第 47 卷第 4 期Vol. 47 No. 4
2017 年 8 月Aug 2017

所属栏目:香精香料

正交法优化柠檬醛合成紫罗兰酮工艺
杨海宽,温世坊,李 江,章 挺,汪信东 (江西省林业科学院 国家林业局樟树工程技术研究中心,江西 南昌 330032)
摘 要:以柠檬醛和丙酮为原料,在氢氧化钠催化条件下,经羟醛缩合反应先制备假性紫罗兰酮,再在磷酸催化条件下,经环化反应制备紫罗兰酮。采用正交法研究了一锅法条件下,柠檬醛合成紫罗兰酮工艺条件。合成假性紫罗兰酮优化工艺条件是:物料比n(柠檬醛) ∶ n(丙酮)=1 ∶ 6,催化剂用量比w(10%NaOH) ∶ w(柠檬醛)=4%,反应温度60℃,反应时间3 h。合成紫罗兰酮优化工艺条件:物料比n(柠檬醛) ∶ n(H3PO4)=1 ∶ 1,反应温度40℃,反应时间3 h。
关键词:柠檬醛;紫罗兰酮;正交法
中图分类号:TQ655  文献标识码:A  文章编号:1009-9212(2017)04-0036-03
Synthesis of Ionone from Citral Using Orthogonal Method
YANG Hai-kuan, WEN SHI-fang, LI Jiang, ZHANG Ting, WANG XIN-dong (Camphor Engineering and Technology Research Center for State Forestry Administration, Jiangxi Academy of Forestry, Nanchang 330032, China)
Abstract:The pseudoionone was synthesized from citral and acetone by aldol condensation using sodium hydroxide as catalyst. The ionone was synthesized by cyclization using phosphoric acid as catalyst. The optimized synthesis technology of ionone from citral by one step were studied using orthogonal method. The optimized synthesis technology of pseudoionone were as following: mole ratio of citral to acetone was of 1:6, mass ratio of 10% sodium hydroxide to citral was of 4%, reaction temperature was of 60℃, reaction time was of 3 h. The optimized synthesis technology of ionone were, mole ratio of citral to phosphoric acid was of 1∶6, reaction temperature was of 40℃, reaction time was of 3 h.
Key words:citral; ionone; orthogonal test
基金项目:江西省重大科技专项“樟属珍稀香料植物优良系选育及利用研究”(20143ACF60014)。
作者简介:杨海宽(1985-),男,江西吉安人,助理研究员,硕士,研究方向:林产化学加工工程(E-mail:Yanghaikuan1985@163.com)
收稿日期:2017-08-13