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Preparation method of pyrogallic acid

A technology for pyrogallic acid and gallic acid, which is applied in the field of preparation of pyrogallic acid, can solve the problems of insufficient purity and low yield of pyrogallic acid, and achieves the effects of good product quality, easy operation and low energy consumption

Active Publication Date: 2016-12-07
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

But existing technology, the pyrogallic acid yield of its output is not high, and purity is not enough

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The present embodiment provides a kind of preparation method of pyrogallic acid, comprises the following steps:

[0020] 1) Mix anhydrous gallic acid with N,N-dimethylformamide, absolute ethanol, and polypyrrole in a ratio of 1:1:2:0.1 to obtain a mixed solution; then add 5% of the weight of the mixed solution in benzene Iron sulfonate; then place it in a tubular reaction vessel, and continuously pass an electric current to the solution, with a current intensity of 0.1A; and heat the mixed solution to 50°C, and react for 20minh;

[0021] 2) Put the mixed solution in a heating container, protect it with carbon dioxide gas, heat and concentrate, and concentrate to obtain a solid; the concentration is as follows: heat the solution until it boils and concentrate, and when it is concentrated to 1 / 5 of the original, add 5 times the amount ethanol; repeat "heating to boiling concentration—adding ethanol" more than three times; after adding ethanol for the last time, the soluti...

Embodiment 2

[0024] The present embodiment provides a kind of preparation method of pyrogallic acid, comprises the following steps:

[0025] 1) Mix anhydrous gallic acid with N,N-dimethylformamide, absolute ethanol, and polypyrrole in a ratio of 1:3:4:0.3 to obtain a mixed solution; then add 15% of the weight of the mixed solution in benzene Iron sulfonate; then place it in a tubular reaction vessel, continuously pass an electric current to the solution, and the current intensity is 0.5A; and heat the mixed solution to 70°C, and react for 3h;

[0026] 2) Put the mixed solution in a heating container, protect it with carbon dioxide gas, heat and concentrate, and concentrate to obtain a solid; the concentration is as follows: heat the solution until it boils and concentrate, and when it is concentrated to 1 / 5 of the original, add 5 times the amount ethanol; repeat "heating to boiling concentration—adding ethanol" more than three times; after adding ethanol for the last time, the solution is ...

Embodiment 3

[0029] The present embodiment provides a kind of preparation method of pyrogallic acid, comprises the following steps:

[0030] 1) Mix anhydrous gallic acid with N,N-dimethylformamide, absolute ethanol, and polypyrrole in a ratio of 1:2:3:0.2 to obtain a mixed solution; then add 10% of the weight of the mixed solution in benzene Iron sulfonate; then place it in a tubular reaction vessel, continuously pass an electric current to the solution, and the current intensity is 0.3A; and heat the mixed solution to 60°C, and react for 2h;

[0031] 2) Put the mixed solution in a heating container, protect it with carbon dioxide gas, heat and concentrate, and concentrate to obtain a solid; the concentration is as follows: heat the solution until it boils and concentrate, and when it is concentrated to 1 / 5 of the original, add 5 times the amount ethanol; repeat "heating to boiling concentration—adding ethanol" more than three times; after adding ethanol for the last time, the solution is ...

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Abstract

The invention provides a preparation method of pyrogallic acid, belonging to the technical field of manufacturing in chemical industry. The method comprises the following steps: by using N,N-dimethylformamide and anhydrous ethanol as a solvent, adding conductive high-polymer polypyrrole and an oxidizer iron benzenesulfonate, and carrying out reaction at 50-70 DEG C under the action of electric current to remove decarboxyl. The method has the characteristics of high yield of the product pyrogallic acid, low energy consumption, favorable product quality and the like, and is simple to operate. The high-temperature evaporative concentration step can effectively remove N,N-dimethylformamide, polypyrrole and iron benzenesulfonate in the pyrogallic acid. Thus, the purity of the pyrogallic acid is 95% or above.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and in particular relates to a preparation method of pyrogallic acid. Background technique [0002] Pyrogallol acid, also known as pyrogallol, pyrogallol, and 1,2,3-pyrogallol, is a white needle-like crystal with a specific gravity of 1.453 (4 / 4°C) and a melting point of 131-133°C , with a boiling point of 309°C, sublimates without decomposing when heated slowly, easily oxidized, easily soluble in water, ethanol and ether, insoluble in benzene, xylene and other solvents. [0003] Pyrogallic acid is an important fine chemical and chemical reagent, which is widely used in light industry, food, organic synthesis, synthetic medicine, dyestuff and other industries. and chemical analysis reagents, etc. [0004] The preparation of pyrogallic acid mainly includes gallic acid decarboxylation and chemical synthesis. The decarboxylation of gallic acid to produce pyrogallic acid mainly uses ga...

Claims

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Application Information

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IPC IPC(8): C07C37/50C07C39/10C25B3/00
CPCC07C37/50C25B3/00C07C39/10
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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