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Preparation and characterization of low molecular weight silk fibroin by high‐temperature and high‐pressure method
Author(s) -
Kang GyungDon,
Lee KiHoon,
Shin BongSeob,
Nahm JoongHee
Publication year - 2002
Publication title -
journal of applied polymer science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.575
H-Index - 166
eISSN - 1097-4628
pISSN - 0021-8995
DOI - 10.1002/app.10796
Subject(s) - fibroin , crystallinity , thermogravimetric analysis , differential scanning calorimetry , materials science , carbonization , gravimetric analysis , chemical engineering , polymer chemistry , activated charcoal , thermal analysis , nuclear chemistry , chemistry , silk , organic chemistry , composite material , thermal , adsorption , scanning electron microscope , physics , thermodynamics , engineering , meteorology
Abstract A low molecular weight silk fibroin powder (LMSF) was prepared through high temperature (200°C) and high pressure (20 kgf/cm 2 ), without any addition of chemicals. The carbonized adducts produced during this process were then removed by treatment with activated charcoal. The yield of LMSF by this preparation method was over 60% after the removal of carbonized adducts by using activated charcoal. Amino acid analysis showed an observable decrease in contents of serine and tyrosine in LMSF prepared by this method, as compared to those prepared by neutral salt. The molecular weight of this LMSF was also observably decreased with an increase in the reaction time. From the measurements of differential scanning calorimeter (DSC) and thermal gravimetric analyzer (TGA), thermal properties of LMSF through high temperature and high pressure were also decreased as compared to those produced by neutral salts. In addition, wide‐angle X‐ray diffraction (WAXD) patterns showed that the crystallinity of LMSF differed from that of the original silk fibroin. It can be said that the preparation method of LMSF in this study is a simple, economical, and environmentally compatible process with many advantages. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 2890–2895, 2002