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Method for preparing high-purity glucosamine potassium sulfate and application thereof

A technology of glucosamine and potassium sulfate, applied in the field of glucosamine, can solve the problem of low purity of glucosamine sulfate, and achieve the effects of avoiding impurity removal process, controllable reaction process and improved purity

Inactive Publication Date: 2021-01-29
SHANDONG RUNDE BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, glucosamine hydrochloride is obtained by hydrolysis of raw materials such as chitin, and then neutralized by alkaline materials such as sodium hydroxide, but the glucosamine hydrochloride obtained by this method contains a large amount of substances such as sodium chloride , After converting glucosamine hydrochloride into glucosamine sulfate, the above-mentioned sodium chloride, etc. also entered into glucosamine sulfate, resulting in low purity of glucosamine sulfate

Method used

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  • Method for preparing high-purity glucosamine potassium sulfate and application thereof

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Experimental program
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Effect test

Embodiment 1

[0026]A method for preparing high-purity potassium glucosamine sulfate includes the following steps:

[0027](1) Concentrated hydrochloric acid with a mass concentration of 38% was added to the chitin, and then reacted at 105°C for 3.5 hours to fully hydrolyze the chitin, and a pressure of 0.25 MPa was applied during the hydrolysis.

[0028](2) Add activated carbon to the hydrolyzed liquid obtained in step (1) to decolor the hydrolyzed liquid. After 1.2h, the decolorization of the hydrolyzed liquid is completed, and then the hydrolyzed liquid is filtered to remove the activated carbon and other solid substances in the hydrolyzed liquid to obtain the liquid It is the feed liquid containing glucosamine hydrochloride, ready for use.

[0029](3) Add absolute ethanol to the material solution obtained in step (2) and mechanically stir for 35 minutes to mix the two uniformly, then add potassium hydroxide dropwise to neutralize, monitor the pH of the reaction solution during the reaction When the pH...

Embodiment 2

[0033]A method for preparing high-purity potassium glucosamine sulfate includes the following steps:

[0034](1) Concentrated hydrochloric acid with a mass concentration of 38% was added to the chitin, and then reacted at 100° C. for 4.0 hours to fully hydrolyze the chitin, and a pressure of 0.3 MPa was applied during the hydrolysis.

[0035](2) Add activated attapulgite to the hydrolysate obtained in step (1) to decolor the hydrolysate. After 1.4h, the decolorization of the hydrolysate is completed, and then the hydrolysate is filtered to remove the activated attapulgite and other solid substances in the hydrolysate , The obtained liquid is the feed liquid containing glucosamine hydrochloride, ready for use.

[0036](3) Add anhydrous propanol to the material solution obtained in step (2) and mechanically stir for 45 minutes to mix the two uniformly, then add potassium hydroxide dropwise for neutralization, and monitor the reaction solution during the reaction pH, when the pH of the reaction...

Embodiment 3

[0040]A method for preparing high-purity potassium glucosamine sulfate includes the following steps:

[0041](1) Concentrated hydrochloric acid with a mass concentration of 38% was added to the chitin, and then reacted at 90°C for 4.5 hours to fully hydrolyze the chitin, and a pressure of 0.25 MPa was applied during the hydrolysis.

[0042](2) Add active attapulgite to the hydrolyzed solution obtained in step (1) to decolor the hydrolyzed solution. After 1.5h, the decolorization of the hydrolyzed solution is completed, and then the hydrolyzed solution is filtered to remove the active attapulgite and other solid substances in the hydrolyzed solution , The obtained liquid is the feed liquid containing glucosamine hydrochloride, ready for use.

[0043](3) Add anhydrous methanol to the material solution obtained in step (2) and mechanically stir for 45 minutes to mix the two uniformly, then add potassium hydroxide dropwise for neutralization, and monitor the pH of the reaction solution during th...

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Abstract

The invention relates to a method for preparing high-purity glucosamine potassium sulfate, which comprises the following steps: 1) adding hydrochloric acid into chitin, hydrolyzing chitin under the conditions of heating and pressurizing, decolorizing, and separating out hydrolysate, thereby obtaining a glucosamine hydrochloride-containing feed liquid; 2) adding monohydric alcohol into the feed liquid, uniformly mixing, then adding potassium hydroxide for neutralization, and separating out monohydric alcohol in the obtained reaction liquid after the neutralization is finished, so as to obtain potassium glucosamine salt; and 3) mixing the potassium glucosamine salt with a silver sulfate solution, then carrying out solid-liquid separation, adding organic alcohol into the obtained potassium glucosamine sulfate solution, and separating out precipitated solids, thus obtaining the product. According to the method disclosed by the invention, only one impurity of chloride ions is introduced inthe initial hydrolysis process in the whole preparation process of glucosamine potassium sulfate, so that the variety and content of impurities in the preparation process of glucosamine potassium sulfate are greatly reduced, and the purity of the glucosamine potassium sulfate is effectively improved.

Description

Technical field[0001]The invention relates to the technical field of glucosamine, in particular to a method for preparing high-purity potassium glucosamine sulfate and its application.Background technique[0002]The following content in the background art only refers to the information related to the present invention that the inventor understands. It is intended to increase the understanding of the present invention by explaining some basic technical knowledge related to the present invention. This information does not necessarily constitute a Knowledge known to those of ordinary skill in the art.[0003]Glucosamine (Molecular Formula C6H13NO5) Is a natural amino sugar, obtained by refining after the hydrolysis of chitin. It is extremely unstable and needs to be preserved in the form of a salt. Glucosamine sulfate is one of the forms of glucosamine salt. At present, glucosamine hydrochloride is obtained by hydrolyzing raw materials such as chitin and then neutralizing alkaline raw mate...

Claims

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Application Information

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IPC IPC(8): C07H5/06C07H1/06C07H1/00C07H11/00C13K13/00A61P19/02
CPCA61P19/02C07H1/00C07H1/06C07H5/06C07H11/00C13K13/00
Inventor 卢健行刘长峰张新平水清洋卢建功卢建智
Owner SHANDONG RUNDE BIOTECH CO LTD