有机溶剂法合成聚马来酸酐:聚合残液的分析与循环利用  

Synthesis of Polymaleic Anhydride by Organic Solvent Method:Analysis and Recycling of Polymerization Residue

作　　者：徐华[1] 唐炳涛[1] 袁剑鹏[1] 张淑芬[1] 

机构地区：[1]大连理工大学精细化工国家重点实验室,辽宁大连116012

出　　处：《精细化工》2010年第4期409-412,共4页Fine Chemicals

基　　金：国家自然科学基金重点基金资助项目(20836001);教育部长江学者与创新团队发展计划(IKT0711)~~

摘　　要：以过氧化苯二甲酰为自由基引发剂,甲苯为溶剂,研究了聚马来酸酐（PMA）最佳合成条件,即引发剂质量分数10%,反应温度95℃,反应时间6 h。通过对聚合残液的MS分析,聚合残液主要成分为马来酸酐（MA）,通过聚合残液的酸值分析,得到MA的利用率为63.5%。针对MA利用率较低,将聚合残液循环利用。循环结果表明,经5次循环使用,MA的累计利用率可达90.3%,并随着循环次数增多,MA的累计利用率逐步增大。所合成聚马来酸酐经FTIR1、HNMR分析,结构正确;凝胶渗透色谱（GPC）分析,每次循环产品PMA的平均相对分子质量变化不大,平均相对分子质量Mn保持在930~940,相对分子质量分布系数为1.12。Polymaleic anhydride（PMA） was synthesized with benzoyl peroxide（BPO） as free radical initiator and toluene as solvent.The optimal synthesis conditions were that：the mass percent of initiator was 10%,the reaction temperature was 95 ℃,and the reaction time was 6 h.The polymerization residue was analyzed by MS and the acid-base titration.Results showed that the major component in the polymerization residue was maleic anhydride（MA） and the utilization ratio of MA was 63.5%.This paper gave a technique for recycling the polymerization residue by analyzing the component and the content of the solute in the residue.The results showed after 5 cycles,the cumulative utilization ratio could reach 90.3%.With the increase of the recycle times,the cumulative utilization ratio increased gradually.The structure of PMA was characterized by FTIR and 1HNMR.The analysis of the gel permeation chromatography（GPC） of the product showed that there was a little change in the average molecular weight of the polymaleic anhydride produced in each cycle.The number average molecular weight（Mn） of PMA was kept at 930～940 and the distribution of molecular weight was 1.12.

关 键 词：聚马来酸酐 聚合残液 循环利用 表面活性剂 

分 类 号：O631.6[理学—高分子化学]