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Lewatit Ion Exchange Resins

Tailor-made solutions for


GreenFuels production

Edition July. 2012

Pure biodiesel & glycerine with Lewatit ion exchange resins

Lewatit
iex resins

Pure Biodiesel
Pure Glycerine
2

Edition July. 2012

The Lewatit GreenFuels product line for biodiesel / glycerine

GF 101

Esterification catalyst for FFA removal from triglycerides

GF 202

Adsorber for glycerine, soaps, salts, water, MeOH

GF 303

Separation of soaps and salts from glycerine

GF 404

Polisher, cation removal

GF 505

Polisher, anion removal, decolorization

Edition July. 2012

Biodiesel and glycerine purification with Lewatit GF-Resins


GF 101

Triglycerides

(FFA removal)

Transesterification

Glycerine
+ soap

FAME

Biodiesel
+ impurities

Edition July. 2012

GF 303

Glycerine
+ salts

(salts remova)

FFA

GF 404

Acid Split
(polishing)

GF 101

GF 505

(esterification)

(polishing)

GF 202
(purification)

Pure biodiesel

Pure Glycerine

Biodiesel molecular structure


Major fatty acid methyl ester components of biodiesel
Methyl palmitate

O
O

CH3

Methyl oleate

CH3

Methyl linoleate

O
O

Edition July. 2012

CH3

Raw oil sources for biodiesel production


Oil types
Palm
Rape seed
Soyabean
Sunflower
Canola
Coconut
Jatropha
Used cooking
Animal fats

High viscosity
Poor combustion

Edition July. 2012

Conversion

Biodiesel

Low viscosity
Good combustion

Raw oils chemical composition


O
O
O

Triglycerides
> 95%

O
O
O

Fatty-Acids:
0.1- 5%

Others:
< 1%

Edition July. 2012

O
OH

Micelles, phospholipids, proteins, mineral salts

Biodiesel quality standards ASTM

Property

ASTM

Flash point

93

Lim its
100 min.

Units
C

Water sediment

2709

0.05 max.

vol. %

Carbon residue

4530

0.050 max.

w t. %

Kin. viscosity 40C

445

1.9 - 6.0

Sulfur

5453

0.05 max.

Cetane

613

40 min.

Cloud point

2500

by customer

Copper corrosion

130

No 3 max.

Acid number

664

0.08 max.

Sulfated ash

874

0.020 m ax.

w t. %

Free glycerine

6584

0.020 m ax.

w t. %

Total glycerine

6584

0.240 max.

w t. %

Edition July. 2012

mm/sec.
w t. %
C
mg KOH/g

Biodiesel quality standards Europe: EN 14214 *


Property

Limits

Flash point

> 101

Water content

Units

Test method

ISO CD 3679e

500

mg/kg

EN ISO 12937

Alkali metals

5 max.

mg/kg

pr EN 14108

Viscosity 40C

3.5 - 5.0

mm/sec.

EN ISO 3104

Sulfur

10 max.

mg/kg

Cetane

51 min.

Acid number

0.5 max.

mg KOH/g

pr EN 14104

Sulfated ash

0.02 m ax.

% (m /m )

ISO 3987

Free glycerine

0.02 m ax.

%(m /m )

pr EN 14105

Monoglycerides

0.8 max

%(m/m)

Diglycerides

0.2 max.

%(m/m)

Triglycerides

0.2 max.

%(m/m)

pr EN 14105

Total glycerine

0.25 max.

w t. %

pr EN 141101

Methanol content

0.2 max.

%(m/m)

EN ISO 5165

* As specified for BD from rape seed oil (not all specs. listed)

Edition July. 2012

Degumming, cleaning of triglycerides


Phosphoric acid
Raw Triglycerides

Heat
Water

Pure Triglycerides

Centrifuge II

Phosphatide waste

Filter
Bleaching earth
10

Edition July. 2012

Centrifuge I

Triglyceride transesterification
O

Purified Triglycerides

Recommended purity
> 95%

O
O
O

Transesterification catalyst

CH3OH
O

Top Layer

Biodiesel phase

OCH3

Glycerine phase
Bottom Layer

11

Edition July. 2012

OH

HO
OH

Transesterification catalysts

The most commonly used transesterification catalysts are NaOH, KOH and their methanolic
alkoxides NaOCH3, KOCH3.
Currently >90% of all large scale industrial plants world-wide use alkoxide catalysts:

12

Reduced soap formation

Better separation of glycerine and biodiesel phases.

Good drying agents

Edition July. 2012

Enhanced soap formation with NaOH / KOH

NaOH, KOH react with FFA to form soap + water


Additional soap is formed by the OH-catalysed hydrolysis of ester
NaOH, KOH double the formation of soap relative to NaOMe, KOMe
O
NaOH +

OH

FFA

ONa

Soap

ONa

Soap

O
H2
O

+
O

CH3OH +
OHO
H2
O
13

Edition July. 2012

OCH3

FAME

Reduced soap formation with alkoxides


With alkoxides, soaps are only formed by neutralisation of FFA:

O
NaOCH3 +

OH

FFA

ONa

Soap

O
CH3OH

In order to reduce alkoxide catalyst costs, Lewatit GF 101 can be utilised to effectively
eliminate FFA from the triglyceride feedstocks.

14

Edition July. 2012

Esterification of free fatty acids with catalyst Lewatit GF 101

Free fatty acid (FFA*)


1 100%

OH
+
HOCH3

GF 101
O

Fatty acid methyl ester


(FAME)

OCH3
+
H2O

*The FFA feeds must be degummed and cleaned prior to passage through the GF 101

15

Edition July. 2012

Esterification of free fatty acids with catalyst Lewatit GF 101


GF 101

Triglycerides

(FFA removal)

Transesterification

Glycerine
+ soap

FAME

Biodiesel
+ impurities

16

Edition July. 2012

GF 303

Glycerine
+ salts

(salts remova)

FFA

GF 404

Acid Split
(polishing)

GF 101

GF 505

(esterification)

(polishing)

GF 202
(purification)

Pure biodiesel

Pure Glycerine

Esterification of free fatty acids with catalyst Lewatit GF 101


Design for an 8,000 to/a esterification unit
for
reduction of free fatty acids (FFAs) from triglycerides
with
Catalyst Lewatit GF 101
GF 101

Upflow operation prevents


bed plugging and enables
long catalyst life

Oil-Feed

Triglycerides with FFAs

Resin volume:

3.0 m3

Diameter

1.0 m

Bed depth

4.0 m

Temperature

90-110C

Oil + MeOH feed

900 kg / h (upflow)

FFA content in oil

1-10%

10-50%

50-100%

Oil feed (kg/h)

700

650

600

MeOH feed (kg/h)

200

250

350

FFA conversion

95%

95%

95%

Catalyst lifetime

3 years
Industrial applications

17

Edition July. 2012

Pilot plants

Esterification of free fatty acids with catalyst Lewatit GF 101


Guard - bed
Triglyceride + FFA

Esterification reactor
Triglyceride + FFA-Methyl ester

MeOH
Prior to the esterification step it is recommendable to include a guard bed with GF 101 for
removal of any potential cationic and amine catalyst poisons, especially in conjunction with
used oils from the foodstuffs industries.
Guard bed sizing:
Bed height:
Replacement:
18

Edition July. 2012

20-30% of the resin volume in the esterification reactor


2m
6-9 monthly intervals (once-use / non-regeneration resin)

Basic plant design for a 2-Step esterification with GF 101


GF 101

GF 101

FAME

MeOH + H2O

MeOH + H2O

MeOH + H2O

MeOH

19

Edition July. 2012

FAME Strip

FAME / FFA

MeOH Dist.

FFA

H2O

FAME

Biodiesel purification with Lewatit GF 202

Lewatit GF 202 removes glycerine, soaps, waxes, salts, water, methanol.

It can replace the conventional water-wash, eliminate costly water stripping


and reduce investment and operating costs.

20

Edition July. 2012

Features of Lewatit GF 202 in biodiesel purification

21

Fulfills the stringent specification requirements of the fuel industries

One liter of GF 202 will typically purify 10 tons biodiesel / year

Regenerable, long resin lifetimes

Can be retrofitted into existing plants using water-wash

All biodiesel qualities irrespective of the triglyceride source can be treated

Usable in plants ranging from 100 1,000,000 to/a

The most cost-effective resin-based purification system in the market

Edition July. 2012

Biodiesel purification with Lewatit GF 202


GF 101

Triglycerides

(FFA removal)

Transesterification

Glycerine
+ soap

FAME

Biodiesel
+ impurities

22

Edition July. 2012

GF 303

Glycerine
+ salts

(salts remova)

FFA

GF 404

Acid Split
(polishing)

GF 101

GF 505

(esterification)

(polishing)

GF 202
(purification)

Pure biodiesel

Pure Glycerine

Classical biodiesel production process


Low-acid
triglycerides

MeOH

MeOK or
KOH

HCl

Baynox
Antioxidant

Water

Water strip

Water
wash

Water strip

Methyl ester phase

MeOH Strip

Esterification

Transesterification

Separation
Glycerine phase

Glycerine purification

23

Edition July. 2012

MeOH Strip

Raw oils with


free fatty acids

MeOH +
Gly. + salts

Water +
Glycerine +
Salts

Glycerine +
Salts

Pure
methyl esters
(Biodiesel)

Purification with Lewatit GF 202


Low-acid
triglycerides

MeOH

MeOK or
KOH

Baynox
Antioxidant

HCl

Separation

Adsorption / desorption

Methyl ester phase

MeOH Strip

Esterification

Transesterification

Lewatit GF 202

Glycerine phase

Glycerine purification

Lewatit
GF 303, 404, 505

24

Edition July. 2012

MeOH Strip

Raw oils with


free fatty acids

MeOH +
glycerine

Glycerine +
Salts

Pure
methyl esters
(biodiesel)

Lewatit GF 202 vs water wash


Purification with Lewatit GF 202

Purification with water wash


Water

Glycerine adsorption / desorption

Edition July. 2012

Water strip

25

Water strip

Water wash
Water +
glycerine +
salts

One column of resin


completely replaces
the water washing
system!!

Lewatit GF 202 vs water wash

Purification with water wash

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 <500 ppm in the
purified biodiesel.
In classical biodiesel plants, dry streams are
wetted and redried at subtantial cost.

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Edition July. 2012

Purification with Lewatit GF 202

With GF 202, 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.

Mechanism of glycerine adsorption


Dry Lewatit GF 202 is
hygroscopic and strongly
hydrogen-bonds to alcohols
and water.
Glycerine is a polar tri-alcohol
and is very efficiently
removed from low polarity
biodiesel esters.

HO
HO

GF 202

Hydrogen bonding

S O

HO
HO

Edition July. 2012

Glycerine

HO

27

OH

HO
Na+

HO
OH

Mechanism of salts and soaps adsorption on GF202


The glycerine layer on the GF 202 adsorbs polar and ionic impurities.
Impurities are not as efficiently adsorbed if no glycerine is present.

Glycerine layer
Mg++

Typical impurities in raw


BD to resin (MeOHstripped)

Cl-

K+
-O2C

H2O

GF 202
-O2C

Na+

MeOH
SO42- Ca++

28

Edition July. 2012

conc. (ppm)
Glycerine < 1500
Soaps
< 500
Water
< 500
MeOH
< 1000
Salts
< 1000

Mechanism of salts and soaps adsorption on GF202

Important notice
Prior to passage through GF 202, the ester phase should

not be pretreated
to remove the glycerine, either by water wash, dry resins,
or inorganic filtration media.
The presence of glycerine is essential for the adsorption of soaps and salts!!

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Edition July. 2012

Plant operating data for Lewatit GF 202


Adsorption of glycerine & soaps from rape seed biodiesel at 2 BV/h, 28C
800

glycerine inlet
soaps inlet
glycerine outlet
soaps outlet

700
600

ppm

500
400

300
200
100
0
5

30

Edition July. 2012

10

15
20
25
Bed volumes biodiesel from rape seed oil

30

35

Impurities adsorption in glycerine


Transesterification
phase separation

Capture of ionic impurities on


glycerine phase of GF 202

Biodiesel phase
+

Biodiesel phase

Small concentrations of
ionic impurities + soaps

clean

GF 202
+

Glycerine phase
Glycerine phase
+
High concentrations of
ionic impurities + soaps

31

Edition July. 2012

+
High concentrations of
ionic impurities + soaps

Structure of Lewatit GF 202


Monodisperse bead sizing, hexagonal closest packing

GF 202 sponge-structure
32

Edition July. 2012

Application mode of Lewatit GF 202


Alternate loading and regeneration
Washing with dry, clean MeOH

Biodiesel + glycerine
The feed must be
MeOH-stripped!!

Lewatit
GF 202

MeOH is either recycled to the transesterification reactor,


the MeOH storage tank, or a MeOH strip column,
depending on the water concentration in the effluent
from Lewatit GF 202
The water concentration is dependent on whether
NaOMe or NaOH / KOH is used in the transesterification
(ref. following slides)

Purified biodiesel

33

Edition July. 2012

The MeOH regeneration is effectively cost neutral !!

MeOH + glycerine
(+ water traces*)

Regeneration / cleaning with methanol

Raw oils
MeOH
Methanol

+
glycerine
+
salts & soaps

GF 202
+
glycerine
+
salts & soaps

Transesterification
GF 202
clean

Methanol

34

Edition July. 2012

Operating conditions
Raw BD (MeOH-stripped)
Impurities
Glycerine
Soaps
Water
MeOH
Salts

Preconditioning of GF 202

Typical conc. (ppm)


< 1500
< 500
< 500
< 1000
< 1000

Fresh GF 202 is water-wet and needs to be


preconditioned by drying with 3-4 bed volumes dry
MeOH at 1-2BV/h, (single pass without recycle!)
The MeOH is then drained and the biodiesel passed
into the reactor. Before the MeOH wash, the
biodiesel is also drained.
Lewatit
GF 202

After preconditioning, GF 202 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

Refined biodiesel
35

Edition July. 2012

Operating conditions
Raw BD (MeOH-stripped)
Impurities
Glycerine
Soaps
Water
MeOH
Salts

Glycerine adsorption by GF 202

Typical conc. (ppm)


< 1500
< 500
< 500
< 1000
< 1000

Lewatit
GF 202

Throughput (LHSV)

1.5 2 (BV* biodiesel / hr)

Temperature:

30C 50 70C

Bed height:

1 2 m**

Freeboard:

20%

Operating capacity:

250 g glycerine / liter (max.)

*BV = bed volumes


** Please refer to us for specific design details

Refined biodiesel
36

Edition July. 2012

Operating conditions
Raw BD (MeOH-stripped)
Impurities
Glycerine
Soaps
Water
MeOH
Salts

Regeneration with methanol

Typical conc. (ppm)


< 1500
< 500
< 500
< 1000
< 1000

Lewatit
GF 202

Refined biodiesel
37

Edition July. 2012

Temperature:

20 60C

Regeneration volume:

3 - 4 BV MeOH
at 2 BV/h

Cycle time between regen.:

8-10 days

Resin life:

4-5 years (average)

Operating conditions
MeOH regeneration of GF202 vs glycerol / MeOH in Me-ester

Glycerol (ppm)

Bed vols Me-ester


through GF202
between MeOH
regenerations

MeOH (%) in Me-Ester


Example: Biodiesel / glycerol stripped down to 0.5% MeOH after transesterification equilibrates to approx 800 ppm glycerol
in the ester phase after phase separation, enabling passage of 220 BV through GF202 between MeOH regenerations.

Glycerol binding capacity of GF 202: at 0.1% MeOH approx. 200 g/l ; at 4% MeOH approx 160 g/l. (Soap < 0.1%)

38

Edition July. 2012

Operating conditions
Raw BD (MeOH-stripped)
Impurities
Glycerine
Soaps
Water
MeOH
Salts

MeOH displacement after regeneration

Typical conc. (ppm)


< 1500
< 500
< 500
< 1000
< 1000

The reactor is first drained then blown through with


nitrogen to displace residual methanol from the void
volume between the beads.

Lewatit
GF 202

Biodiesel is introduced from the bottom of the reactor


at 2 BV/h, to displace any nitrogen bubbles.
As MeOH is less dense than biodiesel, it is
initially carried out of the reactor as a separate phase
and can be recycled to the transesterification.
The first 5-7 bed vols of biodiesel can either be passed
upflow or downflow through the bed at 2 BV/h, or
downflow at 4 BV/h, at temperatures in the range
25-50C. This biodiesel should be MeOH-stripped.

Refined biodiesel
39

Edition July. 2012

The next approx 8-20 bed volumes can also be stripped


or sent to storage for further dilution with subsequently
eluted BD (ref. MeOH elution profile on next page)

Elution profile of GF 202 after regeneration with methanol


Throughput: 2 BV/h.
MeOH concentration in BD effluent (%)

1,2
MeOH strip until the specification level is reached

Or
Biodiesel to storage for dilution
with BD containing MeOH < 0.2%

MeOH strip

0,8

0,6

0,4

0,2
MeOH specification level

0
0

10

15

Bed volumes biodiesel

40

Edition July. 2012

20

25

Plant configuration
Depending on the the amount of biodiesel produced and manufacturing site
infrastructure, any of the configurations A-C can be used.
We recommend the classical lead-lag setup, whereby the freshly MeOH
regenerated reactor is switched to the lag-position.

A: Single unit

GF 202

41

Edition July. 2012

B: 1x in operation, 1x in standby

GF 202

GF 202

C: 2 units in series: lead-lag

GF 202

GF 202

Basic design for a 100,000 to/a biodiesel purification unit


Capacity

100,000 to/a*
30 mio. gal/a

Annual operation
Throughput

8,000 h
12.5 to/h
15,600 l/h

69 gal./min.
LHSV
Bed volume
Bed height
Pressure drop
Glycerine capacity

42

2 bed vols/h
7,800 liters GF 202
2 meter
0.4 bar
150-250 g/liter resin**

Glycerine conc

800 ppm

Cycle time

156 h

Resin lifetime

Edition July. 2012

This basic design can be scaled


linearly for plant sizing ranging
from 100 1,00,000 to/a

5 years

**Variable, depending on the


influent glycerine concentration.

Summary biodiesel purification with Lewatit GF 202

Substitutes conventional water-wash


Generates specification-grade BD
pH neutral operation, no impurities emitted by the resin

Regenerable system
Cost-neutral regeneration
Applicable in 100 1,000,000 to/a plants

> 10 years production experience

43

Edition July. 2012

Cost comparison: Lewatit GF 202 vs alternative technologies


Alternatives to Lewatit GF 202 for biodiesel purification are conventional water wash,
once-use inorganic silicate-based filtration media and once-use dried ion
exchange resins.
Handling- and cost-comparisons are summarised in the following tables.
Lewatit GF 202

Dry resins

Resin disposal every 5 years

Resin disposal several times / year

Clean, smooth operation

Regular opening of reactor & waste handling

No regular BD loss

Regular BD loss in resin during dispoal

No swelling relative to delivery form

Resin swelling of 100-150%

90% utilization of reactor volume

30% utilization of reactor volume

44

Edition July. 2012

Cost comparison: Lewatit GF 202 vs alternative technologies

Application

45

Cost / ton biodiesel ($)

Lewatit GF 202 (lifetime 5 years minimum)

0.35

Dry resins (one way application)

13.00

Inorganic filtration media (one way application)

20.00

Water wash

25.00

Edition July. 2012

Reactor configuration: Lewatit vs dry resin in BD purification


Lewatit purification unit

Dry resin purification unit

2 reactors / train

4 reactors / train

GF 202

46

Edition July. 2012

GF 202

Lewatit GF 202 reference plants


Lewatit GF 202 has been used in
industrial-scale biodiesel purification since
1996.

Of the numerous companies using Lewatit


biodiesel purification know-how,
Oil.B located near Milano, Italy, has
generously permitted the citation of its
plant as a reference.

The first batch of GF 202 was used for

7 years.

For further information please contact


your local Lewatit agent.

47

Edition July. 2012

Company
Location
Capacity
Startup

Oil.B
Solbiate Olona, Milano, Italy
250,000 to/a (3 x 8 cbm reactors, 2 trains)
2001

Glycerine processing with GF 303, GF 404, GF 505


GF 101

Triglycerides

(FFA removal)

Transesterification

Glycerine
+ soap

FAME

Biodiesel
+ impurities

48

Edition July. 2012

GF 303

Glycerine
+ salts

(salts remova)

FFA

GF 404

Acid Split
(polishing)

GF 101

GF 505

(esterification)

(polishing)

GF 202
(purification)

Pure biodiesel

Pure Glycerine

Salts-removal from glycerine with Lewatit GF 303

Lewatit GF 303 is a chromatography resin designed for


salts removal from glycerine by ion exclusion.
Raw glycerine from the acid split is introduced into the top
of the resin bed.
The glycerine is then eluted with demineralised water.
The effluent is fractionated and monitored by refractive
index (RI) and conductivity (S).
Salts are eliminated first through ion exclusion, followed by
glycerine.
RI & S

49

Edition July. 2012

The principle of Ion Exclusion


GF 303

Na+
Na+
SO3-

SO3-

Na+

Na+

Na+

SO3-

Edition July. 2012

Na+
SO3

+
-

SO3-

Na+ SO - SO 3
3

SO3-

50

GF 303

+
-

+
-

The principle of Ion Exclusion

Na+ Cl- Na+ Cl- Na+ Cl- Na+ Cl- Na+ Cl-

+
-

+
-

51

Edition July. 2012

+ +
-

+
+

+
-

+
-

The principle of Ion Exclusion


Net effect = ions
pass around the resin beads

Na+
Cl-

Cl-

Na+ Cl-

+
-

Na+
Cl-

+
-

52

Edition July. 2012

Na+

ClNa+ ClCl- Na+

Na+ Cl-

+
-

Cl-

GF 303

Na+

Cl-

+
-

ClNa+
Cl-

+
-

Na+

+
-

Ion Exclusion
Glycerine hydrogen bonds to the water in the GF 303

OH

HO
OH

+
-

Edition July. 2012

OH

+
-

53

OH

HO

+
-

Ion Exclusion with Lewatit GF 303

HO

OH
OH
Na+ Cl-

Glycerine and salt


from the acid split
are pulsed as an
80% concentrate
in demineralised
water every 0.8
bed volumes of
throughput onto
the top of the
column

54

Edition July. 2012

HO

Glycerine and salt


are pushed
through the bed
with demineralised
water at 0.5 bed
volumes/h
This dilutes the
Glycerine.

OH
OH
Na+ Cl-

OH

HO
OH

GF 303

Glycerine is
retained and
elutes later

GF 303
Na+ Cl-

Salt is chargerepelled and


elutes first

Glycerine purification with Lewatit GF 303

Salts [*100 S/cm]

GF 303

60

60

50

50

40

40

30

30

20

20

10

10

0
0,2

0,4

0,6

Filtered bed volume

55

Edition July. 2012

0,8

)%( Glycerine

Separation of glycerine and salts from acid split

Lab arrangement for glycerine purification


Column diameter

cm

Column square area

sqcm

19.63

Resin bed depth

mm

2000

Resin volume

ml

3926

Flow rate

ml/min

NaCl

Fractions

Glycerol injection

minutes

6.25

Glycerol conc. feed

Glycerol injection

ml/cycle

200

ml/fract
NaCl ppm

80

1920

g/cycle

250

m/h

0.98

glyc/cycle

200

bv/h

0.48

g gly /l
resin

50

Rinse water flow

ml/min

32

Water injection

minutes

73.75

ml/cycle

2,360

Total cycle length

min

Total volume/cycle

ml

Cycles / day

56

32

Feed

ml/h

ppm

Temperature

5,0

Edition July. 2012

16
1,300
20

50,000

80
2560
18

80

1 to/d glycerine requires 1 cbm resin

ml/fract
NaCl ppm

1,260
49,980

Deashing of glycerine from rape seed oil glycerine


Test procedure
column

temperature
feed

RI & S

57

Edition July. 2012

glas column with heating jacket,


diameter: 50 mm,
bed depth: 200 cm = 3930 ml resin
70 C
glycerine from rape seed oil
83 % Glycerol
4.7 % NaCl

eluent

demin. water (conductivity 0.4 S)

Injection / pulse:

200 ml glycerine solution

flow rate

32 ml/ min = 100 cm/h

Test result of glycerine-NaCl separation


2.500

1,365
Conductivity NaCl

Refractive index glycerine


1,36

2.000

1,355

1,35

RI

1.500

1.000
1,345
500

1,34

0
0

200

400

600

time (min)
58

Edition July. 2012

800

1000

1,335
1200

Glycerine purification with Lewatit GF 303


Raw glycerine

99.8% deashed glycerine

GF 303

Color

650 IU

Color

200 IU

NaCl

50,000 ppm

NaCl

100 ppm

Glycerine

80% in water

Glycerine

20% in water

Strongly acidic,
monodisperse
gel-type
cation exchange
resin

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Edition July. 2012

Plant for a 10,000 to/a fixed-bed glycerine deashing unit


Design for a 10,000 to/a glycerine purification unit
via
Ion Exclusion Chromatography
with
Lewatit GF 303

GF 303

60

Edition July. 2012

Feed

Glycerine from BD transesterification

Resin volume

30 m3

Diameter

2.5 m

Bed depth

6.0 m

Loading / cycle

1.8 to. glycerine in 0.5 to. water

Salts conc. in raw glycerine

5-7 wt%

Eluent

demin. water

Temperature

80 C

LHSV (bed vol./h)

0.5

Effluent concentration

1.8 to. glycerine in 7.2 to. water []

Resin lifetime

5 years

Glycerine polishing with Lewatit GF 404 / GF 505


Salts-free glycerine

Polished glycerine

GF 404

GF 505

Color

200 IU

Color

< 1 IU

NaCl

100 ppm

NaCl

< 1 ppm

Glycerine

20% in water

Glycerine

20% in water

Strongly acidic,
monodisperse
macroporous
cation exchange
resin

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Edition July. 2012

Intermediate-basic
monodisperse
macroporous
anion exchange
resin

Plant for a 10,000 to/a glycerine polishing unit

NaOH

HCl

GF 404
5cbm

62

NaCl

100 ppm

Color

200 ICU

Glycerine

20% in water

Flow rate

20 cbm/h

Temp.

60C

Capacity

3000 cbm / cycle

Cycle time

150 h

Edition July. 2012

NaCl

<1 ppm

Color

<1 ICU

Glycerine

20% in water

GF 505
6 cbm

Waste

Biodiesel and glycerine purification with Lewatit iex resins

Transesterification
GF 101

GF 202

GF 303
Biodiesel phase
GF 404

Glycerine phase

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Edition July. 2012

GF 505

For additional Information

www.lewatit.com

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Edition July. 2012

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.
Lewatit is a registered trademark of Lanxess Deutschland GmbH.

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Edition July. 2012

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