Reaction rectification device and method for preparing cyclohexanol by hydrating cyclohexene

A cyclohexene water and reactive rectification technology is applied in the field of reactive rectification devices for preparing cyclohexanol by hydration of cyclohexene, and can solve the problems of accelerating cyclohexene hydration reaction speed, slow hydration reaction speed, poor mechanical strength and the like , to improve the one-way conversion rate and solve the effect of high energy consumption

Inactive Publication Date: 2018-12-14
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

In 2014, it was reported that macroporous resin 15 catalyst was used to simulate reactive distillation process. In 2017, Fuzhou University used ion exchange resin A-36 catalyst to simulate reactive distillation process. However, macroporous resin 15 and ion exchange resin A -36 has disadvantages such as poor mechanical strength, poor thermal stability, and short service life.
Although the reactive distillation method can theoretically greatly increase the conversion rate of cyclohexene and reduce the energy consumption of the system, the hydration reaction speed is slow. This process increases the concentration of cyclohexene in water by adding a co-solvent to the reactive distillation system. Solubility, speed up the hydration reaction rate of cyclohexene, can be used to solve the existing problems in the current industrial production

Method used

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  • Reaction rectification device and method for preparing cyclohexanol by hydrating cyclohexene

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Experimental program
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Embodiment 1

[0038] (1) The diameter of the reactive distillation column is 450mm, the column height is 14500mm, and the total number of plates is 29; (2) The process conditions in the reactive distillation column: the flow rate of cyclohexene is 80kmol / h, the flow rate of ethylene glycol ether 80kmol / h, water flow rate 320kmol / h, ZSM-5 molecular sieve catalyst mass concentration 30%, reaction temperature 120°C, reaction pressure 0.5MPa; (3) water and catalyst enter from the 6th tray The feed port is added to the reactive distillation tower, and water and catalyst flow between the sieve plates of the reactive distillation tower in a slurry state; (4) cyclohexene and ethylene glycol ether are fed from the feed port at the 17th tray Added to the reactive distillation tower, it turns into steam at high temperature, enters the slurry through the sieve holes on the sieve plate, contacts the slurry in reverse, and under the catalysis of the catalyst, cyclohexene reacts with water to form cyclohex...

Embodiment 2

[0041] (1) The diameter of the reactive distillation column is 450mm, the column height is 14500mm, and the total number of plates is 29; (2) The process conditions in the reactive distillation column: the flow rate of cyclohexene is 70kmol / h, and the flow rate of propylene glycol methyl ether is 42kmol / h, water flow rate is 70kmol / h, ZSM-5 molecular sieve catalyst mass concentration is 10%, reaction temperature is 110°C, reaction pressure is 0.3MPa; (3) Water and catalyst feed from the sixth tray (4) Cyclohexene and propylene glycol methyl ether are fed into the reactive distillation tower from the inlet of the 17th tray. In the reactive distillation tower, it turns into steam at high temperature, enters the slurry through the sieve holes on the sieve plate, contacts the slurry in reverse, and under the catalysis of the catalyst, cyclohexene reacts with water to form cyclohexanol; (5) unreacted cyclohexene Hexene, propylene glycol methyl ether and water vapor enter the conden...

Embodiment 3

[0044] (1) The diameter of the reactive distillation column is 450mm, the column height is 14500mm, and the total number of plates is 29; (2) The technological conditions in the reactive distillation column: the flow rate of cyclohexene is 60kmol / h, and the flow rate of dimethylformamide The flow rate is 48kmol / h, the water flow rate is 120kmol / h, the mass concentration of ZSM-5 molecular sieve catalyst is 15%, the reaction temperature is 130°C, and the reaction pressure is 0.4MPa; The feed inlet is added to the reactive distillation tower, and water and catalyst flow between the sieve plates of the reactive distillation tower in a slurry state; (4) cyclohexene and dimethylformamide are fed from the 17th tray The feed port is added to the reactive distillation tower, which turns into steam at high temperature, enters the slurry through the sieve holes on the sieve plate, and contacts the slurry in reverse, and under the catalysis of the catalyst, cyclohexene reacts with water t...

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Abstract

The invention belongs to the technical field of a chemical process and equipment, and relates to a reaction rectification device and a reaction rectification method for preparing cyclohexanol by hydrating cyclohexene. The device comprises four parts, namely a reaction rectification tower, a settling separator, a separation tower and a liquid storage tank. Steam and slurry in the reaction rectification tower are in reverse contact to generate violent disturbance, so that the cyclohexene hydration reaction process is realized; reaction products are subjected to settling separation and only the organic phase is added into a stripping section, so that reverse reaction of the cyclohexanol can be inhibited; in the settling separator, the aqueous phase and the organic phase are separated, and water and a catalyst can be recycled; the cyclohexene, a cosolvent and the cyclohexanol in the separation tower are separated to obtain high-purity cyclohexanol, and the cyclohexene and the cosolvent canbe recycled; and the high-purity cyclohexanol is stored in the liquid storage tank. By the device and the method, the problems that conversion per pass of the cyclohexene is low and the reaction energy consumption is high in the cyclohexene hydration reaction; moreover, the device and the method has the following advantages: the whole flow can be operated continuously and stably, the water and the catalyst can be recycled, and the cyclohexene and the cosolvent can be recycled.

Description

technical field [0001] The invention belongs to the technical field of chemical technology and equipment, and relates to a reactive distillation device and method for preparing cyclohexanol through hydration of cyclohexene. Background technique [0002] Cyclohexanol is an excellent organic chemical product with a medium to high boiling point, mainly used as an intermediate raw material for the production of important chemical products such as adipic acid, caprolactam and polyamide-66; in the coating industry as a solvent for paint, shellac and varnish, It has good emulsifying ability; it can be used as a dye solvent and matting agent in the textile industry; it can also be used as a stabilizer for water-soluble latex. Traditional methods for producing cyclohexanol include phenol hydrogenation and cyclohexane oxidation, but these methods have problems such as complex raw material preparation process, poor operation safety, low conversion rate, high raw material cost, and larg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/04C07C29/80C07C35/08
CPCC07C29/04C07C29/80C07C2601/14C07C35/08Y02P20/10Y02P20/584
Inventor 姜海超刘小熙王建臣胡永琪赵风云
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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