| 烷基铝/氢化铝锂还原体系还原液体端羧基氟橡胶 |
| Reduction of Liquid Carboxyl-terminated Fluorine Rubber by Alkyl Aluminum/Lithium Aluminum Hydride Reduction System |
| 投稿时间：2022-01-04 修订日期：2022-01-04 |
| DOI：10.12136/j.issn.1000-890X.2022.12.0891 |
| 中文关键词: 液体端羧基氟橡胶 液体端羟基氟橡胶 还原 二异丁基氢化铝 三异丁基铝 氢化铝锂 |
| 英文关键词: liquid carboxyl-terminated fluorine rubber liquid hydroxyl-terminated fluorine rubber reduction DIBAl-H Al（i-Bu）3 LiAlH4 |
| 基金项目:国家自然科学基金资助项目（83118020） |
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| 中文摘要: |
| 采用两种还原体系二异丁基氢化铝（DIBAl-H）/氢化铝锂（LiAlH4）和三异丁基铝[Al（i-Bu）3]/LiAlH4，将液体端羧基氟橡胶（LTCFs）还原得到液体端羟基氟橡胶（LTHFs）。傅里叶转换红外光谱、核磁共振氢谱和核磁共振氟谱分析均表明，两种还原体系均能将LTCFs中的碳-碳双键和羧基分别还原成碳-碳单键和和羟基。进一步对比两种还原体系的还原能力发现，DIBAl-H/LiAlHM4更适合还原LTCFs，且在反应温度为60 ℃、反应时间为8 h、羰基/LiAlH4/DIBAl-H物质的量比为1/1/2的最优条件下LTCFs的还原率可达到88%。与传统强还原剂LiAlH4相比，DIBAl-H/LiAlH4可降低反应温度，且减小还原剂用量。 |
| 英文摘要: |
| 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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