Method for preparing diphenyl ether

A technology of diphenyl ether and phenol is applied in the field of preparation of flame retardants and fragrance intermediates, which can solve the problems of many by-products and high reaction temperature, and achieve the effects of good product quality, high yield and lower production cost.

Active Publication Date: 2011-08-10
SHANDONG TIANYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the reaction product chlorinated diphenyl ether will also react with phenate to produce by-p

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 170g of molten phenol, put it into a four-necked flask, add 30g of sodium hydroxide, 15g of potassium hydroxide, and then raise the temperature to 85°C to obtain a molten mixture; add 5.5g of copper sulfate pentahydrate and 50g of Molten diphenyl ether is heated up to 130°C, and is allowed to stand at this temperature for 0.5 hours, and then stirred for 1 hour to make it evenly mixed to obtain a mixed liquid containing phenol, diphenyl ether and phenol salt solution. Add 170g of chlorinated benzene to the mixed liquid under certain conditions, and then gradually increase the temperature to distill all the chlorinated benzene and water to obtain a reaction mixture. It is best to add chlorinated benzene in a dropwise manner, so that water and chlorinated benzene can be formed. The azeotropic mixture is refluxed and distilled together to achieve complete removal of the water contained and generated in the system; under the condition of stirring and a temperature of 19...

Embodiment 2

[0024] Weigh 170g of molten phenol, add it to a four-necked flask, add 85g of potassium hydroxide therein, and then raise the temperature to 65°C to obtain a molten mixture; add 2.5g of copper sulfate pentahydrate and 30g of molten diphenyl ether to the mixture , heated up to 110°C, and stood at this temperature for 1 hour, then stirred for 2 hours to make it evenly mixed to obtain a mixed liquid containing phenol, diphenyl ether and phenol salt solution, and added to the mixed liquid under stirring Add 200g of chlorinated benzene to the mixture, then gradually heat up to distill all the chlorinated benzene and water to obtain a reaction mixture. Chlorinated benzene is preferably added dropwise, so that an azeotropic mixture of water and chlorinated benzene can be formed. Reflux and steam together to achieve complete removal of the water contained and generated in the system; under the condition of stirring and a temperature of 220°C, start to add 150g of chlorinated benzene dr...

Embodiment 3

[0026] Weigh 170g of molten phenol, add it to a four-necked flask, add 30g of sodium hydroxide, 50g of potassium hydroxide, and then heat up to 80°C to obtain a molten mixture; add 6g of cuprous chloride wet material to the mixture ( 10% water content) and 80g of molten diphenyl ether, heated to 120°C, and stood at this temperature for 1 hour, then stirred for 2 hours to make it evenly mixed, and prepared a salt solution containing phenol, diphenyl ether and phenol Add 250g of chlorinated benzene to the mixed liquid under agitation, then gradually heat up to distill all the chlorinated benzene and water out to obtain a reaction mixture. Chlorinated benzene is preferably added dropwise, so that An azeotropic mixture of water and chlorinated benzene is formed, and they are refluxed and distilled together to achieve complete removal of the water contained and generated in the system; under the condition of stirring and a temperature of 210°C, start to add 170g of chlorinated benze...

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Abstract

The invention discloses a method for preparing diphenyl ether, which comprises the following steps of: generating saline solution of phenol through phenol and alkali; removing water in a system by back flow of benzene chloride; and under the condition of the existence of a catalyst, performing Ullmann reaction by dripping benzene chloride to generate a target compound. In the method, phenol is used as the raw material and is also used as a solvent; and the catalyst is a wet material of blue vitriol or cuprous chloride or a mixture of the wet materials of blue vitriol or cuprous chloride. The method has low production cost. No solid waste is generated. The yield is high. The product has high quality.

Description

technical field [0001] The invention relates to a preparation process of a flame retardant and a fragrance intermediate. Specifically relates to a preparation method of diphenyl ether. Background technique [0002] Diphenyl ether compounds are important pesticide and pharmaceutical intermediates. Among them, diphenyl ether can be used as an intermediate to prepare flame retardants and fragrances, and produce diphenyl ether brominated flame retardant products and fragrances. Medicines and pesticides, among which the difenoconazole compound is a pesticide with a large dosage and good bactericidal effect; moreover, it can also be used as a heat transfer medium, synthetic resin and other raw materials for organic synthesis; at the same time, diphenyl ether and its The downstream product polyaminodiphenyl ether can also be used as a monomer for the synthesis of polymer compounds, so diphenyl ether has important application value. [0003] There are several different methods tha...

Claims

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Application Information

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IPC IPC(8): C07C43/275C07C41/01
Inventor 邢晓华李善清王丹孟烨赵庭栋闫晓红
Owner SHANDONG TIANYI CHEM
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