化工进展 ›› 2015, Vol. 34 ›› Issue (1): 229-233.DOI: 10.16085/j.issn.1000-6613.2015.01.041

• 精细化工 • 上一篇    下一篇

3-甲基-2-丁烯-1-醇的制备新工艺

周宝强, 宋林林, 张楠, 高瑞昶   

  1. 天津大学化工学院, 天津 300072
  • 收稿日期:2014-05-30 修回日期:2014-07-03 出版日期:2015-01-05 发布日期:2015-01-05
  • 通讯作者: 高瑞昶,副教授。E-mail pharmacy@tju.edu.cn。
  • 作者简介:周宝强(1990-),男,硕士研究生。

A new process on the preparation of 3-methyl-2-butene-1-ol

ZHOU Baoqiang, SONG Linlin, ZHANG Nan, GAO Ruichang   

  1. School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China
  • Received:2014-05-30 Revised:2014-07-03 Online:2015-01-05 Published:2015-01-05

摘要: 研究了以溴代异戊烯水解工艺和精馏分离工艺为基础来制备3-甲基-2-丁烯-1-醇的新工艺。通过优化溶剂种类得到当水解溶剂为偶极类溶剂乙腈时,得到产物的选择性最高。并通过进一步优化实验操作条件,得到当溶剂加入量为v(乙腈):v(溴代异戊烯)=1:1,水解温度为70℃,碱用量为n(NaOH):n(溴代异戊烯)=1.2:1和反应时间为25min时,水解部分3-甲基-2-丁烯-1-醇的转化率最高可达63.35%。水解后的料液通过间歇精馏得到纯的3-甲基-2-丁烯-1-醇,最终的3-甲基-2-丁烯-1-醇总收率达到57.4%。

关键词: 溴代异戊烯, 3-甲基-2-丁烯-1-醇, 甲基丁烯醇, 水解, 精馏, 溴代异戊烯, 3-甲基-2-丁烯-1-醇, 水解, 精馏

Abstract: A new technology for the preparation of 3-methyl-2-butene-1-ol was investigated based on the hydrolysis of brominated isoamylene and distillation separation technology. By choosing a dipolar solvent, acetonitrile, for the hydrolysis the products showed the highest selectivity. And through further the optimization of experimental operating conditions, hydrolysis yield of 3-methyl-2-butene-1-ol reached 63.35% under the condition of the solvent amount v(acetonitrile):v(bromo-3-ene) = 1:1, hydrolysis temperature 70℃, base amount n(NaOH):n(bromo-3-ene) = 1.2:1 and reaction time 25 minutes. The pure 3-methyl-2-butene-1-ol was made of the feed liquid after hydrolysis by batch distillation operation, and the final total yield of 3-methyl-2-butene-1-ol reached 54%.

Key words: brominated isoamylene, 3-Methyl-2-buten-1-ol, 3-methyl-2-butene-l-ol , hydrolysis , distillation, brominatedisoamylene, 3-methyl-2-buten-1-ol, hydrolysis, distillation

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