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Process development for extraction and purification of bioproducts

(2)

PROCESS DEVELOPMENT FOR

EXTRACTION AND PURIFICATION OF

BIOPRODUCTS

Ashwani Kumar

AMTEC, Kuala Lumpur

May 2009

(3)

Lei Xu

NRCan’s-CBIN

Karen Lamb

NRC-NBP &

Linda Layton

AAFC-ABIP

Pinghai Shao

Nikhil Kawachale

(4)

• Introduction – importance of biomass

• NRC’s National Bioproduct Program

• Research Projects –two recent examples

– Nutraceuticals – process development

– Recovery and purification of chemicals in biochemical

conversion of biomass components

(5)

• Canada’s biomass harvest

143

Mt Carbon / year

• Available residue/waste

60

Mt Carbon / year

• Energy content

1.5-2.2 EJ/year (E=10

18

)

• Represents 18-

27% of Canada’s annual energy needs

• Challenge - biomass conversion

– Renewable energy and products comparable to fossil

fuel-derived products,

– Profitable,

– Significant environmental and social benefits

(6)

Primary

– unprocessed - direct combustion

Secondary- extraction of value-added compounds.

processed

– charcoal, gases, liquid fuel

Thermo-chemical

pyrolysis, gasification

– synthesis

gas, bio-oil,

source of chemicals

Physico-chemical

– seed oil, conversion to

biodiesel

Bio-chemical

– biological processes – ethanol,

biogas,

chemicals (e.g. diols)

(7)

Focus - Thermo-chemical & Physico-chemical

Biomass

Bio-oil

Gases

Bio-refinery concept

Nutraceuticals

Basic chemicals

Phenols,

Flavoring agents,

Polymers

CO, H

2

, CH

4

Fuel

Syngas, hydrogen

Feed pre-treatment

Reaction Engineering,

Fractionation

Material development

Characterization

Process development

Pilot scale studies

(8)

Focus

– Biochemical Conversion

Biomass

Bio-refinery Concept

Cellulose

Hemi-cellulose

Pentoses

Lignins

Butanediol,

ethanol,

acetoine

Recovery and purification

of butanediol

(9)

• Bio-oil – stabilization and characterization

• Extraction and purification from biomass extracts – nutraceuticals

• Recovery and purification of butanediol – membrane process

• Biogas Upgrading – new membranes

• CO

2

Capture

– new membranes

• CFD Studies – membrane test cells

(10)

• Skim Soymilk – whey contained 1/3 of the total isoflavones

(Daidzein and genistein as glucoside and esters)

• Recovery of isoflavones using a membrane-based process

– (UF/diafiltration, RO)

• Soy-based isoflavones –estrogenic activity – health concerns

• Alternate source – red clover flowers – biochanin A, formononetin

(Genistiein and daidzein as glucosides)

J. Am Oil Chemists Soc., 81 (2004) 91-96.

Food Research International 37 (2004) 867

–874.

(11)

• Dried - organically grown red clover flowers

• Water extraction under varying temperature and pH

• Adsorption of isoflavones on polyvinylprrolidone

• Elution by ethanol and recovery

(12)

Effects of Temperature & pH

0 10 20 30 40 50 0 30 60 90 120 150 180 210 Is of la vone c onc e nt ra ti on (( μ g/ g)

Extraction time (min)

22 (room temperature) 60 70 80 90 0 10 20 30 40 50 60 70 80 0 30 60 90 120 150 180 210 Is of la von e con ce nt ra tion ( ( μg /g )

Extraction time (min)

3.0 9.0

9.5 10.0

10.5

(13)

Adsorption - PVP

0 10 20 30 40 50 60 70 80 90 100 5% 10% 15% 20% 30% Is o fl a v o n e s a d so rb e d (a s % o f e xt ra ct e d a mo u n t)

PVP to red clover ratio (w/w)

0 10 20 30 40 50 60 70 80 90 100 1 2 3 4 5 Is of la v one s a ds or be d (a s % of e xt ra ct e d a m ount )

(14)

Ethanol-Water - Extraction

0 10 20 30 40 50 60 70 0 50 100 150 200 Is o fl a v o n e co n ce n tr a ti o n ( μ g /m L )

Extraction time (minutes)

0% 30% 40% 50% 100% 0 10 20 30 40 50 60 70 80 90 100 0 20 40 60 80 100 E x tr a ct a b il it y ( %) Ethanol concentration (%, v/v)

(15)
(16)
(17)

Focus

– Biochemical Conversion

Biomass

Bio-refinery Concept

Cellulose

Hemi-cellulose

Pentoses

Lignins

Butanediol,

ethanol,

acetoine

Recovery and purification

of butanediol

(18)

Butanediol

• Manufacturing

– Petroleum

– Biosynthesis

• Potential usage

– Rubber synthesis

intermediate

– Polyester monomer

– Plasticizer

– Bio-fuel

• Physicochemical properties

– High boiling point (183 deg.

C)

– High affinity for water

– Big molecular size

(19)

Status

Recovery methods

– Distillation

– Solvent extraction

– Membrane pervaporation

– Integrated process

(20)

Membranes and Analysis

PDMS & PDMS/PVDF Composite

Chitosan/PVDF Composite Membrane

GC Analysis (HAYESEP D column)

Lab Scale Pervaporation (CM-Celfa AG)

i

P

P

j

i

j

i

i

j

X

X

Y

Y

j

i

i

j

P

P

(21)
(22)

Partition Coefficients

Solvent

Partition

Coefficient

Selectivity

2,3-butanediol

4

(wt. %)

3-ethyl-1-butanol

1

0.31

2.4

12.8

0.40

2.8

14.9

2-ethyl-1-hexanol

2

0.36

20.6

20.0

0.38

17.3

26.7

1-butanol

3

0.62

3.2

2.7

0.77

3.7

6.0

0.91

3.7

9.3

0.95

3.2

13.0

(23)

Temperature (PDMS)

i

C

Ln

P

Ln

Ea

LnQ

(

0

)

22

(24)

Enrichment

–PDMS/PVDF &

Chitosan/PVDF

(25)

Product purity and recovery

360 kg/h

– 5% 2,3-butanediol

PDMS memb. 5 m

Simulation

99.9% product purity

122 m

2

Tradeoff

– purity & recovery

98% & 52%

(26)

Conclusions

An integrated process

– solvent extraction &

pervaporation

PDMS membrane - plasticization

Simulations

– 98% pure 2,3-butanediol at 52%

recovery

(27)

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