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Preparation method for 2,2',4,4'-tetrehydroxybenzophenone

A technology of tetrahydroxybenzophenone and dihydroxybenzoic acid is applied in the field of preparation of 2,2',4,4'-tetrahydroxybenzophenone, and can solve the problems of high unit consumption of raw materials, complex by-products, and reaction Difficult to control and other problems, to achieve the effect of reducing production energy consumption, shortening process time, and accelerating catalytic speed

Inactive Publication Date: 2012-01-11
HUBEI MEIKAI CHEM
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation of 2,2',4,4'-tetrahydroxybenzophenone is usually based on 2,4-dihydroxybenzoic acid and resorcinol as starting materials, zinc chloride and phosphorus oxychloride as compound Catalyst and sulfolane are used as solvent for the reaction. This method has poor operation safety, difficult to control the reaction, easy to solidify, complex by-products and difficult to separate, high unit consumption of raw materials, long process time, low product purity and low yield

Method used

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  • Preparation method for 2,2',4,4'-tetrehydroxybenzophenone
  • Preparation method for 2,2',4,4'-tetrehydroxybenzophenone
  • Preparation method for 2,2',4,4'-tetrehydroxybenzophenone

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Experimental program
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Effect test

Embodiment 1

[0023] Drop into 54kg phosphorus oxychloride, 37.5kg sulfolane, 37.5kg dichloroethane, 50kg 2,4-dihydroxybenzoic acid in the reactor, add 4kg phosphorus trichloride, 50kg m-benzene Diphenol and 42kg zinc chloride, start to heat up, and the temperature in the control still is 64 ℃, and insulation reaction makes reaction completely in 90 minutes. After the reaction is over, transfer the product to a kettle with a water temperature below 15°C and a water volume of 1500L to hydrolyze the catalyst. After the hydrolysis is completed, cool down to below 15°C, discharge and filter, then transfer to a kettle with a water volume of 1500L, and put 6kg of activated carbon into it , heated up to 90-100°C, kept stirring for 10 minutes, then discharged and filtered, crystallized, centrifuged, and dried to obtain 65.72 kg of light yellow-green powder.

[0024] The final product of this embodiment is characterized by infrared spectroscopy (see figure 1 ), and with the infrared spectrum of 2,2...

Embodiment 2～3

[0030] Keep the feed intake of 50kg 2,4-dihydroxybenzoic acid, 50kg resorcinol, 37.5kg sulfolane, and 37.5kg dichloroethane constant, the mass ratio of catalyst phosphorus oxychloride, zinc chloride, phosphorus trichloride Without changing the total amount of the catalyst, other operating conditions and product characterization methods were the same as in Example 1 to obtain 2,2',4,4'-tetrahydroxybenzophenone. The catalyst dosage and test results are shown in Table 1.

[0031] Table 2. Embodiment 2~3 catalyst total amount and test result

[0032]

Embodiment 4～5

[0034] Keep the feeding amount of 50kg 2,4-dihydroxybenzoic acid, 50kg resorcinol, 54kg phosphorus oxychloride, 42kg zinc chloride, 4kg phosphorus trichloride constant, solvent sulfolane, dichloroethane mass ratio constant , changing the dosage of the solvent, other operating conditions and product characterization methods are the same as in Example 1 to obtain 2,2',4,4'-tetrahydroxybenzophenone. The solvent dosage and test results are shown in Table 3.

[0035] Table 3. Embodiment 4~5 solvent total amount and test result

[0036]

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Abstract

The present invention discloses a preparation method for 2,2',4,4'-tetrehydroxybenzophenone. The method comprises: adding phosphorus oxychloride, sulfolane and 2,4-dihydroxybenzoic acid to a reaction container according to a certain ratio; adding phosphorus trichloride, resorcinol and zinc chloride to the reaction container while stirring; slowly heating to a temperature of 62-65 DEG C, then holding the temperature and carrying out complete reaction; adding water to carry out hydrolysis after completing the reaction; cooling the temperature to less than 15 DEG C; discharging the material and carrying out suction filtration; then carrying out treatments of refining, crystallization, centrifugation and drying to obtain the 2,2',4,4'-tetrehydroxybenzophenone finished product. The method provided by the present invention has characteristics of simple process, safe and convenient operation, low environmental pollution and low cost. In addition, the product yield and the product purity are high.

Description

technical field [0001] The invention relates to a preparation method of 2,2',4,4'-tetrahydroxybenzophenone as a light stabilizer. Background technique [0002] 2,2',4,4'-Tetrahydroxybenzophenone, commonly known as BP-2, benzophenone-2, is an anti-ultraviolet additive for oil-based cosmetics, widely used in various sunscreen creams, creams, honey, In sunscreen cosmetics such as emulsion and oil, the application in plastics, resins, synthetic rubber, photosensitive materials and high-grade paints and coatings is also increasingly valued. [0003] At present, the preparation of 2,2',4,4'-tetrahydroxybenzophenone is usually based on 2,4-dihydroxybenzoic acid and resorcinol as starting materials, zinc chloride and phosphorus oxychloride as compound The catalyst and sulfolane are used as the solvent for the reaction. This method has poor operational safety, is difficult to control the reaction, is easy to solidify, has complex by-products and is not easy to separate, high unit co...

Claims

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Application Information

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IPC IPC(8): C07C49/83C07C45/45
Inventor 胡林松王志刚李小林阮长友张兴江
Owner HUBEI MEIKAI CHEM
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