碳酸钾催化反应蒸馏技术合成β-二醇二苯甲酸酯  

Synthesis of β-dioldibenzoates through reactive distillation catalyzed by K_2CO_3

作　　者：冯再兴[1] 孙竹芳[1] 赵思文[1] 赵思源[1] 田宇[1] 谢伦嘉[1] 

机构地区：[1]中国石化北京化工研究院,北京100013

出　　处：《石油化工》2016年第5期542-547,共6页Petrochemical Technology

摘　　要：以碳酸钾为催化剂,利用反应蒸馏技术合成β-二醇二苯甲酸酯,考察了反应温度、催化剂加入量、苯甲酸甲酯加入量、苯甲酸酯种类、共沸剂等对合成β-二醇二苯甲酸酯反应的影响,研究了苯甲酸甲酯和催化剂的回收再利用。实验结果表明,合成β-二醇二苯甲酸酯适宜的反应条件为：n（2,4-戊二醇）∶n（苯甲酸甲酯）∶n（碳酸钾）=1∶3.00∶0.030、反应温度150~160℃、甲苯为共沸剂,在此条件下,2,4-戊二醇的转化率达99.9%以上,2,4-戊二醇二苯甲酸酯的选择性达99.9%,收率为99.9%;回收的苯甲酸甲酯不经处理即可被使用,回收的催化剂使用3次后,产物仍具有较高的选择性,可提高原料的利用率,降低生产成本。A reactive distillation method for the synthesis of β-diol dibenzoates through transesterification was established with K_2CO_3 as the catalyst. The effects of reaction temperature,molar ratio of catalyst to methyl benzoate and β-diol,benzoate type and azeotropic agent on the synthesis were investigated. The recovery and reuse of the methyl benzoate and catalyst were also studied. Under the optimal reaction conditions of n（2,4-pentanediol）∶n（methyl benzoate）∶n（K_2CO_3） 1∶3.00∶0.030,reaction temperature 150-160 ℃ and toluene as the azeotropic agent,the conversion of 2,4-pentanediol,selectivity to 2,4-pentanediol dibenzoate and yield of 2,4-pentanediol dibenzoate reached more than 99.9%,99.9% and 99.9%,respectively. The recovered methyl benzoate could be reused without any treatment and the catalyst could be reused 3 times.

关 键 词：酯交换反应 β-二醇二苯甲酸酯 碳酸钾 反应蒸馏技术 

分 类 号：TQ245.2[化学工程—有机化工]