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Preparation method of 2,3,4,4'-tetrahydroxyldiphenylketone

A technology of tetrahydroxybenzophenone and p-hydroxybenzoic acid is applied in the preparation of carbon-based compounds, the preparation of organic compounds, chemical instruments and methods, etc. Large-scale production, long resin regeneration time and other problems, achieve the effect of complete catalytic reaction, low production cost, mild and safe reaction

Inactive Publication Date: 2010-02-10
HUNAN SHINEWAY ENTERPRISE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem of this method is that tri-n-propylphosphorus oxide is highly toxic, expensive, and difficult to recycle, causing serious environmental pollution and high production costs.
Although this method has a high yield, the resin regeneration time is long and the process is complicated, so it is not suitable for large-scale production

Method used

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  • Preparation method of 2,3,4,4'-tetrahydroxyldiphenylketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: Preparation of supported Lewis acid catalyst

[0028] 15.0g of purified montmorillonite was acidified in 600g of 30% sulfuric acid solution at 100°C for 4 hours, washed with deionized water and filtered, dried at 100°C for 8 hours to obtain acidified soil support, and then immersed in 21.8 g Commercially available anhydrous ZnCl 2 In the 1000mL methanol solution, after natural drying, place it in a muffle furnace and pass N at 120℃ 2 Protected roasting activation for 8 hours, after activation placed in P 2 O 5 Cool in a desiccator to obtain 32.4g of the ZnCl with a loading capacity of 6mmol / g 2 / Montmorillonite catalyst.

Embodiment 2

[0030] The impregnation solution contains 21g of commercially available anhydrous AlCl 3 1000mL methanol solution, the calcination temperature is 100℃, and other conditions are the same as in Example 1, 31.5g of the AlCl with a loading amount of 6mmol / g can be obtained 3 / Montmorillonite catalyst.

[0031] Implementation column 3

[0032] 25.0g of purified montmorillonite was acidified in 1200g of 30% sulfuric acid solution at 100°C for 4 hours, washed with deionized water and filtered, dried at 100°C for 8 hours to obtain acidified soil support, and then immersed in 35g Commercially available anhydrous ZnBr 2 In 1000mL methanol solution, after natural drying, place it in a muffle furnace and pass N at 200℃ 2 Protected roasting activation for 8 hours, after activation placed in P 2 O 5 Cool in a desiccator to obtain 54.0 g of the ZnBr with a loading capacity of 6 mmol / g 2 / Montmorillonite catalyst.

Embodiment 4

[0034] As in Example 3, the preparation of the acidified soil support was the same, and the acidified soil support was immersed in 28 g of commercially available anhydrous ZnBr 2 In 1000mL methanol solution, after natural drying, place it in a muffle furnace and pass N at 200℃ 2 Protected roasting activation for 8 hours, after activation placed in P 2 O 5 Cool in a desiccator to obtain 46.0 g of the ZnBr with a loading capacity of 4 mmol / g 2 / Montmorillonite catalyst.

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Abstract

The invention provides a preparation method of 2,3,4,4'-tetrahydroxyldiphenylketone, comprising the following steps: adopting sulfolane as solvent and pyrogallol as raw materials to perform a reactionat 120-160 DEG C for 6-10h in the presence of a catalyst system containing supported Lewis acid and phosphorus oxychloride, recycling supported Lewis acid catalyst through filtration, reducing pressure to recycle partial solvent sulfolane, neutralizing, adding a defined amount of distilled water, cooling to precipitate crystal, washing with water and finally drying to obtain the yellow target compound, wherein the yield can reach above 80% and the supported Lewis acid is 4-6mmol / g of ZnCl2 / montmorillonite, ZnBr2 / montmorillonite or AlCl3 / montmorillonite. Compared with the prior art, the invention has the advantage that (1) the catalysis efficiency of the supported catalyst is high and can be separated and recycled after the reaction, thus reducing the production cost; (2) the product yieldis high, the product is environmentally friendly and is applicable to mass industrialized production.

Description

Technical field [0001] The invention belongs to the field of fine organic chemicals, and relates to a preparation method of 2,3,4,4'-tetrahydroxybenzophenone, in particular to a supported Lewis acid catalytic system of para-hydroxybenzoic acid and pyrogallic acid A method for preparing 2,3,4,4'-tetrahydroxybenzophenone through Friedel-Crafts acylation reaction. Background technique [0002] 2,3,4,4'-Tetrahydroxybenzophenone is an important organic intermediate, which can be used in photoresist, pharmaceutical intermediate, ultraviolet absorber, resin stabilizer, In dyes and other fields, especially in the microelectronics industry, the demand for high-purity 2,3,4,4'-tetrahydroxybenzophenone and other polyhydroxybenzophenone products is rapidly increasing. To this end, my country has listed the technology of converting gallic tannins into electronic industrial grade 2,3,4,4'-tetrahydroxybenzophenone as a key scientific and technological research topic in the national "Eleventh F...

Claims

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Application Information

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IPC IPC(8): C07C49/83C07C45/54B01J27/16B01J27/138B01J27/10B01J37/02B01J37/08
CPCY02P20/584
Inventor 罗伟
Owner HUNAN SHINEWAY ENTERPRISE
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