CN101811934A - Preparation method of mannitol - Google Patents
Preparation method of mannitol Download PDFInfo
- Publication number
- CN101811934A CN101811934A CN201010150278A CN201010150278A CN101811934A CN 101811934 A CN101811934 A CN 101811934A CN 201010150278 A CN201010150278 A CN 201010150278A CN 201010150278 A CN201010150278 A CN 201010150278A CN 101811934 A CN101811934 A CN 101811934A
- Authority
- CN
- China
- Prior art keywords
- preparation
- deionized water
- extracted
- membrane system
- ultrafiltration membrane
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of mannitol. The technique comprises the following steps: extracting glossy privet leaf of triterpenic acid as a raw material, using 15-20 times (V/W) of deionized water to extract for 1.5-2 hours, carrying out ultrafiltration on extracting solution by an ultrafiltration membrane system with molecular weight cut off of 20000, heating and concentrating permeate till the relative density is 1.30-1.32, standing and crystallizing, using the deionized water to dissolve coarse crystal, boiling for 5 minutes, filtering with heat, recrystallizing for three times, using ether to clean, and drying at the temperature of 80-90 DEG C to obtain a product. The technique has simple operation, lower cost and higher purity and is beneficial to large-scale production operation.
Description
Technical field
The present invention relates to a kind of preparation method of N.F,USP MANNITOL, especially a kind of method of from Leaf of Glossy Privet extraction residue, extracting N.F,USP MANNITOL.
Background technology
N.F,USP MANNITOL claims D-mannitol, manna alcohol again, and the isomers for sorbyl alcohol is hexavalent alcohol.
English name: Mannitol
Molecular formula: C
6H
14O
6
Molecular weight: 182.17
White, needle-shaped crystals.166 ℃ of fusing points, relative density 1.52,1.489 (20 ℃), boiling point 290-295 ℃ (467kPa).These product of 1g dissolve in about 5.5ml water (about 18%, 25 ℃), 83ml alcohol, are dissolved in hot water morely, are dissolved in pyridine and aniline, are insoluble to ether.The aqueous solution is alkalescence.Chemical property with polyvalent alcohol can be esterified, etherificate, oxidation, dehydration, is only a kind of nonhygroscopic crystal in the polyvalent alcohol.
In the prior art, N.F,USP MANNITOL uses chemical synthesis usually, but has a lot of problems: glucose electrolytic process efficient is low, and energy consumption is big, and purity is low; The reduction method product of polyose has the isomery problem, cost height and purity is low; Seminose reduction method raw material sources are a problem etc.The extraction method of N.F,USP MANNITOL mainly is raw material with the sea-tangle, and gained N.F,USP MANNITOL is of poor quality, filtration is difficult, and the production cost height, need be further purified.
Summary of the invention
Technical problem to be solved by this invention provides a kind of simple to operate, and cost is lower, the N.F,USP MANNITOL preparation method that purity is higher.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
1) water is carried: get raw material, adding 15-20 doubly measures the deionized water heating of (V/W) and extracted 1.5-2 hour, filters, and gets extracting solution;
2) ultrafiltration: said extracted liquid is collected and is seen through liquid by ultrafiltration membrane system;
3) condensing crystal: in the time of will being concentrated into relative density and being 1.30-1.32 through liquid heating, blowing be let alone crystallisation by cooling in cylinder, coarse crystallization;
4) refining: coarse crystallization is dissolved in the 5min that seethes with excitement in the deionized water, and recrystallization is 3 times under the agitation condition, and the ether washing is dried under the 80-90 ℃ of temperature, promptly gets product.
Above-mentioned preparation method is characterized in that described raw material is the waste residue that Leaf of Glossy Privet extracted triterpenic acid.
Above-mentioned preparation method is characterized in that it is 75-80 ℃ that described water is put forward the Heating temperature of step.
Above-mentioned preparation method is characterized in that described ultrafiltration membrane system is poly-alum hollow fiber ultrafiltration membrane system, and molecular weight cut-off is 20000.
Above-mentioned preparation method is characterized in that the each crystallization deionized water of described purification step consumption is that the 1.0-1.2 of coarse crystallization doubly measures (V/W), and the ether consumption is that the 0.1-0.2 of coarse crystallization doubly measures (V/W).
In sum, there is following advantage in the present invention: this process using extraction method prepares N.F,USP MANNITOL, and problems such as isomerization impurity in the no synthesis method or catalysts are simple to operate; Raw material adopts Leaf of Glossy Privet to extract the residue of triterpenic acid, has saved resource, has reduced cost; Ultrafiltration also has good decolorizing effect except that the performance with tangible filtering colloidal impurity; The solubility with temperature of N.F,USP MANNITOL in water changes responsive, and crystallization effect is good; Consumption of organic solvent is few, and toxicity is low, produces safer.
Adopt technique scheme to prepare N.F,USP MANNITOL, simple to operate, cost is lower, and purity is higher, is beneficial to big production operation.
Below in conjunction with embodiment the present invention is further elaborated, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1
Get the residue 1kg that Leaf of Glossy Privet extracted triterpenic acid, add the 15L deionized water, heat 75 ℃ and extracted 1.5 hours, filter, get extracting solution.Extracting solution is collected and is seen through liquid through the poly-alum hollow fiber ultrafiltration membrane system decolouring of molecular weight cut-off 20000.See through the liquid heating and be concentrated into relative density 1.30-1.32, leave standstill crystallisation by cooling, get coarse crystallization 52g.Coarse crystallization adds the 52ml deionized water, puts cold crystallization after boiling 5min, and to separating out crystal with condition recrystallization 2 times, crystal adds the washing of 6L ether, and 80 ℃ of oven dry promptly get N.F,USP MANNITOL 3.8g, and through the HPLC detection, purity is 98.5%.
Embodiment 2
Get the residue 1kg that Leaf of Glossy Privet extracted triterpenic acid, add the 16L deionized water, heat 80 ℃ and extracted 1.5 hours, filter, get extracting solution.Extracting solution is collected and is seen through liquid through the poly-alum hollow fiber ultrafiltration membrane system decolouring of molecular weight cut-off 20000.See through the liquid heating and be concentrated into relative density 1.30-1.32, leave standstill crystallisation by cooling, get coarse crystallization 54g.Coarse crystallization adds the 60ml deionized water, puts cold crystallization after boiling 5min, and to separating out crystal with condition recrystallization 2 times, crystal adds the washing of 7L ether, and 90 ℃ of oven dry promptly get N.F,USP MANNITOL 3.9g, and through the HPLC detection, purity is 98.6%.
Embodiment 3
Get the residue 1kg that Leaf of Glossy Privet extracted triterpenic acid, add the 18L deionized water, heat 75 ℃ and extracted 2 hours, filter, get extracting solution.Extracting solution is collected and is seen through liquid through the poly-alum hollow fiber ultrafiltration membrane system decolouring of molecular weight cut-off 20000.See through the liquid heating and be concentrated into relative density 1.30-1.32, leave standstill crystallisation by cooling, get coarse crystallization 53g.Coarse crystallization adds the 55ml deionized water, puts cold crystallization after boiling 5min, and to separating out crystal with condition recrystallization 2 times, crystal adds the washing of 8L ether, and 80 ℃ of oven dry promptly get N.F,USP MANNITOL 3.8g, and through the HPLC detection, purity is 99.2%.
Embodiment 4
Get the residue 1kg that Leaf of Glossy Privet extracted triterpenic acid, add the 20L deionized water, heat 80 ℃ and extracted 2 hours, filter, get extracting solution.Extracting solution is collected and is seen through liquid through the poly-alum hollow fiber ultrafiltration membrane system decolouring of molecular weight cut-off 20000.See through the liquid heating and be concentrated into relative density 1.30-1.32, leave standstill crystallisation by cooling, get coarse crystallization 60g.Coarse crystallization adds the 70ml deionized water, puts cold crystallization after boiling 5min, and to separating out crystal with condition recrystallization 2 times, crystal adds the washing of 6L ether, and 85 ℃ of oven dry promptly get N.F,USP MANNITOL 4.0g, and through the HPLC detection, purity is 99.5%.
Claims (5)
1. the preparation method of a N.F,USP MANNITOL is characterized in that comprising following steps:
1) water is carried: get raw material, adding 15-20 doubly measures the deionized water heating of (V/W) and extracted 1.5-2 hour, filters, and gets extracting solution;
2) ultrafiltration: said extracted liquid is collected and is seen through liquid by ultrafiltration membrane system;
3) condensing crystal: in the time of will being concentrated into relative density and being 1.30-1.32 through liquid heating, leave standstill and let alone crystallisation by cooling, coarse crystallization;
4) refining: coarse crystallization is dissolved in the 5min that seethes with excitement in the deionized water, and recrystallization is 3 times under the agitation condition, and the ether washing is dried under the 80-90 ℃ of temperature, promptly gets product.
2. preparation method as claimed in claim 1 is characterized in that described raw material is the waste residue that Leaf of Glossy Privet extracted triterpenic acid.
3. preparation method as claimed in claim 1 is characterized in that it is 75-80 ℃ that described water is put forward the Heating temperature of step.
4. preparation method as claimed in claim 1 is characterized in that described ultrafiltration membrane system is poly-alum hollow fiber ultrafiltration membrane system, and molecular weight cut-off is 20000.
5. preparation method as claimed in claim 1 is characterized in that the each crystallization deionized water of described purification step consumption is that the 1.0-1.2 of coarse crystallization doubly measures (V/W), and the ether consumption is that the 0.1-0.2 of coarse crystallization doubly measures (V/W).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010150278A CN101811934A (en) | 2010-04-08 | 2010-04-08 | Preparation method of mannitol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010150278A CN101811934A (en) | 2010-04-08 | 2010-04-08 | Preparation method of mannitol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101811934A true CN101811934A (en) | 2010-08-25 |
Family
ID=42619325
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010150278A Pending CN101811934A (en) | 2010-04-08 | 2010-04-08 | Preparation method of mannitol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101811934A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432432A (en) * | 2010-09-29 | 2012-05-02 | 苏州瑞蓝博中药技术开发有限公司 | Preparation method of cordycepic acid |
| CN105152861A (en) * | 2015-09-11 | 2015-12-16 | 中国科学院过程工程研究所 | Method for preparing mannitol from broomrape oligosaccharide syrup |
| CN109320400A (en) * | 2018-09-30 | 2019-02-12 | 湖南华诚生物资源股份有限公司 | A method of natural mannitol is extracted from mogroside production waste liquid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112543A (en) * | 1994-08-13 | 1995-11-29 | 国家***杭州水处理技术研究开发中心 | Method for extracting mannitol from laminaria leach liquor |
-
2010
- 2010-04-08 CN CN201010150278A patent/CN101811934A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112543A (en) * | 1994-08-13 | 1995-11-29 | 国家***杭州水处理技术研究开发中心 | Method for extracting mannitol from laminaria leach liquor |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432432A (en) * | 2010-09-29 | 2012-05-02 | 苏州瑞蓝博中药技术开发有限公司 | Preparation method of cordycepic acid |
| CN105152861A (en) * | 2015-09-11 | 2015-12-16 | 中国科学院过程工程研究所 | Method for preparing mannitol from broomrape oligosaccharide syrup |
| CN109320400A (en) * | 2018-09-30 | 2019-02-12 | 湖南华诚生物资源股份有限公司 | A method of natural mannitol is extracted from mogroside production waste liquid |
| CN109320400B (en) * | 2018-09-30 | 2021-08-10 | 湖南华诚生物资源股份有限公司 | Method for extracting natural mannitol from waste liquid of mogroside production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108658858B (en) | Preparation and refining method of hydroxychloroquine and preparation method of sulfate thereof | |
| CN101812009B (en) | Novel technique for extracting L-tryptophan from fermentation broth | |
| CN102766185B (en) | Method for respectively recovering ursodesoxycholic acid and chenodeoxycholic acid from ursodesoxycholic acid waste mother liquor | |
| CN102399146B (en) | Method for preparing high purity chlorogenic acid | |
| CN102372702A (en) | Preparation method for thiamethoxam | |
| CN101811934A (en) | Preparation method of mannitol | |
| CN109553645B (en) | Method for extracting low-content erythromycin A in fermentation solution | |
| CN102399200B (en) | Suspension crystallization method for preparing crystal form I of linezolid | |
| CN110590587A (en) | Synthetic method of 3-chloro-L-alanine methyl ester hydrochloride | |
| CN112300071B (en) | Synthetic method of high-purity chloroquine phosphate | |
| CN102399205A (en) | Mycophenolic acid purification process | |
| CN104591999A (en) | Long chain organic acid purifying method | |
| CN112142697B (en) | Vc ethyl ether production process | |
| CN106883227B (en) | The method for preparing ergometrine by ergot fermentation waste | |
| CN102311379A (en) | Method for preparing 1-deoxynojirimycin by membrane separation technology | |
| US9206099B2 (en) | Method for producing hydrogenated biphenol | |
| CN105566223A (en) | Crude iminostilbene product recrystallization method | |
| CN114933588A (en) | Refining method of rabeprazole sodium crude product | |
| CN101560188A (en) | Method for separating and purifying 2-methylimidazole crystal impurity | |
| CN112094184B (en) | Method for extracting shikimic acid from ginkgo leaf extract chromatographic wastewater | |
| CN106966980A (en) | The preparation method of high-purity Eptazocine intermediate | |
| CN102603696A (en) | Method for extracting luteolin in peanut hull through supercritical CO2 | |
| CN102559943B (en) | Process method for separating glucose from ionic liquid | |
| CN101781214A (en) | Overdosed esterification production technology for n-octyl gallate | |
| CN100506763C (en) | Method for purifying biphenyl by elution crystallization |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| DD01 | Delivery of document by public notice |
Addressee: Zhang Yi Document name: Notification of Passing Preliminary Examination of the Application for Invention |
|
| SE01 | Entry into force of request for substantive examination | ||
| DD01 | Delivery of document by public notice |
Addressee: Suzhou Baozetang Medical Technology Co.,Ltd. Zhang Yi Document name: the First Notification of an Office Action |
|
| DD01 | Delivery of document by public notice |
Addressee: Suzhou Baozetang Medical Technology Co.,Ltd. Document name: Notification that Application Deemed to be Withdrawn |
|
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100825 |