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有机化学
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有机化学 ›› 2003, Vol. 23 ›› Issue (12): 1380-1386. 上一篇    下一篇

研究论文

a,ω-二羧基-甲基丙烯酸丁酯低聚物的合成及MS分析

刘平桂;赫丽华;陈文章;刘俊能;丁鹤雁;熊少祥;益小苏   

  1. 北京航空材料研究院;中国科学院化学研究所
  • 发布日期:2003-12-25

Synthesis and MS Characterization of a , ω-Dicarboxyl Terminated Oligo (butyl Methacrylate)

Liu Pinggui;He Lihua;Chen Wenzhang;Liu Junneng;Ding Heyan;Xiong Shaoxiang;Yi Xiaosu   

  1. Beijing Institute of Aeronautical Materials;Institute of Chemistry, Chinese Academy of Science
  • Published:2003-12-25

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利用传统自由基聚合法，在四氢呋喃溶液中自由基引发聚合甲基丙烯酸丁酯单 体而得到w-羧基-甲基丙烯酸丁酯低聚物(CTBMA)(分子量在1500左右)；利用CTBMA 末端酯基的反应特性，在二氧六环／水／KOH混合溶液中皂化CTBMA，使之转化为a ，w-羧基甲基丙烯酸丁酯低聚物(di-CTBMA)；研究了溶剂的类别、反应时间等反应 条件对皂化产物结构的影响；利用MALDI-TOF-MS及LSIMS对皂化各阶段产物进行了 分析监测．实验表明，在适当的皂化条件下，CTBMA皂化时主要为末端酯基转化为 羧基，相应得到的产物di-CTMBA具有很好的结构特性，其官能团度 (functionality)接近2．

关键词: 甲基丙烯酸酯;低聚物;自由基聚合;质谱法;四氢呋喃;二氧六环, 水;氢氧化钾;皂化作用

A novel method combining a conventional free-radical solution polymerization with a chemical saponification was used to synthesize a, cu-dicarboxyl terminated oligo (butyl methacrylate) s (di-CTBMA) with molecular weight below 1500. Here, cn-carboxyl terminated oligo (butyl methacrylate) s (CTBMA) were firstly synthesized by the free-radical polymerization in THF, where 4,4'-azobis(4-cyanovaleric acid) was used as initiator, thioglycolic acid as chain transfer agent, then CTBMA were transformed into di-CTBMA via saponifying CTBMA in dioxane/H_2O/KOH solution. The influences of important reaction parameters, such as the type of organic solvent, react time on the structures of the saponified substances were monitored by determination of functionality / via acid-base titration, MALDI-TOF-MS and ISMS analysis. It shows that di-CTBMA with the functionality of about 2 could be obtained under a certain reaction parameter.

Key words: METHYLPROPENOIC ACID ESTER;LOW POLYMER;FREE REDICAL POLYMERIZATION, MS;DIOXANE;WATER;POTASSIUM HYDROXIDE;SAPONIFICATION

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