CN101125892A - Method for producing aminoglucose hydrochloride - Google Patents
Method for producing aminoglucose hydrochloride Download PDFInfo
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- CN101125892A CN101125892A CNA2007101319029A CN200710131902A CN101125892A CN 101125892 A CN101125892 A CN 101125892A CN A2007101319029 A CNA2007101319029 A CN A2007101319029A CN 200710131902 A CN200710131902 A CN 200710131902A CN 101125892 A CN101125892 A CN 101125892A
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- filtrate
- purifying
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- aminoglucose hydrochloride
- crystallization
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- Polysaccharides And Polysaccharide Derivatives (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a production method of gluvosamine hydrochloride relating to a production technique of chemical raw material. The production method comprises acidolysis, decolouration, press filtration, purification, concentration, crystallization, baking, grinding, cribration, and packaging. In the process of production, the products of the invention regulates the proportion between hydrochloric acid and chitin to 5 to 1 under the temperature of 85 DEG C to 88 DEG C for three hours, activated carbon is added in a reaction container directly to decolor without refrigeration and crystallization, which omits the steps of separation of crude crystallization and water solution, thus saving time and water. The crude liquid after being filtered through a press filter is not directly concentrated but is filtered by ultrafiltration system to remove oil and fat and inorganic salts, which solves the problem of clarity and luminous transmittance of products and improves production quality.
Description
Technical field
The present invention relates to a kind of production technique of industrial chemicals.
Background technology
Glucosamine hydrochloride claims Portugal's amine sugar hydrochloride again, it is a kind of natural mucopolysaccharide, contain a large amount of cellulosics, certified products is a white crystalline powder, pharmaceutically has extensive use, can be used as bacterial-infection resisting and immunological adjuvant, is the activator of human body resisiting influenza virus, also have imitate treatment rheumatic arthritis, strengthen function of human body, the effect of anti-ageing, vessel softening and anti-cancer.Traditional method for producing aminoglucose hydrochloride adopts the chitin acid hydrolyzation usually, as, the patent No. is that preparation method's processing step of the glucosamine hydrochloride of 01127784.X is: acidolysis, filtration, concentrate, purifying, reconcentration, cooling, filtration, sprinkling ethanol, pump ethanol, oven dry is at last made.Though reduced the required consumption of ethanol of washing hydrochloric acid, operational path is long and complicated, can not reach the purpose of low cost production, also can't overcome pollution problems.In addition, owing to adopt big water gaging in the reaction process, complex operation, power consumption is high, quantity of wastewater effluent is big.
Summary of the invention
The object of the invention is to invent the production method of a kind of pollution-free, high quality, low cost production glucosamine hydrochloride.
The present invention includes following steps:
1) acidolysis: below 50 ℃, hydrochloric acid and chitin are dropped into reactor with 5: 1 weight, after material was thrown, the control temperature of reaction kettle was 85 ℃～88 ℃, and is incubated 3 hours, makes crude liquid;
2) decolouring, press filtration: add activated carbon decolorizing in the crude liquid, be cooled to 50 ℃ after, carry out press filtration after, obtain filtrate;
3) purifying: filtrate through two-pass reverse osmosis system purifying, is obtained the filtrate of purifying;
4) concentrate, crystallization: with the filtrate of purifying-0.09～-0.1Mpa pressure, 50～55 ℃ of temperature under Concentrated and crystallized in vacuum, cooling blowing when crystal occurring;
5) with crystal washing earlier, dry then to water content be below 0.5%;
6) pulverize, sieve, pack.
Product of the present invention has been adjusted the ratio of hydrochloric acid and chitin in process of production, be controlled at 5: 1, temperature is controlled at 85 ℃～88 ℃, time was controlled at 3 hours, need not crystallisation by cooling, directly in reaction vessel, add activated carbon decolorizing simultaneously, saved the crude product crystalline and separated and water dissolution, save time and water.Crude liquid does not directly concentrate after pressure filter filters, but grease and inorganic salt are dispeled in filtration through ultrafiltration system, have solved the clarity and the transmittance difficult problem of finished product, have improved quality product.Spissated xln is through washing, oven dry, crushing screening, packing, delivery.
Characteristics of the present invention:
1, non-wastewater discharge
This production technique is not introduced water dissolution, and the acid that participates in reaction is fully recycled, and does not waste and discharges.All water coolants are through air-cooled repeated use, and are not subjected to any pollution to belong to cleaning water.
2, the introducing of hyperfiltration
The purified water treatment unit has been introduced in the filtration of finished product filtrate, and filtrate concentrates behind secondary infiltration purifying.Reverse osmosis unit has been dispeled grease and inorganic salt effectively after repacking, reduced the ash of finished product and eliminated grease, has further improved quality product.
Two-pass reverse osmosis of the present invention system purifying is after earlier filtrate being the membrane filtration of Ф 0.45mm through diameter, to be the membrane filtration of Ф 0.22mm through diameter again.Purpose is fully to remove inorganic salt and impurity, reaches better purifying filter effect.
In addition, in the step 5) of the present invention, remove mother liquor, wash to the crystal look that bleaches with alcohol, then oven dry with centrifuging.Bake out temperature is 90～100 ℃.
Embodiment
Concrete technological operation step:
1, acidolysis
In the reactor that cleans up, drop into 10kg chitin and hydrochloric acid 50kg, temperature is controlled at below 50 ℃.After material has been thrown, be warming up to 85 ℃ of insulations 3 hours, temperature is controlled at 85 ℃～88 ℃.Through acidolysis, make crude liquid.
2, decolouring, press filtration
Directly add the 1kg medicinal carbon and decolour in the 60kg crude liquid, the time was controlled at more than 30 minutes, was cooled to 50 ℃ of press filtrations, and filtrate enters in the middle turning barrel.
3, hyperfiltration
After earlier filtrate being the membrane filtration of Ф 0.45mm through diameter, be the membrane filtration of Ф 0.22mm through diameter again, the filtrate of purifying enters concentrated, and the feed liquid that blowdown goes out is returned decolouring again.
4, concentrated, crystallization
The filtrate of purifying is sucked in the concentration kettle with vacuum, control pressure-0.09～-0.1Mpa, temperature between 50～55 ℃, Concentrated and crystallized in vacuum, cooling blowing when a large amount of crystal.
5, washing, oven dry
Pour crystal into the whizzer mother liquor of leaving away, with twice of alcohol washing to the crystal look that bleaches, put into oven for drying, temperature is controlled at 90～100 ℃, and moisture controlled is below 0.5%.
6, pulverize, sieve
Divide the variable grain degree that the oven dry crystal is sieved according to customer requirement, big particle is pulverized.
7, packing
Press the 25KG/ bucket, double-layer plastic bag packing, outer packaging is a full paper barrel.
Claims (4)
1. method for producing aminoglucose hydrochloride is characterized in that may further comprise the steps:
1) acidolysis: below 50 ℃, hydrochloric acid and chitin are dropped into reactor with 5: 1 weight, after material was thrown, the control temperature of reaction kettle was 85 ℃～88 ℃, and is incubated 3 hours, makes crude liquid;
2) decolouring, press filtration: add activated carbon decolorizing in the crude liquid, be cooled to 50 ℃ after, carry out press filtration after, obtain filtrate;
3) purifying: filtrate through two-pass reverse osmosis system purifying, is obtained the filtrate of purifying;
4) concentrate, crystallization: with the filtrate of purifying-0.09～-0.1Mpa pressure, 50～55 ℃ of temperature under Concentrated and crystallized in vacuum, cooling blowing when crystal occurring;
5) with crystal washing earlier, dry then to water content be below 0.5%;
6) pulverize, sieve, pack.
2. according to the described method for producing aminoglucose hydrochloride of claim 1, it is characterized in that in the step 3) that described two-pass reverse osmosis system purifying is after earlier filtrate being the membrane filtration of Φ 0.45mm through diameter, to be the membrane filtration of Φ 0.22mm through diameter again.
3. according to the described method for producing aminoglucose hydrochloride of claim 1, it is characterized in that removing mother liquor with centrifuging in the step 5), wash to the crystal look that bleaches with alcohol, then oven dry.
4. according to the described method for producing aminoglucose hydrochloride of claim 1, it is characterized in that in the step 5) that bake out temperature is 90～100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101319029A CN101125892A (en) | 2007-09-12 | 2007-09-12 | Method for producing aminoglucose hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101319029A CN101125892A (en) | 2007-09-12 | 2007-09-12 | Method for producing aminoglucose hydrochloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101125892A true CN101125892A (en) | 2008-02-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101319029A Pending CN101125892A (en) | 2007-09-12 | 2007-09-12 | Method for producing aminoglucose hydrochloride |
Country Status (1)
| Country | Link |
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| CN (1) | CN101125892A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550170A (en) * | 2008-04-02 | 2009-10-07 | 徐州海吉亚生物制品有限公司 | Production technology hydrolytically separating glucosamine hydrochloride from mushrooms |
| CN101314609B (en) * | 2008-06-20 | 2010-10-27 | 天津大学 | Process for preparing D-glucosamine hydrochlorate |
| CN101475611B (en) * | 2008-11-20 | 2011-05-11 | 浙江海力生制药有限公司 | Method for preparing high-purity aminoglucose hydrochloride |
| CN101775045B (en) * | 2009-12-07 | 2011-12-07 | 汪昔奇 | Method for preparing glucosamine hydrochloride |
| CN102492000A (en) * | 2011-12-15 | 2012-06-13 | 石狮市华宝海洋生物化工有限公司 | Method for preparing D-glucosamine hydrochloride |
| CN103170155A (en) * | 2013-04-01 | 2013-06-26 | 舟山市普陀新兴医药化工有限公司 | Method for concentrating and crystallizing in reaction kettle |
| CN105218598A (en) * | 2015-11-10 | 2016-01-06 | 扬州日兴生物科技股份有限公司 | Microwave-assisted hydrolysis chitin prepares the method for D-glucosamine hydrochloride |
| CN105237591A (en) * | 2015-11-12 | 2016-01-13 | 扬州日兴生物科技股份有限公司 | Process for preparing glucosamine from chitin through external circulation microwave-assisted acidolysis |
-
2007
- 2007-09-12 CN CNA2007101319029A patent/CN101125892A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550170A (en) * | 2008-04-02 | 2009-10-07 | 徐州海吉亚生物制品有限公司 | Production technology hydrolytically separating glucosamine hydrochloride from mushrooms |
| CN101314609B (en) * | 2008-06-20 | 2010-10-27 | 天津大学 | Process for preparing D-glucosamine hydrochlorate |
| CN101475611B (en) * | 2008-11-20 | 2011-05-11 | 浙江海力生制药有限公司 | Method for preparing high-purity aminoglucose hydrochloride |
| CN101775045B (en) * | 2009-12-07 | 2011-12-07 | 汪昔奇 | Method for preparing glucosamine hydrochloride |
| CN102492000A (en) * | 2011-12-15 | 2012-06-13 | 石狮市华宝海洋生物化工有限公司 | Method for preparing D-glucosamine hydrochloride |
| CN103170155A (en) * | 2013-04-01 | 2013-06-26 | 舟山市普陀新兴医药化工有限公司 | Method for concentrating and crystallizing in reaction kettle |
| CN103170155B (en) * | 2013-04-01 | 2015-02-18 | 舟山市普陀新兴医药化工有限公司 | Method for concentrating and crystallizing in reaction kettle |
| CN105218598A (en) * | 2015-11-10 | 2016-01-06 | 扬州日兴生物科技股份有限公司 | Microwave-assisted hydrolysis chitin prepares the method for D-glucosamine hydrochloride |
| CN105218598B (en) * | 2015-11-10 | 2018-07-20 | 扬州日兴生物科技股份有限公司 | The method that microwave radiation technology hydrolysis chitin prepares D- aminoglucose hydrochlorides |
| CN105237591A (en) * | 2015-11-12 | 2016-01-13 | 扬州日兴生物科技股份有限公司 | Process for preparing glucosamine from chitin through external circulation microwave-assisted acidolysis |
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Open date: 20080220 |