全文下载:2012050445
王开明1,2, 李国强3*
(1. 青岛科技大学 化学与分子工程学院, 山东 青岛 266042;2.山东理工职业学院 化工新材料工程系,山东 济宁 272067;
3. 中国海洋大学 医药学院, 山东 青岛 266003)
摘要: 以丙烯醛二乙缩醛为原料,通过单因素实验建立了优化的温和液相反应条件。合成3-甲基吡啶的优化工艺条件为:以乙酸为溶剂,反应温度130 ℃,料比n(丙烯醛二乙缩醛)∶n(乙酸铵)∶n(乙酸)=1∶9.48∶21.33。溶剂为酸性,可以极大地促进反应的正向进行,起到了催化剂的作用。在优化条件下,实现了丙烯醛二乙缩醛转化率100%,3-甲基吡啶收率65.90%。
关键词: 3-甲基吡啶;丙烯醛二乙缩醛;液相反应;工艺优化
中图分类号: TQ 253.2 文献标志码: A
收稿日期:2012-02-27
基金项目: 国家自然科学基金项目(20975094).
作者简介: 王开明(1987—),男,硕士研究生.*通信联系人.
Preparation of 3-Picoline by Mild Liquid Phase Reaction of Acrolein Diethyl Acetal
WANG Kai-ming1,2,LI Guo-qiang3
(1.CollegeofChemistryand Molecular Engineering,QingdaoUniversityof Science and Technology,Qingdao266042,China;
2.Department of Chemical Engineering and New Materials,Shandong Career Development College,Jining 272067,China;
3.SchoolofMedicineand Pharmacy,OceanUniversityofChina,Qingdao266003,China)
Abstract: The synthesis of 3-picoline by mild liquid phase reaction using acolein diethyl acetal as raw material. The reaction conditions were optimized and the obtained optimum conditions were using acetic acid as solvent, temperature130℃, n(acolein diethyl acetal)∶n(acetic ammonium)∶n(acetic acid)=1∶9.48∶21.33. Under above conditions, the conversion of acolein diethyl acetal was almost 100% and the yield of 3-picoline was 65.90%.
Key words: 3-picoline; acolein diethyl acetal; liquid phase reaction; process optimization
孟祥奎, 杨慧, 王涛, 曹长青*
(青岛科技大学 化工学院,山东 青岛 266042)