草酸二丁酯合成工艺优化  

Synthesis process optimization of dibutyl oxalate

作　　者：龚旌[1] 

机构地区：[1]闽江学院化学与化学工程系,福建福州350121

出　　处：《闽江学院学报》2013年第5期114-117,共4页Journal of Minjiang University

基　　金：福建省省属高校科研专项(JK2012036)

摘　　要：探索用环己烷作带水剂,草酸和正丁醇作原料,硫酸氢钠作催化剂合成草酸二丁酯的工艺,在单因素实验的基础上,进行了二次回归正交试验,建立了回归方程数学模型,同时得出最优反应条件为:催化剂用量为反应物总质量的1.41%,n(环己烷)∶n(草酸)=1.5∶1,正丁醇和草酸比例为3.01∶1(物质的量比),温度115℃,回流反应45 min,减压蒸馏,酯收率达83.97%.产物通过阿贝折光仪和红外光谱仪分析,折光率与文献值接近,红外谱图显示有丁酯特征峰,表明产物为草酸二丁酯.Using cyclohexane as dehydration, sodium bisulfate as catalyst, dibutyl oxalate was synthesized by oxalic acid and n-butanol, On the basis of single-factor experiment, second regression of central com- posite design, and establish to a mathematical models of regression equation. The optimal comditions were as follows： the amount of catalyst was 1.41% of total reactant, n （cyclohexane）：n （oxalic acid） = 1.5： 1, n（n-butanol） ： n（ oxalic acid） = 3.01 ： 1, reaction temperature was 115℃ , reflux reaction time was 45 minutes, adopts vacuum distillation, reach the optimal reaction yield was 83.97%. The product was ana- lyzed by FT-IR and Abbe refractometer, refractive index is consistent with the literature values, FT-IR analysis showed that there are characteristic peaks dibutyl, proved the product was dibutyl oxalate.

关 键 词：草酸二丁酯 合成 催化 

分 类 号：TQ425.23[化学工程]