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Method for preparing aminoglucose hydrochloride

A technology of glucosamine hydrochloride and hydrochloric acid, which is applied in the field of preparation of glucosamine hydrochloride, can solve the problems of reducing product purity, increasing cost, sticking to pans, etc., and achieves improving purity and yield, saving cost and reducing dosage. Effect

Inactive Publication Date: 2008-07-02
谢锐权
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to obtain a relatively high product yield, it is generally achieved by increasing the concentration of hydrochloric acid or increasing the reaction temperature of hydrolysis. In the existing preparation process, the concentration of hydrochloric acid is 36-38%, but glucosamine hydrochloride is at a higher concentration. Under the condition of acid liquid and heat, it will cause complex compound and decomposition reactions, which not only deepens the color of the crude product, but also reduces the purity of the product and the yield of the product; when the concentration of hydrochloric acid decreases, the reaction temperature must be increased, generally to above 95°C-100°C, but blindly increasing the reaction temperature will also cause decomposition reactions, and it is easy to cause sticking phenomenon, which will affect the purity and yield of the product
In addition, the existing preparation process all adopts the method of hydrolyzing and filtering while hot. However, due to the high solubility of oil and impurities at high temperature, the impurities are easily filtered out together with the mother liquor, which not only affects the purity of the product, but also makes the subsequent The decolorization process needs to consume a large amount of activated carbon, which increases the cost of preparation

Method used

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  • Method for preparing aminoglucose hydrochloride

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Embodiment 1

[0022] Weigh 600Kg of chitin and 1200Kg of hydrochloric acid with a concentration of 30%, prepare the vacuum reactor in advance, suck the prepared hydrochloric acid into the reactor, close the feed valve, start stirring, open the feed port, and start to put in chitin. Turn on the steam and raise the temperature to 40°C, stop the steam, close the temperature rise after the feeding is completed, control the vacuum in the reactor to not exceed 0.3MPa, start to calculate the holding time when it reaches 88°C, the holding time is 4.5 hours, open the cooling water inlet and outlet valve, Let the temperature in the kettle drop to 40°C, open the vent valve, and transfer the feed liquid to the double-layer vacuum filtration tank for cooling and crystallization for 3.5 hours. The first layer of filter cloth in the double-layer vacuum filtration tank is 300 mesh, and the second layer of filter cloth 500 mesh; turn on the vacuum pump and open the feed valve, suck the mother liquor into the...

Embodiment 2

[0024] Weigh 300Kg of chitin and 800Kg of hydrochloric acid with a concentration of 32%, prepare the vacuum reactor in advance, suck the prepared hydrochloric acid into the reactor, close the feed valve, start stirring, open the feeding port, and start to put in chitin. Turn on the steam and raise the temperature to 40°C, stop the steam, close the heating after the feeding is completed, control the vacuum in the reactor to not exceed 0.3MPa, and start to calculate the holding time when it reaches 85°C, the holding time is 3.5 hours, open the cooling water inlet and outlet valve, Let the temperature in the kettle drop below 40°C, open the vent valve, and transfer the feed liquid to a double-layer vacuum filter tank for cooling and crystallization for 3.5 hours. The first layer of filter cloth in the double-layer vacuum filter tank is 300 mesh, and the second layer of filter cloth The cloth is 500 mesh; turn on the vacuum pump and open the feed valve, suck the mother liquor into ...

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Abstract

The invention provides a new method that prepares glucosamine hydrochloride by adopting chitosan, which comprises the steps of the hydrolysis of hydrochloric acid, the cooling crystallization of mother liquid, the concentration of filter liquid, the cooling crystallization of concentrated solution, decolorization, the crystallization of decolorized liquid, fining, etc. The preparation method of the invention adopts the cooling crystallization firstly after the hydrolysis and the concentration of filter liquid to cause the glucosamine hydrochloride to be separated from the liquid that contains relatively high impurity content and also cause grease and impurities to be separated and suspended at the top layer of crystalline solids, thus being beneficial for removing the grease and the impurities. The preparation method of the invention can obtain the glucosamine hydrochloride with high purity and high yield in the condition that hydrochloric acid concentration is 30-32 percent and reaction temperature is 85-88 DEG C and greatly reduces the dosage of activated carbon, thus greatly saving manufacturing cost.

Description

technical field [0001] The invention relates to a method for preparing glucosamine hydrochloride, in particular to a method for preparing D-glucosamine hydrochloride from chitin extracted from marine organisms such as shrimp and crab shells. Background technique [0002] Glucosamine hydrochloride (that is, D-glucosamine hydrochloride) is a drug for treating bone and joint diseases and an antibiotic synergist, as well as a sweetener and antioxidant for food, and can also be used as a nutritional supplement for diabetics. It can also inhibit the growth of cancer cells and is the main raw material for the synthesis of new anticancer drug chlorurecin. Glucosamine hydrochloride and its derivatives have broad application prospects in medicine, light industrial cosmetics and other fields. [0003] The method of preparing glucosamine hydrochloride from chitin generally adopts the hydrochloric acid hydrolysis method, that is, adding chitin to a certain concentration of hydrochloric ...

Claims

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Application Information

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IPC IPC(8): C07H5/06
Inventor 谢锐权
Owner 谢锐权
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