Thermoplasticization of High Amylose Starch by Chemical Modification Using Reactive Extrusion

Jacqueline Stagner, Vanessa Dias Alves, Ramani Narayan, Adelaide Beleia

Research output: Contribution to journalArticle

  • 10 Citations

Abstract

Modified thermoplastic high amylose starch (MTPS) was synthesized by reactive extrusion in the presence of maleic anhydride (MA) as an esterification agent in a twin-screw extruder. The objective of this work was the preparation of reactive thermoplastic starch in the presence of glycerol and with different amounts of maleic anhydride (MA) and free-radical initiator, in order to improve processability and reactivity. The concentration of MA added varied from 2 to 6 wt% (of starch + glycerol), and the free-radical initiator, 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane, also called Luperox 101, varied from 0.1 to 0.5 wt% (of starch + glycerol). Characterization of maleated thermoplastic starch was performed using dynamic light scattering and thermal analysis. Further, proof of chemically modified extrudate was determined by Fourier transform infrared spectroscopy and by soxhlet extraction with acetone. The modified high amylose corn starch (20 or 30% glycerol) could be pelletized and gave pellets that were more transparent than thermoplastic starches not modified with maleic anhydride. There was negligible change in hydrodynamic radius as the percentage of maleic anhydride increased. However, as the percentage of Luperox 101 increased, the hydrodynamic radius decreased. It could be inferred that the molecular weight decreased as the percentage of free-radical initiator increased. Using the maximum temperature in the extrusion process of 165 °C instead of 135 °C caused a decrease in the hydrodynamic radius, due to the high influence of the temperature profile on the molecular weight of the thermoplastic starch. The MTPS samples presented higher melting temperatures compared to TPS samples. The soxhlet studies indicated that the plasticizer, glycerol, was chemically linked to the starch. Using the maximum temperature of 165 °C versus 135 °C in the extrusion temperature profile resulted in more interaction between glycerol and starch.

LanguageEnglish (US)
Pages589-597
Number of pages9
JournalJournal of Polymers and the Environment
Volume19
Issue number3
DOIs
StatePublished - Sep 2011

Profile

Amylose
Chemical modification
Starch
Extrusion
Maleic Anhydrides
Glycerol
Thermoplastics
Maleic anhydride
Free radicals
Free Radicals
Hydrodynamics
Molecular weight
Plasticizers
Temperature
Esterification
Extruders
Dynamic light scattering
Acetone
Thermoanalysis
Fourier transform infrared spectroscopy

Keywords

  • Biodegradable
  • Maleation
  • Reactive extrusion
  • Thermoplastic starch

ASJC Scopus subject areas

  • Environmental Engineering
  • Polymers and Plastics
  • Materials Chemistry

Cite this

Thermoplasticization of High Amylose Starch by Chemical Modification Using Reactive Extrusion. / Stagner, Jacqueline; Alves, Vanessa Dias; Narayan, Ramani; Beleia, Adelaide.

In: Journal of Polymers and the Environment, Vol. 19, No. 3, 09.2011, p. 589-597.

Research output: Contribution to journalArticle

Stagner, Jacqueline ; Alves, Vanessa Dias ; Narayan, Ramani ; Beleia, Adelaide. / Thermoplasticization of High Amylose Starch by Chemical Modification Using Reactive Extrusion. In: Journal of Polymers and the Environment. 2011 ; Vol. 19, No. 3. pp. 589-597
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abstract = "Modified thermoplastic high amylose starch (MTPS) was synthesized by reactive extrusion in the presence of maleic anhydride (MA) as an esterification agent in a twin-screw extruder. The objective of this work was the preparation of reactive thermoplastic starch in the presence of glycerol and with different amounts of maleic anhydride (MA) and free-radical initiator, in order to improve processability and reactivity. The concentration of MA added varied from 2 to 6 wt{\%} (of starch + glycerol), and the free-radical initiator, 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane, also called Luperox 101, varied from 0.1 to 0.5 wt{\%} (of starch + glycerol). Characterization of maleated thermoplastic starch was performed using dynamic light scattering and thermal analysis. Further, proof of chemically modified extrudate was determined by Fourier transform infrared spectroscopy and by soxhlet extraction with acetone. The modified high amylose corn starch (20 or 30{\%} glycerol) could be pelletized and gave pellets that were more transparent than thermoplastic starches not modified with maleic anhydride. There was negligible change in hydrodynamic radius as the percentage of maleic anhydride increased. However, as the percentage of Luperox 101 increased, the hydrodynamic radius decreased. It could be inferred that the molecular weight decreased as the percentage of free-radical initiator increased. Using the maximum temperature in the extrusion process of 165 °C instead of 135 °C caused a decrease in the hydrodynamic radius, due to the high influence of the temperature profile on the molecular weight of the thermoplastic starch. The MTPS samples presented higher melting temperatures compared to TPS samples. The soxhlet studies indicated that the plasticizer, glycerol, was chemically linked to the starch. Using the maximum temperature of 165 °C versus 135 °C in the extrusion temperature profile resulted in more interaction between glycerol and starch.",
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