聚癸二酸丙二醇酯的优化合成与表征

Optimized Synthesis and Characterization of Poly(propylene glycol sebacate)

以癸二酸,1,2-丙二醇,2-甲基-1,3-丙二醇为原料,以钛酸四正丁酯为催化剂,分别经酯化、缩合过程合成了聚癸二酸丙二醇酯系列聚酯增塑剂;使用傅立叶变换红外光谱仪、核磁共振氢谱仪、热重分析仪、差示扫描量热仪、凝胶色谱仪分别对聚酯产品的结构、热稳定性、玻璃化转变温度和分子量进行了系统表征。结果显示,反应条件为醇酸物质的量之比1.25∶1,催化剂用量为二元酸质量的0.06%,反应温度为180℃,反应时间为8 h,抽真空时间为2 h,此时得到了聚癸二酸1,2-丙二醇酯和聚癸二酸2-甲基-1,3-丙二醇酯产品,其数均分子量分别为924,1 668,分解温度分别为417.8℃和449.7℃,具有较好的热稳定性。

Using tetra-n-butyl titanate as catalyst,2-methyl 1,3-propanediol and 1,2-propanediol sebacic acid as raw material, series polyester products were prepared via polyesterification reaction. The Fourier transform infrared spectrum（FTIR）,nuclear magnetic resonance apparatus,thermogravimetric analyzer,differential scanning calorimetry and gel permeation chromatograph were used to measure the structure,thermostability,glass transition temperature and molecular weight of the prepared products. The results show that stuff molar ratio of diol/diacid is 1.25∶1,the content of catalyst used is 0.06%mass of the carboxylic acid used, the reaction temperature is 180 ℃ and the reaction time is 8 h,the vacuum pumping time is 2 h. The number average molecular weight and the decomposed temperature of the prepared poly-1,2-propylene glycol sebacate and poly-2-methyl-1,3-propylene glycol sebacate is 924,1 668 and 417.8℃,449.7℃. The products have higher thermostability.