CN102464679A - Production process for preparing high-purity D-glucosamine hydrochloride from citric acid fermentation residues - Google Patents
Production process for preparing high-purity D-glucosamine hydrochloride from citric acid fermentation residues Download PDFInfo
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- CN102464679A CN102464679A CN2010105330620A CN201010533062A CN102464679A CN 102464679 A CN102464679 A CN 102464679A CN 2010105330620 A CN2010105330620 A CN 2010105330620A CN 201010533062 A CN201010533062 A CN 201010533062A CN 102464679 A CN102464679 A CN 102464679A
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Abstract
The invention discloses a production process for preparing high-purity D-glucosamine hydrochloride from citric acid fermentation residues. The production process comprises the following steps of: performing acid treatment on the citric acid fermentation residues; filtering; hydrolyzing; filtering; concentrating; filtering; dissolving for decoloring; filtering; performing nanofiltration; concentrating; performing alcohol precipitation; performing centrifugal filtering; and drying to obtain the high-purity D-glucosamine hydrochloride. Due to the adoption of the process disclosed by the invention, impurities such as inorganic salts and the like in a product can be removed effectively, the content of ignition residues is lower than 0.1 percent, the application range is wider, the added value is higher, recycling of wastes is realized, and great economic benefit and social benefit are achieved.
Description
Technical field
The present invention relates to a kind of production technique for preparing the high-purity aminoglucose hydrochloride in vegetalitas source, especially relate to a kind of production technique of utilizing the citric acid fermentation slag to prepare high-purity aminoglucose hydrochloride.
Background technology
Glucosamine hydrochloride, odorlessness, slightly pleasantly sweet, soluble in water, be slightly soluble in methyl alcohol, be insoluble to organic solvents such as ethanol.It has the important physical function to human body, has the anti-inflammatory liver protection effect, stimulates divergent bacillus growth in the baby intestinal, and treatment rheumatism joint inflammation and stomach ulcer are had good curative effect.Glucosamine hydrochloride is a kind of medicine intermediate, is the main raw material of synthetic antibiotic and cancer therapy drug NSC-178248.Also can be applicable to food, in makeup and the fodder additives, purposes is quite extensive.
Raw material sources character according to preparation is divided, and the suitability for industrialized production glucosamine hydrochloride mainly contains two kinds of animal source and plant-sourceds at present.Wherein the animality source mainly is from the shell of crustacean, to extract.This raw material is confined to the coastland, and receives the influence in season bigger, and corrupt owing to organizing in the production process, in the acidolysis alkaline hydrolysis, causes severe contaminations such as stench, waste liquid easily.Along with the change, particularly developed countries such as Japan, America and Europe of the environmental consciousness enhancing and the consumption consciousness, the ammonia sugar hydrochloride pay attention to day by day that people obtain the vegetalitas source, demand grows with each passing day.The glucosamine hydrochloride of plant origin is developed research and utilization, become the focus of current field of medicine and chemical technology research.
The correlative study report and the patent that have the glucosamine hydrochloride of originating about vegetalitas are both at home and abroad at present delivered, and raw material mainly contains fungi, aspergillin, mucormycosis, penicillium spp, oyster cap fungus solid fermentation material, Streptomycin sulphate waste residue, citric acid fermentation slag etc.Make a general survey of the correlative study report and the patent report situation that can find both at home and abroad, do not have to find to prepare the performance of content at 99% above high-purity aminoglucose hydrochloride.Tracing it to its cause, is not have effectively to remove inorganic salt impurity wherein, causes the residue on ignition of products obtained therefrom to exceed standard.
Summary of the invention
The purpose of this invention is to provide a kind of content of product that can make and prepare the production technique of high-purity aminoglucose hydrochloride up to the citric acid fermentation slag that utilizes more than 99%.
The problem that will solve required for the present invention is to realize through following technical scheme: it may further comprise the steps: (1) s.t.: use concentration is 1～10% hydrochloric acid soln immersion citric acid fermentation slag; The volume of hydrochloric acid soln and the weight ratio of fermentation residue are 1～6: 1; Soak time is 0.5～4 hour; Centrifuging, and with the suitable quantity of water washing, filter cake is subsequent use; (2) hydrolysis: the concentration that filter cake is added 4～6 times of weight is in 30～36% the concentrated hydrochloric acid, to be warming up to 60～100 ℃, reacts 6～12 hours; (3) filter: after hydrolysis finishes, filter, and wash filter residue, collect clear liquid with massive laundering with filter cloth; (4) concentrate: feed liquid is concentrated into a large amount of crystal separates out; (5) filter: centrifuging, and wash crystalline substance with an amount of ethanol, obtain the pearl crystal;
(6) dissolving decolouring: crystal adds proper amount of active carbon and decolours with 4～8 times of weight water dissolution, and gac and crystalline weight ratio are 1: 10～20, and bleaching time is 15～60 minutes; (7) filter: obtain the water white transparency settled solution; (8) nanofiltration: above-mentioned solution is carried out nanofiltration with nf membrane, further remove the inorganic salt in the feed liquid; (9) concentrate: the nanofiltration liquid concentrator further is concentrated into solid content 30～70%; (10) alcohol is analysed: stir, in liquid concentrator, add ethanol and carry out alcohol and analyse, and left standstill 4～8 hours, said consumption of ethanol is an ethanol volume liter and the weight kilogram ratio of concentrated feed liquid is 1: 1～3, and concentration of ethanol is 85%～100%; (11) centrifuging and wash crystalline substance, promptly obtain after the crystal oven dry content greater than 99%, residue on ignition is less than 0.1% high-purity aminoglucose hydrochloride.
The above-mentioned technology that the present invention adopts; Utilization originates widely that the citric acid fermentation slag is raw material, can effectively remove the impurity such as inorganic salt in the product, and residue on ignition is lower than 0.1%; Range of application is wider; Value added is higher, has not only realized the utilization again of refuse, and has huge economic benefit and social benefit.
Embodiment
Embodiment 1:
Dispose 20 liters of concentration and be 1% hydrochloric acid soln, pour 8 kilograms of citric acid fermentation slags into, stir and make the fermentation residue swelling, soak after 4 hours, centrifuging, and wash with suitable quantity of water.Filter cake poured in 40 liter 31% the concentrated hydrochloric acid, stir, the chuck heating makes the material temperature be warming up to 100 ℃ gradually, reacts 10 hours.After hydrolysis finishes, blowing, feed liquid is filtered with filter cloth, and washs filter residue with massive laundering, merging filtrate and washings.Feed liquid is concentrated into a large amount of crystal and separates out, and normal temperature left standstill crystallization 72 hours.Stir feed liquid, centrifuging, and wash crystalline substance with an amount of ethanol, obtain the pearl crystal.Crystal with 4 times of weight water dissolution, is added proper amount of active carbon and decolours, and gac and crystalline weight ratio are 1: 10, decolour 1 hour and filtration.Filtrating is concentrated into solid content 50% after nanofiltration; Stir on one side; Adding on one side ethanol carries out alcohol and analyses; Add continued and stirred 1 hour, and leave standstill crystallization centrifuging after 8 hours, promptly obtain after the crystal oven dry after washing crystalline substance content greater than 99%, residue on ignition is less than 0.1% high-purity aminoglucose hydrochloride.
Embodiment 2:
Dispose 10 liters of concentration and be 4% hydrochloric acid soln, pour 8 kilograms of citric acid fermentation slags into, stir and make the fermentation residue swelling, soak after 2 hours, centrifuging, and wash with suitable quantity of water.Filter cake poured in 35 liter 36% the concentrated hydrochloric acid, stir, the chuck heating makes the material temperature be warming up to 95 ℃ gradually, reacts 8 hours.After hydrolysis finishes, blowing, feed liquid is filtered with filter cloth, and washs filter residue three times with massive laundering, merging filtrate and washings.Feed liquid is concentrated into a large amount of crystal and separates out, and leaves standstill crystallization 80 hours.Feed liquid centrifuging, and wash crystalline substance with an amount of ethanol.Crystal adds proper amount of active carbon and decolours with 8 times of weight water dissolution, and gac and crystalline weight ratio are 1: 20, decolour 45 minutes, filters rear filtrate and uses the nf membrane nanofiltration again, and nanofiltration liquid further is concentrated into solid content 60%.Stir on one side, carry out alcohol and analyse Yi Bian add ethanol, and left standstill crystallization 6 hours, suction filtration is also washed crystalline substance.Promptly obtain after the crystal oven dry content greater than 99%, residue on ignition is less than 0.1% high-purity aminoglucose hydrochloride.
Obviously, the above embodiment of the present invention only be for clearly the present invention is described and is done for example, and be not to be qualification to embodiment of the present invention.For the those of ordinary skill in affiliated field, on the basis of above-mentioned explanation, can also make other multi-form variation or changes.Here need not also can't give all embodiments exhaustive, and these belong to conspicuous variation or the change that spirit of the present invention draws and still are among protection scope of the present invention.
Claims (1)
1. a citric acid fermentation slag prepares the production technique of high-purity aminoglucose hydrochloride, it is characterized in that may further comprise the steps:
(1) s.t.: use concentration is 1～10% hydrochloric acid soln immersion citric acid fermentation slag, and the volume of hydrochloric acid soln and the weight ratio of fermentation residue are 1～6: 1, and soak time is 0.5～4 hour, centrifuging, and with the suitable quantity of water washing, filter cake is subsequent use;
(2) hydrolysis: the concentration that filter cake is added 4～6 times of weight is in 30～36% the concentrated hydrochloric acid, to be warming up to 60～100 ℃, reacts 6～12 hours;
(3) filter: after hydrolysis finishes, filter, and wash filter residue, collect clear liquid with massive laundering with filter cloth;
(4) concentrate: feed liquid is concentrated into a large amount of crystal separates out;
(5) filter: centrifuging, and wash crystalline substance with an amount of ethanol, obtain the pearl crystal;
(6) dissolving decolouring: crystal adds proper amount of active carbon and decolours with 4～8 times of weight water dissolution, and gac and crystalline weight ratio are 1: 10～20, and bleaching time is 15～60 minutes;
(7) filter: obtain the water white transparency settled solution;
(8) nanofiltration: above-mentioned solution is carried out nanofiltration with nf membrane, further remove the inorganic salt in the feed liquid;
(9) concentrate: the nanofiltration liquid concentrator further is concentrated into solid content 30～70%;
(10) alcohol is analysed: stir, in liquid concentrator, add ethanol and carry out alcohol and analyse, and left standstill 4～8 hours, said consumption of ethanol is an ethanol volume liter and the weight kilogram ratio of concentrated feed liquid is 1: 1～3, and concentration of ethanol is 85%～100%;
(11) centrifuging and wash crystalline substance, promptly obtain after the crystal oven dry content greater than 99%, residue on ignition is less than 0.1% high-purity aminoglucose hydrochloride.
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| CN2010105330620A CN102464679A (en) | 2010-11-04 | 2010-11-04 | Production process for preparing high-purity D-glucosamine hydrochloride from citric acid fermentation residues |
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| CN2010105330620A CN102464679A (en) | 2010-11-04 | 2010-11-04 | Production process for preparing high-purity D-glucosamine hydrochloride from citric acid fermentation residues |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319547A (en) * | 2013-04-10 | 2013-09-25 | 扬州日兴生物科技股份有限公司 | Preparation method for glucosamine hydrochloride |
| CN103450289A (en) * | 2013-08-27 | 2013-12-18 | 上海应用技术学院 | Preparation method of D-glucosamine hydrochloride |
| CN103694280A (en) * | 2013-11-29 | 2014-04-02 | 安徽丰原发酵技术工程研究有限公司 | Method for extracting glucosamine hydrochloride from glucosamine hydrochloride-containing mother liquor |
| CN106589008A (en) * | 2016-12-20 | 2017-04-26 | 广西大学 | Preparation method of glucosamine monomer |
| CN113981026A (en) * | 2021-11-19 | 2022-01-28 | 青岛海辰生物技术有限公司 | High-purity glucosamine hydrochloride and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101429221A (en) * | 2008-12-19 | 2009-05-13 | 王纪杰 | Method for producing D-glucosamine hydrochlorate |
| CN101503433A (en) * | 2009-03-06 | 2009-08-12 | 石勇 | Preparation of plant source glucosamine hydrochloride |
| CN101628921A (en) * | 2009-07-30 | 2010-01-20 | 扬州日兴生物科技股份有限公司 | Preparation method of plant source D-glucosamine hydrochloride |
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2010
- 2010-11-04 CN CN2010105330620A patent/CN102464679A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101429221A (en) * | 2008-12-19 | 2009-05-13 | 王纪杰 | Method for producing D-glucosamine hydrochlorate |
| CN101503433A (en) * | 2009-03-06 | 2009-08-12 | 石勇 | Preparation of plant source glucosamine hydrochloride |
| CN101628921A (en) * | 2009-07-30 | 2010-01-20 | 扬州日兴生物科技股份有限公司 | Preparation method of plant source D-glucosamine hydrochloride |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319547A (en) * | 2013-04-10 | 2013-09-25 | 扬州日兴生物科技股份有限公司 | Preparation method for glucosamine hydrochloride |
| CN103319547B (en) * | 2013-04-10 | 2015-07-01 | 扬州日兴生物科技股份有限公司 | Preparation method for glucosamine hydrochloride |
| CN103450289A (en) * | 2013-08-27 | 2013-12-18 | 上海应用技术学院 | Preparation method of D-glucosamine hydrochloride |
| CN103694280A (en) * | 2013-11-29 | 2014-04-02 | 安徽丰原发酵技术工程研究有限公司 | Method for extracting glucosamine hydrochloride from glucosamine hydrochloride-containing mother liquor |
| CN103694280B (en) * | 2013-11-29 | 2015-11-25 | 安徽丰原发酵技术工程研究有限公司 | From containing the method extracting glucosamine hydrochloride glucosamine hydrochloride mother liquid |
| CN106589008A (en) * | 2016-12-20 | 2017-04-26 | 广西大学 | Preparation method of glucosamine monomer |
| CN113981026A (en) * | 2021-11-19 | 2022-01-28 | 青岛海辰生物技术有限公司 | High-purity glucosamine hydrochloride and preparation method thereof |
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Application publication date: 20120523 |