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Preparation method of chloroxylenol

A technology for p-chloro-m-xylenol and xylenol, which is applied in the field of preparation of p-chloro-m-xylenol, can solve problems such as difficulty in realizing large-scale production, occurrence of side reactions, large environmental pollution, etc., and achieves less reaction pollution, Less side effects and better safety

Active Publication Date: 2013-07-24
常熟紫金知识产权服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When chlorine is used as the chlorinating agent, carbon tetrachloride is used as the solvent, expensive catalysts are used, side reactions occur, the cost is high, and the environmental pollution is relatively large
When sulfuryl dichloride is used as the chlorinating agent, expensive catalysts and chlorinating agents are used, the production cost is high, it is difficult to realize large-scale production, and side reactions occur in the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] Example 1: Add m-xylenol 12g, chlorosuccinimide 13.08g, carbon tetrachloride 100g and catalyst aluminum trichloride 0.24g in the reaction kettle, and react at a temperature of 70-80°C for 60min; the reaction is completed, Cool the solution, filter, wash, evaporate most of the solvent carbon tetrachloride, place it to crystallize, filter and wash to obtain the crude product of p-chloro-m-xylenol; then recrystallize with chloroform, decolorize with activated carbon, and dry to obtain p-chloro-m-xylenol 9.8 g of white crystals of cresol, yield 64%.

Embodiment 2

[0008] Example 2: Add m-xylenol 12g, chlorosuccinimide 14.4g, carbon tetrachloride 120g and catalyst ferric trichloride 0.36g in the reaction kettle, and react at a temperature of 70-80°C for 70min; the reaction is completed, Cool the solution, filter, wash, evaporate most of the solvent carbon tetrachloride, and place it to crystallize to obtain the crude product of p-chloro-m-xylenol; then recrystallize with chloroform, decolorize with activated carbon, and dry to obtain the white color of p-chloro-m-xylenol. Crystal 10.5g, yield 69%.

Embodiment 3

[0009] Embodiment 3: add m-xylenol 12g, chlorosuccinimide 15.3g, carbon tetrachloride 140g and catalyst zinc chloride 0.48g in the reaction kettle, the temperature is 70-80 ℃ of reaction 80min; The solution is cooled, filtered, washed, and most of the solvent carbon tetrachloride is evaporated, and placed to crystallize to obtain the crude product of p-chloro-m-xylenol; then recrystallized with chloroform, decolorized with activated carbon, and dried to obtain white crystals of p-chloro-m-xylenol 11.9g, yield 78%.

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PUM

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Abstract

The invention discloses a preparation method of chloroxylenol, which comprises the following steps of: putting 3, 5-xylenol, a chlorinated succinimide chlorating agent, a carbon tetrachloride solvent and a catalyst into a reaction kettle in a certain proportion, and carrying out reaction for a period of time at a certain temperature; after the reaction is completed, carrying out cooling, crystallization, suction filtering and washing on a solution, extracting most of the carbon tetrachloride solvent through evaporation, and carrying out cooling, crystallization, suction filtering and washing on the obtained object so as to obtain a coarse chloroxylenol product; and carrying out recrystallization on the coarse chloroxylenol product by using chloroform, carrying out activated carbon decoloration on the product, and drying the obtained product so as to obtain white chloroxylenol crystals. The preparation method disclosed by the invention is mild in reaction conditions; the direct utilization of chlorine is avoided, therefore, the method is good in safety, less in side effects, and easy to realize purification; only a small amount of catalyst is required, therefore, the production cost is low; and the method is simple in post-processing, less in pollution, high in yield, energy-saving, and environment-friendly.

Description

Technical field [0001] The invention relates to a preparation method of p-chlorom-xylenol. Background technique [0002] Para-chlorometa-xylenol is an internationally accepted disinfectant. It is a safe, efficient and broad-spectrum antifungal and antibacterial agent. It can kill more than 160 kinds of bacteria, viruses, molds and fungi. It is non-irritating and has no drug resistance. It is the preferred bactericidal drug recognized by the U.S. Food and Drug Administration and has been used by major international companies including Dettol. Because of its low side effects, low irritation, and ability to come into direct contact with the skin, it is widely used in personal care products such as disinfectants, clothing sterilizers, and women's lotions. It can also be used as a preservative and antifungal agent in glue, coatings, paints, textiles, leather, paper and other industrial fields. Since p-chlorometaxylenol has excellent bactericidal and antiseptic functions, its de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/62C07C39/28
CPCY02P20/52
Inventor 支三军韦长梅安礼涛唐果东
Owner 常熟紫金知识产权服务有限公司
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