摘要
为了确定合成端羧基超支化聚酯的工艺参数,以柠檬酸为单体,SOCl2为酰氯化试剂,THF为溶剂,采用微波合成仪,缩聚合成了端羧基超支化聚酯.通过考察催化剂用量和聚合时间对酯化率的影响,确定了较优的工艺参数.经红外、核磁共振、差示扫描量热仪和凝胶色谱仪对产物进行了初步表征及简单的性能检测.结果表明:以柠檬酸为单体,微波法缩聚可以制得超支化聚酯.SOCl2用量为2.5 g,聚合时间为30 min时,酯化率为93%,产物分子量为2 385 g/mol.
The carboxyl-terminated hyperbranehed polyesters were synthesized with citric acid as monomer,SOCl2 as aeylchloride reagent, THF as solvent by microwave instrument. The influences of the amount of catalyst, polymerization time and temperature on esterification rate, the preparation process were studied. And it was characterized by FT IR,1H NMR, DSC and SEC. It was found that the reaction speed and esterification rate using microwave method were greatly increased. When SOC12 2. 5 g,reaction time 30 min,esterification rate was 93%. The molecular weight was 2 385 g/mol, and the molecular weight distribution expressed as multiple peaks. Tg of the result polymer was 167℃.
出处
《西安工业大学学报》
CAS
2010年第2期150-154,共5页
Journal of Xi’an Technological University
基金
陕西省自然科学基金(SJ08B17)
陕西省教育厅自然科学专项(08JK308)
关键词
超支化聚酯
柠檬酸
氯化亚砜
微波法
hyperbranched polyester
citric acid
SOC12
microwave synthesis