Abstract:

In order to solve the key technical problems such as similar boiling points of cyclohexanol distillation residues and the difficulty of separation by conventional separation methods, the 3-cyclohexylcyclohexene, 1-cyclohexylcyclohexene and dicyclohexylidene were reduced to cyclohexylcyclohexane by catalytic hydrogenation and the boiling point difference between the two components was enlarged. High purity cyclohexylcyclohexane and dicyclohexyl ether were obtained by vacuum distillation. Using Pd/C as catalyst, the optimum conditions for catalytic hydrogenation of 3-cyclohexylcyclohexene, 1-cyclohexylcyclohexene and dicyclohexylidene to cyclohexylcyclohexane in residual solution were obtained. The reaction temperature was 120℃, the reaction time was 4 h, the reaction pressure was 4 MPa, the stirring speed was 550 r/min, the amount of Pd/C catalyst was 0.4% of the mass of the material, the selectivity was more than 99.5% and the conversion rate of the materials was 98.7%. After vacuum distillation, the purity of cyclohexylcyclohexane and dicyclohexyl ether is more than 99.5%.

Key words: residual liquid of cyclohexanol distillation tower, dicyclohexyl ether, cyclohexylcyclohexane, hydrogenation, separation, optimization

摘要：

针对环己醇精馏残液中各组分沸点相近，常规分离方法分离难度大等技术问题，采用催化加氢的方法将环己醇精馏残液中的3-环己基环己烯、1-环己基环己烯和环己亚基环己烷还原为双环己烷，扩大分离组分间的沸点差，经减压精馏分离，得到高纯度的双环己烷和二环己基醚。以Pd/C为催化剂，通过对比实验获得了环己醇精馏残液中的3-环己基环己烯、1-环己基环己烯和环己亚基环己烷催化加氢转化为双环己烷的最佳工艺条件：反应温度120℃、反应压力4 MPa、反应时间4 h、搅拌速度550 r/min、Pd/C催化剂用量为物料质量的0.4%，原料转化率为98.7%，双环己烷的选择性大于99.5%；经减压精馏分离后，双环己烷和二环己基醚的纯度大于99.5%。

关键词: 环己醇精馏残液, 二环己基醚, 双环己烷, 加氢, 分离, 优化