钛络合物均相催化合成聚六氢苯酐二甘醇酯

Synthesis of polydiglycol cyclohexane 1,2-dicarboxylate catalyzed by titanium complex

以六氢苯酐和二甘醇为原料,钛络合物钛酸正四丁酯为催化剂合成聚六氢苯酐二甘醇酯。结果表明,钛酸正四丁酯催化合成聚六氢苯酐二甘醇酯的最佳反应条件为:醇酸摩尔比为1.1∶1,催化剂用量为0.8%(以六氢苯酐质量计),反应温度为220℃,反应时间为5 h,-0.095 MPa压强下减压时间为2.5 h,减压温度为220℃,酯化率大于99.0%。合成产物聚六氢苯酐二甘醇酯的数均分子量Mn为14000,重均分子量Mw为15000,分子量具有窄分布物性。

Poly diglycol cyclohexane 1,2-dicarboxylate was prepared from hexahydrophthalic anhydride and diethylene glycol,catalyzed by titanium complex tetrabutyl titanate.The best reaction conditions of esterification were determined as follows：molar ratio of diethylene glycol to hexahydrophthalic anhydride 1.1∶1,amount of catalyst 0.8%（based on the mass of hexahydrophthalic anhydride）,reaction temperature 220 ℃,reaction time 5 h,vacuum reaction time 2.5 h,vacuum reaction temperature 220 ℃ under vacuum（-0.095 MPa）,and esterification yield could be up to 99.0%.Number-average molecular weight of the product poly diglycol cyclohexane 1,2-dicarboxylate was 14000,and weight-average molecular weight of the product was 15000.Molecular weight distribution of the product was narrow.