Decoloring method of chlorobenzene glyceryl ether

A technology of chlorphenesin and products, which is applied in the field of decolorization of chlorphenesin products, can solve the problems of prolonged decolorization time, high production cost, unsatisfactory decolorization effect, etc., and achieves simple and reasonable process route, short decolorization treatment time, The effect of white appearance of the product

Active Publication Date: 2021-05-11
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The single solvents used, such as methanol, ethanol, chloroform, etc., these organic solvents have low boiling points, high volatility, poisonous, harmful, flammable, explosive, and there are problems such as large safety hazards and dangerous operation, and the single dissolution results in poor decolorization effect Ideal, even if the physical adsorption of adsorbents (such as resin, activated carbon, diatomaceous earth, etc.) is added, it is still difficult to effectively remove the colored substances in the product, and the product quality is low
In order to improve product quality, the method of increasing the amount of solvent and multiple treatments has to be used to achieve effective decolorization of the product, but this not only prolongs the decolorization time, but also greatly increases the product cost.
[0005] The above reflects that there are many problems in the decolorization process of chlorphenesin products, such as the use of toxic and harmful solvents, large safety hazards, environmental hazards, low process efficiency, high production costs, and poor quality improvement. These problems have seriously restricted the relevant enterprises. sustainable and healthy development of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take 100g of the chlorphenesin product recrystallized from a water-alcohol mixed solvent, 150g of pure water, and 1.0g of potassium hydroxide, and add them to a 500ml three-necked flask in turn, stir the materials in the flask at a speed of 110r / min, and heat the materials to make them warm up to 58°C, then add 5g of sodium hypochlorite, react for 1h, then add 0.5g of activated carbon, react for 0.5h, use a funnel with a precision of 10um to vacuum filter while hot to obtain the filtrate, keep it at 58°C for 0.5h, and use pure Melt in water at 80°C for 0.5h, then stir water and cool to 25°C to crystallize, filter under reduced pressure at a vacuum of 0.09MPa or above, and dry the filtered crystals under reduced pressure at a temperature of 90°C to moisture The detection is less than 0.3%, and a qualified product is obtained. The appearance of the product is white powder, the content is 99.7%, and the molten state is close to a colorless transparent liquid.

Embodiment 2

[0018] Take 150g of the chlorphenesin product recrystallized from a water-alcohol mixed solvent, 280g of pure water and 2.0g of sodium hydroxide, and add them to a 500ml three-neck flask in turn, stir the materials in the flask at a speed of 120r / min, and heat the materials to make them warm up to 69°C, then add 5g of calcium hypochlorite, react for 1h, then add 0.8g of activated carbon, react for 0.5h, use a funnel with an accuracy of 8um to vacuum filter while hot to obtain the filtrate, keep it at 69°C for 0.5h, and the product The phase is melted and translucent with water alcohol at 50°C for 0.5h, then stirred with water and cooled to 20°C to crystallize, and then filtered under reduced pressure at a vacuum of 0.09MPa or above, and decompressed the filtered crystals under the condition of a vacuum of 0.09MPa or above and a temperature of 98°C Dried until the water content is less than 0.3%, to obtain a qualified product. The appearance of the product is white powder, the ...

Embodiment 3

[0020] Take 200g of chlorphenesin product, 400g of pure water and 1.0g of sodium carbonate recrystallized in a water-alcohol mixed solvent, and add them to a 1000ml three-necked flask in turn, stir the contents of the flask at a speed of 130r / min, and heat the contents to a temperature of 69 ℃, then add 8g of calcium hypochlorite, react for 2h, then add 1.5g of diatomaceous earth, react for 1h, use a funnel with a precision of 8um to vacuum filter while it is hot, and obtain the filtrate, keep it at 69°C for 0.6h to separate the liquid, the product The phase is melted and translucent with water alcohol at 50°C for 0.5h, then stirred with water and cooled to 20°C to crystallize, and then filtered under reduced pressure at a vacuum of 0.09MPa or above, and decompressed the filtered crystals under the condition of a vacuum of 0.09MPa or above and a temperature of 120°C Dried until the water content is less than 0.3%, to obtain a qualified product. The appearance of the product is...

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PUM

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Abstract

The invention discloses a decoloring method of chlorobenzene glyceryl ether. The method comprises the following process steps of: adding a chlorobenzene glyceryl ether product recrystallized by a water-alcohol mixed solvent into a heating reaction kettle, and adding pure water and alkali into the reaction kettle; stirring the materials in the reaction kettle and heating the materials to 50-80 DEG C; after the materials are uniformly dissolved, adding an oxidizing agent into the dissolved solution, and carrying out heat preservation reaction for 1-3 hours; adding an adsorbent into the reaction liquid and reacting for 0.5-1 hour; filtering while hot to obtain filtrate, standing and separating to obtain a product phase; and obtaining the product by recrystallizing, filtering and drying the product phase. The product is white powder in appearance and almost colorless in a molten state, the purity of the product reaches 99.5% or above, the product quality is obviously improved, the process concept of high efficiency, safety and quality and efficiency improvement is achieved, and conditions are created for industrial application of the product.

Description

technical field [0001] The invention belongs to the technical field of preparation of daily-use chemical products, and relates to a processing method for an anti-mold and antibacterial agent chlorphenesin, and in particular to a decolorization method for a chlorphenesin product. Background technique [0002] Chlorphenesin (chlorphenesin), also known as chlorophenol ether, chlorphenesin, is a kind of antifungal inhibitor with excellent performance. In medicine, chlorphenesin as an antifungal drug is suitable for antifungal, bacteria, vaginal mold, trichomonas and other diseases; in cosmetics, chlorphenesin can effectively resist Gram-positive and negative bacteria In recent years, this product has been widely used in products such as nail polish, skin care agents and hair dyes in the world. [0003] The appearance of the standard chlorphenesin product should be white, but in the preparation process of chlorphenesin, due to the Williamson ether formation reaction mechanism, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/44C07C41/36C07C41/40C07C43/23
CPCC07C41/44C07C41/36C07C41/40C07C43/23
Inventor 郑阿龙沈寒晰张金峰郭鹏涛习娟刘彦婷徐亚霞
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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