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Method for producing high-purity 2,4-dichlorophenol

A dichlorophenol, high-purity technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of high production cost and difficult process operation, and achieve the effect of high raw material conversion rate

Active Publication Date: 2019-06-07
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The present invention solves the technical problems of high production cost, difficult process operation, and need for rectification and purification in the method for producing high-purity 2,4-dichlorophenol in the prior art, and further provides a method that can reduce production cost, A method for producing high-purity 2,4-dichlorophenol with low operating difficulty and no need for rectification and purification

Method used

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  • Method for producing high-purity 2,4-dichlorophenol
  • Method for producing high-purity 2,4-dichlorophenol
  • Method for producing high-purity 2,4-dichlorophenol

Examples

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Embodiment 1

[0028] In this embodiment, phenol and chlorine are used as raw materials, and the mixed catalyst is composed of diphenyl sulfide, ferric chloride, and trifluoromethanesulfonic acid. In the mixed catalyst, diphenyl sulfide, ferric chloride, and trifluoromethanesulfonic acid The molar ratio is 2:2:1. The method for producing high-purity 2,4-dichlorophenol in the present embodiment may further comprise the steps:

[0029] (1) 50g of raw material phenol is heated and melted and stirred, and the stirring speed is 2000r / min, and the mixed catalyst prepared in proportion is added to the raw material being stirred, and the addition amount of the mixed catalyst accounts for the raw material in terms of mass percentage 0.05% by weight of phenol;

[0030] (2) Heating the material prepared in step (1) and maintaining it at 70°C, starting to feed chlorine gas slowly and evenly, the feeding time is 3h, and the total amount of chlorine gas feeding is calculated as 2.2 moles of raw material ...

Embodiment 2-5

[0033] Embodiment 2-5 only changes the quality of mixed catalyst in example 1, and all the other are the same as example 1, and concrete data see table 1. The 2,4-dichlorophenol products of Examples 1-5 are analyzed by gas chromatography, wherein the gas chromatography conditions are: the temperature of the inlet is 50°C, the temperature of the FID detector is 280°C, and the initial temperature is 50°C. 2min, the final temperature is 260°C, hold for 30min, and the heating rate is 10°C / min. Before analysis, the sample is diluted with solvent to equal multiples, and the solvent used is acetone. The experimental results are shown in Table 1.

[0034] Table 1

[0035]

Embodiment 6

[0037] In this embodiment, phenol and chlorine are used as raw materials, and the mixed catalyst is composed of diphenyl sulfide, ferric chloride, and trifluoromethanesulfonic acid. In the mixed catalyst, diphenyl sulfide, ferric chloride, and trifluoromethanesulfonic acid The molar ratio is 2:2:1. The method for producing high-purity 2,4-dichlorophenol in the present embodiment may further comprise the steps:

[0038] (1) 50g of raw material phenol is heated and melted and stirred, and the stirring speed is 2000r / min, and the mixed catalyst prepared in proportion is added to the raw material being stirred, and the addition amount of the mixed catalyst accounts for the raw material in terms of mass percentage 0.06% by weight of phenol;

[0039] (2) Heat the material prepared in step (1) and keep it at 70°C, start slowly and uniformly feeding chlorine gas for 3 hours, the total amount of chlorine gas feeding is 2.2 times the molar number of raw material phenol, after catalytic...

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Abstract

The invention provides a method for producing high-purity 2,4-dichlorophenol. The method comprises the following steps: (1) performing heating melting on a raw material, and adding a mixed catalyst into the raw material, wherein the raw material is at least one selected from phenol, o-chlorophenol or p-chlorophenol, and the mixed catalyst is a mixture of diphenyl sulfide, ferric chloride and trifluoromethanesulfonic acid; (2) maintaining the temperature of the material at 40-100 DEG C, introducing a chlorinating agent into the material, and performing a chlorination catalytic reaction to obtain crude 2,4-dichlorophenol,wherein the chlorinating agent is at least one selected from chlorine gas and sulfuryl chloride; and (3) performing melt crystallization on the crude 2,4-dichlorophenol to obtain the 2,4-dichlorophenol product. According to the method provided by the invention, the chlorinating agent used in the method can be the sulfuryl chloride or the chlorine gas, and when the sulfuryl chloride or the chlorine gas is used, a higher conversion rate of the raw material can be achieved; the crude product obtained by the catalytic chlorination reaction in the method does not need rectification, and the 2,4-dichlorophenol product with purity of 99% can be obtained only by the melt crystallization.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a production method for producing high-purity 2,4-dichlorophenol by catalytic chlorination of phenol, o-chlorophenol or p-chlorophenol. Background technique [0002] 2,4-Dichlorophenol is an important raw material for many pesticides and pharmaceutical intermediates. In terms of pesticides, organophosphorus insecticide prothion, herbicide 2,4-D, 2,4-dibutyl ester, dipropen, methylpyramid, pyrenzazone, propargyl oxadiazone and The new fungicide cyanohydrin etc. In medicine, it can be used as an important raw material for the drug thiobisdichlorophene. [0003] The production methods of 2,4-dichlorophenol in the prior art mainly include phenol direct catalytic chlorination method, p-chlorophenol catalytic chlorination method, o-chlorophenol catalytic chlorination method and the like. Most of the production methods in the prior art have the problems that the product pur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/30C07C37/62C07C37/84
Inventor 孙晓岩赵文英王一鑫夏力毕荣山项曙光
Owner QINGDAO UNIV OF SCI & TECH
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