CN102964395A - Method for improving purity of glucosamine hydrochloride - Google Patents
Method for improving purity of glucosamine hydrochloride Download PDFInfo
- Publication number
- CN102964395A CN102964395A CN2012105340725A CN201210534072A CN102964395A CN 102964395 A CN102964395 A CN 102964395A CN 2012105340725 A CN2012105340725 A CN 2012105340725A CN 201210534072 A CN201210534072 A CN 201210534072A CN 102964395 A CN102964395 A CN 102964395A
- Authority
- CN
- China
- Prior art keywords
- glucosamine hydrochloride
- vacuum
- purity
- support
- rotary body
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Saccharide Compounds (AREA)
- Paper (AREA)
Abstract
The invention provides a method for improving the purity of glucosamine hydrochloride. According to the method provided by the invention, precision filtration is added after a dissolution decolouration filtration process in a refining process, and a 0.45Mum precision filter element is adopted, so that fine impurities, foreign matters and insoluble matters which are larger than 0.45Mum are completely eliminated and the purity of a terminal product is greatly improved; in a concentration crystallization washing process of the refining stage, the pH value of eluate is strictly controlled to be more than or equal to 5.0, and residual mother liquor after washing can be controlled to be extremely little, so that the purity of the terminal product is greatly improved; and in the vacuum drying process of the refining stage, the existing vacuum machine is improved, the vacuum machine is improved in a manner that a vacuumizing device rotates with a double-cone revolving body synchronously, and the phenomenon that glucosamine hydrochloride is polluted as a sealing filler wearer is brought into the double-cone revolving body when the double-cone revolving body rotates and the vacuumizing device does not rotate is avoided, so that foreign matter is reduced to the utmost extent and the purity of the terminal product is improved.
Description
Technical field
The present invention relates to the preparation of glucosamine hydrochloride, specifically a kind of method that improves glucosamine hydrochloride purity.
Background technology
The natural compounds that glucosamine synthesizes in human body, it is made of a glucose and an amino.Studies show that glucosamine is in and plays the part of pivotal player in the lubricating status helping to keep and keep all joints of health.Stimulate synthetic mucopolysaccharide in the body, mucopolysaccharide is the main chemical compositions of cartilaginous tissue.Glucosamine simultaneously can promote element sulphur to enter in the cartilaginous tissue to go.
At present tradition preparation glucosamine hydrochloride method mainly adopts Hydrochloric Acid Hydrolysis Method production, the method is take chitin as raw material, adopt hydrochloric acid as degradation agents, be hydrolyzed for a long time through high temperature, at last by precipitation, separation, filtration, centrifugal and dry acquisition finished product.In the production practice process of reality, find that the glucosamine hydrochloride finished product purity that this method prepares is lower, so that inefficiency in the large-scale industrial production, as purifying follow-up, has increased again the cost burden of enterprise undoubtedly.
Summary of the invention
The present invention is to provide a kind of method that improves glucosamine hydrochloride purity, its main purpose is to solve the problems referred to above that prior art exists:
Technical scheme of the present invention is as follows:
A kind of method that improves glucosamine hydrochloride purity was got a certain amount of chitin and is positioned in the retort, adds hydrochloric acid, to retort heating, back hydrolysis 2.0-2.5 hour; After the cryoprecipitation, carry out centrifuge dehydration, get solid crude product, liquid filtrate; Filtrate is heated concentrated, distills afterwards condensation, reclaims crude product and hydrochloric acid; Crude product adds deionized water and activated carbon, filters after 1-1.5 hour, obtains yellow solution, again this solution is carried out secondary filter, gets rid of fine impurity, foreign matter and insolubles; In yellow solution vacuum suction concentration tank, heating, vacuum concentration and recovery hydrochloric acid is controlled the rate of recovery of this hydrochloric acid about 70%-80%, can stop to concentrate; With the concentrated material centrifuge dehydration later elaboration that must wet, it is dry that the wet elaboration after the alcohol washing is put into vacuum machine, and the time is 4-4.5 hour, can obtain the finished product crystallization.
Improve as the first of the present invention, what described secondary filter was adopted is 0.45 μ m precision Filter element.
Improve as the second of the present invention, in the operation of condensing crystal washing, the pH value of control elutant 〉=5.0.
As the third improvement of the present invention, described vacuum machine comprises support, be positioned at motor on the support, the rotating bipyramid rotary body with opening for feed and discharge port that is positioned on the support, be arranged in the rotation axis of bipyramid rotary side end, described rotation axis is fixed by the bearing that is fixed on the support, the rotation axis outer cover of a described wherein side is provided with a hinge wheel that is fixed on the support, hinge wheel is connected in motor by chain gear, be arranged with vacuum extractor in this rotation axis, the end that this vacuum extractor stretches into bipyramid rotary body inside is provided with vacuum filter; Be provided with inlet pipe and escape pipe in the rotation axis of opposite side, described inlet pipe and escape pipe are connected with swivel joint, the outside of described bipyramid rotary body is provided with a shell, form container cavity between described shell and the bipyramid rotary body, described container cavity is connected in swivel joint by inlet pipe and escape pipe.
Further, also be provided with a controller on the described support, this controller control linkage is in motor.
By the above-mentioned description of this invention as can be known, be compared with existing technology, the invention has the advantages that:
One, the present invention increases secondary filter after refining workshop section dissolving decolorization filtering operation is filtered, adopted 0.45 μ m precision Filter element, fine impurity, foreign matter, insolubles greater than 0.45 μ m all is eliminated, thereby greatly improves the purity of end product.
Two, the present invention strictly controls the pH value of elutant 〉=5.0 in refining workshop section condensing crystal washing procedure, the residue of mother after the washing can be controlled in few scope, thereby greatly improve the purity of finished product of terminal company.
Three, the present invention is in refining workshop section vacuum-drying operation, improved existing vacuum machine, vacuum machine has been improved, made vacuum extractor and bipyramid rotary body synchronous rotary, avoid the rotation of bipyramid rotary body, and vacuum extractor is brought the lock packing wearer in the bipyramid rotary body into when not rotating, and pollutes glucosamine hydrochloride, so the minimizing foreign substance pollution of larger limit, the purity of raising final finished.
Four; the present invention is by several measures; in the glucosamine hydrochloride preparation process of reality; reduce the foreign material content in the glucosamine hydrochloride, improved the purity of glucosamine hydrochloride, had very strong practicality; avoid enterprise after the glucosamine hydrochloride preparation is finished, also to need the step of further purifying; reduced the production cost of enterprise, and to enterprise with certain economical efficiency, be fit to the large-scale industrial production.
Description of drawings
Fig. 1 is the structural representation of the vacuum machine of the embodiment of the invention three.
Embodiment
Embodiment one
A kind of method that improves glucosamine hydrochloride purity was got a certain amount of chitin and is positioned in the retort, adds hydrochloric acid, to retort heating, back hydrolysis 2.0-2.5 hour; After the cryoprecipitation, carry out centrifuge dehydration, get solid crude product, liquid filtrate; Filtrate is heated concentrated, distills afterwards condensation, reclaims crude product and hydrochloric acid; Crude product adds deionized water and activated carbon, filters after 1-1.5 hour, obtains yellow solution, again this solution is carried out secondary filter, and what secondary filter was adopted is 0.45 μ m precision Filter element; Get rid of fine impurity, foreign matter and insolubles; In yellow solution vacuum suction concentration tank, heating, vacuum concentration and recovery hydrochloric acid is controlled the rate of recovery of this hydrochloric acid about 70%-80%, can stop to concentrate; With the concentrated material centrifuge dehydration later elaboration that must wet, it is dry that the wet elaboration after the alcohol washing is put into vacuum machine, and the time is 4-4.5 hour, can obtain the finished product crystallization.
The present invention increases secondary filter after refining workshop section dissolving decolorization filtering operation is filtered, adopted 0.45 μ m precision Filter element, fine impurity, foreign matter, insolubles greater than 0.45 μ m all is eliminated, thereby greatly improves the purity of end product.
Embodiment two
Present embodiment and embodiment one are roughly the same, and its key distinction is in the operation of condensing crystal washing, the pH value of control elutant 〉=5.0.
The present invention strictly controls the pH value of elutant 〉=5.0 in refining workshop section condensing crystal washing procedure, the residue of mother after the washing can be controlled in few scope, thereby greatly improve the purity of finished product of terminal company.
Embodiment three
Present embodiment and embodiment one and embodiment two are roughly the same, and its key distinction is the improvement of vacuum machine.
As shown in Figure 1, vacuum machine comprises support 1, be positioned at motor 2 on the support, the rotating bipyramid rotary body 3 with opening for feed 31 and discharge port 32 that is positioned on the support 1, be arranged in the rotation axis 4 of bipyramid rotary body 3 sides, rotation axis 4 is fixing by the bearing 5 that is fixed on the support 1, wherein rotation axis 4 outer cover of a side are provided with a hinge wheel 41 that is fixed on the support 1, hinge wheel 41 is connected in motor 2 by chain gear, be arranged with vacuum extractor 5 in this rotation axis 4, this vacuum extractor 5 stretches into bipyramid rotary body 3 inside, and its end that stretches into bipyramid rotary body 3 inside is provided with vacuum filter 51; Be provided with inlet pipe 61 and escape pipe 62 in the rotation axis 4 of opposite side, inlet pipe 61 and escape pipe 62 are connected with swivel joint 63, the outside of bipyramid rotary body 3 is provided with a shell 33, form container cavity 34 between shell 33 and the bipyramid rotary body 3, container cavity 34 is connected in swivel joint 63 by inlet pipe 61 and escape pipe 62; Also be provided with a controller 7 on the support 1, these controller 7 control linkages also can be controlled the turnover of steam in motor 3.
By opening for feed 31 and discharge port 32 turnover glucosamine hydrochlorides, controller 7 can be controlled motor 2 and open and close, motor 2 starts, rotate by chain gear hinge wheel 41, and then drive vacuum extractor 5 and 3 rotations of bipyramid rotary body, and vacuum extractor 5 can be being evacuated in the bipyramid rotary body 3, and vacuum filter 51 is then avoided the materials in the bipyramid rotary body 3 are extracted out, block vacuum extractor 5, affect the use of vacuum extractor 5; Inlet pipe 61 can be to the container cavity 34 interior delivering vapors that form between shell 33 and the bipyramid rotary body 3, so that the glucosamine hydrochloride in the bipyramid rotary body 3 is dried, escape pipe 62 then transfers out gas, and 63 of swivel joints are the normal uses of being convenient to inlet pipe 61 and escape pipe 62 when bipyramid rotary body 3 rotation.
The present invention is in refining workshop section vacuum-drying operation, improved existing vacuum machine, vacuum machine is improved, make vacuum extractor and bipyramid rotary body synchronous rotary, avoid bipyramid rotary body rotation, and vacuum extractor is not when rotating, the lock packing wearer is brought in the bipyramid rotary body, pollute glucosamine hydrochloride, thus the minimizing foreign substance pollution of larger limit, the purity of raising final finished.
The present invention is by several measures; in the glucosamine hydrochloride preparation process of reality; reduced the foreign material content in the glucosamine hydrochloride; improve the purity of glucosamine hydrochloride; have very strong practicality, avoid enterprise after the glucosamine hydrochloride preparation is finished, also to need the step of further purifying, reduced the production cost of enterprise; and to enterprise with certain economical efficiency, be fit to the large-scale industrial production.
Above-mentionedly only be the embodiment of invention, but design concept of the present invention is not limited to this, 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 (5)
1. a method that improves glucosamine hydrochloride purity is characterized in that: get a certain amount of chitin and be positioned in the retort, add hydrochloric acid, to retort heating, back hydrolysis 2.0-2.5 hour; After the cryoprecipitation, carry out centrifuge dehydration, get solid crude product, liquid filtrate; Filtrate is heated concentrated, distills afterwards condensation, reclaims crude product and hydrochloric acid; Crude product adds deionized water and activated carbon, filters after 1-1.5 hour, obtains yellow solution, again this solution is carried out secondary filter, gets rid of fine impurity, foreign matter and insolubles; In yellow solution vacuum suction concentration tank, heating, vacuum concentration and recovery hydrochloric acid is controlled the rate of recovery of this hydrochloric acid about 70%-80%, can stop to concentrate; With the concentrated material centrifuge dehydration later elaboration that must wet, it is dry that the wet elaboration after the alcohol washing is put into vacuum machine, and the time is 4-4.5 hour, can obtain the finished product crystallization.
2. a kind of method that improves glucosamine hydrochloride purity according to claim 1, it is characterized in that: what described secondary filter was adopted is 0.45 μ m precision Filter element.
3. a kind of method that improves glucosamine hydrochloride purity according to claim 1 is characterized in that: in the operation of condensing crystal washing, and the pH value of control elutant 〉=5.0.
4. a kind of method that improves glucosamine hydrochloride purity according to claim 1, it is characterized in that: described vacuum machine comprises support, be positioned at motor on the support, the rotating bipyramid rotary body with opening for feed and discharge port that is positioned on the support, be arranged in the rotation axis of bipyramid rotary side end, described rotation axis is fixed by the bearing that is fixed on the support, the rotation axis outer cover of a described wherein side is provided with a hinge wheel that is fixed on the support, hinge wheel is connected in motor by chain gear, be arranged with vacuum extractor in this rotation axis, the end that this vacuum extractor stretches into bipyramid rotary body inside is provided with vacuum filter; Be provided with inlet pipe and escape pipe in the rotation axis of opposite side, described inlet pipe and escape pipe are connected with swivel joint, the outside of described bipyramid rotary body is provided with a shell, form container cavity between described shell and the bipyramid rotary body, described container cavity is connected in swivel joint by inlet pipe and escape pipe.
5. a kind of method that improves glucosamine hydrochloride purity according to claim 4, it is characterized in that: also be provided with a controller on the described support, this controller control linkage is in motor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105340725A CN102964395A (en) | 2012-12-12 | 2012-12-12 | Method for improving purity of glucosamine hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105340725A CN102964395A (en) | 2012-12-12 | 2012-12-12 | Method for improving purity of glucosamine hydrochloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102964395A true CN102964395A (en) | 2013-03-13 |
Family
ID=47794855
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012105340725A Pending CN102964395A (en) | 2012-12-12 | 2012-12-12 | Method for improving purity of glucosamine hydrochloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102964395A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861005A (en) * | 2015-05-26 | 2015-08-26 | 华东理工大学 | Electric field and flow field coupling and regulation nanofiltration and separation method of glucosamine |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335322A (en) * | 2001-08-24 | 2002-02-13 | 广东梅县梅雁蓝藻有限公司 | Prepn of aminoglucose hydrochloride |
| JP2004059475A (en) * | 2002-07-26 | 2004-02-26 | Unitika Ltd | Method for purifying reducing sugar |
| CN201335593Y (en) * | 2008-12-31 | 2009-10-28 | 太仓市正信干燥设备厂 | Bipyramid vacuum drier |
| CN101671374A (en) * | 2009-09-18 | 2010-03-17 | 连云港澳兴生物科技有限公司 | New technique for extracting D-glucosamine hydrochloride |
| CN201757571U (en) * | 2010-06-24 | 2011-03-09 | 安徽东健化工科技有限公司 | Rotary type vacuum drying machine |
-
2012
- 2012-12-12 CN CN2012105340725A patent/CN102964395A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335322A (en) * | 2001-08-24 | 2002-02-13 | 广东梅县梅雁蓝藻有限公司 | Prepn of aminoglucose hydrochloride |
| JP2004059475A (en) * | 2002-07-26 | 2004-02-26 | Unitika Ltd | Method for purifying reducing sugar |
| CN201335593Y (en) * | 2008-12-31 | 2009-10-28 | 太仓市正信干燥设备厂 | Bipyramid vacuum drier |
| CN101671374A (en) * | 2009-09-18 | 2010-03-17 | 连云港澳兴生物科技有限公司 | New technique for extracting D-glucosamine hydrochloride |
| CN201757571U (en) * | 2010-06-24 | 2011-03-09 | 安徽东健化工科技有限公司 | Rotary type vacuum drying machine |
Non-Patent Citations (1)
| Title |
|---|
| 刘意，等: "甲壳素水解制备氨基葡萄糖盐酸盐的优化工艺条件", 《应用化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861005A (en) * | 2015-05-26 | 2015-08-26 | 华东理工大学 | Electric field and flow field coupling and regulation nanofiltration and separation method of glucosamine |
| CN104861005B (en) * | 2015-05-26 | 2020-12-04 | 华东理工大学 | Electric field and flow field coupling regulation nanofiltration separation method of glucosamine |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102212149B (en) | Preparation process for extracting crude sodium heparin from pig lungs | |
| CN101628921B (en) | Preparation method of plant source D-glucosamine hydrochloride | |
| CN106397630A (en) | Method for extracting sodium hyaluronate based on membrane separation technology | |
| CN105622776A (en) | Flos farfarae polysaccharide extraction and purification method | |
| CN103665192B (en) | A kind of method extracting sodium heparin and co-producing protein powder from chitterlings | |
| CN101550199A (en) | Method for preparing sodium hyaluronate from hyaluronic acid zymotic fluid | |
| CN104480228A (en) | Method for preparing glucosamine by utilizing shrimp and crab shells | |
| CN102146144A (en) | Method for extracting and refining inulin | |
| CN102952204A (en) | Novel production technique of heparin sodium | |
| CN101671294A (en) | Method for continuously extracting and separating 1-deoxynojirimycin (DNJ) and flavone from folium mori | |
| CN210170984U (en) | Filter equipment of pharmacy extract | |
| CN104628802B (en) | Method for extracting and purifying nemadectin from fermentation liquid | |
| CN102964395A (en) | Method for improving purity of glucosamine hydrochloride | |
| CN102775511B (en) | Method for extracting pepper polysaccharide from pepper residue | |
| CN104195195B (en) | A kind of extracting method of ferroheme | |
| CN103819572A (en) | Extraction technology for production of polysaccharide from mulberry leaf | |
| CN103724456A (en) | Technology for normal-temperature salt-free extraction of heparin sodium | |
| CN104610385A (en) | Refining method of D-glucosamine hydrochloride | |
| CN103641886B (en) | A kind of process for purification of glutamine dipeptide | |
| CN205313446U (en) | Chestnut shell pigment extraction device | |
| CN102746421B (en) | Impurity removing technology of crude heparin sodium | |
| CN102584611A (en) | Production method for medical grade valine | |
| CN107641161A (en) | A kind of optimal reparation technology of casing accessory substance liquaemin | |
| CN103936639A (en) | Production process for extracting cystine by hair | |
| CN113980090A (en) | Method for recovering biological source protein by using biological medicine fermentation fungus residues |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130313 |