A method for preparing gallic acid and pyrogallic acid from tannin biomass

A technology of pyrogallic acid and gallic acid, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate/lactone, etc., can solve the problems of low yield and purity, and achieve high analytical purity and total The effect of high yield

Active Publication Date: 2018-12-18
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 its yield and purity are not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] This embodiment provides a method for preparing gallic acid and pyrogallic acid from tannin biomass, comprising the following steps:

[0018] 1) Add pulverized tannin-containing biomass, deionized water, absolute ethanol, and formamide into the autoclave, wherein the ratio of tannin-containing biomass, deionized water, absolute ethanol, and formamide is 1: 1:2:0.5; turn on the agitator, raise the temperature to boiling at normal temperature and pressure, and pass in carbon dioxide to replace the air in the reaction kettle; the tannin biomass described is gall or tara

[0019] 2) Close the valve of the reactor, continue to heat up to 170°C, and react for 30 minutes;

[0020] 3) Open the valve of the reaction kettle and protect it with carbon dioxide gas, add formamide of 1 times the amount of the solution, then heat the solution to 110°C, evaporate the deionized water and absolute ethanol, and stop when the content of the two is less than 1%. ;

[0021] 4) Place the so...

Embodiment 2

[0026] This embodiment provides a method for preparing gallic acid and pyrogallic acid from tannin biomass, comprising the following steps:

[0027] 1) Add pulverized tannin-containing biomass, deionized water, absolute ethanol, and formamide into the autoclave, wherein the ratio of tannin-containing biomass, deionized water, absolute ethanol, and formamide is 1: 3:4:1; turn on the agitator, raise the temperature to boiling at normal temperature and pressure, and pass in carbon dioxide to replace the air in the reaction kettle; the tannin biomass described is gall or tara

[0028] 2) Close the valve of the reactor, continue to heat up to 190°C, and react for 60 minutes;

[0029] 3) Open the valve of the reaction kettle, protect it with carbon dioxide gas, add formamide of 1 times the amount of the solution, then heat the solution to 115°C, evaporate the deionized water and absolute ethanol, and stop when the content of the two is less than 1%. ;

[0030] 4) Place the solutio...

Embodiment 3

[0035] This embodiment provides a method for preparing gallic acid and pyrogallic acid from tannin biomass, comprising the following steps:

[0036] 1) Add pulverized tannin-containing biomass, deionized water, absolute ethanol, and formamide into the autoclave, wherein the ratio of tannin-containing biomass, deionized water, absolute ethanol, and formamide is 1: 2: 3: 0.8; turn on the agitator, heat up to boiling at normal temperature and pressure, and pass in carbon dioxide to replace the air in the reactor; the tannin biomass described is gall or tara

[0037] 2) Close the valve of the reactor, continue to heat up to 180°C, and react for 45 minutes;

[0038] 3) Open the valve of the reaction kettle, protect it with carbon dioxide gas, add formamide of 1 times the amount of the solution, then heat the solution to 113°C, evaporate the deionized water and absolute ethanol, and stop when the content of the two is less than 1%. ;

[0039] 4) Place the solution in step 3) in a ...

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Abstract

The invention provides a method for preparing gallic acid and pyrogallic acid with tannin biomass and belongs to the technical field of chemical production. A mixed solution of deionized water, absolute ethyl alcohol and formamide is utilized to carry out acid-base catalysis and special dissolvability in high-temperature liquid state, Chinese gall or tara is enabled to be decomposed into gallic acid or pyrogallic acid to undergo strongly acidic styrene type cation exchange resin reaction in the microwave environment after dehydration and ethanol removal, Chinese gall or tara is enabled to be hydrolyzed fully, and gallic acid and pyrogallic acid products processed via some processing steps are high in analysis purity and total yield. Test proves that the analysis purity of gallic acid and pyrogallic acid products are above 90wt% and 95wt%. Total yield of products is over 75%.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and in particular relates to a method for preparing gallic acid and pyrogallic acid from tannin biomass. Background technique [0002] Gallic acid (Gallic Acid, GA), chemical name 3,4,5-trihydroxybenzoic acid, also known as beilic acid, gallic acid, gallic acid is white or light yellow needle crystal or powder, usually in the form of monohydrate Existence, specific gravity 1.694, melting point 235-240°C. Gallic acid has a wide range of applications and can be used in organic synthesis, coatings, dyes, medicine, food, chemical industry, daily chemicals, agriculture, minerals, etc. It is mainly used in the manufacture of medicines, dyes, and inks, and is also used as food antioxidants and preservatives , metal extractant, ultraviolet absorber, disinfectant, hemostatic astringent, developer, etc. At present, gallic acid is usually prepared from tannin-containing biomass such as gallnut...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/09C07C65/03C07C37/055C07C39/10
CPCC07C37/0555C07C51/09C07C65/03C07C39/10
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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