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Method for preparing gallic acid by sulfuric acid hydrolysis

A technology for hydrolysis of gallic acid and sulfuric acid, which is applied in the preparation of carboxylate/lactone, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems such as the inability to meet the demand of gallic acid, Achieve the effect of reducing decolorization treatment time, improving yield, and avoiding excessive hydrolysis

Inactive Publication Date: 2016-11-23
遵义市倍缘化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But in spite of this, it still can not meet the market demand for gallic acid, so that the production process of gallic acid needs to be further improved, so that the production process of gallic acid can be generalized, routine, and the yield and activity of gallic acid etc. are better; meanwhile, this is also the direction that those skilled in the art are constantly pursuing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Grind 1kg gallnut, add it to a high-pressure reactor, add 2.5L of water, heat up to boiling, and add a compound mixture of sulfuric acid with a mass concentration of 1% and tartaric acid with a mass concentration of 3%, and mix and add it according to the ratio of 1kg of sulfuric acid and 3kg of tartaric acid , the addition amount of the mixture is 2% of the water quality, stirring while adding, after the addition is completed, seal the reaction kettle, control the temperature at 100 ° C, react for 2 hours, and heat filter to obtain the filtrate and filter residue; the filtrate is cooled and crystallized, filtered, The solid and liquid are obtained, the liquid is returned and mixed with water and added to the reactor, the solid is dissolved in hot water, decolorized by activated carbon adsorption, filtered, crystallized, and dried under a vacuum of 0.02 MPa.

[0022] The crude product yield of gallic acid is 59.6%, the crude product yield of gallic acid by the simple sul...

Embodiment 2

[0024] Grind 1kg gallnut, add it to a high-pressure reactor, add 3.5L of water, heat up to boiling, and add a compound mixture of sulfuric acid with a mass concentration of 20% and tartaric acid with a mass concentration of 3%, and mix and add it according to the ratio of 1kg of sulfuric acid and 7kg of tartaric acid , the addition of the mixture is 4% of the water quality, stirring while adding, after the addition is completed, seal the reactor, control the temperature at 130 ° C, react for 4 hours, and heat filter to obtain the filtrate and filter residue; the filtrate is cooled and crystallized, filtered, Obtain solid and liquid, return the liquid and mix it with water and add it to the reaction kettle. After the solid is dissolved in hot water, it is decolorized by activated carbon adsorption, filtered, crystallized, and dried under a vacuum of 0.08 MPa.

[0025] The crude product yield of gallic acid is 58.3%, the crude product yield of gallic acid by the simple sulfuric a...

Embodiment 3

[0027] Grind 1kg of tara, add it to a high-pressure reaction kettle, add 3L of water, heat up to boiling, and add a compound mixture of sulfuric acid with a mass concentration of 10% and tartaric acid with a mass concentration of 3%, and mix and add it according to the ratio of 1kg of sulfuric acid and 5kg of tartaric acid , the addition of the mixture is 3% of the water quality, stirring while adding, after the addition is completed, seal the reactor, control the temperature at 110 ° C, react for 3 hours, and heat filter to obtain the filtrate and filter residue; the filtrate is cooled and crystallized, filtered, The solid and liquid are obtained, the liquid is returned and mixed with water and added to the reactor, the solid is dissolved in hot water, decolorized by activated carbon adsorption, filtered, crystallized, and dried under a vacuum of 0.06 MPa.

[0028] The crude product yield of gallic acid is 58.7%, the crude product yield of gallic acid by the simple sulfuric ac...

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PUM

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Abstract

The invention relates to the technical field of gallic acid prepared by sulfuric acid hydrolysis, in particular to a method for preparing the gallic acid by the sulfuric acid hydrolysis. Composite catalysts are added, so that reaction conditions are tenderly treated, improper control in the simple sulfuric acid hydrolysis process is effectively controlled, excessive hydrolysis is avoided, the impurity appearance rate of the gallic acid caused by carbonization or other reasons is reduced, a large number of steps removing impurities for the gallic acid are avoided, discoloration treatment time is shortened, production cycle is shortened, the yield of the gallic acid is improved, and production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of preparing gallic acid by hydrolysis of sulfuric acid, in particular to a method for preparing gallic acid by hydrolysis of sulfuric acid. Background technique [0002] Gallic acid, also known as gallic acid, chemically named as 3, 4, 5-trihydroxybenzoic acid, is a white or light yellow needle crystal or powder, is an important chemical raw material, and is widely used in the market, such as organic synthesis , coatings, dyes, medicines, food, daily chemicals and so on. In the prior art, the production of gallic acid is mainly obtained by hydrolyzing gallnuts and tara as raw materials by chemical hydrolysis. The most chemical hydrolysis methods here are acid hydrolysis and alkali hydrolysis. [0003] Acid hydrolysis is to directly use sulfuric acid to hydrolyze tannic acid in gallnuts. The auxiliary materials used in the hydrolysis process are few, the purity is high, and the gallic acid has strong activ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/09C07C65/03B01J31/04B01J27/10
CPCC07C51/09B01J27/02B01J27/10B01J31/04B01J35/19C07C65/03
Inventor 张基明杨长满杨金明蒋家均胡敬
Owner 遵义市倍缘化工有限责任公司
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