CN102391322A - Method for recovering glucosamine hydrochloride from hydrolytic mother liquid of glucosamine hydrochloride - Google Patents
Method for recovering glucosamine hydrochloride from hydrolytic mother liquid of glucosamine hydrochloride Download PDFInfo
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- CN102391322A CN102391322A CN2011104188139A CN201110418813A CN102391322A CN 102391322 A CN102391322 A CN 102391322A CN 2011104188139 A CN2011104188139 A CN 2011104188139A CN 201110418813 A CN201110418813 A CN 201110418813A CN 102391322 A CN102391322 A CN 102391322A
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Abstract
The invention relates to a method for recovering a glucosamine hydrochloride from a hydrolytic mother liquid of the glucosamine hydrochloride. According to the method, chitin is added to concentrated hydrochloric acid with the concentration of 30-31% according to a weight ratio of 1:2.5 and is hydrolyzed for 3.5-4.5h at 90-95DEG C, the obtained liquid is cooled, the deposition is crystallized, the mother liquid generated by centrifuge dewatering is added with a special crystal induction agent at 40-50DEG C, is stirred for 25-35min by an anchor stirrer, is cooled to below 10DEG C by refrigerated water, and stands for not less than 4h at the temperature, the supernatant is sucked out by a vacuum tube, and the deposition is centrifuged to dryness to obtain crude crystals. The method allows the energy consumption to be low, the operation time to be short, and the recovery rate to reach 80-85%. Compared with present traditional high-temperature (85-90DEG C) long-time (10h) vacuum concentration recovery methods, the method of the invention allows the recovery rate of the glucosamine hydrochloride to be increased by about 20%, the crude crystal quality to be obviously better because of the low temperature deposition mode, the comprehensive energy consumption to be reduced, the production period to be shortened, the labor cost and the equipment maintenance cost to be reduced, and the production cost to be lower.
Description
Technical field
The present invention relates to the biochemical technology field, be meant a kind of method that from the glucosamine hydrochloride hydrolysising mother liquid, reclaims glucosamine hydrochloride specifically.
Background technology
The glucosamine hydrochloride production process adds to carry on as before in the chitinous hydrolysising mother liquid that produces of concentrated hydrochloric acid hydrolysis and so contains the 10-15% glucosamine hydrochloride of having an appointment and be dissolved in the mother liquor and must reclaim.
Existing tradition reclaims long-time (10 hours) the vacuum concentration absorption method of process using high temperature (85-90 ℃); This method consumes great amount of cost, such as energy consumption steam and electricity, and labour cost and maintenance of the equipment expense etc.; And the recovery of glucosamine hydrochloride bullion 60-65% only in the mother liquor; About 20% glucosamine hydrochloride bullion destroys decomposition because of long-time heating high temperature burns wall, can't realize reclaiming, and causes huge waste and loss.
Summary of the invention
The present invention provides a kind of method that from the glucosamine hydrochloride hydrolysising mother liquid, reclaims glucosamine hydrochloride, and its main purpose is to solve the problems referred to above that prior art exists.
Technical scheme of the present invention is following:
A kind of method that from the glucosamine hydrochloride hydrolysising mother liquid, reclaims glucosamine hydrochloride, chitin add in the concentrated hydrochloric acid of concentration 30-31%, at 90-95 ℃ of hydrolysis 3.5-4.5 hour by weight 1:2.5; The cryoprecipitation crystallization is after the mother liquor that centrifuge dehydration produces; Mother liquor adds special use and lures brilliant agent in the time of temperature 40-50 ℃, stirs 25-35 minute with anchor stirrer; Connect and be cooled to below 10 ℃ with refrigerated water; Keep this temperature to leave standstill and be not less than 4 hours, the back is inhaled with valve tube and is removed supernatant, and the deposition part is taken off the dried crystal crude product that obtains through centrifugal again.
It is that the former powder of oyster shells, precipitated silica and crystallite chitosan powder are made that said special use lures brilliant agent, by weight being 1:0.5:2.
Special use lures brilliant agent and mother liquor by weight being 2:1000.
Can know by the above-mentioned description of this invention, compare, the invention has the advantages that with existing conventional art:
One, adopt low temperature and lure brilliant agent to reclaim novel process.In this mother liquor, add a certain proportion of crystallization and lure brilliant agent, and change steam-heated cal(l)andria into the refrigerated water cooling, this method not only consumes energy low, and the running time is short, and the recovery of glucosamine hydrochloride can reach 80-85% in the mother liquor.
Two, compare with long-time (10 hours) the vacuum concentration absorption method of at present traditional high temperature (85-90 ℃), the glucosamine hydrochloride recovery can increase about 20% in the mother liquor.Cause is the low-temperature sludge mode, and the quality of recovery article obviously is better than traditional technology, and reduces comprehensive power consumption, shortening production cycle, reduction labour cost and maintenance of the equipment expense, makes production cost lower.
Three, the present invention is novel, and design is unique, have very strong practicality, so the present invention has broad application prospects.
Embodiment
Embodiment one
Present embodiment is a kind of method that from the glucosamine hydrochloride hydrolysising mother liquid, reclaims glucosamine hydrochloride; Chitin adds in the concentrated hydrochloric acid of concentration 30% by weight 1:2.5; 90 ℃ of hydrolysis 3.5 hours, the cryoprecipitation crystallization was after the mother liquor that centrifuge dehydration produces, and mother liquor is when 40 ℃ of temperature; Add special use and lure brilliant agent; It is that the former powder of oyster shells, precipitated silica and crystallite chitosan powder are made that special use lures brilliant agent, and by weight being 1:0.5:2, special use lures brilliant agent and mother liquor by weight being 2:1000.Stirred 25 minutes with anchor stirrer, connect and be cooled to below 10 ℃ with refrigerated water, keep this temperature to leave standstill and be not less than 4 hours, the back is inhaled with valve tube and is removed supernatant, and the deposition part is taken off the dried crystal crude product that obtains through centrifugal again.
This bullion continues rectification flow by common technology.
Embodiment two
Present embodiment is a kind of method that from the glucosamine hydrochloride hydrolysising mother liquid, reclaims glucosamine hydrochloride; Chitin adds in the concentrated hydrochloric acid of concentration 31% by weight 1:2.5; 95 ℃ of hydrolysis 4.5 hours, the cryoprecipitation crystallization was after the mother liquor that centrifuge dehydration produces, and mother liquor is when 50 ℃ of temperature; Add special use and lure brilliant agent; It is that the former powder of oyster shells, precipitated silica and crystallite chitosan powder are made that special use lures brilliant agent, and by weight being 1:0.5:2, special use lures brilliant agent and mother liquor by weight being 2:1000.Stirred 35 minutes with anchor stirrer, connect and be cooled to below 10 ℃ with refrigerated water, keep this temperature to leave standstill and be not less than 4 hours, the back is inhaled with valve tube and is removed supernatant, and the deposition part is taken off the dried crystal crude product that obtains through centrifugal again.
This bullion continues rectification flow by common technology.
Embodiment three
Present embodiment is a kind of best practice that from the glucosamine hydrochloride hydrolysising mother liquid, reclaims glucosamine hydrochloride; Chitin adds in the concentrated hydrochloric acid of concentration 30.5% by weight 1:2.5; 92.5 ℃ of hydrolysis 4 hours, the cryoprecipitation crystallization was after the mother liquor that centrifuge dehydration produces, and mother liquor is when 45 ℃ of temperature; Add special use and lure brilliant agent; It is that the former powder of oyster shells, precipitated silica and crystallite chitosan powder are made that special use lures brilliant agent, and by weight being 1:0.5:2, special use lures brilliant agent and mother liquor by weight being 2:1000.Stirred 30 minutes with anchor stirrer, connect and be cooled to below 10 ℃ with refrigerated water, keep this temperature to leave standstill and be not less than 4 hours, the back is inhaled with valve tube and is removed supernatant, and the deposition part is taken off the dried crystal crude product that obtains through centrifugal again.
This bullion continues rectification flow by common technology.
Adopt low temperature and lure brilliant agent to reclaim novel process.In this mother liquor, add a certain proportion of crystallization and lure brilliant agent, and change steam-heated cal(l)andria into the refrigerated water cooling, this method not only consumes energy low, and the running time is short, and the recovery can reach 80-85%.
Compare with long-time (10 hours) the vacuum concentration absorption method of at present traditional high temperature (85-90 ℃), the glucosamine hydrochloride recovery can increase about 20% in the mother liquor.Cause is the low-temperature sludge mode, and the quality of recovery article obviously is better than traditional technology, and reduces comprehensive power consumption, shortening production cycle, reduction labour cost and maintenance of the equipment expense, makes production cost lower.
The present invention is novel, and design is unique, have very strong practicality, so the present invention has broad application prospects.
The above-mentioned embodiment that is merely invention, but design concept of the present invention is not limited thereto allly utilizes this design that the present invention is carried out the change of unsubstantiality, all should belong to the behavior of invading protection domain of the present invention.
Claims (3)
1. method that from the glucosamine hydrochloride hydrolysising mother liquid, reclaims glucosamine hydrochloride, chitin adds in the concentrated hydrochloric acid of concentration 30-31%, at 90-95 ℃ of hydrolysis 3.5-4.5 hour by weight 1:2.5; The cryoprecipitation crystallization is after centrifuge dehydration produces mother liquor; It is characterized in that: mother liquor adds special use and lures brilliant agent in the time of temperature 40-50 ℃, stirs 25-35 minute with anchor stirrer; Connect and be cooled to below 10 ℃ with refrigerated water; Keep this temperature to leave standstill and be not less than 4 hours, the back is inhaled with valve tube and is removed supernatant, and the deposition part is taken off the dried crystal crude product that obtains through centrifugal again.
2. method that from the glucosamine hydrochloride hydrolysising mother liquid, reclaims glucosamine hydrochloride, it is characterized in that: it is that the former powder of oyster shells, precipitated silica and crystallite chitosan powder are made that said special use lures brilliant agent, by weight being 1:0.5:2.
3. method that from the glucosamine hydrochloride hydrolysising mother liquid, reclaims glucosamine hydrochloride is characterized in that: special use lures brilliant agent and mother liquor by weight being 2:1000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110418813.9A CN102391322B (en) | 2011-12-15 | 2011-12-15 | Method for recovering glucosamine hydrochloride from hydrolytic mother liquid of glucosamine hydrochloride |
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| CN201110418813.9A CN102391322B (en) | 2011-12-15 | 2011-12-15 | Method for recovering glucosamine hydrochloride from hydrolytic mother liquid of glucosamine hydrochloride |
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| CN102391322A true CN102391322A (en) | 2012-03-28 |
| CN102391322B CN102391322B (en) | 2014-06-04 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105753914A (en) * | 2016-04-27 | 2016-07-13 | 山东凯尔海洋生物科技有限公司 | Method for treating D-glucosamine hydrochloride acid pickle |
| CN112645992A (en) * | 2020-12-25 | 2021-04-13 | 山东润德生物科技有限公司 | Method for recovering glucosamine hydrochloride mother liquor and application thereof |
| CN115340582A (en) * | 2021-05-13 | 2022-11-15 | 山东润德生物科技有限公司 | Method for recovering glucosamine hydrochloride mother liquor |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1056331A (en) * | 1963-01-18 | 1967-01-25 | Rotta Res Lab | Process for preparing glucosamine salts |
| FR2701030A1 (en) * | 1993-01-20 | 1994-08-05 | Aber Technologies | Process for the hydrolysis of chitin and/or of chitosan and D-glucosamine hydrochloride oligomers obtained |
| CN1335322A (en) * | 2001-08-24 | 2002-02-13 | 广东梅县梅雁蓝藻有限公司 | Prepn of aminoglucose hydrochloride |
| KR20020023016A (en) * | 2000-09-22 | 2002-03-28 | 신용규 | Preparation of glucosamine hydrochloride |
| US6486307B1 (en) * | 2001-08-23 | 2002-11-26 | Alberta Research Council Inc. | Preparation of glucosamine hydrochloride |
| CN1467227A (en) * | 2002-07-09 | 2004-01-14 | 邵建华 | Closed path circulation and comprehensive utilization for waste liquor of chitin and derivative production |
| CN101210035A (en) * | 2007-12-25 | 2008-07-02 | 谢锐权 | Method for preparing aminoglucose hydrochloride |
| CN101671374A (en) * | 2009-09-18 | 2010-03-17 | 连云港澳兴生物科技有限公司 | Novel process for extracting D-glucosamine hydrochloride |
| CN101775045A (en) * | 2009-12-07 | 2010-07-14 | 汪昔奇 | Method for preparing glucosamine hydrochloride |
-
2011
- 2011-12-15 CN CN201110418813.9A patent/CN102391322B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1056331A (en) * | 1963-01-18 | 1967-01-25 | Rotta Res Lab | Process for preparing glucosamine salts |
| FR2701030A1 (en) * | 1993-01-20 | 1994-08-05 | Aber Technologies | Process for the hydrolysis of chitin and/or of chitosan and D-glucosamine hydrochloride oligomers obtained |
| KR20020023016A (en) * | 2000-09-22 | 2002-03-28 | 신용규 | Preparation of glucosamine hydrochloride |
| US6486307B1 (en) * | 2001-08-23 | 2002-11-26 | Alberta Research Council Inc. | Preparation of glucosamine hydrochloride |
| CN1335322A (en) * | 2001-08-24 | 2002-02-13 | 广东梅县梅雁蓝藻有限公司 | Prepn of aminoglucose hydrochloride |
| CN1467227A (en) * | 2002-07-09 | 2004-01-14 | 邵建华 | Closed path circulation and comprehensive utilization for waste liquor of chitin and derivative production |
| CN101210035A (en) * | 2007-12-25 | 2008-07-02 | 谢锐权 | Method for preparing aminoglucose hydrochloride |
| CN101671374A (en) * | 2009-09-18 | 2010-03-17 | 连云港澳兴生物科技有限公司 | Novel process for extracting D-glucosamine hydrochloride |
| CN101775045A (en) * | 2009-12-07 | 2010-07-14 | 汪昔奇 | Method for preparing glucosamine hydrochloride |
Non-Patent Citations (2)
| Title |
|---|
| 仇立干: "D-氨基葡萄糖盐酸盐的研制", 《苏州大学学报(自然科学)》, vol. 16, no. 3, 31 July 2000 (2000-07-31), pages 86 - 90 * |
| 李建，等: "氨基葡萄糖盐酸盐的研制", 《青岛化工学院学报》, vol. 23, 30 September 2002 (2002-09-30), pages 24 - 25 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105753914A (en) * | 2016-04-27 | 2016-07-13 | 山东凯尔海洋生物科技有限公司 | Method for treating D-glucosamine hydrochloride acid pickle |
| CN112645992A (en) * | 2020-12-25 | 2021-04-13 | 山东润德生物科技有限公司 | Method for recovering glucosamine hydrochloride mother liquor and application thereof |
| CN112645992B (en) * | 2020-12-25 | 2022-01-21 | 山东润德生物科技有限公司 | Method for recovering glucosamine hydrochloride mother liquor and application thereof |
| CN115340582A (en) * | 2021-05-13 | 2022-11-15 | 山东润德生物科技有限公司 | Method for recovering glucosamine hydrochloride mother liquor |
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| CN102391322B (en) | 2014-06-04 |
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Denomination of invention: Method for recovering glucosamine hydrochloride from hydrolytic mother liquid of glucosamine hydrochloride Effective date of registration: 20180509 Granted publication date: 20140604 Pledgee: Industrial Bank Limited by Share Ltd Shishi subbranch Pledgor: Shishi City Well Able Marine Organism Chemical Co., Ltd. Registration number: 2018350000042 |
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