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Process for synthesizing 4,4'-dihydroxy diphenylketone

A technology of dihydroxybenzophenone and synthetic methods, applied in 4 fields, can solve problems such as environmental pollution, achieve the effects of reducing production costs, easy handling and storage, and realizing resource utilization

Inactive Publication Date: 2008-09-24
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] Judging from the current situation, the common problem in the synthesis process of diaryl ketones by the carbon tetrachloride method is environmental pollution. Therefore, it is necessary to find a high-efficiency catalyst application that does not increase production costs and does not have the problem of "three wastes". It is imminent to synthesize diaryl ketones

Method used

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  • Process for synthesizing 4,4'-dihydroxy diphenylketone
  • Process for synthesizing 4,4'-dihydroxy diphenylketone
  • Process for synthesizing 4,4'-dihydroxy diphenylketone

Examples

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Embodiment 1

[0030] Embodiment 1: the preparation of solid superacid catalyst

[0031] FeCl 3 ·6H 2 O10g was dissolved in 100mL distilled water, and 25% (w / w) ammonia water was added to adjust the pH to 8 to obtain ferric hydroxide sol, which was filtered, and the filter cake was washed with distilled water to remove Cl - , dried, placed in 0.25mol / L H 2 SO 4 Solution (15mL / g) was impregnated, then filtered, dried, and roasted at 500°C to obtain the solid superacid catalyst (SO 4 2- / Fe 2 o 3 ).

Embodiment 2

[0033] Take commercially available Fe(NO 3 ) 3 9H 2 O10g was dissolved in 100mL distilled water, and urea was added to adjust the pH to 9 to obtain ferric hydroxide sol, which was filtered, and the filter cake was washed with distilled water to remove NO 3 -, dried, placed in 0.50mol / L (NH 4 ) 2 SO 4 Solution (15mL / g) was impregnated, then filtered, dried, and roasted at 550°C to obtain the solid superacid catalyst (SO 4 2- / Fe 2 o 3 ).

Embodiment 3

[0035] commercially available anhydrous AlCl 3 Dissolve 5 g in 50 mL of distilled water, add 25% (w / w) ammonia water to adjust the pH to 8, obtain aluminum hydroxide sol, filter, and wash the filter cake with distilled water to remove Cl - , dried, placed in 2.50mol / L H 2 SO 4 Solution (15mL / g) was impregnated, then filtered, dried, and roasted at 600°C to obtain the solid superacid catalyst (SO 4 2- / Al 2 o 3 ).

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Abstract

The present invention provides a synthetic method of 4, 4'-dihydroxy benzophenone (I). In the method, carbon tetrachloride and phenol are used as raw materials and react for 3 to 20 hours at the temperature of 80 to 200 DEG C, with solid superacid catalytic, then the mixture is cooled to be at the room temperature, an appropriate amount of ice water is added for mixing and hydrolysis for 20 to 60 minutes; after the hydrolysis reaction, the reaction solution is separated and purified to prepare the 4, 4'-dihydroxy benzophenone; the formula of the solid super acidic catalyst can be one of the following: SO4<2-> / Fe2O3, SO4<2-> / Al2O3, SO4<2-> / SnO2, and SO4<2-> / Sb2O3. The method has the following beneficial effects: the carbon tetrachloride is used as the raw material to synthesize the 4, 4'-dihydroxy benzophenone, which realizes the resource utilization of the carbon tetrachloride and reduces the production cost; the solid super acidic catalyst can be easily treated and stored and has no corrosion to the equipment; the catalyst can be separated from the reaction mixture after the reaction is completed; and the catalyst can be recycled and has little pollution.

Description

(1) Technical field [0001] The invention relates to a synthesis method of 4,4'-dihydroxybenzophenone, in particular to a method for synthesizing 4,4'-dihydroxybenzophenone by catalyzing carbon tetrachloride and phenol with a solid superacid. (2) Background technology [0002] 4,4'-Dihydroxybenzophenone (4,4'-Dihydroxybenzophenone) is a very important organic synthesis intermediate, which is widely used in the fields of photosensitization, medicine, dyestuff, pesticide and so on. With the increasing demand for photosensitive materials, pharmaceutical raw material cyclofenyl and other products in domestic and foreign markets, the synthesis of 4,4'-dihydroxybenzophenone has received great attention again. [0003] There are many reports on its synthesis, most of which use p-hydroxybenzoic acid and phenol as raw materials. Among them, Japanese Patent JP 3123752 reports that p-hydroxybenzoic acid and phenol are used as raw materials, and polyphosphoric acid is directly used as a...

Claims

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Application Information

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IPC IPC(8): C07C49/83C07C45/43
CPCY02P20/584
Inventor 裴文林晶王艳峰
Owner ZHEJIANG UNIV OF TECH
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