Method for preparing gallic acid and pyrogallic acid with 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 high yield effect

Active 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

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Problems solved by technology

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Method used

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Examples

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Example Embodiment

[0016] Example one

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

[0018] 1) Add crushed tannin-containing biomass, deionized water, absolute ethanol, and formamide into the autoclave, and the ratio of tannin-containing biomass, deionized water, absolute ethanol, and formamide is 1: 1:2:0.5; turn on the stirrer, heat up to boiling at room temperature and pressure, and introduce carbon dioxide to replace the air in the reactor; the tannin biomass 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 reactor and protect it with carbon dioxide gas, add 1 times the amount of formamide to the solution, then heat the solution to 110°C, evaporate deionized water and absolute ethanol, and stop when the content of both is less than 1% ;

[0021] 4) Place the solution of step 3) in a microwave heater, add 1...

Example Embodiment

[0025] Example two

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

[0027] 1) Add crushed tannin-containing biomass, deionized water, anhydrous ethanol, and formamide into the autoclave, and the ratio of tannin-containing biomass, deionized water, absolute ethanol, and formamide is 1: 3:4:1; turn on the stirrer, heat up to boiling at room temperature and pressure, and pass the air in the carbon dioxide replacement reactor; the tannin biomass 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 reactor and protect it with carbon dioxide gas, add 1 times the amount of formamide to the solution, then heat the solution to 115°C, evaporate deionized water and absolute ethanol, and stop when the content of both is less than 1% ;

[0030] 4) Place the solution of step 3) in a microwave heater, and add 3%...

Example Embodiment

[0034] Example three

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

[0036] 1) Add crushed tannin-containing biomass, deionized water, absolute ethanol, and formamide into the autoclave, and the ratio of tannin-containing biomass, deionized water, absolute ethanol, and formamide is 1: 2:3:0.8; turn on the stirrer, heat up to boiling at room temperature and pressure, and pass the air in the carbon dioxide replacement reactor; the tannin biomass 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 reactor and protect it with carbon dioxide gas, add 1 times the amount of formamide to the solution, then heat the solution to 113°C, evaporate deionized water and absolute ethanol, and stop when the content of both is less than 1% ;

[0039] 4) Place the solution of step 3) in a microwave heater, add 2% ...

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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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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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