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A method for preparing gallic acid by hydrolysis of hydrochloric acid

A technology of gallic acid and hydrochloric acid, applied in the preparation of carboxylate/lactone, organic chemistry, etc., can solve the problems of high raw material cost, high energy consumption, environmental pollution, etc., and achieve improved hydrolysis recovery rate, reduced consumption, and reduced cost effect

Active Publication Date: 2019-01-22
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

[0003] Acid hydrolysis usually uses components such as sulfuric acid and hydrochloric acid, which are added as a catalyst to realize acid hydrolysis. During the hydrolysis process, the concentration of sulfuric acid or hydrochloric acid used is relatively high, at least reaching a mass concentration of more than 4%. This makes the requirements for the equipment in the hydrolysis process higher and the cost is higher, and in the process of extraction and concentration, the acid volatilizes or remains in the hydrolyzate, and after extraction, it is discharged with the waste liquid, causing environmental pollution
[0004] In addition, the yield and purity of the gallic acid product obtained by acid hydrolysis are poor, and the preparation process is long and the cost is high
[0005] In view of this, some researchers began to consider that in the preparation process of gallic acid hydrolysis, it directly adopts high-pressure water phase without adding catalyst production treatment, so that under high-pressure water phase, it realizes the hydroxide ion or hydrogen ion of water ionization, making the solution After the state of weak acid or weak base appears, the hydrolysis of gallic acid can be realized; however, in the process of treatment, the temperature needs to be increased by more than 160°C, and the pressure is gradually increased with the production of water vapor, so the requirements for equipment are relatively high. High, large energy consumption, making the cost of preparing gallic acid higher
[0006] Furthermore, for alkaline hydrolysis, there are still many defects, such as strong corrosion of equipment, and the need for neutralization reaction treatment, the amount of raw material preparation is large, resulting in high raw material cost and complicated process flow
[0007] The fermentation method is to extract the tannic acid-containing substances, and then use glucose as a carbon source to carry out microbial fermentation treatment. Because the conditions in the fermentation treatment process are relatively harsh, the cost of using this method to prepare gallic acid is relatively high.

Method used

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  • A method for preparing gallic acid by hydrolysis of hydrochloric acid
  • A method for preparing gallic acid by hydrolysis of hydrochloric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Gallnuts from Duyun, Guizhou were selected as raw materials and ground into powder.

[0023] In the reaction kettle, add Galla gall powder 10g, and add hydrolyzate 40mL thereinto, the hydrolyzate is the hydrochloric acid solution that mass concentration is 0.1%, and temperature is 50 ℃. Adjust the pressure of the reactor to 0.002MPa, use a frequency of 5kHz, ultrasonically treat for 20min, and use a filter to separate the solid and liquid to obtain a primary liquid and a primary solid; cool and crystallize the primary liquid until the solid does not increase, and use a filter for secondary separation Separation of secondary solid and liquid to obtain secondary liquid and secondary solid; the secondary solid is dissolved in water at a temperature of 50°C, decolorized by activated carbon, recrystallized at a temperature of 10°C, and dried under a vacuum of 0.02MPa to obtain gall Acid 5.45g.

Embodiment 2

[0025] Gallnuts from Zunyi, Guizhou were selected as raw materials and ground into powder.

[0026] In the reaction kettle, 10 g gallnut powder was added, and 30 mL of a hydrolyzate was added thereto. The hydrolyzate was a hydrochloric acid solution with a mass concentration of 1%, and the temperature was 70° C. Adjust the pressure of the reaction kettle to 0.05MPa, use a frequency of 10kHz, and perform ultrasonic treatment for 80 minutes. Use a filter to separate the solid and liquid to obtain a primary liquid and a primary solid; Separation of secondary solid and liquid to obtain secondary liquid and secondary solid; the secondary solid is dissolved in water at a temperature of 60°C, decolorized by activated carbon, recrystallized at a temperature of 20°C, and dried under a vacuum of 0.08MPa to obtain gall Acid 5.12g.

Embodiment 3

[0028] Gallnuts along the river in Guizhou are selected as raw materials and ground into powder.

[0029] In the reaction kettle, 10 g of Galla gall powder was added, and 50 mL of a hydrolyzate was added thereto. The hydrolyzate was a hydrochloric acid solution with a mass concentration of 0.5%, and the temperature was 60° C. Adjust the pressure of the reactor to 0.03MPa, use a frequency of 7kHz, and ultrasonically treat for 50 minutes. Use a filter to separate the solid and liquid to obtain a primary liquid and a primary solid; cool and crystallize the primary liquid until the solid does not increase, and use a filter for secondary Separation of secondary solid and liquid to obtain secondary liquid and secondary solid; the secondary solid is dissolved in water at a temperature of 55°C, decolorized by activated carbon, recrystallized at a temperature of 15°C, dried under a vacuum of 0.06MPa, and gallium is obtained Acid 5.53g.

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Abstract

The invention relates to the technical field of production of gallic acid through hydrochloric acid hydrolysis, and especially relates to a method for preparing gallic acid through hydrochloric acid hydrolysis. The mass concentration of hydrochloric acid is controlled to be 0.1-1% and the pressure in a reaction kettle is adjusted to 0.02-0.05 MPa to realize synergism in order to improve the hydrolysis recovery rate of gallic acid in a tannin-containing substance, and a subsequent processing technology is combined to make gallic acid have high purity and good quality, so the concentration of hydrochloric acid is effectively reduced, the use amount of hydrochloric acid is reduced, and the cost is reduced.

Description

technical field [0001] The invention relates to the technical field of preparing gallic acid by hydrolysis of hydrochloric acid, in particular to a method for preparing gallic acid by hydrolysis of hydrochloric acid. Background technique [0002] Gallic acid, also known as gallic acid, has a chemical name of 3,4,5-trihydroxybenzoic acid, a molecular weight of 188.4, white needle-like crystals, easily soluble in water, ethanol, glycerin, insoluble in chloroform and benzene, and is widely used In the pharmaceutical, food and electronics industries. In the prior art, in the hydrolysis preparation process of gallic acid, it mainly adopts acid hydrolysis, alkali hydrolysis, fermentation method, etc. to hydrolyze gallic acid in substances containing tannic acid, and then concentrate it, extract and purify it Get the product. [0003] Acid hydrolysis usually uses components such as sulfuric acid and hydrochloric acid, which are added as a catalyst to realize acid hydrolysis. Duri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C65/03C07C51/09
CPCC07C51/09C07C65/03
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