磁载钛硅分子筛TS-1/NiFe_2O_4催化环己酮氨肟化反应研究

Study on ammoximation of cyclohexanone catalyzed by magnetic titanium silicalite molecular sieve TS-1 /NiFe_2O_4

钛硅分子筛(TS-1)是绿色催化领域具有原子经济特征的新型催化剂,环己酮肟是化学工业重要的中间体,本文采用磁载钛硅分子筛(MTS-1)作为催化剂,研究了环己酮氨肟化制备环己酮肟,实验考察了物料比、温度、反应时间、催化剂用量、溶剂比等工艺参数对催化反应的影响。研究结果表明:以叔丁醇-水体系为溶剂,叔丁醇与水体积比为1∶1,原料环己酮/过氧化氢/氨水摩尔比为1∶1.2∶1.8,反应温度80℃,反应时间2.5h,磁载钛硅分子筛用量为0.2g/g环己酮,环己酮转化率、环己酮肟选择性和环己酮肟收率可分别达到96%、98%和94%。

Titanium silicalite（ TS-1 ）had been known as a new type atom-economic characteristics of the catalyst in green chemical industry field. Cyclohexanone oxime was an important intermediate in chemical industry. Ammoximation of cyclohexanone was cata- lyzed by magnetic titanium silicalite molecular sieve（ MTS-I ）in this paper. The influences of the reactants ratios,temperature,reac- tion time,MTS-1 amount and the ratio of solvent were investigated. The experiments results indicated that the optimum operating conditions were a mixture of water and t-butanol with volume ratio of 1 ： 1 as reaction solvent system and an cyclohexanone/hydrogen peroxide/ammonia molar ratio of 1：1.2：1.8 at a reaction temperature of 80℃and a residence time about 2. 5h, the catalyst/cyclohexanone ratio was 0. 2g/g. The cyclohexanone conversion,oxime selectivity and oxime yield could amount to 96% ,98% and 94% respectively.