文献类型：期刊文献

中文题名：乙醛酸法合成香兰素过程研究

英文题名：Study on synthesis process of vanillin by glyoxylic acid

作者：曹仲良[1];潘鹤林[1];束铭杰[1];凌昊[1]

机构：[1]华东理工大学化工学院,上海200237

年份：2016

卷号：45

期号：8

起止页码：1542

中文期刊名：应用化工

外文期刊名：Applied Chemical Industry

收录：CSTPCD;;北大核心:【北大核心2014】；CSCD:【CSCD_E2015_2016】；

语种：中文

中文关键词：香兰素;乙醛酸;愈创木酚;合成

外文关键词：vanillin; glyoxylic acid; guaiacol; synthesis

摘要：以乙醛酸与愈创木酚为原料合成香兰素,分别对其缩合反应、氧化反应做了考察。结果表明,缩合反应较优反应条件为:物料滴加加入,反应温度为35℃,反应时间为6 h,n(乙醛酸)∶n(愈创木酚)∶n(氢氧化钠)=1∶2∶3,未反应愈创木酚先用甲苯萃取,再用氢氧化钠溶液反萃取,用于下次反应;氧化反应较优反应条件为:硫酸铜为氧化剂,n(硫酸铜)∶n(3-甲氧基-4-羟基扁桃酸)=2.4∶1,反应温度为95℃,反应体系pH=13,反应时间为7 h,氧化剂使用双氧水再生。缩合产物收率达到89.5%,氧化产物收率达到98.2%,香兰素精品收率可达到80%,纯度>99.8%,高于以往文献报道。
Vanillin was synthesized by the reaction of glyoxylic acid with guaiacol,its condensation reaction and oxidation reaction were investigated.The results show that the optimal process conditions of condensation reaction is the reaction temperature is 35 ℃,the reaction time is 6 h,n（glyoxylic acid）：n（guaiacol）：n（sodium hydroxide） =1：2：3,unreacted guaiacol extracted with toluene,and then back-extracted with sodium hydroxide /or the next reaction;the optimal process conditions of oxidation reaction is CuSO4 as oxidant,n（CuSO4）：n（3-methoxy-4-hydroxylmandelic acid） =2.4：1,the reaction temperature is 95 ℃,reaction system pH =13,the reaction time is 7 h pxidant regenerated with hydrogen peroxide solution.The yield of condensation product reached 89.5%,the yield of oxidation product reached〉 98.2%,the yield of fine vanillin can reach 80%,and purity 99.8%,higher than that reported in previous studies.