Preparation method for 3,4'dichloro diaryl ether

A technology of dichlorodiphenyl ether and m-dichlorobenzene, applied in 3 fields, can solve problems such as affecting product quality and yield, and achieve the effects of improving product quality, reducing pollution and fast reaction speed

Inactive Publication Date: 2012-06-27
HUBEI XINGHUO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Because benzene is prone to biphenylation reaction at high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A kind of 3, the preparation of 4' dichlorodiphenyl ether, its step is as follows:

[0041] (1) Preparation of potassium methoxide

[0042] Add 50L of petroleum ether (pre-dried) and 10kg of potassium metal into a 200L stainless steel reactor, and start stirring. Add 50L of anhydrous methanol dropwise within 2h. Reflux for 1 hour after the dropwise addition, and cool. A white paste potassium methoxide solution was obtained.

[0043] (2) Preparation of potassium p-chlorophenate

[0044] Add 40L of self-made potassium methoxide solution and 26kg of p-chlorophenol into a 200L stainless steel reaction kettle, pass nitrogen gas under stirring, react for 0.5h, and then heat up to 100°C to distill off the solvent to obtain white anhydrous potassium phenolate.

[0045] (3) Preparation of cuprous chloride

[0046] Add copper oxide to saturated sodium chloride hydrochloric acid solution, react at 100°C, then add copper powder, and stir until the solution becomes colorless an...

Embodiment 2

[0050]A kind of 3, the preparation of 4' dichlorodiphenyl ether, its step is as follows:

[0051] (1) Preparation of potassium methoxide

[0052] Add 50L of petroleum ether (pre-dried) and 10kg of potassium metal into a 200L stainless steel reactor, and start stirring. Add 50L of anhydrous methanol dropwise within 2h. Reflux for 1 hour after the dropwise addition, and cool. A white paste potassium methoxide solution was obtained.

[0053] (2) Preparation of potassium p-chlorophenate

[0054] Add 40L of self-made potassium methoxide solution and 26kg of p-chlorophenol into a 200L stainless steel reaction kettle, pass nitrogen gas under stirring, react for 0.5h, and then heat up to 100°C to distill off the solvent to obtain white anhydrous potassium phenolate.

[0055] (3) Preparation of cuprous chloride

[0056] Add copper oxide to saturated sodium chloride hydrochloric acid solution, react at 100°C, then add copper powder, and stir until the solution becomes colorless and...

Embodiment 3

[0060] A kind of preparation method of 3,4' dichlorodiphenyl ether, its step is as follows:

[0061] (1) Preparation of sodium methoxide

[0062] Add 50L of petroleum ether (pre-dried) and 6kg of metallic sodium into a 200L stainless steel reactor, and start stirring. Add 50L of absolute ethanol dropwise within 2h. Reflux for 1 hour after the dropwise addition, and cool. A white paste potassium methoxide solution was obtained.

[0063] (2) Preparation of potassium p-chlorophenate

[0064] Add 40L of self-made potassium methoxide solution and 26kg of p-chlorophenol into a 200L stainless steel reaction kettle, pass nitrogen gas under stirring, react for 0.5h, and then heat up to 100°C to distill off the solvent to obtain white anhydrous potassium phenolate.

[0065] (3) Preparation of cuprous chloride

[0066] Add copper oxide to saturated sodium chloride hydrochloric acid solution, react at 100°C, then add copper powder, and stir until the solution becomes colorless and tr...

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Abstract

A preparation method for 3,4'dichloro diaryl ether is disclosed, which comprises the following steps of: (1) preparation for potassium alkoxide or sodium alkoxide; (2) preparation for potassium p-chlorophenolate; (3) preparation for active cuprous chloride; and (4) preparation for 3,4'dichloro diaryl ether. The preparation method has the following advantages that: side reactions are greatly reduced, reaction speed is fast, the pollution caused by the volatilization of benzene solvents is reduced, the utilization rate of equipment and the like are increased, the quality of product is improved, as well as yield and chilling efficiency are increased by using p-chlorophenol waterless salifying process, using newly-prepared catalyst, optimizing the ratio and pouring method of materials, and protecting by inert gas.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of 3,4' dichlorodiaryl ether. Background technique [0002] Diaryl ether is an important intermediate of organic medicine and pesticide. Among them, 3,4' dichlorodiaryl ether is an important intermediate for the production of difenoconazole. Difenoconazole is an important fungicide. At present, domestically produced difenoconazole is mainly used for export, and the supply of the product is in short supply. At present, the common method for producing chlorinated diphenyl ethers is to use the Ullmann etherification process. The process uses chlorobenzene and phenoxide as raw materials, copper powder or copper salt as a catalyst, and at the same time, some phase transfer catalysts need to be added to accelerate the reaction. [0003] Among them, the synthesis of phenate is generally to form a salt with substituted phenol in the form of solid or aqu...

Claims

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Application Information

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IPC IPC(8): C07C43/29C07C41/30
Inventor 曾丹田汪志君
Owner HUBEI XINGHUO CHEM
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