第 38 卷第 1 期Vol. 38 No. 1
2008 年 2 月Feb 2008

所属栏目:有机合成原料

2,2-二甲基-3-羟基丙醛的合成工艺研究
郭振美1,李 强2,李 露1 (1.青岛科技大学 化工学院,山东 青岛 266042;2.烟台万华合成革集团有限公司,山东 烟台 264002)
摘 要:以异丁醛和甲醛为原料,三乙胺为催化剂,羟醛缩合法合成了2,2-二甲基-3-羟基丙醛。考察了物料比、加料方式、反应温度和反应时间对反应结果的影响,同时考察了产品的分离精制工艺。在物料比n(异丁醛) ∶ n(甲醛) ∶n(三乙胺)为1∶1.1∶0.02、反应温度61~65℃的优化反应条件下,反应4~5 h,所得产品经水洗、减压、蒸馏和结晶后,2,2-二甲基-3-羟基丙醛收率达到95%,纯度为99%以上。
关键词:2,2-二甲基-3-羟基丙醛;羟醛缩合;碱催化
中图分类号:TQ031.2  文献标识码:A  文章编号:1009-9212(2008)01- 0044-03
Study on the Synthesis of 2,2-Dimethyl-3-hydroxy Propanal
GUO Zhen-mei1,LI Qiang2,LI Lu1 (1. College of Chemical Engineering,Qingdao University of Science & Technology,Qingdao 266042 ,China;2. Design Institute,Yantai Wanhua Co.,Ltd.,Yantai 264002,China)
Abstract:The preparation of 2,2-dimethyl-3-hydroxy propanal from the condensation of formaldehyde and i-butyraldehyde by using triethylamine as catalyst was studied. The main effect factors. ratio of materials,charging-up mode,reaction time and reaction temperature were examined. The obtained reaction optimum conditions were as follows:n(i-butyraldehyde)∶ n(formaldehyde)∶ n(triethylamine) =1∶ 1.1∶ 0.02,61~65℃,4~5 h. Under above reaction conditions,and after purification,the yield and purity of product reached 95% and more than 99%,respectively.
Key words:2,2-dimethyl-3-hydroxy propanal;condensation;base catalysis
作者简介:郭振美(1965-),女,山东青岛人,工程师,硕士,主要从事有机合成工艺研究。(E-mail:gzhenm@sina.com)
收稿日期:2007-12-10