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Justin R. Barone*,

Maria Medynets

Thermally processed levan

polymers

1

Carbohydrate Polymers

69 (2007) 554-561

Present by : Miss Wilairat Dinsakul


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2

Justin R. Barone

Author

Source: Renewable Materials

Research Group(2007).

www.tourismlogistics.com

Interested in the role protein

nter-molecular interactions play

n:Dynamic and equilibrium

properties of

protein aggregates and gels.

Regulating metabolism in acellular environment.


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Introduction

Levan

glycerol

Objective Experimental

procedures

Film preparation

Polymer processing

Polymer properties

and testing

Results and 3

Outline


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Levan produced from sucrose by the

transfructosylation reaction oflevansucrase

a polymer of fructose linked by-(26) fructofuranosidic bonds

applications in the fields ofcosmetics, foods andpharmaceuticals

Introduction

4

Source: Montana

Polysaccharides.www.polysriacchades.us/aboutlevan_structure.php

G F

sucrose

Transfructo

sylationLevansucreaseLevan

n( )

G F

G F

FG


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Glycerol (C3H

8O3) an organic compound, also called

glycerin or glycerine

can be produced by saponification

of animal fats

It is a colourless , viscous liquid three hydrophilic hydroxyl groups

that are responsible for its

solubility in water 5Source: Glycerin Skelett.svg2007 .en.wiki edia.or /wiki/File:Gl cerin Skelett.sv


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To study thermally processed of

levan through molding and extrusion

techniques.

6

Objective


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Experimental

proceduresFilmpreparati

on

Levanwas

combined with

(DI-H2O)and

glycerol.(various

proportions)

Polymerprocessi

ng

Extrusion

Compression

Molding

Polymerpropertiesand testingMechanic

al

testing

DSC

FT-IR


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8

Materials

1. Levan were ground into a fine powder.

(size of the particles about 53 m)

2. Reagent

grade glycerol


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sample

5 g of

sample

(wt%

)

5 1

0

1

5

2

0

2

5

3

0

4

0

T(oC

)

8

2

8

0

7

2

6

5

5

3

4

6

4

2

9

an

Lev

anGl cerol

40 (wt%)

Glycerol5

,10,15,20,25,30,40 (wt%)

Mixing

proceed(Brabender

mixing head)

Compression

2 min

Compression

molding

90oc , 133,446

N ,

2 min

pression molding

Source: Carver, Inc(2006-09).www.carverpress.com/astm_presses.ht

Levan films(film thickness depended on the

amount of glycerol)

40oC, 15min.Table 1: Pressingconditions for levan filmsGiycer

ol

( wt%)

Film

thicknes

s (cm)

Compressiv

e stress

(MPa)

5 0.022 11.1

10 0.017 8.7

15 0.015 7.7

20 0.014 7.3

25 0.009 4.6

30 0.007 3.6

40 0.009 4.7


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10

Extru

sion Mixed with

min.

Mixed witha Waring

kitchen blender

high speed,2

min.

Levan

water

Levan+ glycerol

+ de-

ionized

water

Extruder

110oc

Source:Denis Razuvaev

http://masters.donntu.edu.ua/2006/fema/razuvaev/diss/disse.htm

Levan

films


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11

Source:Denis Razuvaev

http://masters.donntu.edu.ua/2006/fema/razuvaev/dis

s/disse.htm

Extruder

process

Source:uiengineering.www.uiengineering.com/Html/EN/Tufftride.html


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12

Mechanical

Testing of films Test samples were preparedaccording to

ASTM D882for thin plastic

films.

Results reported asaverage values of

modulus,E

stress at break,Wb

strain at break,Ib

ASTM D882 : American society

fortesting material

Source:Dr.Pakorn(2008)www.v

varticle/18774

Source:DonShockey(2010).www.sri.com/psd/fracture/w

The sample were 2.54 cm/min

wide by 10.16 cm long and a

5.08 cm length.


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Differential scanning

calorimetry (DSC)Assess the effect of glycerol concentration on

glass transition temperature (Tg).Sample size 5 mg were used

in a N2 atmosphere.A heating rate of 10oC/min.Two heat cycles.

A first heating cycle from 0oC to 160oC .

A second heating cycle from 0oC to 400oC .

Source:www.pt.ctw.utwente.nl/organisation/facilitie

s/analysis/Mettler%20Differential%20Scanning%2

0Calorimeter%20(DSC822E).doc/


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Fourier transform-infrared

(FT-IR) spectroscopyFT-IR analysis was

performed with

a Thermo Nicolet Avatar370.

- mode with a flat 45o

ZnSe crystal

Source: The Caran

Research

Group(2010).http://csm

a31.csm.jmu.edu/chemistry/faculty/caran/rese

arch/pix/


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Results and discussion

Glass transition

temperature (Tg)

Result of theDSC analysis

Fig. 1. DSC results for


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Fig. 3. Picture of an

extrudate of the 65:35

levan:glycerol blend

extruded at 110 oc.

Levan

Glycerol T(

o

C) Extrusion Results

85 15 90 Very little flow occurred

through the die at low

speed .75 25 100

65 35 110 A free flowing

extrudate over a wide.

Extrusion

results

The addition of water

made the blends much

softer and therefore it was

not possible to test these

extrudates in tension.


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Fig. 5. Effect of applied

apparent shear stress during

extrusion, , on extrudatephysical properties for the 65:35

aW

Physical

properties

Smodulu

s,EStress at

break,Wb(Strain at

break,Ib


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70:30

levan:glycer

olGlyce

rol

FT-IR

Fig.6. Comparison of the FT-IR spectra for glycerol and 70:30 levan:glycerol

blend cold-mixed and compression-molded at 90o

c. The y-axis is not acommon scale because of the high absorbance of glycerol

Glycerol

Lev

an


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Fig.7(b) . FT-IR spectra 600cm-1 to 1800 cm-1 range for

levan:glycerol blends. The 65:35 levan:glycerol blend waso -

1. 90:10 levan:glycerol2. 80:20 levan:glycerol3. 75:25 levan:glycerol

4. 70:30 levan:glycerol5. 65:35levan:glycerol(extruded)

2.

1.

3.

4.

5.

(CO stretch.)

furanose ring

813,945 cm-1

(CO stretch.)

linkage

1093 ,1165

cm-1(CH bending), (OH

bending)

1370,1398 cm-1

(CHbending)

1248

,1265

cm-1


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Fig. 8. Plot of FT-IR peak intensity, I. as a

function of glycerol concentration (weight


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Levan can be successfullythermally processed through

molding and extrusion

techniques.Assuming levan producedthrough a microbial process, the

molecule to be formed into films

products for polymer

applicationsGlycerol was an effectiveplasticizer and allow for efficient

processing at low temperature.

Conclu

sions


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A critical concentration of 20

weight percent glycerol was

necessary for effective

plasticization of levan.


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Fishman, M.L., Coffin, D. R., Konstance, R.P., & Onwulata, C.I.(2000). Eutrusion of

pectin/startch blends plasticized with

glycerol. Carbohydrate Polymers, 41, 317-

325

Simon, J., Muller, H.P., Koch, R., & Muller, V.

(1998). Thermoplastic and biodegradable

polymers of cellulose. Polymer Degradation

and Stability,59,107-115

Finkenstadt, V. L., & Willet, J. L. ZA(2004b).

Electroactive materials composed of

starch. Journal of Polymers and the

Environment, 12, 43-46

Refere

nces


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The speaker wish to thank

teachers

for give advices on this seminar.

Acknowled

gements


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Lev

an

Glyc

erol

DI-

H2O

The extrudate

65 35 0 The viscosity wasquite high and

strongly shear-

thinning

65 25 10 Extrudate splittingoccurred at

Wa > 0.3 Mpa.

55 35 10 Extrudate split uponexiting the die.

26

Fig. 4. Rheological data for

levan:glycerol:DI-H2O (l:g:w)

blends of (open symbols)65:35:0,

(closed symbols)65:25:10, and (dotted symbols)55:3

The addition of water made the

blends much softer and therefore itwas not possible to test these

extrudates in tension.

Extrusion

rheology

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