水热法制备固体碱CaO-ZrO2催化合成十二烷二酸二异辛酯  

HYDROTHERMAL SYNTHESIS OF CaO-ZrO2 SOLID BASES CATALYSTS AND ITS APPLICATION IN THE SYNTHESIS OF DIISOOCTYL DODECANEDIOATE

作　　者：宋昌盛 王宸 王志德 郑爱华[2] 李为民[2] Song Changsheng;Wang Chen;Wang Zhide;Zheng Aihua;Li Weimin(Taicang Customs,Taicang 215400,Jiangsu,China;College of Petrochemical Engineering,Changzhou University,Changzhou 213164,Jiangsu,China)

机构地区：[1]太仓海关,江苏太仓215400 [2]常州大学石油化工学院,江苏常州213164

出　　处：《精细石油化工》2019年第5期11-16,共6页Speciality Petrochemicals

基　　金：南京海关科技计划项目(2017KJ42);宜兴市基础设施-重大企业研发机构项目(2018)

摘　　要：采用水热改性法制备了CaO-ZrO2固体碱催化剂,并用于以十二烷二酸、异辛醇为原料催化合成十二烷二酸二异辛酯,对催化剂和产物分别进行了结构表征和理化性能分析。考察了反应温度、原料配比、反应时间、催化剂用量等条件对合成反应的影响。实验结果表明:催化剂较佳水热时间为24 h;合成十二烷二酸二异辛酯的较佳反应条件为反应温度220℃、醇酸摩尔比3∶1、反应时间7 h、催化剂用量为酸质量的2.5%,酯化率为99.19%。CaO-ZrO2固体碱催化剂不经处理可循环使用,使用5次以后酯化率可达95.01%。CaO-ZrO2 solid alkali catalystswere prepared by hydrothermal modification method and characterized by XRD, FT-IR, SEM, TEM and EDS.Diisooctyldodecanedioate was synthesized from dodecanedioic acid and 2-ethyl-1-hexanolby the CaO-ZrO2 solid alkali catalysts. The effects of reaction temperature, raw material ratio, reaction time and catalyst dosage on the synthesis reaction were investigated. The results indicate thatthe better time for hydrothermal reaction time is 24 h, and the optimum conditions for synthesis ofdiisooctyldodecanedioateare shown as follows:reaction temperature 220 ℃, molar ratio of alcohol to acid 3∶1, reaction time 7 h, catalyst dosage 2.5% of dodecanedioic acid. Under the optimal condition, the yield of esterification reaches 99.19%. Furthermore, the CaO-ZrO2 solid alkali catalyst can be reused without treatment, and the yield of esterification can still reach 95.01% when the catalyst is reused for five times. The FT-IR, TG and physicochemical properties of the prepared diisooctyldodecanedioate were analyzed.

关 键 词：水热法 固体碱 氧化钙 氧化锆 十二烷二酸 异辛醇 十二烷二酸二异辛酯 

分 类 号：TQ225.242[化学工程—有机化工]