摘要
以马来酸酐为原料,过氧化氢为氧化剂,钨酸盐为催化剂合成环氧琥珀酸,考察了反应温度、反应时间、物料配比、氧化剂及催化剂用量对环氧化反应和水解反应的影响规律,研究了提纯方法。结果表明,反应温度65℃,反应时间1.5h,催化剂用量3%(wt%),氢氧化钠与马来酸酐摩尔比2∶1,过氧化氢与马来酸酐质量比1.2∶1,环氧琥珀酸收率88%。采用间接法计算环氧琥珀酸产率,可精确计算收率。甲醇重结晶法可以提纯环氧琥珀酸,所得产率与间接法计算结果基本一致。经红外光谱仪分析确定产物为环氧琥珀酸。
Epoxysuccinic acid was synthesized using maleic anhydride as raw material, hydrogen peroxide as oxidizer and tungstate as catalyst. The effects of reaction temperature, reaction time, ratio of materials, dosage of oxidizer and catalyst on epoxidation and hydrolysis reaction were investigated. Purification method of epoxysuccinic acid was also researched. The results showed that the yield of epoxysuccinic acid was 88%when the reaction conditions were as followed:reaction temperature 65℃, reaction time 1.5h, catalyst dosage 3%(wt%), molar ratio of sodium hydrate to maleic anhydride 2:1, mass ratio of hydrogen peroxide to maleic anhydride 1.2:1. The yield of epoxysuccinic acid was indirectly obtained. This indirect method could calculate the yield of epoxysuccinic acid precisely and overcome the disadvantage of obtaining inpure product by recrystallization method. Methanol recrystallization method could purify epoxysuccinic acid which had a same conclusion with indirect method. Infrared spectrometer demonstrated that the product was epoxysuccinic acid.
出处
《化工技术与开发》
CAS
2014年第1期9-12,共4页
Technology & Development of Chemical Industry
基金
黑龙江省大学生创新创业训练计划项目资助(CX12018)
黑龙江省普通高校石油与天然气化工重点实验室资助(HXHG2012-01)
关键词
钨酸盐催化剂
环氧琥珀酸
合成规律
产率测定
提纯
表征
tungstate catalyst
epoxysuccinic acid
synthesis regularity
determination of yield
purification
characterization