CN102977158A - Method for preparing glucosamine hydrochloride by use of pleuromutilin waste thalli - Google Patents
Method for preparing glucosamine hydrochloride by use of pleuromutilin waste thalli Download PDFInfo
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- CN102977158A CN102977158A CN2012105068798A CN201210506879A CN102977158A CN 102977158 A CN102977158 A CN 102977158A CN 2012105068798 A CN2012105068798 A CN 2012105068798A CN 201210506879 A CN201210506879 A CN 201210506879A CN 102977158 A CN102977158 A CN 102977158A
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- pleuromutilin
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Abstract
The invention discloses a method for preparing glucosamine hydrochloride by use of pleuromutilin waste thalli, which comprises the steps of preparing chitosan, preparing glucosamine hydrochloride and the like. The method disclosed by the invention effectively removes residual pleuromutilin in waste thalli, does not need additional thallus wall breaking equipment and processes, filters macromolecular impurities through ultrafiltration, realizes comprehensive utilization and turns waste into wealth.
Description
Technical field
The present invention relates to a kind of method for preparing glucosamine hydrochloride with the pleuromutilin waste thallus.
Background technology
Glucosamine hydrochloride is widely used in medicine, chemical industry, food, feed and cosmetic industry, human body had important physiological function, can promote the synthetic of human body mucopolysaccharide, improve the viscosity of knuckle synovia, improve the metabolism of joint cartilage, be considered as the up to now only material that can at all treat bone and joint diseases by medical circle.The main raw material of making glucosamine hydrochloride is chitin, usually chitin is by shrimp shell, the preparation of crab shell, but in recent years because the minimizing of sea-food output, add shrimp shell, crab shell collection difficulty, and be subject to seasonal effect, thereby can not satisfy the demand of production, new raw material sources are all being sought by manufacturing enterprise.
The Mycophyta thalline is found in research, as containing abundant chitin in aspergillus, mould, Mucor or the bacterium of picking up the ears.The main raw material of synthetic microbiotic Tiamulin for animals, valnemulin is pleuromutilin, and pleuromutilin is Basidiomycetes brachymemma the pick up the ears product of bacterium fermentating metabolism of bacterium and Pa Shi of picking up the ears, and the somatic cells dry weight accounts for 4.0%～4.5% of fermented liquid.Contain pleuromutilin 25%～36%, chitin 18%～22%, protein 16%～24%, carbohydrate 8%～12%, lipid 6%～11% in the dry mycelium cell, because pleuromutilin and lipid are suggested, chitin content is up to 24%～31% in the pleuromutilin waste thallus behind the extraction pleuromutilin.Present domestic pleuromutilin output is about 3000 tons, and the pleuromutilin waste thallus behind the extraction pleuromutilin is about 12000 tons.But because the residual a small amount of pleuromutilin of pleuromutilin waste thallus (about 0.3%) is defined as dangerous solid waste, enterprise mostly electric power supply plant burns or landfill, both increased production cost, cause the wasting of resources, contaminate environment again, the processing of pleuromutilin waste thallus has become the thorny problem of each pleuromutilin manufacturing enterprise.
Summary of the invention
The object of the present invention is to provide residual pleuromutilin in a kind of effective removal waste thallus, production cost is low, method is easy prepares the method for glucosamine hydrochloride with the pleuromutilin waste thallus.
Technical solution of the present invention is:
A kind ofly prepare the method for glucosamine hydrochloride with the pleuromutilin waste thallus, it is characterized in that: comprise the following steps:
(1) chitosan preparation
(1) pleuromutilin waste thallus 100 ㎏ are dropped in the enamel reaction still of 1000L with reflux, chitin content is 28.6% in the pleuromutilin waste thallus, adds 5% hydrochloric acid soln 500L, boil insulation 1h, suction filtration, filter residue wash with water to neutrality, and vacuum is drained;
(2) add 15% sodium hydroxide solution 500L, at 80 ℃ of heated in water solution insulation 1h, suction filtration, filter residue wash with water to neutrality, and vacuum is drained;
(3) add 42% sodium hydroxide solution 500L, boil insulation 2.5h, filter, be washed to neutrality, drain;
(4) behind 70 ℃ of vacuum-drying 10h, obtain chitosan 23.56 ㎏, content is 89.6%, and yield 73.8%, product are faint yellow particle, and deacetylation is 85.3%;
(2) glucosamine hydrochloride preparation
(1) hydrolysis: 23.56 ㎏ chitosans are dropped in the enamel reaction still of 500L with reflux, add 30% hydrochloric acid soln 200L, be warming up to 95 ℃, insulation hydrolysis 3.5h;
(2) decolouring: after reaction finished, hydrolyzed solution was cooled to 60～70 ℃, added pharmaceutical powder gac 3.5 ㎏, stirred decolouring 2h;
(3) filter: destainer is through Plate Filtration, and filtrate is again through 0.2 μ m fine filter ultrafiltration;
(4), vacuum concentration: 65～70 ℃ of temperature, vacuum tightness-0.06～-0.07MPa, reclaim hydrochloric acid, the feed supplement while concentrating when being concentrated into glucosamine hydrochloride content and being 50%, stops to concentrate;
(5) crystallisation by cooling: concentrated solution Slow cooling, crystallization, mixing speed 30rpm is cooled to 5～8 ℃, static 12h.
(6) centrifugation: the ethanol drip washing of the crystal after the centrifugation, remove the plane of crystal mother liquor;
(7) vacuum-drying: 60 ℃ of drying temperatures, dry 8h obtains white amino glucosamine salt hydrochlorate 12.01 ㎏.
Advantage of the present invention:
1, effectively removes residual pleuromutilin in the waste thallus: just can effectively remove residual pleuromutilin in the waste thallus, all detect without pleuromutilin in work in-process chitosan and the finished product glucosamine hydrochloride.
2, need not increase thalline broken wall equipment and operation newly: the pleuromutilin that fermentation contains in the thalline is with methyl alcohol or ethyl acetate extraction, and endobacillary lipid material also is removed in the time of the extraction pleuromutilin.Microscopic examination is found, along with oozing out of pleuromutilin in the thalline and lipid material, the autolyze of somatic cells wall need not increase thalline broken wall equipment and operation newly, the materials such as protein, nucleic acid are removed easily in the somatic cells behind the broken wall, are conducive to extraction and the purifying of chitosan.
3, by ultrafiltration, filtering macromole impurity: the glucosamine hydrochloride solution behind activated carbon decolorizing, behind Plate Filtration, filtrate is again through 0.2 μ m fine filter ultrafiltration, the residual macromolecular colloid albumen of filtering and pigment are for the quality product of glucosamine hydrochloride provides assurance.
4, fully utilize, turn waste into wealth: by the analysis to pleuromutilin waste thallus composition, find wherein to contain abundant chitin, find the effective ways of removing residual pleuromutilin in the waste thallus, make the technological line that extracts chitosan and glucosamine hydrochloride preparation with the pleuromutilin waste thallus, and the realization industrialization, solved a great problem of puzzlement pleuromutilin manufacturing enterprise.Fully utilize, turn waste into wealth, promote the well-being of mankind, benefit the nation and the people, for cheap raw material sources have been opened up in the production of glucosamine hydrochloride.
The invention will be further described below in conjunction with embodiment.
Embodiment
One, chitosan preparation
1, pleuromutilin waste thallus 100 ㎏ are dropped in the enamel reaction still of 1000L with reflux, chitin content is 28.6% in the pleuromutilin waste thallus, adds 5% hydrochloric acid soln 500L, boil insulation 1h, suction filtration, filter residue wash with water to neutrality, and vacuum is drained.
2, add 15% sodium hydroxide solution 500L, at 80 ℃ of heated in water solution insulation 1h, suction filtration, filter residue wash with water to neutrality, and vacuum is drained.
3, add 42% sodium hydroxide solution 500L, boil insulation 2.5h, filter, be washed to neutrality, drain.
4, behind 70 ℃ of vacuum-drying 10h, obtain chitosan 23.56 ㎏, content is 89.6%, and yield 73.8%, product are faint yellow particle, and deacetylation is 85.3%.
Two, glucosamine hydrochloride preparation
1, hydrolysis: 23.56 ㎏ chitosans are dropped in the enamel reaction still of 500L with reflux, add 30% hydrochloric acid soln 200L, slowly be warming up to 95 ℃, insulation hydrolysis 3.5h.
2, decolouring: after reaction finished, hydrolyzed solution was cooled to 60～70 ℃, added pharmaceutical powder gac 3.5 ㎏, stirred decolouring 2h.
3, filter: destainer is through Plate Filtration, and through 0.2 μ fine filter ultrafiltration, the ultrafiltrated transmittance reaches more than 90% filtrate again.
4, vacuum concentration: 65～70 ℃ of temperature, vacuum tightness-0.06～-0.07MPa, reclaim hydrochloric acid.The feed supplement while concentrating when being concentrated into glucosamine hydrochloride content and being 50%, stops to concentrate.
5, crystallisation by cooling: concentrated solution Slow cooling, crystallization, mixing speed 30rpm is cooled to 5～8 ℃, static 12h.
6, centrifugation: the crystal after the centrifugation is removed the plane of crystal mother liquor with a small amount of ethanol drip washing.
7, vacuum-drying: 60 ℃ of drying temperatures, dry 8h obtains white amino glucosamine salt hydrochlorate 12.01 ㎏, and yield is 56.9%, and product is white crystals, and content is 98.61%, meets food grade glucosamine hydrochloride quality standard.
Claims (1)
1. one kind prepares the method for glucosamine hydrochloride with the pleuromutilin waste thallus, it is characterized in that: comprise the following steps:
(1) chitosan preparation
(1) pleuromutilin waste thallus 100 ㎏ are dropped in the enamel reaction still of 1000L with reflux, chitin content is 28.6% in the pleuromutilin waste thallus, adds 5% hydrochloric acid soln 500L, boil insulation 1h, suction filtration, filter residue wash with water to neutrality, and vacuum is drained;
(2) add 15% sodium hydroxide solution 500L, at 80 ℃ of heated in water solution insulation 1h, suction filtration, filter residue wash with water to neutrality, and vacuum is drained;
(3) add 42% sodium hydroxide solution 500L, boil insulation 2.5h, filter, be washed to neutrality, drain;
(4) behind 70 ℃ of vacuum-drying 10h, obtain chitosan 23.56 ㎏, content is 89.6%, and yield 73.8%, product are faint yellow particle, and deacetylation is 85.3%;
(2) glucosamine hydrochloride preparation
(1) hydrolysis: 23.56 ㎏ chitosans are dropped in the enamel reaction still of 500L with reflux, add 30% hydrochloric acid soln 200L, be warming up to 95 ℃, insulation hydrolysis 3.5h;
(2) decolouring: after reaction finished, hydrolyzed solution was cooled to 60～70 ℃, added pharmaceutical powder gac 3.5 ㎏, stirred decolouring 2h;
(3) filter: destainer is through Plate Filtration, and filtrate is again through 0.2 μ m fine filter ultrafiltration;
(4), vacuum concentration: 65～70 ℃ of temperature, vacuum tightness-0.06～-0.07MPa, reclaim hydrochloric acid, the feed supplement while concentrating when being concentrated into glucosamine hydrochloride content and being 50%, stops to concentrate;
(5) crystallisation by cooling: concentrated solution Slow cooling, crystallization, mixing speed 30rpm is cooled to 5～8 ℃, static 12h.
(6) centrifugation: the ethanol drip washing of the crystal after the centrifugation, remove the plane of crystal mother liquor;
(7) vacuum-drying: 60 ℃ of drying temperatures, dry 8h obtains white amino glucosamine salt hydrochlorate 12.01 ㎏.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210506879.8A CN102977158B (en) | 2012-12-03 | 2012-12-03 | Method for preparing glucosamine hydrochloride by use of pleuromutilin waste thalli |
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| CN201210506879.8A CN102977158B (en) | 2012-12-03 | 2012-12-03 | Method for preparing glucosamine hydrochloride by use of pleuromutilin waste thalli |
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| CN102977158A true CN102977158A (en) | 2013-03-20 |
| CN102977158B CN102977158B (en) | 2015-01-28 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2117673C1 (en) * | 1995-12-26 | 1998-08-20 | Алтайский государственный медицинский университет | Method of chitosan preparing |
| CN1242377A (en) * | 1998-07-20 | 2000-01-26 | 北京化工大学 | Method for preparing chitosan and low polymerized chitosan |
| CN1335322A (en) * | 2001-08-24 | 2002-02-13 | 广东梅县梅雁蓝藻有限公司 | Prepn of aminoglucose hydrochloride |
| CN1642986A (en) * | 2002-02-12 | 2005-07-20 | 克托兹莫股份有限公司 | Cell wall derivatives from biomass and preparation thereof |
| JP4468665B2 (en) * | 2003-07-10 | 2010-05-26 | 株式会社リコム | Production method of plant chitosan |
-
2012
- 2012-12-03 CN CN201210506879.8A patent/CN102977158B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2117673C1 (en) * | 1995-12-26 | 1998-08-20 | Алтайский государственный медицинский университет | Method of chitosan preparing |
| CN1242377A (en) * | 1998-07-20 | 2000-01-26 | 北京化工大学 | Method for preparing chitosan and low polymerized chitosan |
| CN1335322A (en) * | 2001-08-24 | 2002-02-13 | 广东梅县梅雁蓝藻有限公司 | Prepn of aminoglucose hydrochloride |
| CN1642986A (en) * | 2002-02-12 | 2005-07-20 | 克托兹莫股份有限公司 | Cell wall derivatives from biomass and preparation thereof |
| JP4468665B2 (en) * | 2003-07-10 | 2010-05-26 | 株式会社リコム | Production method of plant chitosan |
Non-Patent Citations (4)
| Title |
|---|
| P. POCHANAVANICH，等: ""Fungal chitosan production and its characterization"", 《LETTERS IN APPLIED MICROBIOLOGY》, vol. 35, 31 December 2002 (2002-12-31), pages 17 - 21 * |
| 张淑红: ""常见食用菌子实体中壳聚糖的提取和检测"", 《北方园艺》, no. 18, 31 December 2010 (2010-12-31), pages 203 - 204 * |
| 王军，等: ""壳聚糖酸解制备氨基葡萄糖盐酸盐的研究"", 《郑州轻工业学院学报》, vol. 25, no. 1, 28 February 2010 (2010-02-28), pages 36 - 38 * |
| 赵春燕，等: ""从几种常见真菌中筛选壳聚糖高产菌株的研究"", 《食品与发酵工业》, vol. 35, no. 3, 31 December 2009 (2009-12-31), pages 68 - 70 * |
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