Synthesis of Polyester-diol and Exfoliation of Nanoclay through Esterification between Adipic Acid and Diethylene Glycol

Adipic Acid와 Diethylene Glycol의 에스테르 반응을 통한 나노점토의 박리와 폴리에스테르형 디올의 합성

  • Kim, Byung-Ju (Department of Chemical Engineering, Dong-A University) ;
  • Lee, Sang-Ho (Department of Chemical Engineering, Dong-A University)
  • 김병주 (동아대학교 화학공학과) ;
  • 이상호 (동아대학교 화학공학과)
  • Published : 2009.12.31

Abstract

We synthesized polyester-diol containing Cloisite 30B which is exfoliated during the synthesis. First, esterification was conducted with excess adipic acids and two 2-hydroxyethyl groups of the tertiary ammonium tethered to Cloisite 30B silicate layer. Due to the small molecular size of adipic acid ($d{\approx}3.0\;{\AA}$, $L{\approx}9.3\;{\AA}$), it penetrated into the interlayer of Cloisite 30B, reacted with the 2-hydroxyethyl groups, and produced the tertiary ammonium that has the two ethyl-ester adipic acid groups, one methyl group, and one hydrogenated alkyl group. Through the esterification, the molecular size of the tertiary ammonium increased and as the result, the basal space of Cloisite 30B increased from $18.4\;{\AA}$ to more than $58.3\;{\AA}$. The produced ethyl-ester adipic acid and unreacted adipic acid reacted with excess diethylene glycol ([COOH]/[OH]${\approx}0.6$) to be polyester-diol. The COOH conversion calculated from the acid value of the reactant mixture was 94%. The number average molecular weight and PDI of the produced polyester-diol were 830 g/mol and 1.2, respectively.

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