熔融/固相缩聚法合成聚乙醇酸及其性能表征  

Research on the Synthesis and Property of Poly(glycolic) Acid via Melt/Solid Polycondensation

作　　者：崔爱军[1] 陆卫良[1] 王泽云[1] 田俊凯[1] 陈群[1] 何明阳[1] 

机构地区：[1]常州大学江苏省精细石油化工重点实验室,常州213164

出　　处：《高分子通报》2013年第2期73-78,共6页Polymer Bulletin

基　　金：江苏省高校自然科学研究重大项目(11KJA430007)

摘　　要：采用熔融/固相缩聚法合成了聚乙醇酸(PGA)可降解高分子材料,其基本反应步骤为:以乙醇酸为原料,先在190℃熔融状态下将乙醇酸脱水制成分子量为2万左右的低聚物,然后将制得的低聚物在190℃下进行固相缩聚以进一步提高分子量,所制备的PGA产物通过IR、DSC、XRD等手段进行表征。重点考察了不同催化剂,催化剂用量、是否熔融、反应温度、反应时间等因素对固相缩聚的影响,并得出熔融/固相缩聚法合成高分子量的聚乙醇酸的较佳工艺条件:反应温度190℃,二水合醋酸锌与等摩尔量的对甲苯磺酸作为催化剂(质量分数为0.4%),熔融缩聚2h后制得低聚物,然后在190℃下进行固相缩聚,40h后熔融一次,产品粉碎后继续固相缩聚60小时,PGA的重均分子量可达74000左右。Ploy（glycolic） acid （PGA）, as a biodegradable material, was synthesized via melt/solid polycondensation with glycolic as starting material. A general procedure for preparation was as follows： At first, oligomer was prepared by melt-polycondensation of glycolic acid （GA） at 190℃, and then it was subjected to solid-state polycondensation at the same temperature to increase the molecular weight. PGA product was characterized by IR, DSC and X-ray diffractometry. By examining the effect of different catalysts, catalyst amount, melting or not, reaction temperature and time on the polymerization, optimum conditions of the PGA synthesis was obtained as follows： reaction temperature 190℃, 0.4 % zinc acetate dihydrate and p-toluene sulfonic acid of same Molar as catalyst, melting one time after 40 hours solid polycondensation, then continuous 60 hours solid polycondensation after being crashed into pieces.

关 键 词：生物可降解材料 聚乙醇酸 固相缩聚 熔融缩聚 

分 类 号：O631.3[理学—高分子化学]