以3-甲基-2-丁烯-1-氯为原料,合成3-甲基-2-丁烯-1-醇的催化水解工艺,利用气相色谱、红外光谱和核磁共振对所得产物进行了表征。通过正交试验讨论了催化剂种类、助催化剂种类、水解温度和水解液pH值对氯代烃的转化率和不饱和醇的选择性的影响。结果表明,最佳工艺条件为:n(氯代烃)∶n(CuCl)∶n(NaI)=1∶0.02∶0.02,水解温度为60℃,水解液pH=6。在此条件下,氯代烃的转化率达到97.83%,不饱和醇的选择性保持在94.19%。此外,研究了催化水解反应中副产物的产生机理及控制措施,提出了水解液循环利用过程中的催化效率保持的方法。
3-Methyl-2-buten-1-ol was prepared from isopentenyl chloride by the catalytic hydrolysis method,and characterized by GC,IR and 1 H NMR.The effects of catalyst type,cocatalyst type,temperature and solution pH on the catalytic hydrolysis reaction were investigated by the orthogonal experiment method.The results indicated that the optimal conditions were:n(isopentenyl chloride)∶n(CuCl)∶n(NaI)=1∶0.02∶0.02,the temperature was 60 ℃,the solution pH was 6.Under the best conditions,the conversion of isopentenyl chloride was up to 97.83%,and the selectivity of 3-methyl-2-buten-1-ol was94.19%.Besides,the generating mechanism and the control measure of the byproduct,and the method of keeping catalytic efficiency in the recycle of hydrolysis solution was proposed.