熔融-固相酯化法合成季戊四醇四氯乙酸酯  

Synthesis of chloroacetic pentaerythritol tetraester by melt solid esterification method

作　　者：郑晓凤[1] 刘海舰[1] 张然[2] 

机构地区：[1]曲阜师范大学化学与化工学院,山东曲阜273165 [2]滨州学院材料化学研究所,山东滨州256600

出　　处：《工业催化》2014年第10期804-808,共5页Industrial Catalysis

基　　金：山东省教育厅高等学校科技计划(J12LD04)资助项目;曲阜师范大学科研启动基金(BSQD20110120)资助项目;滨州学院青年人才基金(BZXYQNLG200704)资助项目

摘　　要：季戊四醇衍生物分子具有高度对称性,在科研和工业领域用途广泛。季戊四醇与氯乙酸缩合反应,由于季戊四醇的溶解局限性,难以实现溶液合成。在无溶剂条件下,以SO2-4/TiO2-SnO2固体超强酸为催化剂,通过熔融-固相酯化法进行季戊四醇四氯乙酸酯的合成,考察催化剂用量、反应物物质的量比、反应时间和反应温度等对酯化反应的影响。结果表明,在催化剂用量为反应物总质量的4%、n(季戊四醇)∶n(氯乙酸)=1∶4.2、反应温度170℃和反应时间6 h条件下,季戊四醇四氯乙酸酯产率为98.7%。对产物进行了IR和1H NMR表征。Pentaerythritol derivatives with high symmetrical molecular structures have wide application in the fields of research and industry. It is difficult to achieve the esterification reaction of pentaerythritol and ehloroacetic acid in solution due to the dissolution limitation of pentaerythritol. In this paper, using SO2-/ TiO2-SnO2 solid superacid as the catalyst, ehloroacetic pentaerythritol tetraester was synthesized by melting solid esterification method under solvent-free condition. The influence of catalyst dosage, molar ratio of reactants, reaction time and reaction temperature on the esterification was investigated. The results showed that chloroaeetic pentaerythritol tetraester yield of 98.7% was attained under the optimal reaction condition as follows ： catalyst dosage 4% of the total mass of the reactants, n （pentaerythritol） ： n （ chloroacetic acid） = 1：4.2, reaction temperature 170 ℃ and reaction time 6 h. The product was characterized by IR and 1H NMR techniques.

关 键 词：精细化学工程 季戊四醇四氯乙酸酯 固体超强酸 熔融-固相酯化法 

分 类 号：TQ223.164[化学工程—有机化工] TQ426.94