苯基缩水甘油醚加成物及酯的合成研究

Studies on the Preparation of Phenyl Glycidyl Ether Adduct and Its Carboxylate

以C8-10醇和环氧乙烷为原料,反应合成了六聚氧乙烯醚,再与苯基缩水甘油醚形成加合物,苯基缩水甘油醚加成物与马来酸酐进行酯化反应形成产物苯基缩水甘油醚加成物马来酸单酯,并考察了反应条件。实验表明,在C8-10醇与环氧乙烷物质的量比为1∶6,压力为0.5MPa,反应温度150℃条件下反应,环氧乙烷结合率大于98%;六聚氧乙烯醚与苯基缩水甘油醚物质的量比为1∶1,催化剂三氟化硼乙基络合物为反应原料总物质的量的0.4%,温度50℃,反应时间45min,加合物收率达到91.6%;加合物与马来酸酐物质的量比1∶1,催化剂三正丁基胺为原料的1%(wt),反应时间4h,反应温度90℃,加合物马来酸单酯的收率达99%。

The Ca-10 mixed alcohol and ethylene oxide were used as raw materials in the process for synthesizing fatty alcohol polyoxyethylene ether; the phenyl glycidyl ether adduct was prepared by the additive reaction between fatty alcohol polyoxyethylene ether and phenyl glycidyl ether; then the phenyl glycidyl ether adduct reacted with maleic anhydride by esterification reaction to produce phenyl glycidyl ether adduct maleic acid monoester. The conditions for synthesis were studied by experiments. The binding rate of ethylene oxide would be 98.1% when the molar ratio of C8-10 mixed alcohol to ethylene oxide was 1：6, the reaction pressure was 0.5MPa and reaction temperature was 150%. When the molar ratio of fatty alcohol polyoxyethylene ether to phenyl glycidyl ether was 1：1, the content of catalyst boron trifluoride ethyl complex was 0.4% of the total reactant, and the reaction temperature and time was 50℃ and 45rain respectively, the yield of adduct would be 91.1%. The optimum conditions for preparing phenyl glycidyl ether adduct maleic monoester were shown as follows： the molar ratio of phenyl glycidyl ether adduct to maleic anhydride was 1：1, the weight percent of catalyst tributylamine was 1% of total reactant, the reaction temperature and time was 90℃ and 4h respectively; And the yield of phenyl glycidyl ether adduct maleic acid monoester was 99%.