键合法固载酸性离子液体催化贝克曼重排合成己内酰胺

Catalytic synthesis of caprolactam by Beckmann rearrangement over acidic ionic liquid immobilized by bonding method

以硅胶为载体、3-氯丙基三乙基氧基硅烷为硅烷偶联剂、咪唑和1,3-丙烷磺内酯为功能基、硫酸为质子酸,设计合成了硅胶键合咪唑型酸性离子液体催化剂。将该催化剂用于催化环己酮肟重排合成己内酰胺,考察了催化剂的催化活性、反应时间、溶剂用量、反应温度、催化剂用量和催化剂重复使用等因素对该反应的影响,得到了合成己内酰胺的最优条件。结果表明,该催化剂在己内酰胺合成中表现出了极高的活性,使用该催化剂具有易分离,反应条件温和,产品纯度好,收率高等特点。

Using silica gel as carrier,3-chloropropyltriethoxysilane as silane coupling agent,imidazole and 1,3-propane sulfonolactone as functional groups,sulfuric acid as proton acid,silica gel bonded imidazole acid ionic liquid catalyst was designed and synthesized.The catalyst was used to catalyze the rearrangement of cyclohexanone oxime to caprolactam.The influences of catalytic activity,reaction time,dosage of solvent,reaction temperature,dosage of catalyst,and recycle of catalyst were discussed,the best reaction conditions was found.The results showed that the catalyst exhibited high activity in the synthesis of caprolactam.This method takes the advantages of easy separation of catalyst,mild reaction conditions,high purity and yield of the product.