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A kind of industrial production method of crude glycyrrhizic acid

A production method and technology of glycyrrhizic acid, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of low cold water extraction rate, many extraction impurities, long time consumption, etc., and achieve easy industrial operation and purification process. Simple and easy to operate, the effect of saving purification steps

Active Publication Date: 2018-05-15
CHENGUANG BIOTECH GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of many impurities in alcohol extraction and alkaline water extraction in the existing glycyrrhizic acid production methods, low cold water extraction rate and long time consumption, the present invention provides an industrial production method of crude glycyrrhizic acid, which adopts hot water liquid-solid countercurrent circulation Extraction, which not only reduces water consumption, improves the extraction rate of glycyrrhizic acid, but also avoids excessive impurities from being mixed into the product, and simplifies the purification process route

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 350kg of licorice raw material after wire drawing, the content of glycyrrhizic acid in the raw material is 3.5%, the extraction temperature is 45°C, the number of extraction units is 5, the mass ratio of solid to liquid is 1:6, and each extraction is 1.5h. The extraction rate was 98.6%; the extract was immediately cooled to 20°C, centrifuged after 30 minutes to remove impurities, and then the feed liquid was transferred to the acid sink tank for acid adjustment. The stirring speed during the acid adjustment process was 50 rpm, with 10% Sulfuric acid adjusted the acidity of the feed solution to pH 1.3, and left it to settle for 2 hours.

[0028] Filter the feed liquid plate and frame after acid precipitation. The initial filtration temperature of the feed liquid is 25°C. After 20 minutes of filtration, the temperature of the feed liquid reaches 55°C due to the heat generated by the pump. Then switch to the cooling channel and cool down through the cooling tower for 2...

Embodiment 2

[0031] Take 400kg of powdered licorice raw material after wire drawing, the content of glycyrrhizic acid in the raw material is 2.80%, the extraction temperature is 65°C, the number of extraction units is 5, the mass ratio of solid to liquid is 1:5, each extraction is 1.2h, and a total of 8 pots of glycyrrhizic acid are fed. The extraction yield was 97.9%; the feed liquid was immediately cooled to 15°C, centrifuged after 60 minutes to remove impurities, and then the feed liquid was transferred to an acid sink tank for acid adjustment. The stirring speed during the acid adjustment process was 200 rpm. % hydrochloric acid to acidify the feed solution to pH 1.5, then let it settle for 3 hours.

[0032] Filter the feed liquid plate and frame after acid precipitation. The initial filtration temperature of the feed liquid is 20°C. After 40nin of filtration, the temperature of the feed liquid reaches 51°C due to the heating of the pump, and then switch to the cooling channel, and cool...

Embodiment 3

[0035] Take 700kg of licorice raw material after wire drawing, the content of glycyrrhizic acid in the raw material is 3.81%, the extraction temperature is 80°C, the number of extraction units is 6, the mass ratio of solid to liquid is 1:7, each time of extraction is 1h, and a total of 7 pots are fed, and the glycyrrhizic acid is extracted rate of 97.0%; the feed liquid was immediately cooled to 20°C, centrifuged after 1.5 hours to remove impurities, and then the feed liquid was transferred to an acid sink tank for acid adjustment. The stirring speed during the acid adjustment process was 100 rpm, with 30% After adjusting the feed solution to pH 1.7 with sulfuric acid, let it settle for 2.5 hours.

[0036] Filter the feed liquid plate and frame after acid precipitation. The initial filtration temperature of the feed liquid is 25°C. After 30 minutes of filtration, the temperature of the feed liquid reaches 58°C due to the heating of the pump, and then switch to the cooling chann...

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Abstract

The invention discloses an industrial production method of rough glycyrrhizic acid. The industrial production method comprises the following steps: drawing liquorice roots into shreds or powder through a drawing machine; extracting by taking hot water as an extracting solvent to obtain an extracting solution; cooling extracted material liquid; after finishing cooling, centrifuging to obtain clarified material liquid; carrying out acid regulation on the centrifuged material liquid in an acid tank; after finishing the acid regulation, standing and carrying out acid precipitation for 2h to 5h; filtering material liquid subjected to the acid precipitation; washing a filtered solid with water to obtain a wet product; drying the wet product to obtain a rough glycyrrhizic acid product. By adopting hot water countercurrent circular extraction and combining a cooling and impurity removing process, a water resource is saved and the extraction rate of the product is guaranteed; a post-period purification process is simple and easy to operate and the unit content of the obtained rough glycyrrhizic acid product is more than or equal to 45 percent; industrial production is easy to realize.

Description

technical field [0001] The invention belongs to the technical field of natural extracts, in particular to an industrial production method of crude glycyrrhizic acid. Background technique [0002] Glycyrrhizic acid is the main compound in licorice. At present, glycyrrhizic acid is mainly used in food, medicine, daily chemical and other fields, and has good physiological functions. [0003] At present, there are many ways to extract glycyrrhizic acid. The main extraction solvents are dilute alcohol solution, dilute ammonia water and ammoniacal ethanol solution. Extraction with these solvents will cause a large amount of impurity components to be extracted, which will burden the purification of later products. For example, in the patent with publication number CN102304165A, dilute alcohol is used as the solvent for the extraction of glycyrrhizic acid, and ion exchange resin is needed for purification in the later stage, which not only wastes time but also has the risk of solven...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/08
CPCC07H1/08C07H15/256C07J63/008
Inventor 张志明杨香瑜额尔敦巴雅尔安晓东连运河
Owner CHENGUANG BIOTECH GRP CO LTD
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