters Left to Right: RBD Palm Oil, Palm Methyl Ester (Palm Biodiesel), Crude
and glycerol (as by-product). Glycerine (80%)

This chemical reaction is called

“Transesterification”.

Biodiesel Process
LIPICO Biodiesel Process
LIPICO biodiesel process is
based on a complete integration
of the following:
a) Transesterification
Reaction
LIPICO’s proprietary reactor
design allows continuous
removal of glycerol during
reaction in order to achieve
maximum conversion.
Glycerine is separated from
biodiesel using separator.
Washing
The use of counter-current
washing reduces water
consumption by 50% as
compared to one-stage
washing.
Centrifugal separator is
used in this application.
Drying
Residual moisture in methyl
ester is dried in vacuum
dryer before sending to
product storage tanks.
Typical 1,050 tpd biodiesel production plant.
Plant footprint 12m x 24 m
b) Glycerine-water treatment
Mixture of by-products
containing residual catalyst,
excess methanol, soap,
glycerine, and washed water
will undergo acid treatment
where strong acid (such as
hydrochloric acid) is used to
neutralize the residual
catalyst and to acidulate the
soap for converting into fatty
matter.
The treated glycerine-water-
methanol mixture is then
dosed with a controlled
amount of caustic to adjust
the pH of mixture to ~pH 7
prior to methanol
rectification.
c) Methanol Rectification
The mixture is heated and
distilled in the rectification
column where high purity
methanol is fully recovered
and recycled back to the
transesterification reaction.
d) Glycerine Evaporation
Glycerine-water from
methanol rectification plant
is evaporated to a purity of
78 ~ 82%.
Multiple-effect evaporator is
used to achieve high steam
economy.
Clean evaporated water is
re-used in the washing
section.
Biodiesel Cold Filtration:
Purification to produce haze-free biodiesel

What is Sterol Glucosides?

Sterol glucosides occur naturally
in vegetable oils and fats in
acylated sterol glucosides
(ASG) which is oil-soluble.

However, ASG are hydrolyzed

to free sterol glucosides (SG)
during alkali-catalyzed trans-
esterification process of the oil
for biodiesel production.

Due to low solubility of free SG

in biodiesel and its high melting
point (240 °C), it can be seen as
dispersed fine solid particles in
the biodiesel sample, causing
“hazy” appearance to the
biodiesel.

Change of ASG and SG content in oil before and after transesterification

Why Cold Filtration?
For biodiesel used as alternative
to transport fuel, issues such as
filter plugging and deposits on
injectors are detrimental to
engine operation due to
precipitate formation at low
temperature.

The sterol glucosides affect the

biodiesel production process.
For instance, the filter used in
the final polishing can become
filled/blinded with SG-rich solids,
resulting in costly process
interruptions and frequent filter
change-over to clean and
replace filter material.

Crystallization and
agglomeration of SG also
causing sedimentation issue in
the biodiesel storage tanks –
which leads to handling problem
and yield loss.

Cold filtered palm biodiesel are free from hazy appearance

Process Description
Cold filtration is used as a post-
treatment process for biodiesel
product.
It is a simple and direct
approach to removing free SG
which has low solubility in
biodiesel as well as other
particulate contaminants.
The process consists of:-
• Cold Conditioning
• Filtration
Process Flow LIPICO Process Features:
o Optimized condition for
Sterol Glucosides (SG)
precipitation in biodiesel
o Use of filter aid for
complete removal of
precipitated SG
o Reduction of Total
Contamination in filtered
biodiesel
o Consistent product quality

o Proven industrial
a) Cold Conditioning application with largest
During the conditioning step, running plant of 1,050 TPD.
biodiesel is first cooled
and/or chilled to induce the
crystallization of SG.

A suitable conditioning
temperature, sufficient
holding time along with good
agitation in the conditioning
tank is important to ensure a
homogeneous mixing and
complete precipitation of SG
in biodiesel before going
through filtration.

b) Filtration
Sterols are not easy to
handle and behave like
waxes/gums on the filter
septum.

The conditioned biodiesel is

required to be filtered
through a pre-coated filter
with addition of filter aid as
body feed to obtain a clean
and haze free filtered
product.
Biodiesel Distillation:
For producing high-quality distilled biodiesel

Why Biodiesel Distillation? Process Flow

Biodiesel produced from some
commercial plants contains
impurities (particularly
monoglycerides, sterol
glucosides, glycerol and etc)
which cannot be effectively
reduced due to limitation in
transesterification reaction and
conventional washing process.

Besides that, low quality

feedstock used in biodiesel
production will also resulted in
biodiesel with high level of
impurities.

There is a need for a purification

process to improve the final
quality of the biodiesel product
meeting stringent internationally
recognized standards.

Biodiesel Distillation Process

Process Description
Crude biodiesel is first dried and
de-aerated in the deaerator
which operates under vacuum.
This is important to prevent
possible oxidative reaction in the
subsequent operation.
De-aerated crude biodiesel is
then pumped into the distillation
column, which is equipped with
structured packing and
optionally with a heavy end
separation chamber at the
bottom.
Falling film evaporator is used to
ensure gentle thermal
evaporation of methyl esters
(biodiesel) without affecting
product quality.
Heavy residues can be
withdrawn separately or
recycled for partial re-distillation.
Distilled Product
Distilled biodiesel consists of
high ester content and is able to
pass the stringent ASTM cold
soak filtration test (CSFT).
Residue (Heavies)
The heavies contain solid
impurities (such as sterol
glucosides) and other high
boiling components
(monoglycerides, bound
glycerine, natural anti-oxidants,
sterols, etc)

LIPICO Process Features:

o Consistent product quality

o High quality distilled

biodiesel with low MG
content

o Low thermal effect on

product distillate

o Minimum loss as residue

o Optimized energy
consumption with heat
recovery

o Falling-film evaporation
provides short residence
time and reduced thermal
stress

Typical 1,000 tpd biodiesel distillation plant.

Plant footprint 8 m x 12 m
Glycerine Refining:
For Crude Glycerine from biodiesel plant
Source of Crude Glycerine
Different processes in the
oleochemical industry (splitting,
saponification,
transesterification) will produce
different quality of glycerine.
There are 3 most common types
of crude glycerine:
• Sweet water
(From fat splitting process -
Hydrolysis)
• Soap-Lye
(From soap manufacturing
process - Saponification)
• Crude glycerine
(From biodiesel production -
Transesterification)
Process Flow
Impurities in Crude Glycerine
Typical crude glycerine contains
the following:
• Glycerol
• Water
• Organic impurities (MONG)
• Salt (depending on the type
of transesterification
catalyst)
• Residual methanol (possible
if produced from biodiesel
process)
Glycerine Refining Process
Glycerine refining process
involves the following steps:
o Deaeration
o Distillation & Condensation
o Bleaching
o Continuous Salt Removal
Process Description
a) Deaeration
Crude glycerine is first treated
with sodium hydroxide. It is then
heated and de-aerated under
vacuum to remove residual
moisture, methanol (if any) and
un-dissolved gasses.
b) Distillation
Partially dried crude glycerine is
fed to the distillation still for
further heating under high
vacuum. Distillation is carried
out by means of circulation
within force-circulation heater
(using medium pressure steam)
at temperatures of 160 °C. Top
column pressure is maintained
at high vacuum to facilitate good
separation efficiency.
c) Condensation
Condensation of glycerine
vapors is effected in high-
efficiency structured packing
and special distributors.
The high purity distillate 1
(>99.7%) is obtained from a hot
condensation system
The glycerine from 2nd
condensation system is
recovered as technical grade
glycerine (90%) (also known as
yellow glycerine) or recycled
back to glycerine pretreatment
section.
Glycerine Distillation & Bleaching Process
d) Bleaching
Glycerine distillate 1 is filtered
through activated carbon bed at
80 °C to remove color
e) Salt Removal
When glycerine is distilled, the
non-boiling compounds (MONG,
Salt, Soap, etc) are being
concentrated.
Concentrated glycerine is
periodically bled off to decanter
system to remove salt as solid
discharge.
Liquid residue from decanter will
be sent to post distillation still
where glycerine is distilled off
further.
LIPICO Process Features:
o Tailor-made design for
crude glycerine feedstock
with different quality and
impurities
o Guaranteed high yield
with low glycerine loss
o Low ester content and
good color for refined
glycerine
o Continuous salt removing
with decanter system
particularly suitable for
crude glycerine from
biodiesel plant
o High efficiency structured
packing for separation
Re-Esterification:
Converting high FFA oil into feedstock for Biodiesel Plant

Biodiesel Feedstock Process Description

Flexibility
The key factor to profitability of a
biodiesel plant is closely related
to feedstock cost, product yield
and operating cost.
The ability to convert a lower-
cost feedstock, usually
associated with higher free fatty
acid (FFA) content, into
feedstock suitable for biodiesel
plant provide advantage to new
as well as existing biodiesel
plant producer with flexibility to
use feedstock from low to high
FFA content.
LIPICO’s re-esterification
process allows conversion of
low cost, low quality high FFA
fats and oils of vegetable or
animal sources into feedstock
suitable for biodiesel plant
(using transesterification route).
Feedstock containing fatty acid
is mixed with pre-calculated
quantity of glycerine and heated
using heat recovered from the
hot re-esterified product
continuously. The heated
mixture will be stored in a feed
tank and discharge to reactor
batch-wise.
The re-esterification reaction is
batch process. The reaction
mixture is heated to final
reaction temperature using
thermal system/medium
pressure steam whichever
available. The reaction is
operated under vacuum
condition and the water formed
during the reaction is
continuously removed. Once the
reaction is complete, the mixture
is discharge to drop tank.

Re-Esterification Reaction Process Flow

Re-esterification is the reaction
of free fatty acids (FFA) with
glycerol to produce mixture of
monoglycerides (MG),
diglyceride (DG) and triglyceride
(TG) with water is produced
during the reaction. The reaction
occurs under high temperature
of >200 °C and no catalyst is
required.

Reaction Chemistry:
FFA + Glycerol ↔ MG + H2O
FFA + MG ↔ DG + H2O
FFA + DG ↔ TG + H2O
Deacidification Process
For use as biodiesel process
feedstock, the FFA content in
the re-esterified oil need to be
reduced further to <0.1%.
Crude re-esterified oil is heated
to a temperature where fatty
acid is flashed. In the
deacidifcation column, fatty acid
is stripped off using live steam.
Hot deacidified oil is discharge
continuously to economizer for
heat recovery and cooled to
storage temperature.
Re-Esterification Process
Product Applications
Biodiesel Plant Feedstock
Re-Esterified oil is a mixture of
monoglycerides (MG) /
diglycerides (DG) / triglycerides
(TG) with < 0.1% FFA.
Biofuel
For re-esterified oil (without
deacidification treatment) which
contains 2 % ~ 3 % FFA, it can
be used readily as biofuel (fuel
for power generation plant)
LIPICO Process Features:
o Maximum heat recovery
with continuous heat
recovery of feed and re-
esterified product
o Short reaction time and
complete reaction
o No catalyst required
o Multiple feedstock with FFA
ranging from 10% - 100%
o Deacidification process for
converting to feedstock
for biodiesel production
 Process Technology
Process Technology

LIPICO Bioenergy undertakes projects in various renewable energy related and oleochemical processes:

• Biodiesel Technology
o Pretreatment
o Biodiesel Production
o Biodiesel Cold Filtration
o Biodiesel Distillation
o Fatty Acid Esterification
Technology
• Fatty Acid Technology
o Pressure Splitting of Fats and Oils
o Thermal Fractionation
o Straight Distillation
o Wet Fractionation

• Methyl Ester Technology

o Thermal Fractionation
o Straight Distillation
Degumming / Bleaching / Deodorization
• Glycerine Technology
o Biodiesel Crude Glycerine Treatment
o Sweet Water Treatment & Concentration
o Glycerine-Water Evaporation
o Glycerine Distillation / Refining

• PFAD Related Technology

o Calcium Soap Process
o Re-Esterification Process

• Others
o Pilot Plant

Contact Us:
LIPICO Bioenergy Pte Ltd
61 Bukit Batok Crescent
#06-03 Singapore 658078
Tel: +65-63167800
E-mail: sg.biomail@lipico.com

Find out more:

2015/10 Rev0