CN101665545A - Method for preparing chitosan into water-soluble chitosan oligosaccharide - Google Patents
Method for preparing chitosan into water-soluble chitosan oligosaccharide Download PDFInfo
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- CN101665545A CN101665545A CN200910196098A CN200910196098A CN101665545A CN 101665545 A CN101665545 A CN 101665545A CN 200910196098 A CN200910196098 A CN 200910196098A CN 200910196098 A CN200910196098 A CN 200910196098A CN 101665545 A CN101665545 A CN 101665545A
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Abstract
The invention relates to a method for preparing chitosan into water-soluble chitosan oligosaccharide, which takes the chitosan as raw material and comprises the following steps of: treating the chitosan by rinsing and drying technique, and then soaking in material liquid prepared by purified water and food grade hydrogen peroxide; carrying out microwave radiation degradation treatment, and formingthe mixed liquid of low molecular weight chitosan oligosaccharide which can be dissolved in the material liquid and chitosan part of which is not dissolved; after that, filtering and obtaining the residue of the chitosan and the chitosan oligosaccharide solution; and finally, adding the chitosan oligosaccharide solution into absolute alcohol for alcohol precipitation, and then carrying out suction filtration and drying, thus obtaining the finished product of the water-soluble chitosan oligosaccharide. By adopting the microwave radiation degradation treatment technology and exciting energy bya physical method, the higher molecular weight chitosan is degraded into the low molecular weight water-soluble chitosan oligosaccharide with stable structure, no reaction by-product is generated in the degradation process, and no contaminant is produced; furthermore, compared with the preparation method in the prior art, the method has the advantages of advanced technique, simple working procedures, little production facility investment, high purity of the product, stable quality and the like, thus opening up wide market application prospect for preparing the chitosan oligosaccharide by taking the chitosan as raw material.
Description
Technical field
The present invention relates to the mechanical degradation technical field, particularly a kind of method that Preparation of Chitosan is become water-soluble chitosan oligosaccharide.
Background technology
Oligochitosan, also claim chitin oligo saccharide, be that a kind of chitosan with chitin acquisition after taking off the acetyl processing is a raw material, the plain product of producing by high-tech degraded separation means of a kind of natural high reactivity animal fiber, because its unique pharmacological action and consequent wide market application foreground and be concerned by people day by day, even be described as the laudatory title of " human body the 6th vital principle " and " soft gold ".
Chitin is a kind of macromolecular compound of pure natural, extensively be present in Crustaceans such as shrimp, crab and insect, the algae, its annual biosynthesizing stock number is up to more than 10,000,000,000 tons, wherein halobiontic growing amount is the second largest nexhaustible natural biology resource that is only second to vegetable fibre on the earth about more than 1,000,000,000 tons.Owing to chemical property torpescence, the poorly water-soluble of chitin are used extremely restriction.Biologists discover, chitin is taken off the chitosan that obtains after acetyl is handled be dissolvable in water in the part food, thereby obtain topical application.But since the molecular weight of chitosan usually at hundreds of thousands of between millions of, can not be dissolved in the aqueous solvent, thereby still have more serious application limitation.In recent years, biologists have just carried out big quantity research, have obtained the widespread use achievement in research the molecular weight of the chitosan aspect of degrading, the chitosan that the activity of having grasped low-molecular weight chitoglycan can be greatly improved, be lower than certain molecular weight can be dissolved in the aqueous solvent fully, and molecular weight is lower than 10,000 chitosan called after " oligochitosan " after will degrading, and embody its using value widely gradually in fields such as food, medicine, daily-use chemical industry, environmental protection, agriculturals at present.
Become the method for oligochitosan to mainly contain chemical degradation method and enzymolysis process at present Preparation of Chitosan.The shortcoming of chemical degradation method is to be easy to generate byproduct of reaction, finally influences product purity, thereby quality product is than difficult control, less stable; Enzymolysis process is to reach the degraded purpose in the mode of utilizing some enzyme to ftracture, change molecular structure specifically, owing in whole degradation process, there not being the method that other byproducts of reaction become at present many usefulness, its shortcoming is that operation more complicated, degradation efficiency are low, the product cost height, only be in laboratory study, short run trial production stage at present, reach commercial scale production still has the series of process technical problem to solve.
Summary of the invention
The objective of the invention is to provide that a kind of operation is fairly simple, degradation efficiency is high, constant product quality, help reducing product cost and the method that Preparation of Chitosan is become water-soluble chitosan oligosaccharide of carrying out commercial scale production.
Of the present invention Preparation of Chitosan is become the method for water-soluble chitosan oligosaccharide is such: the polymer chitosan that obtains after taking off acetyl with chitin is a raw material, drops into by water purification (H after rinsing, stoving process physical treatment
2O) 80-90% and food grade hydrogen peroxide (H
2O
2) soak in the formulated feed liquid of the weight ratio of 10-20%, obtain the miscellany of chitosan and feed liquid; In the microwave radiation reactor, carry out microwave frequency radiation then, most chitosan becomes lower molecular weight, is dissolved in oligochitosan and the undegradable chitosan residue of small portion in the described feed liquid, the oligochitosan solution that obtains undegradable chitosan residue after filtering and degraded after degraded; Return in the described feed liquid after undegradable chitosan residue compiled and deal with, the alcohol that dehydrated alcohol is housed in the oligochitosan solution of having degraded is sent into is analysed in the container alcohol and is analysed, forms solid-state oligochitosan throw out and useless alcohol; The solid-state oligochitosan that suction filtration falls to give up alcohol, will obtain is done oven dry and is handled, and looks over so as to check then, analysis and classification, obtains the water-soluble chitosan oligosaccharide finished product.In addition, for analyse at alcohol with the suction filtration process in useless alcohol isolated dehydrated alcohol after distilling of obtaining be returned to alcohol and analyse and continue in the container to use, all the other raffinates both can have been made further art breading, extract monose, also can be as the fuel of the useless alcohol of distillation.
In addition, the time that described chitosan soaks in described feed liquid is more than half an hour, serves as preferred with 1-2 hour; Described chitosan and the miscellany of the feed liquid time and the radiating temperature correlation of in the microwave radiation reactor, carrying out microwave frequency radiation after soaking, the radiating time is no less than 5 hours, with 5-6 hour was good, and temperature is not higher than 80 ℃, was good with 60 ℃-80 ℃; Described microwave radiation reactor is common commercially available prod.
Preparation of Chitosan is become the method for water-soluble chitosan oligosaccharide based on the present invention of above-mentioned design, owing to adopted by the feed liquid that includes water purification and hydrogen peroxide, and be equipped with microwave radiation degradation treatment technology, with the sharp energy of penetrating of the method for physics, make difficult water-soluble polymer degradation of chitosan water-soluble for energy, and molecular structure stabilized, relative molecular weight is lower than 3000 oligochitosan, production facility required in whole degradation technique process is few, also contamination-free produces and discharges, also not having other byproducts of reaction in the degradation process generates, thereby compare with the method for preparing water-soluble chitosan oligosaccharide of prior art, has the technology advanced person, operation is simple, economic less investment, product purity is high and quality is steady, and can automatization circulation distinct advantages such as work continuously, favourablely guarantee quality product, improve productive rate, reduce production costs, environmental protection, energy-conservation and commercial scale production, thereby the present invention is will be that the Preparation of Chitosan that raw material is made becomes water-soluble chitosan oligosaccharide to start a kind of effective brand-new route with the chitin, the chemical degradation method and the existing many weak points of enzymolysis process of present more use have effectively been overcome, for being that the chitosan that raw material is made has been opened up wide market application prospect with the chitin, thereby has significant technical advance, extremely strong practicality and valuable economy.
Description of drawings
Accompanying drawing is the process flow diagram of the embodiment of the invention.
Embodiment
Below in conjunction with accompanying drawing and exemplary embodiments the present invention is further described.
In the accompanying drawings, based on the present invention Preparation of Chitosan is become the method for water-soluble chitosan oligosaccharide, its technical process is: the chitosan with private-use class is a raw material, drops in advance by water purification (H after rinsing, stoving process physical treatment
2O) 80-90% and food grade hydrogen peroxide (H
2O
2) soaked 1-2 hour in the formulated feed liquid of the weight ratio of 10-20%; In the microwave radiation reactor, carry out being lower than under 80 ℃ of environment 5-6 hour microwave frequency radiation then in temperature, most chitosan just can be biodegradable into to lower molecular weight, is dissolved in oligochitosan and the undegradable chitosan residue of small portion in the described feed liquid, the oligochitosan solution that obtains undegradable chitosan residue after filtering and degraded, return in the described feed liquid after undegradable chitosan residue compiles and deal with, the oligochitosan solution of having degraded is sent into throw out and the useless alcohol that solid-state oligochitosan was analysed, formed to alcohol in the dehydrated alcohol; The solid-state oligochitosan that suction filtration falls to give up alcohol, will obtain is done oven dry and is handled, and looks over so as to check then, analysis and classification, obtain can be water-soluble, relative molecular weight is lower than 3000 oligochitosan finished product.In addition, for analyse at alcohol with the suction filtration process in useless alcohol isolated dehydrated alcohol after distilling of obtaining be returned to alcohol and analyse and continue in the container to use, all the other raffinates are for use as the fuel of the useless alcohol of distillation.
Claims (6)
1. one kind becomes the method for water-soluble chitosan oligosaccharide with Preparation of Chitosan, it is characterized in that technical process is:
A. the polymer chitosan that obtains after taking off acetyl with chitin is a raw material, drops into by water purification (H after rinsing, stoving process physical treatment
2O) 80-90% and food grade hydrogen peroxide (H
2O
2) soak in the feed liquid that is mixed with of the weight ratio of 10-20%, obtain the miscellany of chitosan and feed liquid;
B. will in the microwave radiation reactor, carry out microwave frequency radiation through the chitosan after soaking and the miscellany of feed liquid, most chitosan becomes lower molecular weight, is dissolved in oligochitosan and the undegradable chitosan residue of small portion in the described feed liquid, the oligochitosan solution that obtains undegradable chitosan residue after filtering and degraded after degraded;
C. return in the described feed liquid after undegradable chitosan residue being compiled and deal with again, the oligochitosan solution of having degraded is sent in the dehydrated alcohol alcohol analyse, form solid-state oligochitosan throw out and useless alcohol;
D. suction filtration falls to give up alcohol, the solid-state oligochitosan that will obtain does oven dry and handle, and looks over so as to check then, analysis and classification, obtains relative molecular weight and is lower than 3000 water-soluble chitosan oligosaccharide finished product.
2. according to claim 1 Preparation of Chitosan being become the method for water-soluble chitosan oligosaccharide, it is characterized in that the time that described chitosan soaks is more than half an hour in described feed liquid, served as preferred with 1-2 hour.
3. the method that Preparation of Chitosan is become water-soluble chitosan oligosaccharide according to claim 1, it is characterized in that described chitosan and the miscellany of feed liquid time of carrying out microwave frequency radiation in the microwave radiation reactor after soaking is no less than 5 hours, with 5-6 hour was good, the temperature of microwave frequency radiation is not higher than 80 ℃, is good with 60 ℃-80 ℃.
4. according to claim 1 Preparation of Chitosan is become the method for water-soluble chitosan oligosaccharide, it is characterized in that described useless alcohol obtains dehydrated alcohol and raffinate after distillation.
5. described Preparation of Chitosan is become the method for water-soluble chitosan oligosaccharide according to claim 1 or 4, it is characterized in that described dehydrated alcohol is sent to alcohol and analyses and continue in the container to use.
6. described Preparation of Chitosan is become the method for water-soluble chitosan oligosaccharide according to claim 1 or 4, it is characterized in that described raffinate extracts monose through further handling the back, or for use as the useless pure fuel of distillation.
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| CN200910196098A CN101665545A (en) | 2009-09-22 | 2009-09-22 | Method for preparing chitosan into water-soluble chitosan oligosaccharide |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102180993A (en) * | 2011-05-05 | 2011-09-14 | 大连鑫蝶泓祥甲壳素有限公司 | Production method of chitooligosaccharide |
| CN102321123A (en) * | 2011-08-12 | 2012-01-18 | 高翔 | Preparation device of water-soluble chitosan oligosaccharide |
| CN103044574A (en) * | 2013-01-11 | 2013-04-17 | 河北工业大学 | Process for preparing narrow-distribution chitosan with controllable molecular weight through microwave-H2O2 combined degradation method |
| CN103073600A (en) * | 2013-01-18 | 2013-05-01 | 上海峰瑜生物科技发展有限公司 | Method for preparing water soluble chitosan oligosaccharide |
| CN103641936A (en) * | 2013-12-09 | 2014-03-19 | 吴彪 | Method for preparing water-soluble chitosan oligosaccharide by adopting ultrafiltration and nanofiltration |
| CN106755208A (en) * | 2016-12-30 | 2017-05-31 | 山东智顺进出口有限公司 | The method that low energy consumption digests shitosan preparation solution body shell oligosaccharides |
| CN109400948A (en) * | 2018-09-10 | 2019-03-01 | 中国科学院金属研究所 | A kind of method that microwave process reinforcing prepares different deacetylations and degree of polymerization series chitooligosaccharide- |
| CN112194736A (en) * | 2020-09-24 | 2021-01-08 | 长春工业大学 | Method for preparing chitosan oligosaccharide by microwave-peroxide coupling degradation of chitosan |
-
2009
- 2009-09-22 CN CN200910196098A patent/CN101665545A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102180993A (en) * | 2011-05-05 | 2011-09-14 | 大连鑫蝶泓祥甲壳素有限公司 | Production method of chitooligosaccharide |
| CN102321123A (en) * | 2011-08-12 | 2012-01-18 | 高翔 | Preparation device of water-soluble chitosan oligosaccharide |
| CN102321123B (en) * | 2011-08-12 | 2014-09-03 | 高翔 | Preparation device of water-soluble chitosan oligosaccharide |
| CN103044574A (en) * | 2013-01-11 | 2013-04-17 | 河北工业大学 | Process for preparing narrow-distribution chitosan with controllable molecular weight through microwave-H2O2 combined degradation method |
| CN103073600A (en) * | 2013-01-18 | 2013-05-01 | 上海峰瑜生物科技发展有限公司 | Method for preparing water soluble chitosan oligosaccharide |
| CN103073600B (en) * | 2013-01-18 | 2015-08-26 | 上海峰瑜生物科技发展有限公司 | A kind of method preparing water-soluble chitosan oligosaccharide |
| CN103641936A (en) * | 2013-12-09 | 2014-03-19 | 吴彪 | Method for preparing water-soluble chitosan oligosaccharide by adopting ultrafiltration and nanofiltration |
| CN103641936B (en) * | 2013-12-09 | 2016-03-23 | 吴彪 | A kind of method adopting ultrafiltration and nanofiltration to prepare water-soluble chitosan oligosaccharide |
| CN106755208A (en) * | 2016-12-30 | 2017-05-31 | 山东智顺进出口有限公司 | The method that low energy consumption digests shitosan preparation solution body shell oligosaccharides |
| CN109400948A (en) * | 2018-09-10 | 2019-03-01 | 中国科学院金属研究所 | A kind of method that microwave process reinforcing prepares different deacetylations and degree of polymerization series chitooligosaccharide- |
| CN109400948B (en) * | 2018-09-10 | 2021-05-28 | 中国科学院金属研究所 | Method for preparing chitosan oligosaccharides with different deacetylation degrees and polymerization degrees in enhanced microwave process |
| CN112194736A (en) * | 2020-09-24 | 2021-01-08 | 长春工业大学 | Method for preparing chitosan oligosaccharide by microwave-peroxide coupling degradation of chitosan |
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Open date: 20100310 |