Cyclic oxidation method and cyclic oxidation device for preparing epsilon-caprolactone

A technology of cyclic oxidation and caprolactone, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve problems such as high energy consumption and risk factor, increase system energy consumption, and difficult water removal, etc., to achieve Reduce energy consumption and danger, reduce difficulty, avoid the effect of peroxyacid and water residue

Inactive Publication Date: 2020-03-13
河南能源化工集团研究总院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst sulfuric acid residue in this process is unfavorable to the subsequent reaction, and a large amount of water in the system must be removed, so the peroxyacid aqueous solution is required to remove water by rectification, and there is a large potential safety hazard
In another process using weak acid catalysis to prepare peroxyacid, the removal of water still needs to be c

Method used

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  • Cyclic oxidation method and cyclic oxidation device for preparing epsilon-caprolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A cyclic oxidation method for preparing ε-caprolactone, comprising the steps of:

[0032] (1) First place the solid acid in a continuous reactor; the hydrogen peroxide reaction solution flows through the solid acid to generate a solid peroxyacid; the solid acid is a weak acid ion exchange resin or an inorganic heteropolyacid;

[0033] (2) Secondly, pass the cleaning liquid through the solid peroxyacid to take away the residual moisture on the surface of the solid peroxyacid;

[0034] (3) Flow the cyclohexanone solution through the solid peroxyacid, react to generate caprolactone, and directly rectify to obtain the caprolactone product; the concentration of the cyclohexanone solution is 30%-100%, and the solvent is a cleaning solution

[0035] (4) The second cleaning solution flows through the continuous reactor to clean the residual cyclohexanone and caprolactone and repeat steps (1)-(4).

[0036] Wherein, the flow rate of the hydrogen peroxide reaction solution in ste...

Embodiment 2

[0045] Reactor preheating

[0046] Reactor R1 was preheated to reaction temperature 60°C using jacketed steam.

[0047] Peroxidation

[0048] Open the valves 1a and 1b, and adjust the opening of the valve to control the flow rate to 2g·h -1 •g -1 固体酸 , the material flows out of R1 and enters into V1, and the peroxidation process is completed after 12 hours. Then, while closing 1a and 1b, open 2a and 2b, and control the flow rate to 2g·h -1 • g -1 固体酸, the material flows out of R1 and then flows into V2, and the removal of residual hydrogen peroxide and water is completed after 2 hours.

[0049] reaction

[0050] While closing 2a and 2b, open 3a and 3b, and adjust the opening of the valve to control the flow rate to 2 g·h -1 •g -1 固体酸 , the material flows out of R1 and then flows into V3, and the ε-caprolactone synthesis reaction is completed after 12 hours. The material concentration obtained at this time is: ε-caprolactone 50%, cyclohexanone 50%, water less than 5...

Embodiment 3

[0054] Reactor preheating

[0055] Reactor R1 was preheated to a reaction temperature of 90 °C using jacketed steam.

[0056] Peroxidation

[0057] Open the valves 1a and 1b, and adjust the opening of the valve to control the flow rate to 10g·h -1 •g -1 固体酸 , the material flows out of R1 and enters into V1, and the peroxidation process is completed after 5 hours. Then, while closing 1a and 1b, open 2a and 2b, and control the flow rate to 10g·h -1 •g -1 固体酸 For solid acid, the material flows out of R1 and then flows into V2, and the residual hydrogen peroxide and moisture removal are completed after 1 hour.

[0058] reaction

[0059] While closing 2a and 2b, open 3a and 3b, and adjust the opening of the valve to control the flow rate to 10 g·h -1 •g -1 固体酸 , the material flows out of R1 and then flows into V3, and the ε-caprolactone synthesis reaction is completed after 5 hours. The material concentration obtained at this time is: ε-caprolactone 30%, cyclohexanone 7...

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Abstract

The invention provides a cyclic oxidation method and a cyclic oxidation device for preparing epsilon-caprolactone. A reactor adopts a fixed bed with a jacket or adopts a tubular reactor, and is filledwith a solid acid. A hydrogen peroxide reaction liquid, a cleaning liquid and a cyclohexanone solution sequentially flows through the reactor in sequence to complete a synthesis reaction of epsilon-caprolactone, the cleaning liquid flows through the reactor finally to complete regeneration, and a next cycle is started. A novel solid peroxy acid oxidation technology used in the invention makes residual water and a sulfuric acid catalyst simply washed off by using an anhydrous solvent, and the used solid organic peroxy acid can be recycled after being washed with a simple solvent washing, so peroxy acid and water residues are avoided, the energy consumption and danger are reduced, and the product quality can be guaranteed.

Description

technical field [0001] The invention relates to the technical field of ε-caprolactone production, in particular to a cyclic oxidation method and equipment for preparing ε-caprolactone. Background technique [0002] The most well-established ε-caprolactone is usually prepared by the Bayer-Williger reaction of cyclohexanone with peroxyacids. The method for preparing peroxyacids at low cost in industry is to react aqueous hydrogen peroxide solution with organic acids under the catalysis of sulfuric acid to prepare corresponding peroxyacids. However, the catalyst sulfuric acid residue in this process is unfavorable to the subsequent reaction, and a large amount of water in the system must be removed. Therefore, rectification of the peroxyacid aqueous solution is required to remove water, and there is a large safety hazard. In another process using weak acid catalysis to prepare peroxyacid, the removal of water still needs to be carried out with water-carrying agent and vacuum d...

Claims

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Application Information

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IPC IPC(8): C07D313/04B01J8/02B01J8/06
CPCB01J8/0285B01J8/06B01J2208/00212C07D313/04
Inventor 闫捷赵立红蒋元力魏灵朝崔发科李丰宋灿梁旭
Owner 河南能源化工集团研究总院有限公司
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