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Preparation method for glucosamine sulfate double salt

A technology of glucosamine sulfate and glucosamine hydrochloride, which is applied in the field of glucosamine sulfate, can solve problems such as high production cost and cumbersome process, and achieve the effects of reducing production cost, shortening process steps, and simplifying the preparation process

Inactive Publication Date: 2020-06-05
厦门蓝湾科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of complicated technical process and high production cost in the prior art, and provide a method for preparing a glucosamine sulfate double salt with simple process steps and low cost, which can achieve a higher yield

Method used

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  • Preparation method for glucosamine sulfate double salt
  • Preparation method for glucosamine sulfate double salt

Examples

Experimental program
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Effect test

Embodiment 1

[0022] In a glass reactor, add 5kg of 31% concentrated hydrochloric acid, then add 2kg of chitin, heat to 85°C, react for 5h, filter under reduced pressure while hot, cool the filtrate to room temperature, and then filter under reduced pressure to obtain crude crystals of glucosamine hydrochloride, 75 Wash the crystals with 1% ethanol until the filtrate is colorless. After vacuum drying (50°C, vacuum degree is -0.1MPa), it is detected that the crystals contain 1.43kg of glucosamine hydrochloride, add 2.8kg of 70°C water to dissolve, add 3.6g of activated carbon and stir for 15min. Filtrate under reduced pressure while it is hot, cool down to 55±5°C, add 0.37kg of sodium sulfate, stir for 2 hours, add 7.1L of absolute ethanol to precipitate crystals, cool down to 10°C, centrifugally filter, and vacuum dry (40°C, vacuum degree - 0.1MPa) to 1.27kg white glucosamine sulfate sodium chloride crystals, the yield is 35.5%, and the content is 99.1%.

Embodiment 2

[0024] In a glass reactor, add 5kg of 34% concentrated hydrochloric acid, then add 2kg of chitin, heat to 90°C, react for 4h, filter under reduced pressure while hot, cool the filtrate to room temperature, and then filter under reduced pressure to obtain crude crystals of glucosamine hydrochloride, 85 % of ethanol to wash the crystals until the filtrate is colorless, after vacuum drying (55°C, vacuum degree is -0.09MPa), it is detected that the crystals contain 1.56kg of glucosamine hydrochloride, add 3.1kg of 80°C water to dissolve, add 7.8g of activated carbon and stir for 20min, Filtrate under reduced pressure while it is hot, cool down to 55±5°C, add 0.43kg of sodium sulfate, stir for 3 hours, add 12.5L of absolute ethanol to precipitate crystals, cool down to 15°C, vacuum dry after centrifugal filtration (45°C, vacuum degree -0.09 MPa) to obtain 1.56kg of white glucosamine sulfate sodium chloride crystals, with a yield of 43.6% and a content of 99.8%.

Embodiment 3

[0026] In a glass reactor, add 5kg of 36% concentrated hydrochloric acid, then add 2kg of chitin, heat to 95°C, react for 3h, filter under reduced pressure while hot, cool the filtrate to room temperature, and then filter under reduced pressure to obtain crude crystals of glucosamine hydrochloride, 95 % of ethanol to wash the crystals until the filtrate is colorless, after vacuum drying (60°C, vacuum degree is -0.08MPa), it is detected that the crystals contain 1.52kg of glucosamine hydrochloride, add 3.0kg of 85°C water to dissolve, add 15.2g of activated carbon and stir for 25min, Filtrate under reduced pressure while it is hot, cool down to 55±5°C, add 0.44kg of sodium sulfate, stir for 2 hours, add 15.2L of absolute ethanol to precipitate crystals, cool down to 10°C, and vacuum dry after centrifugal filtration (50°C, vacuum degree -0.08 MPa) to obtain 1.69kg of white glucosamine sulfate sodium chloride crystals, with a yield of 47.2% and a content of 98.9%.

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Abstract

The invention discloses a preparation method for glucosamine sulfate double salt, and relates to glucosamine sulfate. The preparation method comprises the following steps: 1) adding chitin into concentrated hydrochloric acid with a mass accounting for 2.5 times of the mass of the chitin, and carrying out a reaction under heating; 2) carrying out filtering while an obtained solution is hot under reduced pressure, and cooling a filtrate to a room temperature; 3) carrying out reduced pressure filtration on the filtrate again, and washing an obtained crystal with ethanol with a concentration of 75% or more until the filtrate is colorless; 4) drying the crystal in vacuum, and detecting the content of the glucosamine hydrochloride in the crystal; 5) adding hot water for dissolving, then adding active carbon, carrying out stirring and decolorizing for 15-25 minutes, and carrying out filtering while a solution is hot; 6) cooling a filtrate to 50 to 60 DEG C, adding a sulfate solid, carrying out stirring for 2-3 hours, adding absolute ethyl alcohol to separate out a crystal; and 7) carrying out cooling to 10-20 DEG C, and carrying out centrifugal filtering and vacuum drying so as to obtaina white crystal. The preparation method provided by the invention is simple in process and high in yield, can integrally reduce the production cost of the glucosamine sulfate double salt, and is applicable to large-scale industrial production.

Description

technical field [0001] The invention relates to glucosamine sulfate, in particular to a preparation method of glucosamine sulfate double salt. Background technique [0002] Glucosamine sulfate is mainly used for the treatment of osteoarthritis, and is widely used in medicine, health food, food and other fields. Currently, the glucosamine sulfate that has been on the market is mainly glucosamine sulfate double salt and glucosamine sulfate without metal salts. Due to its better stability, glucose double salt has become the main glucosamine sulfate product in the current market, which is mainly divided into glucosamine sulfate sodium chloride double salt and glucosamine sulfate potassium chloride double salt. [0003] According to existing literature, as the preparation method of U.S. Patent (US5847107) glucosamine sulfate double salt mainly is to utilize glucosamine hydrochloride and sulfate to add water to dissolve, then add organic reagent to separate out crystal and obtain,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/06C07H1/06C07H1/00
CPCC07H1/00C07H1/06C07H5/06
Inventor 林颖珺朱浩邓美健张倩赵坐都张慧兰周炜方建华张水兰黄建波
Owner 厦门蓝湾科技有限公司
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