CN101215383B - Method for preparing acid and base amphiprotic dissoluble chitosan - Google Patents
Method for preparing acid and base amphiprotic dissoluble chitosan Download PDFInfo
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- CN101215383B CN101215383B CN2008100591364A CN200810059136A CN101215383B CN 101215383 B CN101215383 B CN 101215383B CN 2008100591364 A CN2008100591364 A CN 2008100591364A CN 200810059136 A CN200810059136 A CN 200810059136A CN 101215383 B CN101215383 B CN 101215383B
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Abstract
The invention relates to a process for preparing chitosan whose acid and alkali can be dissolved, and the process comprises dissolving chitosan whose molecular weight is 3 million to 10 million and degree of deacetylation is 80% to 90.2%, and adding alcohol and acetic anhydride to evenly mixed, and standing, standing to form gel after adding excess alcoholic-water solution of alkali to completely react, filtering the gel, repeatedly immersing, washing, filtering , drying and disintegrating with distilled water to get chitosan whose acid and alkali can be dissolved. The chitosan which is prepared by the invention can not only be dissolved in acid, but also can be dissolved in alkali to form stable solution, and the problem that chitosan is degraded in acid is avoided, and the invention is convenient for processing the chitosan into chitosan products. The chitosan whose acid and alkali can be dissolved which is prepared by the invention has wide application scope in the aspect of the processing and shaping of chitosan.
Description
Technical field
The present invention relates to the preparation method of chitosan, especially the preparation method of acid and base amphiprotic dissoluble chitosan.
Background technology
Chitosan is processed by the natural macromolecular chitin, it is the renewable green resource of environmental protection, have nontoxic, tasteless, moisture absorption, preserve moisture, breathe freely, antibiotic characteristics such as mothproof, and has an excellent biological compatibility, excellent properties such as biodegradability can be widely used in all many-sides such as medical treatment, health textile and environmental protection.But its molecular arrangement is regular, and intermolecular have an intensive hydrogen bond action, causes its processing characteristics relatively poor, and is the same with intermolecular other polysaccharide macromolecular with strong hydrogen bonding effect, and chitosan is easy dehydration carbonization when heating, promptly decomposes.But present chitosan is unstable in acid, very easily degraded, and be insoluble to alkali, thereby the chitosan forming process can only be used solution method, chitosan is dissolved in the diluted acid moulding in alkali then earlier.The chitosan product mechanical property that processes is not good enough, thereby has limited the development and the application of chitosan.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method that all can the dissolved chitosan in acidity and alkaline environment.
The preparation method of acid and base amphiprotic dissoluble chitosan of the present invention may further comprise the steps:
1) chitosan with the deacetylation 80%-90.2% of molecular weight 300,000-1,000,000 is dissolved in the acetic acid solution that mass concentration is 1%-30%, add pure and mild acetic anhydride then, chitosan: acetate: alcohol: the weight ratio of acetic anhydride is 1: 15-95: 8-75: 0.1-1.5, mix, leave standstill 10-30h;
2) adding excessive volumetric molar concentration is the alcohol-water solution of 0.3-1.5mol/L alkali, and the volume ratio of alcohol-water is 2: 1-1: 4, fully after the reaction, leave standstill the formation gel;
3) with gel-filtration, to soak repeatedly, wash, filter with distilled water, oven dry, pulverizing obtain acid and base amphiprotic dissoluble chitosan.
Above-mentioned chitosan can be the commercial goods.Said alcohol can adopt ethanol or methyl alcohol.
Beneficial effect of the present invention is:
The chitosan of the present invention's preparation can be dissolved in acid, can be dissolved in alkali again and form stable solution, be convenient to chitosan is processed into the chitosan goods, the degradation problem of having avoided chitosan to process in acid and having caused, the acid and base amphiprotic dissoluble chitosan of the present invention's preparation is having wide practical use aspect the machine-shaping of chitosan.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1:
1) chitosan of the deacetylation 80% of molecular weight 700,000 being dissolved in mass concentration is in 25% the acetic acid solution, stir and form clear solution, add methyl alcohol and acetic anhydride then, chitosan: acetate: methyl alcohol: the weight ratio of acetic anhydride is 1: 15: 75: 1.5, mix, leave standstill 30h;
2) adding excessive volumetric molar concentration is the alcohol-water solution of 0.3mol/L alkali, and the volume ratio of alcohol-water is 1: 2, fully after the reaction, leaves standstill the formation gel;
3) with gel-filtration, to soak repeatedly, wash, filter with distilled water, oven dry, pulverizing obtain acid and base amphiprotic dissoluble chitosan.
The chitosan of above-mentioned gained dissolves in the acid solution of pH≤3, also dissolves in the alkaline solution of pH 〉=12.
Embodiment 2:
1) deacetylation 86% chitosan of molecular weight 300,000 being dissolved in mass concentration is in 1% the acetic acid solution, stir and form clear solution, add ethanol and acetic anhydride then, chitosan: acetate: ethanol: the weight ratio of acetic anhydride is 1: 95: 8: 0.1, mix, leave standstill 10h;
2) adding excessive volumetric molar concentration is the alcohol-water solution of 1.5mol/L alkali, and the volume ratio of alcohol-water is 2: 1, fully after the reaction, leaves standstill the formation gel;
3) with gel-filtration, to soak repeatedly, wash, filter with distilled water, oven dry, pulverizing obtain acid and base amphiprotic dissoluble chitosan.
The chitosan of above-mentioned gained dissolves in the acid solution of pH≤3, also dissolves in the alkaline solution of pH 〉=12.
Embodiment 3:
1) deacetylation 90.2% chitosan of molecular weight 1,000,000 being dissolved in mass concentration is in 30% the acetic acid solution, stir and form clear solution, add ethanol and acetic anhydride then, chitosan: acetate: ethanol: the weight ratio of acetic anhydride is 1: 40: 60: 0.6, mix, leave standstill 12h;
2) adding excessive volumetric molar concentration is the alcohol-water solution of 1mol/L alkali, and the volume ratio of alcohol-water is 1: 3, fully after the reaction, leaves standstill the formation gel;
3) with gel-filtration, to soak repeatedly, wash, filter with distilled water, oven dry, pulverizing obtain acid and base amphiprotic dissoluble chitosan.
The chitosan of above-mentioned gained dissolves in the acid solution of pH≤3, also dissolves in the alkaline solution of pH 〉=12.
Claims (1)
1. the preparation method of acid and base amphiprotic dissoluble chitosan may further comprise the steps:
1) chitosan with the deacetylation 80%-90.2% of molecular weight 300,000-1,000,000 is dissolved in the acetic acid solution that mass concentration is 1%-30%, add pure and mild acetic anhydride then, chitosan: acetate: alcohol: the weight ratio of acetic anhydride is 1: 15-95: 8-75: 0.1-1.5, mix, leave standstill 10-30h;
2) adding excessive volumetric molar concentration is the alcohol-water solution of 0.3-1.5mol/L alkali, and the volume ratio of alcohol-water is 2: 1-1: 4, fully after the reaction, leave standstill the formation gel;
3) with gel-filtration, to soak repeatedly, wash, filter with distilled water, oven dry, pulverizing obtain acid and base amphiprotic dissoluble chitosan;
Above-mentioned alcohol is methyl alcohol or ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100591364A CN101215383B (en) | 2008-01-14 | 2008-01-14 | Method for preparing acid and base amphiprotic dissoluble chitosan |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100591364A CN101215383B (en) | 2008-01-14 | 2008-01-14 | Method for preparing acid and base amphiprotic dissoluble chitosan |
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| Publication Number | Publication Date |
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| CN101215383A CN101215383A (en) | 2008-07-09 |
| CN101215383B true CN101215383B (en) | 2010-06-09 |
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| CN2008100591364A Expired - Fee Related CN101215383B (en) | 2008-01-14 | 2008-01-14 | Method for preparing acid and base amphiprotic dissoluble chitosan |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974105B (en) * | 2010-11-12 | 2012-05-23 | 上海海洋大学 | Method for rapidly preparing amphipathic soluble chitosan |
| CN102028966B (en) * | 2010-12-29 | 2013-04-17 | 苏州方策科技发展有限公司 | Manufacturing method of chitosan hemostatic membrane with high water-absorbing swelling performance |
| CN102140177B (en) * | 2011-04-20 | 2012-11-28 | 浙江大学 | Alkaline solvent for dissolving high-molecular-weight chitosan and using method thereof |
| CN107955185A (en) * | 2017-10-27 | 2018-04-24 | 扬州日兴生物科技股份有限公司 | A kind of high-efficiency dissolution method for the chitin that ferments |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1367183A (en) * | 2002-02-04 | 2002-09-04 | 玉环县海洋生物化学有限公司 | Preparation method for hyaluronic acid-like chitosan |
| CN1594406A (en) * | 2004-06-24 | 2005-03-16 | 上海交通大学 | Process for preparing water-soluble chitosan packing film |
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2008
- 2008-01-14 CN CN2008100591364A patent/CN101215383B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1367183A (en) * | 2002-02-04 | 2002-09-04 | 玉环县海洋生物化学有限公司 | Preparation method for hyaluronic acid-like chitosan |
| CN1594406A (en) * | 2004-06-24 | 2005-03-16 | 上海交通大学 | Process for preparing water-soluble chitosan packing film |
Non-Patent Citations (3)
| Title |
|---|
| JP昭58-045202A 1983.03.16 |
| 陈长春.甲壳素的酰基化及其在生物材料上的应用.功能高分子学报第10卷 第2期.1997,第10卷(第2期),276-280. |
| 陈长春.甲壳素的酰基化及其在生物材料上的应用.功能高分子学报第10卷 第2期.1997,第10卷(第2期),276-280. * |
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