四氯化锡掺杂聚苯胺催化合成环己酮1，2-丙二醇缩酮

Catalytic Synthesis of Cyclohexanone 1,2-Propanediol Ketal on Polyaniline Doped with Stannic Chloride

以聚苯胺(PAn)和SnCl_4为原料,制备了掺杂率为11.1%(质量分数)的SnCl_4掺杂PAn(PAn-SnCl_4)催化剂。以PAn-SnCl_4为催化剂、环己酮和1,2-丙二醇为原料合成了环己酮1,2-丙二醇缩酮;考察了PAn-SnCl_4催化剂对缩酮化反应的催化活性;通过单因素实验及正交实验,考察了原料配比、催化剂用量、带水剂用量、反应时间等因素对环己酮1,2-丙二醇缩酮收率的影响。实验结果表明,在n(环己酮):n(1,2-丙二醇)=1:1.5、催化剂用量占反应物料总质量的2.5%、带水剂环己烷用量18 mL、反应时间1.0 h的优化条件下,环己酮1,2-丙二醇缩酮的收率达85.86%,产品纯度为99.54%。催化剂的重复使用性好,重复使用5次后环己酮1,2-丙二醇缩酮的收率仍达80.02%。

Cyclohexanone 1,2-propanediol ketal was synthesized from cyclohexanone and 1,2- propanediol on polyaniline doped with stannic chloride pentahydrate as catalyst. The catalyst was prepared from polyaniline and stannic chloride pentahydrate. Doping amount （mass fraction） of the latter was 11.1%. Factors influencing product yield were discussed and optimum reaction conditions were found by single factor experiments and orthogonal experiments. Under optimal conditions： n（cyclohexanone） ：n（ 1,2-propanediol） 1： 1.5, mass fraction of polyaniline doped with stannic chloride 2.5%, cyclohexane 18 mL and reaction time 1.0 h, yield and purity （ mass fraction） of cyclohexanone 1,2-propanediol ketal are 85.86% and 99.54%, respectively. After catalyst was reused 5 times, yield to cyclohexanone 1,2-propanediol ketal still kept at 80.02%. Preparation of polyaniline doped with stannic chloride pentahydrate catalyst is simple in procedure. The obtained catalyst is high in activity and good in repeatability, with convenient final treatment.