利用微波辅助氧化降解法制备液体端羧基氟橡胶及其结构
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大连海事大学交通运输工程学院材料科学与工程系

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国家自然科学基金资助项目(51873026)


Preparation and Characterization of Liquid Carboxyl-Terminated Fluororubber by Microwave Assisted Oxidation Degradation Method
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    摘要:

    以246型固体氟橡胶为原料,过氧化氢(H2O2)/ KOH为氧化降解体系,利用微波辅助一步氧化降解方法,制备了液体端羧基氟橡胶(LCTF)。采用FTIR、1H-NMR、19F-NMR、GPC和化学分析方法对其结构、分子量和分子分布、羧基含量进行了表征,证明246型固体氟橡胶被高效地氧化降解成LCTF,并且LCTF的分子量和羧基含量可控。系统研究了微波功率和加热时间、溶剂品种和用量、KOH溶液浓度、H2O2 /KOH摩尔比、H2O2和KOH溶液用量、相转移催化剂 (PTC) 品种和用量等因素对LCTF分子量和羧基含量的影响。结果表明,随着影响因素的变化,Mn和羧基含量均呈现完全相同的变化规律。在微波功率为480W、微波加热时间为11min、四氢呋喃(THF)为175ml或丙酮为150ml、KOH溶液浓度为45wt%、H2O2 /KOH摩尔比为1.50/1.00、H2O2和KOH溶液用量分别为35.32g和48.18g、相转移苄基三乙基氯化铵(BTEAC)用量为0.0165 mol时,LCTF的Mn最低,羧基含量最高。微波加热极大地加快了氧化降解反应时间。

    Abstract:

    The liquid carboxyl-terminated fluororubber (LCTF) was prepared using 246 type solid fluororubber and peroxide (H2O2)/KOH as the reaction raw materials and the oxidative degradation system respectively by microwave assisted one-steps oxidation degradation method. The structure and molecular weight and distribution, carboxyl content of the LCTF were characterized by FTIR, 1H-NMR, 19F-NMR, GPC and chemical analysis methods. The results proved that 246 solid fluororubber was efficiently oxidized and degraded into LCTF, controlled degradation of molecular weight (Mn) and carboxyl content of LCTF was achieved. The effects of microwave power and heating time, type and amount of solvent, KOH concentration, H2O2 / KOH molar ratio, amount of H2O2 and KOH solution, type and amount of phase transfer catalyst (PTC) on molecular weight and carboxyl content of LCTF were systematically studied. Results showed that with the change of affecting factors, the content of Mn and carboxyl group showed the same change rule. When the microwave power was 480W, microwave heating time was 11min, THF was 175mL or acetone was 150mL, KOH solution concentration was 45%, the molar ratio of H2O2 / KOH was 1.50/1.00, the amount of H2O2 solution and KOH solution was 35.32g and 48.18g, and the amount of PTC (BTEAC) was 0.0165 mol, the content of Mn and carboxyl was the lowest and the content of carboxyl was the highest. Microwave assisted heating greatly accelerated the process of oxidative degradation and shortened the reaction time.

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  • 收稿日期:2021-09-23
  • 最后修改日期:2022-04-02
  • 录用日期:2022-04-18
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