CN102417525A - Preparation method of synthesized D-glucosamine sulfate sodium - Google Patents
Preparation method of synthesized D-glucosamine sulfate sodium Download PDFInfo
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- CN102417525A CN102417525A CN2010102947652A CN201010294765A CN102417525A CN 102417525 A CN102417525 A CN 102417525A CN 2010102947652 A CN2010102947652 A CN 2010102947652A CN 201010294765 A CN201010294765 A CN 201010294765A CN 102417525 A CN102417525 A CN 102417525A
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- sodium sulfate
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- glucosamine
- dissolving
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Abstract
The invention provides a preparation method of a synthesized D-glucosamine sulfate sodium. The method comprises the following steps of dissolving, crystallization and drying. The synthesized D-glucosamine sulfate sodium of the present invention has advantages of simple process flow, low cost and benefit for industrialized production; and the synthesized D-glucosamine sulfate sodium prepared by the method of the invention has high purity, little impurity and good curative effect.
Description
Technical field
The invention belongs to oceanic resources and pharmaceutical chemistry technical field, be specifically related to a kind of preparation method of synthetic D-glucosamine sodium sulfate salt.
Background technology
The glucosamine sulphate of prior art is extremely unstable, has water absorbability, and is oxidized easily.And density is different, degree of uniformity is relatively poor between the GS sodium sulfate salt material of existing employing physical mixed.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of preparation method of synthetic D-glucosamine sodium sulfate salt is provided.
Technical scheme of the present invention is: a kind of preparation method of synthetic D-glucosamine sodium sulfate salt may further comprise the steps:
A, dissolving: in reactor drum, add entry, being heated to temperature is 70 ℃～80 ℃, under agitation condition, adds sodium sulfate; Treat to cool the temperature to 60 ℃～65 ℃ after its dissolving, add the D-glucosamine hydrochloride, continue to stir; Treat after its dissolving solution temperature to be risen to 65 ℃～75 ℃, add organic solvent, be cooled to 15 ℃～25 ℃; Continue to stir 10～15 hours, make all materials in reactor drum, fully react;
B, crystallization: the material that above-mentioned reaction is accomplished is cooled to 0 ℃～-10 ℃, and crystallization is 90～120 minutes under agitation condition, in whizzer, gets the white crystals body then after the centrifuge dehydration;
C, drying: above-mentioned white crystals body after centrifugal is obtained synthetic D-glucosamine sodium sulfate salt after oven dry under the vacuum condition of 55 ℃～65 ℃ of temperature.
Beneficial effect: the preparation method of synthetic D-glucosamine sodium sulfate salt of the present invention has the advantage that technical process is simple, cost is low, help suitability for industrialized production; And high, few, the good effect of impurity of the synthetic D-glucosamine sodium sulfate salt purity of utilizing preparing method's preparation of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is described further:
Embodiment 1
A kind of preparation method of synthetic D-glucosamine sodium sulfate salt may further comprise the steps:
A, dissolving: in reactor drum, add entry, being heated to temperature is 70 ℃, under agitation condition, adds sodium sulfate; Treat to cool the temperature to 60 ℃ after its dissolving, add the D-glucosamine hydrochloride, continue to stir; Treat after its dissolving solution temperature to be risen to 65 ℃, add organic solvent, be cooled to 15 ℃; Continue to stir 10 hours, make all materials in reactor drum, fully react;
B, crystallization: the material that above-mentioned reaction is accomplished is cooled to 0 ℃, and crystallization is 90 minutes under agitation condition, in whizzer, gets the white crystals body then after the centrifuge dehydration;
C, drying: above-mentioned white crystals body after centrifugal is obtained synthetic D-glucosamine sodium sulfate salt after oven dry under the vacuum condition of 55 ℃ of temperature.
Embodiment 2
A kind of preparation method of synthetic D-glucosamine sodium sulfate salt may further comprise the steps:
A, dissolving: in reactor drum, add entry, being heated to temperature is 80 ℃, under agitation condition, adds sodium sulfate; Treat to cool the temperature to 65 ℃ after its dissolving, add the D-glucosamine hydrochloride, continue to stir; Treat after its dissolving solution temperature to be risen to 75 ℃, add organic solvent, be cooled to 25 ℃; Continue to stir 15 hours, make all materials in reactor drum, fully react;
B, crystallization: the material that above-mentioned reaction is accomplished is cooled to-10 ℃, and crystallization is 120 minutes under agitation condition, in whizzer, gets the white crystals body then after the centrifuge dehydration;
C, drying: above-mentioned white crystals body after centrifugal is obtained synthetic D-glucosamine sodium sulfate salt after oven dry under the vacuum condition of 65 ℃ of temperature.
Embodiment 3
A kind of preparation method of synthetic D-glucosamine sodium sulfate salt may further comprise the steps:
A, dissolving: in reactor drum, add entry, being heated to temperature is 75 ℃, under agitation condition, adds sodium sulfate; Treat to cool the temperature to 62 ℃ after its dissolving, add the D-glucosamine hydrochloride, continue to stir; Treat after its dissolving solution temperature to be risen to 70 ℃, add organic solvent, be cooled to 20 ℃; Continue to stir 12 hours, make all materials in reactor drum, fully react;
B, crystallization: the material that above-mentioned reaction is accomplished is cooled to-5 ℃, and crystallization is 105 minutes under agitation condition, in whizzer, gets the white crystals body then after the centrifuge dehydration;
C, drying: above-mentioned white crystals body after centrifugal is obtained synthetic D-glucosamine sodium sulfate salt after oven dry under the vacuum condition of 60 ℃ of temperature.
Claims (1)
1. the preparation method of a synthetic D-glucosamine sodium sulfate salt is characterized in that: may further comprise the steps:
A, dissolving: in reactor drum, add entry, being heated to temperature is 70 ℃～80 ℃, under agitation condition, adds sodium sulfate; Treat to cool the temperature to 60 ℃～65 ℃ after its dissolving, add the D-glucosamine hydrochloride, continue to stir; Treat after its dissolving solution temperature to be risen to 65 ℃～75 ℃, add organic solvent, be cooled to 15 ℃～25 ℃; Continue to stir 10～15 hours, make all materials in reactor drum, fully react;
B, crystallization: the material that above-mentioned reaction is accomplished is cooled to 0 ℃～-10 ℃, and crystallization is 90～120 minutes under agitation condition, in whizzer, gets the white crystals body then after the centrifuge dehydration;
C, drying: above-mentioned white crystals body after centrifugal is obtained synthetic D-glucosamine sodium sulfate salt after oven dry under the vacuum condition of 55 ℃～65 ℃ of temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102947652A CN102417525A (en) | 2010-09-28 | 2010-09-28 | Preparation method of synthesized D-glucosamine sulfate sodium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2010102947652A CN102417525A (en) | 2010-09-28 | 2010-09-28 | Preparation method of synthesized D-glucosamine sulfate sodium |
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| Publication Number | Publication Date |
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| CN102417525A true CN102417525A (en) | 2012-04-18 |
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| CN2010102947652A Pending CN102417525A (en) | 2010-09-28 | 2010-09-28 | Preparation method of synthesized D-glucosamine sulfate sodium |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102850412A (en) * | 2012-10-12 | 2013-01-02 | 江苏澳新生物工程有限公司 | Preparation method of D-glucosamine sulfate sodium chloride salt |
| CN104530144A (en) * | 2014-12-09 | 2015-04-22 | 厦门蓝湾科技有限公司 | Reactor and method for preparing glucosamine sulfate |
| CN110862426A (en) * | 2019-12-09 | 2020-03-06 | 山东润德生物科技有限公司 | Method for preparing high-purity glucosamine sulfate |
| CN114853826A (en) * | 2022-05-12 | 2022-08-05 | 山西辅仁恒峰药业有限公司 | Preparation method of glucosamine sulfate sodium chloride double salt |
-
2010
- 2010-09-28 CN CN2010102947652A patent/CN102417525A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102850412A (en) * | 2012-10-12 | 2013-01-02 | 江苏澳新生物工程有限公司 | Preparation method of D-glucosamine sulfate sodium chloride salt |
| CN102850412B (en) * | 2012-10-12 | 2015-07-22 | 江苏澳新生物工程有限公司 | Preparation method of D-glucosamine sulfate sodium chloride salt |
| CN104530144A (en) * | 2014-12-09 | 2015-04-22 | 厦门蓝湾科技有限公司 | Reactor and method for preparing glucosamine sulfate |
| CN104530144B (en) * | 2014-12-09 | 2017-05-24 | 厦门蓝湾科技有限公司 | Reactor and method for preparing glucosamine sulfate |
| CN110862426A (en) * | 2019-12-09 | 2020-03-06 | 山东润德生物科技有限公司 | Method for preparing high-purity glucosamine sulfate |
| CN114853826A (en) * | 2022-05-12 | 2022-08-05 | 山西辅仁恒峰药业有限公司 | Preparation method of glucosamine sulfate sodium chloride double salt |
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Application publication date: 20120418 |