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Preparation method for 2,4-dichlorophenol, and preparation method for 2,4-dichlorophenolate

A technology of dichlorophenol and dichlorophenate, applied in the chemical industry, can solve problems such as poor appearance of products, influence on use, etc., and achieve the effects of simple process, guaranteed reaction rate, and improved selectivity

Inactive Publication Date: 2018-08-21
SHANDONG RUNBO BIOTECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The Chinese patent with the publication number CN105777499A discloses a method for directional synthesis of 2,4-dichlorophenol and 2,4,6-trichlorophenol with sulfuryl chloride plus a composite catalyst. It is mentioned that 98% of 2, 4-dichlorophenol, but due to the use of expensive sulfuryl chloride, and the subsequent use of molten crystallization for separation, it will inevitably lead to the mixing of low-melting catalysts and oxidative and discolored substances during chlorination into the target product, resulting in poor appearance of the product and containing Certain impurities will affect subsequent use and make it difficult to implement industrialization

Method used

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  • Preparation method for 2,4-dichlorophenol, and preparation method for 2,4-dichlorophenolate

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[0030] The invention provides a preparation method of 2,4-dichlorophenol, comprising: S) chlorinating phenol, an accelerator and sulfuryl chloride in an organic solvent under low temperature conditions to obtain 2,4-dichlorophenol Chlorophenol; the accelerator is selected from one or more of dimethyl sulfide, phenylene sulfide and isopropyl ether.

[0031] The present invention has no special limitation on the sources of all raw materials, which can be commercially available.

[0032] Phenol, accelerator and sulfuryl chloride are chlorinated in an organic solvent under low temperature conditions; the accelerator is one or more of dimethyl sulfide, phenylene sulfide and isopropyl ether; the The quality of the accelerator is 0.1% to 10% of the phenol mass, more preferably 0.5% to 5%; the organic solvent is an organic solvent well known to those skilled in the art, and there is no special limitation. In the present invention, it is preferably One or more in methylene dichloride,...

Embodiment 1

[0044] 1.1 Dissolve 100g of phenol and mix with 100g of tetrachlorethylene, then add 0.5g of dimethyl sulfide, lower to -10°C, then add 287g of sulfuryl chloride dropwise, and carry out chlorination reaction. The dropwise addition time is 5h. After the reaction is completed, the mixture containing The reaction solution of 2,4-dichlorophenol; the normalized content of 2,4-dichlorophenol is 99.53%, and the yield is 99.3%.

[0045]1.2 Add 30% sodium hydroxide solution to the reaction liquid containing 2,4-dichlorophenol until the pH of the solution is 12, and the neutralization temperature is 50°C, and let stand to separate to obtain the aqueous phase and the organic phase; The water phase was dehydrated to obtain 197.5 g of anhydrous 2,4-dichlorophenol sodium salt, with a yield of 99.2%; the organic phase was refluxed with water, and the water was extracted until the water content was less than 0.2%, and then returned to 1.1, and phenol was added , cooling and then adding sulfur...

Embodiment 2

[0047] 200g ethanol, 95g (1mol) chloroacetic acid and 0.1g concentrated sulfuric acid were mixed and stirred, and desolvated and dehydrated for 5h to obtain ethyl chloroacetate; 186g (1mol) of 2,4-dichlorophenate sodium obtained in Example 1 was added and kept warm Stir for 3 hours, filter out the solid sodium chloride generated by the reaction, remove ethanol from the filtrate to obtain ethyl 2,4-dichlorophenoxyacetate, add 125g of 32% sodium hydroxide solution, keep stirring at 100°C for 2 hours, add 50% sulfuric acid 100 g was crystallized at 10°C for 1 h, filtered, and the filter cake was dried to obtain 221 g of 2,4-dichlorophenoxyacetic acid solid with a purity of 99.5% and a yield of 99.5%.

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Abstract

The invention provides a preparation method for 2,4-dichlorophenol. The preparation method comprises the following steps: S) adding phenol, a promoter and sulfuryl chloride into an organic solvent andcarrying out chlorination under low temperature conditions to obtain 2,4-dichlorophenol, wherein the promoter is one or more selected from the group consisting of dimethyl sulfide, phenyl sulfide andisopropyl ether. Compared with the prior art, the preparation method provided by the invention has the advantage that selectivity is improved due to the reaction under low temperature conditions; andthe promoter is added at the same time to ensure a reaction rate.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of 2,4-dichlorophenol and a preparation method of 2,4-dichlorophenate. Background technique [0002] 2,4-Dichlorophenol is used as a solvent, pesticide and pharmaceutical intermediate for the synthesis of biben, 2,4-D, ibifos (EPBP), dukesan, glyphosate and the drug thiobisdichlorophene, The annual demand is tens of thousands of tons. [0003] The production methods of 2,4-dichlorophenol mainly include: phenol direct chlorination method, mixed phenol chlorination method, o-chlorophenol selective chlorination method, p-chlorophenol chlorination method and phenol catalytic chlorination method. [0004] The direct chlorination of phenol is a traditional production process at home and abroad. The process is simple and the cost is low. However, because the physical properties of the by-product 2,6-dichlorophenol are very close to those of 2,...

Claims

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Application Information

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IPC IPC(8): C07C37/66C07C37/62C07C39/30
Inventor 孙国庆侯永生陈桂元赵广理
Owner SHANDONG RUNBO BIOTECH CO LTD
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