Thermally processed levan polymers

Justin R. Barone*, Maria Medynets Carbohydrate Polymers 69 (2007) 554-561 Present by : Miss Wilairat Dinsakul

Author
Justin R. Barone Interested in the role protein inter-molecular interactions play in: Dynamic and equilibrium properties of protein aggregates and gels. Regulating metabolism in a cellular environment.

Source: Renewable Materials Research Group(2007). www.tourismlogistics.com

Outline

Introduction Levan glycerol Objective Experimental procedures Film preparation Polymer processing Polymer properties and testing Results and discussions

Introduction

Levan

produced from sucrose by the transfructosylation reaction of levansucrase a polymer of fructose linked by -(2 6) fructofuranosidic bonds applications in the fields of cosmetics, foods and pharmaceuticals Transfructo G F
n

sucrose

Levansucrease Levan sylation

Source: Montana Polysaccharides.www.polysriacchades.us/aboutlevan_st ructure.php

Glycerol (C3H8O3)

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 Glycerin Skelett.svg Source: water 5 (2007).en.wikipedia.org/wiki/File:Glycerin_Skelett.sv

Objective
To study thermally processed of levan through molding and extrusion techniques.

Film preparati on Levan was combine d with (DI-H2O) and glycerol.

(various proportions)

Experimental procedures
Polymer processi ng

Extrusion Compres sion Molding

Polymer properties and testing Mechanic al testing DSC FT-IR

Materials
1. Levan were ground into a fine powder. (size of the particles about 53 m) 2. Reagent grade glycerol

ompression molding
Lev an Glycerol
5 ,10,15,20,25,30, 40 (wt%)

Table 1: Pressing 40oC, 15min. Mixingconditions for levan films Giycer (wt% 5 1 Compressiv Film 1 2 2 3 4 proceed ol ) 0 5 0 thicknes 5 e0stress 0 (Brabender T(oC 8 8 7 6 5 4 4 ( s (cm) (MPa) mixing head) wt%)
5 10 15 20 25 30
3 55g of 6 2 0.022 11.1 Compression sample ) 2 0 2

molding8.7 0.017

90oc , 133,446 0.015 7.7 N, 0.014 2 min 7.3

0.009 0.007 3.6 (film thickness depended on the amount of glycerol) 0.009 4.7

Levan films

4.6

Source: Carver, Inc(200609).www.carverpress.com/astm_presses.ht ml

40

Extru sion Levan

+ glycerol + deionized water

Mixed with a Waring kitchen blender high speed,2 min.

Extruder 110oc

Levan films

Source:Denis Razuvaev http://masters.donntu.edu.ua/2006/fema/razuvaev/dis s/disse.htm

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Extruder process

Source:Denis Razuvaev http://masters.donntu.edu.ua/2006/fema/razuvaev/dis s/disse.htm

Source:uiengineering.www.uiengineering.c om/Html/EN/Tufftride.html

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Mechanical Testing of were prepared films Test samples

Source:Dr.Pakorn(2008)www.vch varticle/18774

according to ASTM D882 for thin plastic films. D882 : American society ASTM for testing material The sample were 2.54 cm/min wide by 10.16 cm long and a 5.08 cm length. Results reported as average values of modulus,E stress at break,Wb Source:Don strain at break,Ib

Shockey(2010).www.sri.com/psd/fracture/w elded_steel.html

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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) spectroscopy

FT-IR analysis was performed with a Thermo Nicolet Avatar 370. - mode with a flat 45o ZnSe crystal

Source: The Caran Research Group(2010).http://csm a31.csm.jmu.edu/chem istry/faculty/caran/rese arch/pix/

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Results and discussion

Result of the DSC analysis Glass transition temperature (Tg)

Fig. 1. DSC results for levan-glycerol blends.

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Lev Glyc an erol 85 75 15 25

Extrusion results

T(o C)

Extrusion Results

90 Very little flow occurred 100 through the die at low speed . 65 35 110 A free flowing extrudate The addition of water over a wide.

made the blends much softer and therefore it was not possible to test these extrudates in tension.

Fig. 3. Picture of an extrudate of the 65:35 levan:glycerol blend extruded at 110 oc.

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Physical properties S modulu at Stress s,E break,Wb (Strain at break,Ib

Fig. 5. Effect of applied Wa apparent shear stress during extrusion, , on extrudate physical properties for the 65:35 levan:glycerol extruded blend.

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FT-IR
Glycero l

Lev an

70:30 levan:glycer Glyce ol rol

Fig.6. Comparison of the FT-IR spectra for glycerol and 70:30 levan:glycerol blend cold-mixed and compression-molded at 90oc. The y-axis is not a common scale because of the high absorbance of glycerol

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levan:glycerol 2. 80:20 levan:glycerol 3. 75:25 levan:glycerol 4. 70:30 levan:glycerol 5. 65:35 levan:glycerol(extru 5. ded)

4.
O-H stretch. (3282 cm-1)

3. 2. 1.

Fig.7(a) . FT-IR spectra full IR range

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(CO stretch.) 1. 90:10 levan:glycerol furanose ring 2. 80:20 levan:glycerol 5. 3. 75:25 levan:glycerol 813,945 cm-1 4. 70:30 levan:glycerol (CH 5. 65:35 bending) levan:glycerol(extruded (CO stretch.) 1248 ) 4. linkage ,1265 1093 ,1165 cm-1 cm-1 3. (CH bending), (OH bending) 2. 1370,1398 cm-1

1.

Fig.7(b) . FT-IR spectra 600cm-1 to 1800 cm-1 range for levan:glycerol blends. The 65:35 levan:glycerol blend was 20 extruded at 110oC. They y-axis is a common scale.

Fig. 8. Plot of FT-IR peak intensity, I. as a function of glycerol concentration (weight fraction)

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Levan can be successfully thermally processed through molding and extrusion Assuming levan produced techniques. through a microbial process, the molecule to be formed into films products for polymer Glycerol was an effective applications plasticizer and allow for efficient processing at low temperature. 22

Conclu sions

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, 317325 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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Acknowled gements
The speaker wish to thank teachers for give advices on this seminar.

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Extrusion rheology
Lev Glyc DIan erol H2O 65 35 0 The extrudate
The viscosity was quite high and strongly shearthinning Extrudate splitting occurred at Wa > 0.3 Mpa.

65

25

10

The addition of water made split upon the Extrudate 55 35 10 blends much softer and therefore it exiting the die. was not possible to test these extrudates in tension.

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)55:35:

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