3,3-二甲基-1-丁烯合成条件的优化

Optimization of Synthetic Conditions of 3,3- Dimethyl-1-butene

探讨了合成3,3-二甲基-1-丁烯(新己烯)的最佳工艺条件。以叔丁醇和盐酸为原料,浓硫酸为催化剂合成氯代叔丁烷,探讨了反应温度和反应时间对收率的影响;采用加压方法,无水AlCl3为催化剂,以氯代叔丁烷和乙烯为原料合成氯代新己烷(2,2-二甲基丁烷);确定了合适的加成反应条件,以N-甲基吡咯烷酮为溶剂,采用反应精馏的方法,氯代新己烷脱氯化氢制备新己烯。实验确定的最佳工艺条件:合成氯代叔丁烷的最佳反应温度为20℃,最佳反应时间为60 min;合成氯代新己烷的最佳反应压力为0.75 MPa,最佳反应温度为45℃;脱氯化氢制备新己烯的最佳溶剂为N-甲基吡咯烷酮。

The best process conditions of the synthesis of 3,3- dimethyl-1-butene（new hexene） were discussed. With tertiary butyl alcohol and hydrochloric acid as raw materials, concentrated sulfuric acid as catalyst for synthesis of chlorinated tertiary butane, the influence of reaction temperature and reaction time on the yield were discussed.Using compression method with anhydrous AlCl3 as catalyst, chlorinated new hexane（2, 2- dimethyl butane） was synthesized with chlorinated tertiary butane and ethylene as raw materials. The suitable addition reaction conditions were determined,with N- methyl pyrrolidone as solvent, adopting the method of reaction distillation,neohexene was prepared after hydrogen chloride was removed from chlorinated new hexane.The obtained best process conditions were that in the synthesis of chlorinated tertiary butane,the optimum reaction temperature was 20 ℃, and the best reaction time was 60 min; in the synthesis of chlorinated new hexane,the optimum reaction pressure was 0.75 MPa, the best reaction temperature was 45℃;N- methyl pyrrolidone was the best solvent for the preparation of nehexene by dehydrochlorination.