凍結乾燥フィブロインの結晶構造と熱的性質について

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  • On the crystal structure and thermal property of lyophilized fibroin
  • トウケツ カンソウ フィブロイン ノ ケッショウ コウゾウ ノ ネツテキ セイシツ ニ ツイテ

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抄録

On the lyophilized samples prepared by different methods from fibroin aqueous solutions, which extracted from posterior section of silk gland and prepared from raw silk by Cu-En method, the crystaline structures and the thermal properties were investigated. The following results were obtained:<br>1) On the fibroin samples, which prepared by lyophilization of fibroin aqueous solution water-extracted from posterior section of silk gland and by lyophilization of fibroin precipitated from the same solution, the conformations of these samples were fl-structures and the positions of the amide I lay 1650 and 1630cm-1. The decomposition temperatures were observed at 318-320°C and the thermodecomposition began at lower temperature than other samples and were stepwise.<br>2) The fibroin sample, which was prepared by lyophilization of fibroin aqueous solution prepared from degummed silk by Cu-En method, was amorphous and the band of the amide I appeared at 1660cm-1 and the decomposition temperature was 305°C. The broad and weak endothermic peak in the thermogram was observed about 180-230°C and at this temperature the X-ray diffraction pattern changed to that of β-structure and the band of the amide I appeared newly about 1630cm-1.<br>3) The fibroin sample, which prepared by lyophilization of the alcohol-precipitate from the aqueous solution of degummed silk by Cu-En method, gave an X-ray diffraction pattern of β-structure, and the amide I was observed about 1650 and 1630cm-1, and the sample thermodecomposed at 315°C. The lyophilized fibroin precipitated with ammonium sulfate gave X-ray diffraction pattern of α-structure, and the position of amide I was at 1645cm-1 alone. The thermodecomposition temperature was 310°C and the transconformation to β-structure by heating did not occured.<br>4) On the IR-spectra of degummed silk, the positions of the amide I were observed about 1660 and 1630cm-1 and the sample decomposed at 350°C. The spectra was similar that of the lyophilized fibroin except the absorption band about 1700cm-1.<br>Generally, on the change of IR-spectrum by heating, the absorption band about 1700cm-1 occured with elevating temperature and the intensities of the amide II and amide III decreased remarkably about thermodecomposition.

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