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A kind of purification method of chlorophenyl glycerol

A technology of chlorphenesin and a refining method, which is applied in the field of antifungal and antibacterial agents, can solve the problems of large amount of purification solvent, flammable solvent, explosive and poisonous, etc., and achieve simplified purification treatment process, easy waste liquid, and reduced treatment cost effect

Active Publication Date: 2022-07-01
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the deficiencies of the above-mentioned prior art, the object of the present invention is to provide a method for refining chlorphenesin, which solves the problem that in the production process of chlorphenesin products, the amount of product purification solvent is large, the time is long, and the solvent is flammable and explosive. Toxic and many other problems, in line with the principles of safety and environmental protection, to reduce production costs and improve product environmental protection and economic benefits

Method used

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  • A kind of purification method of chlorophenyl glycerol

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Effect test

Embodiment 1

[0027] 150g of the crude product of chlorophenyl glycerol obtained by the experimental synthesis, with a product content of 90%, was added to a 500ml three-necked flask, heated by an electric heating mantle, nitrogen protection, decompressed by 0.095mpa, collected 216-218 ℃ fraction 125g, and then added the fraction to 380g, In 0.3% hot lye, the temperature is 75°C, the ratio of stirring to liquid level height is 0.6, the speed is 168r / min, the temperature is 25°C, air cooling, the cooling time is 3.5h, and the product is completely precipitated when it is lowered to room temperature, and vacuumed at 0.09mpa Filtration, using 100g of deionized water, and rinsing in three times to obtain a product filter cake. After drying, liquid phase analysis was used to determine the product content of 99.85%, and the phenol content was found to be no. The product yield is 90%, which meets the requirements of the invention process index.

Embodiment 2

[0029] 145g of the crude product of chlorophenyl glycerol obtained by the experimental synthesis, with a product content of 91%, was added to a 500ml three-necked flask, heated by an electric heating mantle, nitrogen protection, decompressed by 0.096mpa, collected 128g of 216-217 ℃ fraction, and then added the fraction to 400g, In 0.3% hot lye solution, the temperature is 75°C, the ratio of stirring to liquid level height is 0.62, the speed is 160r / min, the temperature is 25°C, air cooling, the cooling time is 3.5h, and the product is completely precipitated when it is lowered to room temperature, and vacuumed at 0.09mpa Filtration, using 100g of deionized water, and washing in three times to obtain a product filter cake. After drying, the product content was determined to be 99.88% by liquid phase analysis, and the phenol content was found to be no. The product yield is 91%, which meets the requirements of the invention process index.

Embodiment 3

[0031] 130g of the crude product of chlorophenyl glycerol obtained by the experimental synthesis, with a product content of 91%, was added to a 500ml three-necked flask, heated by an electric heating mantle, nitrogen protection, decompressed by 0.095mpa, collected 118g of 216-218 ℃ fraction, and then added the fraction to 420g, In 0.25% hot lye, the temperature is 75°C, the ratio of stirring to liquid level height is 0.6, the speed is 156r / min, the temperature is 25°C, air cooling, the cooling time is 3.5h, and the product is completely precipitated when it is lowered to room temperature, and the vacuum is 0.09mpa. Filtration, using 96g of deionized water, and washing in three times to obtain a product filter cake. After drying, liquid phase analysis was used to determine the product content of 99.79%, and no phenol content was detected. The product yield is 90.5%, which meets the requirements of the invention process index.

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Abstract

A method for purifying chlorophenyl glycerol, comprising the following steps: after the reaction is completed, a crude product of chlorophenyl glycerol is obtained, under the protection of nitrogen, heating with an electric heating mantle, a distillation flask, and a Y-shaped distillation head with a glass packing ring under a vacuum degree of 0.095 Mpa or more , collect 216-218 ℃ fraction products, reuse the front fraction, and treat the residue harmlessly. The distillate product is dissolved in a certain amount of lye solution, crystallized by cooling, filtered, and the amount of the mother liquor is about 3-4 times that of the product, and the filter cake is heated and dried in a vacuum step to obtain a product with a content of more than 99.8%. The content of p-chlorophenol is There is no test result, and the product yield is 70%. The process of the invention simplifies the refining process of the chlorophenyl glycerol product, shortens the time, improves the efficiency, reduces the amount of waste liquid, the waste liquid is easy to handle, reduces the processing cost, is green and safe, and has little environmental harm, and is created for its industrial application. condition.

Description

technical field [0001] The invention belongs to the technical field of anti-mildew and bacteriostatic agents, relates to the separation and treatment of products of the anti-mildew and anti-bacterial agent Chlorphenesin, which is applied to industries such as daily chemicals, detergents and coatings, and in particular relates to a method for purifying Chlorphenesin. Background technique [0002] Chlorphenesin is a kind of excellent performance, anti-mold and bacteriostatic agent, it has good inhibitory effect on various bacteria, especially anti-fungal, bacteria, vaginal mold, Trichomonas disease. Its current synthesis method has about nine process routes. The process raw materials mainly use p-chlorophenol and 3-chloro-1,2-propylene glycol or 3-chloro-propylene oxide. Its preparation is the classic Williamson ether-forming reaction between p-chlorophenol sodium salt and halohydrin, which is a bimolecular nucleophilic reaction of SN2 to generate the main product, as well as...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/42C07C41/40C07C43/23
CPCC07C41/42C07C41/40C07C43/23
Inventor 郑阿龙沈寒晰张金峰吴素芳刘彦婷习娟
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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