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Preparation method of parachlorometaxylenol

A technology of p-chloro-meta-xylenol and dimethylphenol, applied in the field of basic chemical industry, can solve the problems of unclear industrialization prospect, long reaction time, large energy consumption and the like

Inactive Publication Date: 2013-10-16
JIANGSU HUANXIN NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it takes 3-4 multi-stage temperature control steps to obtain p-chloro-m-xylenol, and the reaction time is long, the energy consumption is huge, the process operation rules are cumbersome, and the industrialization prospect is unclear.

Method used

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  • Preparation method of parachlorometaxylenol

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preparation example Construction

[0028] The present invention proposes a kind of preparation method of p-chloro-m-xylenol, which comprises the following steps or operations.

[0029] Step 1, compounding water, inorganic acid and organic solvent into M system. The M system here is an abbreviation for the compound solution made of water, inorganic acid and organic solvent. The following solutions A, B, etc. are also referred to as abbreviations.

[0030] In one embodiment, this step can be specifically performed as follows: water, inorganic acid and organic solvent are compounded into an M system, wherein the inorganic acid is selected from hydrochloric acid with a mass concentration of 10-35% or 10-40% Any one of the sulfuric acid, the product yield of the sulfuric acid system is slightly better than that of the hydrochloric acid system; the organic solvent is selected from any one of tetrachlorethylene or ethylene dichloride; the inorganic acid and the 3,5- The weight ratio of dimethylphenol is 0.25:1~10:1,...

Embodiment 1

[0047] Add 300g of 10% hydrochloric acid and 30g of tetrachlorethylene into a 500ml three-necked flask to prepare the M system, add 122g of 3,5-dimethylphenol into the M system, then start the stirring or mixing device, and keep warm at 15- Between 25°C, slowly add 135g of sulfuryl chloride dropwise at this temperature, the dropping time is 4 hours, after the dropwise addition is completed, the temperature is raised to 85°C, and then cooled to 25°C, standing for stratification, and the lower organic phase is separated, the result For: 3,5-dimethylphenol: 1.78%, 4-chloro-3,5-dimethylphenol: 86.43%, 2-chloro-3,5-dimethylphenol: 9.84% and 2,4- Dichloro-3,5-dimethylphenol: 1.56%.

[0048] The material was suction filtered and washed with water, and dried to obtain 123g of white crystalline solid. The results of gas chromatography analysis were: 3,5-dimethylphenol: 0.51%, 4-chloro-3,5-dimethylphenol: 99.01%, 2 -Chloro-3,5-dimethylphenol: 0.23% and 2,4-dichloro-3,5-dimethylphenol: ...

Embodiment 2

[0050] Add 300g of 20% hydrochloric acid and 30g of dichloroethane into a 500ml three-necked flask to prepare the M system, add 122g of 3,5-dimethylphenol into the M system, then start the stirring or mixing device, and keep warm at 15- Between 25°C, slowly add 135g of sulfuryl chloride dropwise at this temperature, and the dropping time is 5 hours. After the dropwise addition is completed, the temperature is raised to 85°C, and then cooled to 25°C. For: 3,5-dimethylphenol: 0.88%, 4-chloro-3,5-dimethylphenol: 89.21%, 2-chloro-3,5-dimethylphenol: 8.45% and 2,4 -Dichloro-3,5-dimethylphenol: 1.23%.

[0051] The material was filtered and washed with water, and dried to obtain 123.3 g of white crystalline solids. The results of gas chromatography analysis were: 3,5-dimethylphenol: 0.52%, 4-chloro-3,5-dimethylphenol: 99.22%, 2-Chloro-3,5-dimethylphenol: 0.11% and 2,4-dichloro-3,5-dimethylphenol: 0.12%.

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Abstract

The invention discloses a preparation method of parachlorometaxylenol. The method includes: adding a proper amount of tetrachloroethylene or dichloroethane into acidic water to prepare a composite solvent, i.e. an M system, letting a chlorinating agent sulfuryl chloride and a substrate 3, 5-dimethylphenol undergo a chlorination reaction in the M system so as to produce the target product parachlorometaxylenol. The method not only can avoid use of catalysts that are expensive and are difficult to recover, but also can reduce the use of organic solvents, and reduce energy consumption during production. At the same time, the method can improve the conversion per pass of the product and the first-time qualification rate. Moreover, the process also can significantly reduce the exhaust gas and waste in the production process, such as volatilization of organic solvents, discharge of inactivated metal catalysts, and can improve the production environment, thus being conducive to environmental protection.

Description

technical field [0001] The invention belongs to the field of basic chemical industry, in particular to a preparation method of p-chloro-m-xylenol. Background technique [0002] p-Chloro-m-xylenol (also known as: 4-chloro-3,5-dimethylphenol, CAS number: 88-04-0, English abbreviation PCMX) is an important microbial killer, as an antibacterial agent, Antifungal agent, disinfectant, widely used in industry and cosmetic industry, it has excellent inhibitory effect on bacteria, mold and most fungi. [0003] In recent years, with the ravages of epidemic diseases, people's health awareness has become stronger and stronger. As a traditional low-toxicity disinfectant p-chloro-m-xylenol will also have greater development potential, and its structural formula is as follows: [0004] [0005] p-Chloro-m-xylenol is prepared by the electrophilic substitution reaction of sulfuryl chloride and 3,5-dimethylphenol. Since 1866, Dubois reacted with equimolar sulfuryl chloride and molten phe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/28C07C37/62
Inventor 倪廷王润谦袁照晨戚晶晶朱汉文陈健明
Owner JIANGSU HUANXIN NEW MATERIAL CO LTD
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