生物质基平台化合物制备乙酰丙酸缩酮酯的工艺  

Preparation of levulinic acid ketal ester from biomass-based platform compounds

作　　者：郭鹏坤 徐艳丽[1] 李攀[1,2] 常春 肖泽[1] 白净 方书起[1,2] GUO Peng-kun;XU Yan-li;LI Pan;CHANG Chun;XIAO Ze;BAI Jing;FANG Shu-qi(School of Chemical Engineering and Energy,Zhengzhou University,Zhengzhou 450001,China;Henan Outstanding Foreign Scientists’Workroom,Zhengzhou 450001,China;Key Laboratory of Biomass Chemical Engineering of Ministry of Education,Zhejiang University,Hangzhou 310027,China)

机构地区：[1]郑州大学化工与能源学院,河南郑州450001 [2]河南省杰出外籍科学家工作室,河南郑州450001 [3]浙江大学生物质化工教育部重点实验室,浙江杭州310027

出　　处：《高校化学工程学报》2020年第5期1250-1257,共8页Journal of Chemical Engineering of Chinese Universities

基　　金：生物质化工教育部重点实验室(浙江大学)开放基金资助项目(2018BCE001);河南省杰出外籍科学家工作室生物质资源加工与高效利用(GZS2018004)。

摘　　要：为了探究由生物质基平台化合物制备乙酰丙酸缩酮酯的工艺路线,以超低酸为催化剂,由乙酰丙酸乙酯(EL)和甘油(GLY)为原料制备乙酰丙酸甘油缩酮乙酯(ELK)。考察并优化ELK生成的工艺条件,在反应温度为127℃、真空度为91 kPa、当EL与GLY摩尔比n(EL):n(GLY)为5.1时,ELK的摩尔收率达到98.9%。在此基础上,利用红外光谱、液质、气质和核磁共振对产物ELK进行表征。结果表明此体系真空度、n(EL):n(GLY)、反应温度等因素对ELK的产率影响显著,经过提纯工艺,获得了纯度95%左右的ELK。In order to explore the process of preparing levulinic acid ketal ester from biomass platform compounds,a method of preparing ELK from ethyl levulinate(EL)and glycerin(GLY)using ultra-low acid as catalyst was proposed.The effects of reaction temperature,reaction pressure,EL and GLY molar ratio n(EL):n(GLY)on ELK yield were investigated,and the process conditions for ELK generation were optimized.When the reaction temperature was 127℃,the vacuum degree was 91 kPa and n(EL):n(GLY)was 5.1,the molar yield of ELK reached 98.9%.Furthermore,ELK was characterized by FT-IR,LC-MS,GC-MS and NMR.The results show that vacuum degree,n(EL):n(GLY),reaction temperature and other factors have significant effects on ELK yield,and ELK with purity of 95%is obtained after purification.

关 键 词：乙酰丙酸乙酯(EL) 甘油(GLY) 乙酰丙酸甘油缩酮乙酯(ELK) 催化 生物质 

分 类 号：S216.2[农业科学—农业机械化工程]