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作 者:王福玲[1] 杨瑞娜[1] 王建莉[1] 马伟[1]
机构地区:[1]河南省科学院化学研究所有限公司,郑州450002
出 处:《河南科学》2013年第9期1349-1351,共3页Henan Science
基 金:河南省产学研项目(122107000035)
摘 要:以六氢邻苯二甲酸和环氧氯丙烷为原料经开环酯化和闭环反应合成了六氢邻苯二甲酸二缩水甘油酯(HADE),研究了物料配比、催化剂种类、碱浓度、碱用量、闭环时间及不同温度对反应的影响.结果表明,最佳反应条件如下(以六氢邻苯二甲酸为0.1 mol计):当六氢邻苯二甲酸与环氧氯丙烷的量的比为1∶16,以十六烷基三甲基溴化铵为催化剂,升温回流时间2 h,50%NaOH用量为0.30 mol,室温闭环反应6 h,HADE的收率达94.2%,纯度为88.5%.Using 1,2-cyclohexanedicarboxylic acid and epoxy chloropropane as the raw materials, diglycidyl 1, 2-eyclohexanedicarboxylate (HADE) was prepared through ring-opening reaction and ring-closing reaction. The effects of molar ratio of reactants, concentration and amount of sodium hydroxide, the time and temperature of the ring-closing reaction were investigated. The results showed that the optimal reaction conditions are as follows (based on 0.1 mol 1,2-cyclohexanedicarboxylie acid):the molar ratio of 1,2-cyclohexanedicarboxylic acid to epoxy chloropropane was 1:16, hexadecyl trimethyl ammonium bromide was used as catalyst,the ring-opening reaction was carried out at refluxing for 2 h, and the ring-closing reaction was completed at room temperature for 6 h using 0.30 mol 50% NaOH aqueous solution. The yield of HADE was 94.2% and the purity was 88.5% under the optimum reaction condition.
关 键 词:六氢邻苯二甲酸二缩水甘油酯 闭环反应 合成
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