Preparation method of 4, 4'-dihydroxy benaophenonel

A technology of dihydroxybenzophenone and p-hydroxybenzoic acid, which is applied in the field of preparation of 4,4'-dihydroxybenzophenone, can solve the problems of difficult recycling of waste phosphoric acid, long holding time, environmental pollution, etc. To achieve the effects of shortening the production cycle, reducing pollution and reducing costs

Inactive Publication Date: 2014-01-08
武汉怡兴化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Calculated according to the current market conditions, it takes about 7 tons of polyphosphoric acid to produce one ton of the target product using this process, and the raw material cost is as high as about 110,000, which is relatively high.
Moreover, the heat preservation time of this process is relatively long, resulting in a long time-consuming process for the entire process, thereby prolonging the production cycle
In addition, a large amount of waste phosphoric acid produced is difficult to recycle, causing environmental pollution

Method used

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  • Preparation method of 4, 4'-dihydroxy benaophenonel
  • Preparation method of 4, 4'-dihydroxy benaophenonel
  • Preparation method of 4, 4'-dihydroxy benaophenonel

Examples

Experimental program
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Effect test

Embodiment 1

[0050] 1. Process formula

[0051] Crude production raw materials: 200kg p-hydroxybenzoic acid, 164kg phenol, 283kg dimethyl sulfoxide, 400kg aluminum chloride, 333kg phosphorus oxychloride, 50+950kg water

[0052] Crude refined ingredients: crude product 320kg, methanol 550kg, water 650+440kg, activated carbon 20kg, 95% alcohol 450kg

[0053] 2. Operation steps

[0054] (1) Put 283kg of measured dimethyl sulfoxide and 164kg of phenol into a 2000L liter reactor, add 200kg of p-hydroxybenzoic acid and 400kg of aluminum trichloride under stirring, stir and heat up to 68-72°C, boil water Cool down, stabilize the temperature, turn on tail gas absorption, add 323 kg of phosphorus oxychloride dropwise, and drop it in about 1.5 hours, the reaction material turns from white to yellow.

[0055] (2) After dropping the phosphorus oxychloride, keep it warm for about 3.5 hours at 68-72°C until the material has no bubbles. After the reaction, the material changes from yellow to orange-red...

Embodiment 2

[0063] 1. Process formula

[0064] Crude production raw materials: 150kg p-hydroxybenzoic acid, 123kg phenol, 215kg dimethyl sulfoxide, 300kg aluminum chloride, 250kg phosphorus oxychloride, 50+700kg water

[0065] Crude refined ingredients: crude product 240kg, methanol 400kg, water 480+330kg, activated carbon 20kg, 95% alcohol 340kg

[0066] 2. Operation steps

[0067] (1) Put 215kg of measured dimethyl sulfoxide and 123kg of phenol into a 1000L liter reactor, add 150kg of p-hydroxybenzoic acid and 300kg of aluminum trichloride under stirring, stir and heat up to 68-72°C, boil water Cool down, stabilize the temperature, turn on tail gas absorption, add 250 kg of phosphorus oxychloride dropwise, and drop it in about 1.5 hours. The reaction material turns from white to yellow.

[0068] (2) After dropping the phosphorus oxychloride, keep it warm for about 3.5 hours at 68-72°C until the material has no bubbles. After the reaction, the material changes from yellow to orange-red...

Embodiment 3

[0076] 1. Process formula

[0077] Crude production raw materials: p-hydroxybenzoic acid 100kg, phenol 82kg, dimethyl sulfoxide 142kg, aluminum chloride 200kg, phosphorus oxychloride 167kg, water 50+400kg

[0078] Crude refined ingredients: crude product 160kg, methanol 280kg, water 330+220kg, activated carbon 10kg, 95% alcohol 230kg

[0079] 2. Operation steps

[0080] (1) Put 142kg of measured dimethyl sulfoxide and 82kg of phenol into a 1000L liter reaction kettle, add 100kg of p-hydroxybenzoic acid and 200kg of aluminum trichloride under stirring, stir and heat up to 68-72°C, boil water Lower the temperature, stabilize the temperature, turn on the tail gas absorption, add 167kg of phosphorus oxychloride dropwise, and drop it in about 1 hour, and the reaction material changes from white to yellow.

[0081] (2) After dropping the phosphorus oxychloride, keep it warm for about 3.5 hours at 68-72°C until the material has no bubbles. After the reaction, the material changes f...

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Abstract

The invention provides a preparation method of 4, 4'-dihydroxy benaophenonel. The preparation method includes: with phosphorus oxychloride and aluminum trichloride as catalysts and dimethyl sulfoxide as solvent, subjecting hydroxybenzoic acid and phenol to synthetic reaction to obtain 4, 4'-dihydroxy benaophenonel. According to the preparation method, with the dimethyl sulfoxide as solvent, the hydroxybenzoic acid and the phenol are subjected to synthetic reaction under the action of the catalysts, and the 4, 4'-dihydroxy benaophenonel is generated; accordingly, the cost is reduced, production cycle is shortened, and no waste causing environmental pollution is generated during the reaction process so that environmental pollution is also reduced.

Description

【Technical field】 [0001] The invention relates to the field of chemical industry, in particular to a preparation method of 4,4'-dihydroxybenzophenone. 【Background technique】 [0002] 4,4'-dihydroxybenzophenone (4.4'-dihydroxy benzophenone), insoluble in water, soluble in organic solvents, is often used as an intermediate for pesticides, pharmaceutical raw materials and dyes, and can also be used as a stabilizer for ultraviolet light It is widely used in cosmetics, plastics, film, films, films, adhesives and coatings, optical fibers, and printed circuit boards. Products, pharmaceutical intermediates. Its molecular structure is shown in the figure below: [0003] [0004] Invention patent No. 200510018620.9 of Wuhan University discloses a preparation method of 4,4-dihydroxybenzophenone. The main process is: under the condition of catalyst, stirring phenyl p-hydroxybenzoate in an organic solvent and raising the temperature Heat up to 70-170°C, react for 3-20 hours, separa...

Claims

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Application Information

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IPC IPC(8): C07C45/46C07C49/83
CPCC07C45/46C07C49/83
Inventor王勤潘明黄雄
Owner武汉怡兴化工股份有限公司