3-甲基-2-丁烯-1-醇的制备新工艺.pdfVIP

学兔兔 化 工 进 展 2015年第34卷第1期 CHEMICAL INDUSTRYAND ENGINEERING PROGRESS ·229· 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．2一丁烯．1一醇的新工艺。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)：’，(溴代异戊烯)=1：l，水解温度为70~C，碱用量为n(NaOH)： (溴代异戊烯)：1．2：1和 反应时间为25min时，水解部分3一甲基一2。丁烯一1．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．1一醇；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 D0I：10．16085~．issn．1000—66l3．2015．01．041 A new process on the preparation of 3-methyl-2-butene-l-ol ZHOUBaoqiang，SONGLinlin，ZHANGNan，GAORuichang (School of Chemical Engineering and Technology，Tianjin University，Tianjin 300072，China) Abstract：A new technology for the preparation of 3-methy1．2．butene一1一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一2一butene一1一o1 reached 63．35％under the condition of the solvent amount v(acetonitrile)：v(bromo．3．ene)=1：1， hydrolysis temperature 70℃，base amount aOH)：n(bromo．3．ene)=1．2：1 and reaction time 25 minutes．The pure 3-methy1—2一butene-1-ol was made of the feed liquid after hydrolysis by batch distillation operation，and the final total yield of3-methy1．2．butene．1一ol reached 54％． Key words：brominatedisoamylene；3-methy