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Synthesis method of high-purity odorless chlorphenesin

A technology for chlorophenesiol and a synthesis method, which is applied in the directions of ether preparation, alkylene oxide preparation of ether, organic chemistry, etc., can solve the problems of incomplete reaction of raw materials in the synthesis process, complex reaction products, potential safety hazards, etc., and achieves no para-chlorine The effect of phenol residue, simple reaction process and high purity

Pending Publication Date: 2021-07-30
渭南畅通药化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the above-mentioned shortcoming of the prior art, solve the defects such as incomplete reaction of raw materials in the existing synthesis process, complex reaction products, potential safety hazards in the reaction raw materials or the reaction process, use of ether-petroleum ether or chloroform in the post-treatment process, etc., Provide a synthetic method that can obtain high-purity, no residual p-chlorophenol, odorless high-quality chlorphenesin

Method used

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  • Synthesis method of high-purity odorless chlorphenesin
  • Synthesis method of high-purity odorless chlorphenesin
  • Synthesis method of high-purity odorless chlorphenesin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A kind of high-purity odorless chlorphenesin synthetic method, concrete operation is as follows:

[0038] S1: Put 300kg of purified water, 7.8kg of sodium hydroxide and 250kg of p-chlorophenol into a 1000L reaction tank and stir for 10 minutes;

[0039] S2: Put 1kg of benzyltriethylammonium chloride into the reaction tank and heat to 50°C;

[0040] S3: Slowly drop 150kg of glycidol into the reaction tank at a constant temperature of 50°C;

[0041] S4: After the reaction is finished, let it stand for stratification, the upper layer is the brine layer, and the lower layer is the product layer;

[0042] Put the brine layer into a 200L crystallization bucket and let it stand for crystallization overnight. The clear liquid is concentrated under reduced pressure, and the distilled wastewater is discharged after three-dimensional electrolysis and biochemical treatment up to standard. The concentrated residue is disposed of as hazardous waste.

[0043] The production waste ga...

Embodiment 2

[0047] A kind of high-purity odorless chlorphenesin synthetic method, concrete operation is as follows:

[0048] S1: Put 300kg of purified water, 8.2kg of sodium hydroxide and 250kg of p-chlorophenol into a 1000L reaction tank and stir for 10 minutes;

[0049] S2: Put 2kg of tetrabutylammonium bromide into the reaction tank and heat to 70°C;

[0050] S3: Slowly drop 150kg of glycidol into the reaction tank at a constant temperature of 70°C;

[0051] S4: After the reaction is finished, let it stand for stratification, the upper layer is the brine layer, and the lower layer is the product layer;

[0052] Put the brine layer into a 200L crystallization bucket and let it stand for crystallization overnight. The clear liquid is concentrated under reduced pressure, and the distilled wastewater is discharged after three-dimensional electrolysis and biochemical treatment up to standard. The concentrated residue is disposed of as hazardous waste.

[0053] The production waste gas (incl...

Embodiment 3

[0057] A kind of high-purity odorless chlorphenesin synthetic method, concrete operation is as follows:

[0058] S1: Put 300kg of purified water, 8.5kg of potassium carbonate and 250kg of p-chlorophenol into a 1000L reaction tank and stir for 10 minutes;

[0059] S2: Put 5kg of chain polyethylene glycol into the reaction tank and heat to 70°C;

[0060] S3: Slowly drop 150kg of glycidol into the reaction tank at a constant temperature of 70°C;

[0061] S4: After the reaction is finished, let it stand for stratification, the upper layer is the brine layer, and the lower layer is the product layer;

[0062] Put the brine layer into a 200L crystallization bucket and let it stand for crystallization overnight. The clear liquid is concentrated under reduced pressure, and the distilled wastewater is discharged after three-dimensional electrolysis and biochemical treatment up to standard. The concentrated residue is disposed of as hazardous waste.

[0063] The production waste gas (...

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Abstract

The invention relates to a synthesis method of high-purity odorless chlorphenesin. The method comprises the steps of S1, adding water, an inorganic base catalyst and parachlorophenol into a reaction tank, and stirring; S2, adding a phase transfer catalyst into the reaction tank, and heating; S3, dropwise adding glycidol into the reaction tank at a constant temperature, and carrying out condensation reaction on the glycidol and parachlorophenol under the catalytic action of an inorganic base catalyst to generate chlorphenesin; and S4, after the reaction is completed, obtaining chlorphenesin through a post-treatment method. According to the synthesis method of the high-purity odorless chlorphenesin, the reaction process is simple, and the obtained chlorphenesin is high in purity, free of parachlorophenol residues and odorless; and no industrial waste salt is generated in the production process, a small amount of generated low-concentration waste brine is subjected to three-dimensional electrolysis to realize open-loop degradation of organic matters in the wastewater, and the wastewater is discharged after being treated by anaerobic treatment, oxygen consumption treatment and other biochemical treatment measures and reaching the standard, so that the water body is not polluted.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and more specifically, the invention relates to a method for synthesizing high-purity odorless chlorphenesin. Background technique [0002] British Patent (GB628497) reported a method for the synthesis of chlorphenesin by reacting p-chlorophenol and glycidol in the presence of pyridine. The reaction process of this method exothermic violently, there is certain potential safety hazard, and the reaction of raw material p-chlorophenol is not complete, ether-petroleum ether or chloroform are used as recrystallization solvent in the post-treatment process, and the residual p-chlorophenol and pyridine have a strong smell , has high requirements on production equipment and environment, it is difficult to recover solvents, and it is difficult to treat waste water and waste gas. [0003] Chinese patent (CN101445436A) provides a method for synthesizing chlorphenesin by reaction with sodium p-chl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/02C07C43/23
CPCC07C41/02C07C43/23
Inventor 古凤强畅水平畅通马宝莉石敏畅快乐传雅萍刘静
Owner 渭南畅通药化科技有限公司
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