Preparation method of potassium glycyrrhizate

Abstract

The invention discloses a preparation method of potassium glycyrrhizate. According to special physicochemical properties of glycyrrhizic acid, glycyrrhizic acid crude powder is used as a raw material and undergoes extraction, decoloring and ammonification; and through specific resin conversion equipment and by the ion replacement principle, potassium glycyrrhizate which has good color and high content and meets the industrial standard is produced. In comparison with the prior art, the invention has the following obvious advantages: a) the technology is novel and simple to operate, is energy-saving and environment friendly and has strong practicality; b) by a resin tank direct stirring treatment mode, the preparation method is operated directly at normal temperature; after a solid intermediate product which is insoluble in a high-concentration alcoholic solution is directly contacted with resin, the solid intermediate product is gradually converted to alcohol-soluble glycyrrhizic acid through resin conversion effect; by the method, feeding quantity is increased, the flow of firstly dissolving and then passing through a resin column is avoided so as to greatly save the operation period, efficiency is raised, and characteristics are good; and c) advantages of an ion exchange resin technology are fully applied, equipment and material costs are low, handling capacity is large, the product has good chroma and high yield and content and is suitable for industrial production, and the product has excellent color, uniform crystal and good quality.

Description

technical field [0001] The invention relates to the field of compound preparation, in particular to a preparation method of potassium glycyrrhizinate. Background technique [0002] Potassium glycyrrhizinate is widely used in medicine, food, cosmetics and other industries, and the market demand is relatively large. At present, there are not many preparation methods of potassium glycyrrhizinate reported in literature and patents. In general, it is mainly through potassium solution and glycyrrhizic acid. Monoammonium salt reaction is made, as in the patent that is called as " the production technology and application of tripotassium glycyrrhizinate " in the application number 00119121.7, the production technology of the disclosed tripotassium glycyrrhizinate is: place crude glycyrrhizic acid in Add ethanol to the reaction kettle in a ratio of 1:3, heat and react at 50°C to 60°C for 6 to 8 hours, cool, vacuum filter, wash the filter cake with ethanol, drain, discard the filter r...

AI Technical Summary

Problems solved by technology

Although this method uses a new technology of resin conversion, it needs to use a higher temperature to dissolve the monoammonium salt raw material before processing, but it will often freeze and condense during the production process, and the resin will be damaged if the temperature is too high; In addition, the cycle of resin column treatment and regeneration is long, which indirectly leads to an increase in cost

In the patent titled "A Preparation Method of Glycyrrhizic Acid Monopotassium Salt or Dipotassium Salt" with the application number 201510005226.5, a method for preparing glycyrrhizic acid potassium salt is disclosed by using the mother liquor produced from the production of glycyrrhizic acid monoammonium salt as raw material. Although the method is also through resin conversion, the actual content of glycyrrhizic acid in the mother liquor involved in this method is very low and there are many impurities. Although the final product has no difference in content when detected by ultraviolet light, it is found by HPLC that it has The content of glycyrrhizic acid is low, which is far from enough to meet the requirements of most customers in the market; in addition, the strength of the resin used in this invention patent is low, and it is difficult to withstand repeated stirring operations for a long time, and the processing and regeneration of the resin column The long cycle also indirectly leads to an increase in cost

[0003] In summary, most of the currently disclosed preparation methods for potassium glycyrrhizinate are prepared by direct chemical reaction, and have high requirements for raw materials. Monoammonium salt is often used as the starting raw material, which has high cost and cannot fully meet the requirements of industrial production.

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