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Preparation method of 2,2'- dyhydroxyl-4,4'-dimethoxybenzophenone

A technology of dimethoxybenzophenone and dihydroxy, which is applied in the field of preparation of ultraviolet absorbers, can solve the problems of difficult transportation of phosgene, large environmental pollution, and high production cost, and achieve easy industrial production, low environmental pollution, The effect of high production safety

Inactive Publication Date: 2013-12-25
SHANDONG WUYANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method for preparing this product is mainly the phosgene method, but phosgene has the disadvantage of being difficult to transport; those skilled in the art have recently provided a preparation method using oxalyl chloride instead of phosgene
Although the two preparation methods have their own advantages, the disadvantages of both are: high production cost, low yield, large environmental pollution, etc.

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0023] A kind of preparation method of 2,2'-dihydroxy-4,4'-dimethoxybenzophenone of the present invention, comprises the following steps:

[0024] ① Put resorcinol and 20%-50% aqueous sodium hydroxide solution into a reaction tank, and dissolve to obtain a mixed solution; the molar ratio of resorcinol to aqueous sodium hydroxide solution is 1:1-1.2;

[0025] ②Heat the mixed solution in step ① to 30°C-45°C, then add dimethyl sulfate, and add 20%-50% aqueous sodium hydroxide solution dropwise at the same time, keep warm for 2-4 hours, dimethyl sulfate and m-benzene The mol ratio of diphenol 2.4-3: 1, the amount of the aqueous sodium hydroxide solution that drips 20%-50% is identical with the aqueous sodium hydroxide solution of 20%-50% in step 1.;

[0026] 3. the solution after step 2. heat preservation reaction is completed is separated, and the organic phase obtained after separation is distilled by a rectifying tower to obtain m-phenylenediyl ether;

[0027] ④Put the organic...

Embodiment 1

[0037] Embodiment 1, concrete steps are as follows:

[0038] 1. Get 42kg resorcinol and 76.3kg 20% ​​sodium hydroxide aqueous solution and put them into a reaction tank to stir and dissolve, and obtain a mixed solution after dissolving;

[0039] ②Heat the mixed solution in step ① to 35°C, add 115.5kg of dimethyl sulfate under stirring, and add 76.3kg of 20% sodium hydroxide aqueous solution dropwise at the same time, and keep warm for 2 hours;

[0040] 3. the solution after the complete insulation reaction in step 2. is separated, and the organic phase obtained after the separation is distilled by a rectifying tower to obtain m-xylylene dimethyl ether;

[0041] ④ Take 300kg of dichloroethane and 50kg of m-xylylene dimethyl ether, put them into the reaction tank, add 23.9kg of anhydrous aluminum chloride and 0.24kg of anhydrous sodium chloride under stirring, and add them within 3.8 hours at 30°C 18kg of phosgene, then heated to 55°C for 12 hours;

[0042] ⑤ Add water and hyd...

Embodiment 2

[0044] Embodiment 2, concrete steps are as follows:

[0045] ①Get 42kg resorcinol and 56kg 30% sodium hydroxide aqueous solution and put them into the reaction tank to stir and dissolve, and obtain the mixed solution after dissolving;

[0046] ②Heat the mixed solution in step ① to 30°C, add 130kg of dimethyl sulfate under stirring, and add 56kg of 30% sodium hydroxide aqueous solution dropwise at the same time, and keep it warm for 4 hours;

[0047] 3. the solution after the complete insulation reaction in step 2. is separated, and the organic phase obtained after the separation is distilled by a rectifying tower to obtain m-xylylene dimethyl ether;

[0048] ④ Take 300kg of dichloroethane and 50kg of m-xylylene dimethyl ether, put them into the reaction tank, add 46.6kg of anhydrous aluminum chloride and 1.6kg of anhydrous sodium chloride under stirring, and add them within 4 hours at 20°C 27kg of phosgene, then heated up to 40°C and kept warm for 18 hours;

[0049] ⑤ Add wa...

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Abstract

The invention provides a preparation method of 2,2'-dyhydroxyl-4,4'-dimethoxybenzophenone. The preparation method comprises the following steps: (1) adding resorcinol and a sodium hydroxide aqueous solution to a reaction tank to dissolve to obtain a mixed solution; (2) heating the mixed solution obtained in step (1), adding dimethyl sulfate, and simultaneously dropping the sodium hydroxide aqueous solution; (3) separating the solution completely subjected to thermal reaction in step (2), and distilling the separated organic phase through a rectifying column to obtain dimethoxy bengene; (4) adding an organic solvent, a composite catalyst and dimethoxy bengene to the reaction tank; (5) hydrating the solution completely reacted in step (4), separating the organic phase, and then performing distilling, acidizing out and filtering to obtain crude 2,2'-dyhydroxyl-4,4'-dimethoxybenzophenone; (6) transferring the crude 2,2'-dyhydroxyl-4,4'-dimethoxybenzophenone into the organic solvent, and performing crystallizing, filtering and drying to obtain 2,2'-dyhydroxyl-4,4'-dimethoxybenzophenone. By adopting the preparation method, the shortcomings in the prior art can be overcome.

Description

[0001] technical field [0002] The invention relates to the preparation of ultraviolet absorbers, which is a preparation method of 2,2'-dihydroxy-4,4'-dimethoxybenzophenone. Background technique [0003] 2,2′-Dihydroxy-4,4′-dimethoxybenzophenone is a kind of ultraviolet absorber, which is widely used in many fields such as industry and agriculture. At present, the method for preparing this product is mainly the phosgene method, but phosgene has the disadvantage of being difficult to transport; those skilled in the art have recently provided a preparation method using oxalyl chloride instead of phosgene. Although the two preparation methods have their own advantages, both have the disadvantages of high production cost, low yield, and large environmental pollution. Contents of the invention [0004] The purpose of the present invention is to provide a preparation method of 2,2'-dihydroxy-4,4'-dimethoxybenzophenone, so as to solve the shortcomings of the prior art. [0005]...

Claims

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Application Information

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IPC IPC(8): C07C49/84C07C45/64
Inventor 张俊祥徐洪涛贾宁刘建国李刚
Owner SHANDONG WUYANG CHEM
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