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Preparation method of 3,5-dimethyl-4-chlorophenol

A technology of dimethylphenol and chlorophenol, which is applied in the field of preparation of 3,5-dimethyl-4-chlorophenol, can solve the problems of low PCMX content, incomplete chlorination reaction, high production cost, and achieve high content , Reduce the generation of by-products, improve the yield and quality

Inactive Publication Date: 2015-02-04
RONGCHENG QINGMU CHEM MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The existing process has disadvantages such as low conversion rate, incomplete chlorination reaction, increased by-products, low PCMX content, a large amount of washing water that has not been recycled, high environmental pollution, and high production costs.

Method used

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  • Preparation method of 3,5-dimethyl-4-chlorophenol
  • Preparation method of 3,5-dimethyl-4-chlorophenol
  • Preparation method of 3,5-dimethyl-4-chlorophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] As shown in the route map, add 1000 kg of tetrachlorethylene and 500 kg (4 kmol) of substrate MX into the chlorination kettle, start stirring, control the temperature between 30 and 45 °C, dissolve the substrate MX, and add benzylthiophenol 0.5 kg, 2 kg of aluminum trichloride, and slowly add 540 kg (4 kmol) of sulfuryl chloride dropwise at this temperature. Add 54 kg (0.4 kmol) of sulfuryl chloride, dropwise for 1~1.5 h. After the dropwise addition is completed, remove tail gas at -0.02~-0.04 MPa and 50~65 °C for 1~2 h, and react according to [ 0029] road map carries out aftertreatment, obtains product 550 kg, yield 85.80% (based on the molar yield of MX), content 99.01%.

Embodiment 2

[0038] As shown in the route map, add 1000 kg of tetrachlorethylene to the chlorination kettle, start stirring with 500 kg (4 kmol) of substrate MX, and control the temperature between 30 and 45 °C to dissolve the substrate, add 0.5 kg of benzylthiophenol, three Aluminum chloride 2 kg, slowly add 560 kg (4.15 kmol) sulfuryl chloride dropwise at this temperature, the dropwise addition time is 4.5~5 h, after the dropwise addition, raise the temperature to 50~65 °C, and then add dropwise 70 kg (0.52 kmol) Sulfuryl chloride, the dropwise addition time is 1~1.5 h. After the dropwise addition is completed, at -0.02~-0.04 MPa, 50~65 ℃, after heat preservation to remove the tail gas for 1~2 h, the reactants are carried out according to the route diagram of [0029]. Processed product 560 kg, yield 87.3% (molar yield based on MX), content 98.81%.

Embodiment 3

[0040] As shown in the route map, add 1000 kg of tetrachlorethylene to the chlorination kettle, start stirring with 500 kg (4 kmol) of substrate MX, and control the temperature between 30 and 45 °C to dissolve the substrate, add 0.5 kg of benzylthiophenol, three Aluminum chloride 2.5 kg, slowly add 560 kg (4.15 kmol) sulfuryl chloride dropwise at this temperature, the dropwise addition time is 4.5~5 h, after the dropwise addition is completed, the temperature is raised to 50~65°C, and then 70 kg (0.52 kmol) is added dropwise Sulfuryl chloride, the dropwise addition time is 1~1.5 h. After the dropwise addition is completed, at -0.02~-0.04 MPa, 50~65 °C, keep removing the tail gas for 1~2 h, and the reactants are carried out according to the route diagram of [0029]. Process to get product 530 kg, yield 82.6% (molar yield based on MX), content 98.58%.

[0041] The directional chlorination process product of each embodiment PCMX, GC analysis result is:

[0042] Example ...

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Abstract

The invention discloses a preparation method of 3,5-dimethyl-4-chlorophenol, which takes tetrachloroethylene as a solvent, benzyl thiophenol and aluminium chloride as cocatalysts, sulfuric chloride as a chloridizing agent, orientation chlorination is carried out through two phases of low-temperature chlorination and high-temperature chlorination, the mass ratio of tetrachloroethylene to MX is 0.5-4: 1; the mass ratio of the cocatalyst to MX is 2.5-6.5:1000; at low temperature chlorination phase, the mass ratio of sulfuric chloride dropping amount to MX is 0.9-1.2: 1; at high temperature chlorination phase, the mass ratio of sulfuric chloride dropping amount to MX is 0.1-0.2: 1; the temperature at the low temperature chlorination phase is controlled at 30-45 DEG C, chlorination is carried out for 4-6 hours; the temperature at high temperature chlorination phase is controlled at 50-65 DEG C, and chlorination is carried out for 1-2 hours, insulation reaction is carried out after the dropping process of sulfuric chloride is completed, tail gas is removed for 1-2 hours, and steps of water-washing layering, cooling and crystallizing, centrifuging and washing, and drying to obtain the product. According to the method, the conversion rate can reach more than 95%, finished product PCMX yield is increased, and the by-product can be effectively reduced.

Description

technical field [0001] The invention belongs to fine chemical chlorination process, and in particular relates to a preparation method of 3,5-dimethyl-4-chlorophenol. Background technique [0002] 3,5-Dimethyl-4-chlorophenol, abbreviated as PCMX, is a safe, efficient, and broad-spectrum fungicide. It is certified by the U.S. Food and Drug Administration (FDA) as the first-choice bactericidal drug, which can kill a variety of bacteria , mold, fungus and germs, widely used in industrial and cosmetic industries. Due to its excellent bactericidal and antiseptic functions, PCMX has a promising development prospect and has been recognized by consumers. [0003] The constructor of PCMX is as follows: [0004] [0005] The second issue of the volume 35 of the journal "Applied Chemical Industry" introduced that Wei Wenlong of Taiyuan University of Technology and others studied the use of m-xylenol and chlorine as raw materials and carbon tetrachloride as a solvent in "New Process...

Claims

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Application Information

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IPC IPC(8): C07C39/28C07C37/62
CPCY02P20/52C07C37/62C07C39/28
Inventor 刘玉美任相忠王晓玲程玉强林海飞孙燕超李晓明
Owner RONGCHENG QINGMU CHEM MATERIALS
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