Reduction of Liquid Carboxyl-terminated Fluorine Rubber by Alkyl Aluminum/Lithium Aluminum Hydride Reduction System |
Received:January 04, 2022 Revised:January 04, 2022 |
DOI:10.12136/j.issn.1000-890X.2022.12.0891 |
Key Words: liquid carboxyl-terminated fluorine rubber;liquid hydroxyl-terminated fluorine rubber; reduction;DIBAl-H;Al(i-Bu)3;LiAlH4 |
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Abstract: |
In this study, liquid hydroxyl-terminated fluorine rubber(LTHFs) was prepared by reduction
of liquid carboxy-terminated fluorine rubber(LTCFs)by using two reduction systems: diisobutylaluminum
hydride(DIBAl-H)/lithium aluminum hydride(LiAlH4) and triisobutylaluminum hydride[Al(i-Bu)3]/
LiAlH4. Fourier transform infrared spectroscopy,nuclear magnetic resonance hydrogen spectroscopy and
nuclear magnetic resonance fluorine spectroscopy analysis showed that both reduction systems could reduce
the carbon-carbon double bond and carboxyl group in LTCFs to carbon-carbon single bond and hydroxyl
group, respectively. Further comparing the reducing capacity of the two reduction systems, it was found
that DIBAl-H/LiAlH4 was more suitable for LTCFs reduction,and the reduction rate could reach 88% at
the optimal condition in which the reaction temperature was 60 ℃,the reaction time was 8 h and the molar
ratio of COOH/LiAlH4/DIBAl-H was 1/1/2. Compared with the traditional strong reducing agent LiAlH4,
DIBAl-H/LiAlH4 could reduce the reaction temperature and reduce the amount of reducing agent. |
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