3甲基2丁烯1醇的制备新工艺.pdfVIP

化 工 进 展 2015 年第34 卷第 1 期 CHEMICAL INDUSTRY AND ENGINEERING PROGRESS ·229 · 研究开发 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 （天津大学化工学院，天津 300072 ） 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; 水解; 精馏 中图分类号：TQ 21 文献标志码：A 文章编号： 1000 –6613 （2015 ）01 –0229 –05 DOI ：10.16085/j.issn.1000-6613.2015.01.041 A new process on the preparation of 3-methyl-2-butene-1-ol ZHOU Baoqiang ，SONG Linlin ，ZHANG Nan ，GAO Ruichang （School of Chemical Engineering and Technology，Tianjin University ，Tianjin 300072 ，China ） 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:brominatedisoamylene; 3-methyl-2-buten-1-ol; hydrolysis ; distillation 3- 甲基