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机构地区:[1]无锡石油化工总厂,江苏无锡214016 [2]蓝星总公司,北京100000 [3]广西大学化工系,530004
出 处:《广州化工》2006年第5期17-18,共2页GuangZhou Chemical Industry
摘 要:由柠檬酸和正丁醇在复合催化剂存在下合成柠檬酸三丁酯。它再与醋酐于复合催化剂下合成乙酰柠檬酸三丁酯。酯化反应的最佳条件为:柠檬酸与正丁醇的物质量之比为1:3.5,于100℃~130℃反应,催化剂质量为柠檬酸的0.8%,反应时间2.8 h,酯化率>99.4%,纯度>99.5%;乙酰化最佳反应条件为:柠檬酸三丁酯与醋酐物质的量之比为1:1.4,于60℃~85℃反应时间为1.4 h,催化剂用量为柠檬酸三丁酯的0.01%(质量),乙酰化转化率>99.5%,纯度为99.5%。Non - toxic tributyl citrate was synthesized by citric acid and n - butanol. The non - toxic acetyl tributyy citrate was synthsized by tributyl citrate and acetyloxide in the presence of compounded catalyst. The optinum esterification conditions were determined as follows: molar ratio of citric acid to n - butanol was 1 : 3.5, reaction temperature 100℃- 130℃, quantity of catalyst accounted for 0.8 % of citric acid and reaction time was 2.8 hs. The final corversion of more than 99.4 % with a purity of more than 99.5 %. The optinun acetyla- tion conditions were determined as follows: molor ratio of tributyl citrate to acetyloxide was 1 : 1.4, reaction temperature 80℃ - 85℃, reaction time 1.4 hs, quanitiy of catalyst accounted for 1% of tributyl citrate. Resulted in final conversion of more than 99.5 %. The optinun acetylation conditions were determined as follows:molor ratio of tributyl citrate to acetyloxide was 1 : 1.4, reaction temperature 80℃ -85℃, reaction time 1.4 hs, quantity of catalyst accounted for 1% of tributyl citrate. Resulted in final conversion of more than 99.5 % with a purity of more than 99.5 %.
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