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Lewatit Ion Exchange Resins
Tailor-made solutions for biodiesel production
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Biodiesel production with Lewatit ion exchange
resins
Lewatit iex resins
Pure Biodiesel
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Biodiesel purification with Lewatit K 2567

• Lewatit K 2567 has specifically been developed
  for biodiesel purification and is used to remove
• glycerine, soaps, salts and to a certain
  extent, monoglycerides.
• It can replace the conventional water-wash,
  eliminate costly water stripping to dry the
  biodiesel
• and thereby reduce operating and
  investment costs.

Biodiesel
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Advantages of using Lewatit K2567

• Biodiesel purified with Lewatit K 2567 fulfills
  the stringent specification requirements
• of the European and American fuel
  industries.
• Lewatit K 2567 is a macroporous cation exchange
  resin with monodisperse bead
• sizing, to optimize break-through and
  pressure drop performance in packed beds.
• One liter of K 2567 will purify 11-14 tons
  biodiesel / year
• It can be reused many times, thus minimizing
  resin disposal costs.
• Resin lifetimes up to 7 years have been obtained.
• Therefore only relatively small beds are
  necessary for cycle times of 710 days
• It can be retrofitted into existing plants.
• All biodiesel qualities irrespective of the
  triglyceride source can be treated.
• It is currently used in plants ranging widely in
  size, from 10,000 ? 350,000 to/a.
• It is the most cost-effective ion exchange resin
  based purification system in the market.
• Lewatit K 2567 has been used for biodiesel
  production in Europe since 1997.

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Biodiesel quality standards ASTM
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Biodiesel quality standards Europe EN 14214
As specified for BD from rape seed oil (not all
specs. listed)
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Raw oil sources
Oil types
Palm Rape seed Soyabean Sunflower Canola Coconut
Jatropha Used cooking Animal fats
Biodiesel
Conversion

• High viscosity
• Poor combustion

Low viscosity Good combustion
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Raw oils chemical composition
Triglycerides
gt 95
O
Fatty-Acids
OH
0.1- 5
Micelles, phospholipids, proteins, mineral salts
Others
lt 1
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Triglyceride transesterification
Purified Triglycerides
gt 95

NaOCH3
CH3OH
Top Layer
Biodiesel phase
Glycerine phase
Bottom Layer
The catalyst Na-methoxide is also a drying
agent and should be used instead of NaOH to
suppress the formation of soap.
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Transesterification byproduct soap
O
Free fatty acid (FFA)
OH

lt 5
NaOCH3
O
Soap
ONa

Methanol
CH3OH
The FFA content of the triglycerides should be
maintained below 0.5 to minimize soap formation
and maximize BD selectivity, i.e. FFAs should be
esterified to Me-esters before transesterification
. FFAs can be esterified with H2SO4 or Lewatit K
2621 as catalysts.
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Free fatty acids removal with Lewatit K 2621
Design for an 8,000 to/a esterification unit
for Reduction of free fatty acids (FFAs) from
triglycerides with Lewatit K 2621
K 2621
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Classical biodiesel production process
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Purification with Lewatit K 2567
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Lewatit K 2567 vs water wash
Purification with water wash
Purification with Lewatit K 2567
Water
Glyc. adsorption desorption
Water strip
Water strip
One column of resin completely replaces the water
washing system!!
Water wash
Water glycerine salts
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Lewatit K 2567 vs water wash
Purification with water wash
Purification with Lewatit K 2567
Many biodiesel plants already use NaOCH3 for
transesterification, i.e. the streams are
already very dry. Water efficiently
removes impurities but needs to be stripped
down down to lt500 ppm in the purified
biodiesel. In classical biodiesel plants, dry
streams are wetted and redried at subtantial
cost.
With K 2567, dry biodiesel streams remain
dry. Only methanol is required as a
washing agent to regenerate the resin. The
washing effluent is recycled to the
transesterification.
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Mechanism of glycerine adsorption
Dry Lewatit K 2567 is hygrosopic and strongly
hydrogen-bonds to alcohols and water. Glycerine
is a polar tri-alcohol and is very efficiently
removed from low polarity biodiesel esters.
Na
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Solvation with glycerine
MeOH-washed, dry resin
Glycerine-solvated resin
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Mechanism of salts and soaps adsorption
Glycerine layer
SO3-
Na
K2567
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Impurities adsorption in glycerine
Transesterification phase separation
Capture of ionic impurities on glycerine phase of
K 2567
Biodiesel phase clean
K 2567 Glycerine phase High concentrations
of ionic impurities soaps
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Structure of Lewatit K 2567
Monodisperse bead sizing, hexagonal closest
packing
K 2567 sponge-structure
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Application mode of Lewatit K2567
Alternate loading and washing
Washing with dry MeOH
Biodiesel glycerine
Lewatit K 2567
Transesterification
Purified biodiesel
MeOH glycerine
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Regeneration / cleaning with methanol
Raw oils
MeOH glycerine salts soaps
Methanol
Transesterification
K 2567 glycerine salts soaps
K 2567 clean
Methanol
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Operating conditions
Preconditioning
Biodiesel from phase separation glycerine 600
4000 ppm soap 10 500 ppm

• Fresh K 2567 is first preconditioned by drying
  with 3-4 bed volumes MeOH at
• 2BV/h. The MeOH is then drained and the
  biodiesel passed into the reactor.
• Before the MeOH wash, the biodiesel is also
  drained.
• After preconditioning, K 2567 is only subjected
  to alternate MeOH / biodiesel
• treatments and never washed with water.
• 100 bed volume water-wet, shrinks to 95 in
  MeOH, further shrinks to 90
• in biodiesel glycerine

Operating parameters Temperature 30C
40C LHSV 1.5 2 (BV biodiesel/hr) Bed
height 1 2 m Freeboard 20 Operating
capacity 250 g glycerine/liter Regeneration
MeOH _at_ 20-35C Regeneration volume 5-10 BV to
transesterification Resin life 4-5 years
(average) BV bed volumes Please refer to
us for specific design details
Lewatit K 2567
Refined biodiesel glycerine lt10 ppm, soap lt 5
ppm
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Plant configuration

• Depending on the the amount of biodiesel
  produced and manufacturing site infrastructure,
• any of the configurations A-C can be used.
• Greatest flexibility is obtained with the
  classical lead-lag setup, whereby the freshly
  MeOH-
• regenerated reactor is switched to the
  lag-position.

B 1x in operation, 1x in standby
A Single unit
C 2 units in series lead-lag
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Operating data
Adsorption of glycerine soaps from rape seed
biodiesel with Lewatit K 2567
at 2 BV/h and 28C
800
glycerine inlet
soaps inlet
700
glycerine outlet
soaps outlet
600
500
ppm
400
300
200
100
0
5
10
15
20
25
30
35
Bed volumes biodiesel from rape seed oil
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Basic design
This basic design can be scaled linearly for
plant sizing ranging from 1,000 ? 300,000 to/a.
bed depth should be kept in the range 1.5
meters (1,000 to/a) to 3 meters (300,000
to/a) Variable, depending on the influent
glycerine concentration.
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Competitive technologies and resin cost of
operation
Competitive ion exchange resin-based biodiesel
purification processes are also available
involving once-only use of disposable resin
without regeneration. A comparison of the two
approaches is summarised in the following tables
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Glycerine salts-removal with Lewatit MDS 1368
Design for a 2000 to/a glycerine purification
unit via Ion Exclusion Chromatography with Lewati
t MDS 1368-Na 350µ
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Glycerine purification with Lewatit MDS 1368
MDS 1368-Na 350µ
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Glycerine polishing with Lewatit S 2528 / S 4268
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Biodiesel and glycerine purification with
Lewatit iex resins
Transesterification
K 2567
Biodiesel phase
MDS 1368
Glycerine phase
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Additional information at www. lewatit.com
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Legal note
This information and our technical advice -
whether verbal, in writing or by way of trials -
are given in good faith but without warranty, and
this also applies where proprietary rights of
third parties are involved. Our advice does not
release you from the obligation to verify the
information currently provided (especially that
contained in our safety data and technical
information sheets) and to test our products as
to their suitability for the intended processes
and uses. The application, use and processing of
our products and the products manufactured by you
on the basis of our technical advice are beyond
our control and, therefore, entirely your own
responsibility. Our products are sold and our
advisory service is given in accordance with the
current version of our General Conditions of Sale
and Delivery.