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Reactive distillation method for preparing cyclohexanol through hydration of cyclohexene and device of method

A cyclohexene hydration and reactive distillation technology, which is applied in the field of cyclohexene hydration to prepare cyclohexanol reactive distillation and its device, can solve the problems of resin catalyst strength pulverization, insufficient reaction speed, adhesion, etc. Achieve the effects of reducing steam flow velocity, increasing single-pass conversion rate, and reducing reaction energy consumption

Inactive Publication Date: 2019-04-19
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1980, DuPont used perfluorosulfonic acid resin as the catalyst for cyclohexene hydration reaction. In 2008, Zhejiang University adopted macroporous strong acid A36wet ion exchange resin as the catalyst for cyclohexene hydration reaction. In 2017, Fuzhou University adopted strong acid cation exchange resin A36wet As a cyclohexene hydration reaction catalyst, but the activity of the acidic resin catalyst is low, and due to the insufficient strength of the resin catalyst, it will cause pulverization, and it is easy to cause loss during operation, which cannot guarantee long-term stable operation.
At present, the ZSM-5 catalyst used in industry has good activity, but there is still a problem that the reaction speed is not fast enough; on the other hand, its shape is fine powder, which cannot be fixed on the tray, and the catalyst in the slurry state will be absorbed by the steam. Entrained and adhered to the bottom of the tray, resulting in blockage and failure of normal operation

Method used

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  • Reactive distillation method for preparing cyclohexanol through hydration of cyclohexene and device of method
  • Reactive distillation method for preparing cyclohexanol through hydration of cyclohexene and device of method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] The diameter of the reactive distillation column is 450mm, the column height is 14500mm, and the total number of trays is 29. Process conditions in the reactive distillation tower: cyclohexene flow rate is 80kmol / h, 18-crown-6 flow rate is 80kmol / h, water flow rate is 320kmol / h, ZSM-5 molecular sieve catalyst mass concentration is 35%, reaction temperature The temperature is 130°C, and the reaction pressure is 0.55MPa. The particle size of the ZSM-5 molecular sieve catalyst is 2.5 μm, and the acidity of the filtrate is 0.22 mmol / g. The air inlet on the non-porous tray assembly is 14mm; the diameter of the U-shaped vapor rising pipe in the non-porous tray assembly is 24mm, and the height is 320mm; the annular gas distribution in the non-porous tray assembly is The diameter of the device is 100 mm, and the opening rate is 15%.

[0059] Water, ZSM-5 molecular sieve catalyst and 18-crown ether-6 are fed into the reactive distillation column from the feed port (a) at the s...

Embodiment 2

[0062] The diameter of the reactive distillation column is 450mm, the column height is 14500mm, and the total number of trays is 29. Process conditions in the reactive distillation tower: cyclohexene flow rate is 70kmol / h, 15-crown-5 flow rate is 49kmol / h, water flow rate is 140kmol / h, ZSM-5 molecular sieve catalyst mass concentration is 15%, reaction temperature is 120°C, and the reaction pressure is 0.35MPa. The particle size of the ZSM-5 molecular sieve catalyst is 1 μm, and the acidity of the filtrate is 0.25 mmol / g. The size of the air inlet on the non-porous tray assembly in the non-porous tray assembly is 10mm; the diameter of the U-shaped vapor rising pipe in the non-porous tray assembly is 15mm, and the height is 200mm; the annular gas distribution in the non-porous tray assembly The diameter of the device is 80mm, and the opening rate is 8%.

[0063] Water, ZSM-5 molecular sieve catalyst and 15-crown ether-5 are fed into the reactive distillation column from the fe...

Embodiment 3

[0066] The diameter of the reactive distillation column is 450mm, the column height is 14500mm, and the total number of trays is 29. The process conditions in the reactive distillation tower: the flow rate of cyclohexene is 60kmol / h, the flow rate of pyridine is 102kmol / h, the flow rate of water is 180kmol / h, the mass concentration of ZSM-5 molecular sieve catalyst is 20%, the reaction temperature is 140°C, the reaction The pressure is 0.45MPa. The particle size of the ZSM-5 molecular sieve catalyst is 1.4 μm, and the acidity of the filtrate is 0.18 mmol / g. The air inlet on the non-porous tray assembly is 12mm; the diameter of the U-shaped vapor rising pipe in the non-porous tray assembly is 19mm, and the height is 240mm; the annular gas distribution in the non-porous tray assembly is The diameter of the device is 85mm, and the opening rate is 10%.

[0067] Water, ZSM-5 molecular sieve catalyst and pyridine are fed into the reactive distillation column from the feed port (a)...

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Abstract

The invention relates to a reactive distillation method for preparing cyclohexanol through hydration of cyclohexene and a device of the method. According to the reactive distillation method and the device thereof, a ZSM-5 molecular sieve is adopted as a reaction catalyst, cyclic crown ether or tertiary amine is adopted as a phase transfer catalyst, and a tower plate of a reactive distillation tower is a non-porous tower plate combination body composed of non-porous tower plates, U-shaped vapor rise pipes and annular gas distributors in form. By means of the reactive distillation method and thedevice thereof, the sieve plate hole channel blockage problem caused when vapor at the high gas velocity drives the catalyst to impact the bottom of a sieve plate can be solved, the single-pass conversion rate of cyclohexene is increased, and the reaction energy consumption is reduced.

Description

technical field [0001] The invention relates to a reactive distillation method and a device for preparing cyclohexanol by hydrating 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. At present, cyclohexanol is usually prepared by the direct hydration reaction of cyclohexene, which has obvious advantages in system safety and product selectivity, and also has the advantages of low raw material cost, saving hydrogen source, and high utilization of carbon atoms, making it It has become the most widely used production me...

Claims

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Application Information

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IPC IPC(8): C07C29/04C07C29/80C07C35/08B01J31/26B01D3/14B01D3/16B01D3/32B01D3/00
CPCB01D3/009B01D3/14B01D3/166B01D3/322B01J8/0453C07C29/04C07C29/80B01J31/26C07C2601/14B01J35/19C07C35/08Y02P20/10
Inventor 刘小熙胡永琪姜海超曹超文刘彩红宁原锋贾云婷赵风云王建英
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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