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A kind of preparation method of glucosamine sulfate

A technology of glucosamine sulfate and bisulfate, which is applied in the field of electrochemical analysis and detection, can solve problems such as damage to the environment and workers' health, consumption of large organic solvents, and difficulty in stable production, so as to save costs, shorten reaction time, and improve catalytic performance. outstanding effect

Inactive Publication Date: 2011-12-14
青州市瑞鑫再生资源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the former production process, hydrochloric acid is used when preparing glucosamine hydrochloride. The pollution caused by hydrochloric acid mist damages the environment and the health of workers. After ion exchange, the mixture needs to be dried by freeze-drying method. Because it contains acetone, it is difficult to freeze-dry, so it is difficult to industrialize large-scale production; the organic strong alkali method first converts glucosamine hydrochloride into glucosamine base, and controls the fuming sulfuric acid by adjusting the pH. The amount of addition, the composition of glucosamine sulfate prepared by each batch is different, and it is difficult to stabilize the production
And use sulfuric acid to directly degrade, this method consumes a large amount of organic solvents, the production cost is higher, and the residual organic solvents and non-monosaccharide compound components greatly affect the purity of the product, and there are still key technologies to be broken through as health care products and pharmaceutical applications. A large amount of concentrated sulfuric acid in production will corrode the reactor, and it is difficult to recover

Method used

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  • A kind of preparation method of glucosamine sulfate
  • A kind of preparation method of glucosamine sulfate
  • A kind of preparation method of glucosamine sulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Weigh 10Kg of chitosan (Aladdin Reagent (Shanghai) Co., Ltd., specification: low viscosity), add 50 liters of 1-H-3-methylimidazolium bisulfate ionic liquid into the vacuum reactor, and heat up to about 55°C , start the stirring, open the feeding port, put the chitosan into it, and add 50Kg distilled water, gradually heat up and stir to make the chitosan dissolve, control the reaction temperature at 90°C, and keep the reaction time for 3.5 hours. After the hydrolysis was completed, 100 grams of activated carbon passed through a 100-mesh sieve was put in and decolorized at 80° C. for 1 hour. Transfer the decolorized feed liquid to a vacuum suction filter tank for suction filtration, then transfer the filtrate to a vacuum concentration kettle, control the temperature at 83°C, and concentrate to remove all water, add 3 times the volume of absolute ethanol to the concentrated liquid, Turn on the stirring and stir thoroughly for 1.5 hours, and let it stand at room temperatur...

Embodiment 2

[0034] Weigh 10Kg of chitosan, add 35 liters of 1-propylsulfonate-3-methylimidazolium bisulfate ionic liquid into the vacuum reactor, heat up to 60°C, start stirring, open the feeding port, and the chitosan Add sugar, and add 30Kg distilled water, gradually raise the temperature and stir to dissolve the chitosan, control the reaction temperature to 80°C, and keep the reaction time for 2.5 hours. After the hydrolysis was completed, 150 grams of activated carbon passing through a 100-mesh sieve was put into the mixture and decolorized at 85° C. for 1.5 hours. The decolorized feed liquid is transferred to a vacuum filtration tank for suction filtration, and the filtrate is then transferred to a vacuum concentration kettle, and the temperature is controlled at 93°C for concentration to remove all water. Add 3 times the volume of methanol to the concentrated solution, start the stirring and stir thoroughly for 1.5 hours, and let it stand at room temperature for 2 hours, crystalliza...

Embodiment 3

[0041] Weigh 10Kg of chitosan, add 40 liters of 1-butyl-3-methylimidazolium bisulfate ionic liquid into the vacuum reactor, heat up to about 55°C, start stirring, open the feeding port, and put chitosan into , and add 60Kg of distilled water, gradually increase the temperature and stir to dissolve the chitosan, control the reaction temperature to 100° C., and keep the reaction time for 2.0 hours. After the hydrolysis was completed, 50 grams of activated carbon passed through a 150-mesh sieve was put in and decolorized at 80° C. for 1.5 hours. The decolorized feed liquid is transferred to a vacuum filter tank for suction filtration, and the filtrate is then transferred to a vacuum concentration kettle, and the temperature is controlled at 80°C for concentration to remove all water. Add 2 times the volume of acetone to the concentrated solution, turn on the stirring and stir thoroughly for 1.5 hours, and let it stand at room temperature for 3 hours, crystals precipitate out, and...

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Abstract

The invention provides a preparation method of glucosamine sulfate. According to the hydrolysis in the preparation method, chitosan and a bisulfate-containing acidic ionic liquid undergo a hydrolysis reaction in water for 2-5 hours, wherein the quality and volume ratio of chitosan to the bisulfate-containing acidic ionic liquid is 1:3-5, the water amount is 3-6 times the weight of chitosan, and the reaction temperature is 80-140 DEG C. According to the method, there is no acid fog and tail gas during the production process; and the product contains no chloride ion and is safe with no pollution. With the use of the bisulfate-containing acidic ionic liquid, the reaction time is short, the yield is high, the ionic liquid can be repeatedly used, the whole production technology is simple, the purity and the yield of the product obtained is high, the cost is low, and the preparation method provided by the invention is a green, environmentally friendly and high efficient production technology.

Description

technical field [0001] The invention belongs to the technical field of electrochemical analysis and detection, and in particular relates to a preparation method of glucosamine sulfate. Background technique [0002] There are currently 355 million people with arthritis worldwide. In Asia, one out of every six people suffers from arthritis, the world's number one disabling disease, at some point in their life. At present, it is estimated that there are more than 100 million arthritis patients in mainland China, and the number is still increasing . Severe pain can lead to loss of working ability, which is a major damage to social development and human health. [0003] Glucosamine sulfate can significantly relieve the pain of arthritis and rheumatism patients and improve, prevent, treat and repair connective tissue damage. It also has certain curative effect on bone and arthritis inflammation, and also helps the healing of acute and chronic inflammation. Therefore, It also ha...

Claims

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Application Information

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IPC IPC(8): C07H5/06C07H1/00B01J31/02
Inventor 胡燚黄和贾儒
Owner 青州市瑞鑫再生资源科技有限公司
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