CN1460687A - Method for preparing high-qualtiy chitosan - Google Patents
Method for preparing high-qualtiy chitosan Download PDFInfo
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- CN1460687A CN1460687A CN 03127930 CN03127930A CN1460687A CN 1460687 A CN1460687 A CN 1460687A CN 03127930 CN03127930 CN 03127930 CN 03127930 A CN03127930 A CN 03127930A CN 1460687 A CN1460687 A CN 1460687A
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- sodium hydroxide
- chitin
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Abstract
The preparation method of high-quality chitosan includes the following steps: making chitin produce reaction in soduium hydroxide solution, then transferring the above-mentioned material into alcoholic solution containing sedium hydroxide, making reflux reaction for 1-5 hr. filtering and washing to neutrality, drying so as to invented finished product with high molecular weight and good colour, and said finished product high quality chitosan is easy to pulverize, can be used for producing medical product with high mesh.
Description
Technical field
The present invention relates to a kind of preparation method of high-quality chitosan.
Background technology
Chitin has another name called chitin, is present in a large number in the crust of ocean arthropods (as shrimp, crab), also is present in the cell walls of insect, alga cells film and higher plant, and annual biosynthesizing amount reaches 10,000,000,000 tons more than.Therefore, it is a kind of inexhaustible, nexhaustible renewable resource.Because the effect of intermolecular and intramolecular hydrogen bond, chitin are insoluble in diluted acid, alkali and the common organic solvent, thereby have limited its widespread use.And chitin removes the product of ethanoyl is chitosan; it is soluble in the dilute acid soln; because have good film forming, preserve moisture, the unique functions such as affinity of absorption and pair cell, obtained widespread use at aspects such as papermaking, weaving, daily use chemicals, water treatment and biomaterial for medical purpose.But different purposes requires different to the molecular weight of chitosan with deacetylation.As utilize the film forming and the absorb oil performance of chitosan, just require high molecular and high deacetylized chitosan; Utilize chitosan to increase the function of immunity and promotion plant-growth, then need low-molecular-weight chitosan.So, seek comparatively convenient or ideal deacetylation method, still be the focus of Recent study.
Have than big difference with its physico-chemical property of chitosan that different reaction conditionss obtains with a kind of chitin.In recent years, relevant low-molecular weight chitoglycan preparation method has obtained than quantum jump.But the research to high-quality high molecular weight chitosan is less.Usually in the aqueous solution, high-alkalinity and high temperature can obtain the chitosan that height takes off acetyl, but have also caused simultaneously deficiencies such as the decline of molecular weight and the jaundice of product color and luster.In order to obtain high molecular and high deacetylized product simultaneously, be necessary existing preparation technology is improved.
Summary of the invention
Purpose of the present invention is exactly the deficiency that overcomes in the above-mentioned background, and a kind of manufacture method that is fit to prepare from different source chitins high molecular, chitosan with high deacetylation degree is provided.
The technical measures that the present invention takes are: chitin is placed sodium hydroxide solution, in 70-100 ℃ of reaction 2-4 hour, change over to then in the alcohol solution that contains sodium hydroxide, back flow reaction 1-5 hour, filter, wash, dry, pulverize the chitosan that promptly gets medical grade.
Among the present invention, concentration sodium hydroxide is between 30-60%wt, and the weight ratio of chitin and sodium hydroxide solution is 1: 10-20.
Among the present invention, sodium hydroxide is 1 with the weight ratio of alcohol in the alcoholic solution of sodium hydroxide: 3-10, used alcohol can be methyl alcohol, ethanol or Virahol.
Among the present invention, used chitin can be to come from shrimp, the crab shell, also can come from fly puparium, duster worm, pine moth and squid bone.
In present method owing to adopted organic solvent, it has stronger perviousness than water, add alcohol and participate in deacetylation with the form of sodium alkoxide in sodium hydroxide solution, it is checked colors and have certain extraction simultaneously, thereby higher deacetylation and color and luster are preferably arranged.This technological reaction temperature is not high, so can obtain the high-molecular weight product.In addition, the alcoholic solution in this technology is recyclable to be utilized again, and production cost is low, the characteristics of operability so have.
According to the chitosan that preparation method of the present invention produces, the sheet that is white in color is easy to pulverize, and molecular weight is greater than 800,000, and deacetylation is greater than 90%.
Embodiment
Below in conjunction with embodiment invention is described further:
Embodiment 1
Take by weighing the clean shrimps chitin of 10g and add in the sodium hydroxide solution of 150ml 60%, be warming up to 80 ℃ of reactions 3 hours, change over to after the filtration in the aqueous isopropanol that contains 20g sodium hydroxide, reflux temperature is reaction 3h down, filters, and washes with water to neutrality, oven dry is pulverized promptly.The molecular weight of products obtained therefrom is 1,180,000, and deacetylation is 92%.
Embodiment 2
Take by weighing the clean crab class of 10g chitin and add in the sodium hydroxide solution of 200ml 47%, be warming up to 90 ℃ of reactions 3 hours, change over to after the filtration in the ethanolic soln that contains 25g sodium hydroxide, reflux temperature is reaction 3h down, filters, and washes with water to neutrality, and oven dry is pulverized promptly.The molecular weight of products obtained therefrom is 1,600,000, and deacetylation is 90%.
Embodiment 3
Take by weighing the clean duster worm of 10g chitin and add in the sodium hydroxide solution of 180ml 50%, be warming up to 90 ℃ of reactions 3 hours, change over to after the filtration in the methanol solution that contains 15g sodium hydroxide, reflux temperature is reaction 4h down, filters, and washes with water to neutrality, oven dry is pulverized promptly.The molecular weight of products obtained therefrom is 820,000, and deacetylation is 93%.
Embodiment 4
Take by weighing 10g squid bone chitin and add in the sodium hydroxide solution of 120ml 40%, be warming up to 100 ℃ of reactions 3 hours, change over to after the filtration in the ethanolic soln that contains 10g sodium hydroxide, reflux temperature is reaction 2h down, filters, and washes with water to neutrality, and oven dry is pulverized promptly.The molecular weight of products obtained therefrom is 3,900,000, and deacetylation is 95%.
The physicochemical property of de-acetyl chitin
| Physical and chemical index | Deacetylation (%) | Molecular weight (* 10 6) | Color and luster | Pulverize complexity |
| Embodiment 1 | ????92 | ?????1.18 | In vain | Easily |
| Embodiment 2 | ????90 | ?????1.60 | In vain | Easily |
| Embodiment 3 | ????93 | ?????0.82 | Little Huang | Be easier to |
| Embodiment 4 | ????95 | ?????3.90 | In vain | Easily |
| Not solubilizing agent and embodiment 1 contrast | ????85 | ?????0.92 | Pale yellow | Be not easy |
Claims (4)
1. the preparation method of a high-quality chitosan, it is characterized in that placing sodium hydroxide solution in 70-100 ℃ of reaction 2-4 hour chitin, change over to then in the alcoholic solution that contains sodium hydroxide, back flow reaction 1-5 hour, filter, wash to neutral, oven dry, pulverize promptly.
2. in accordance with the method for claim 1, it is characterized in that concentration sodium hydroxide between 30-60wt%, the weight ratio of chitin and sodium hydroxide solution is 1: 10-20.
3. in accordance with the method for claim 1, it is characterized in that in the alcoholic solution of sodium hydroxide that sodium hydroxide is 1 with the weight ratio of alcohol: 3-10, used alcohol are methyl alcohol, ethanol or Virahol.
4. according to right 1 described method, its feature is that also the source of chitin obtains from shrimp, crab shell, fly puparium, duster worm shell, pine moth and squid bone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03127930 CN1217957C (en) | 2003-04-24 | 2003-04-24 | Method for preparing high-qualtiy chitosan |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03127930 CN1217957C (en) | 2003-04-24 | 2003-04-24 | Method for preparing high-qualtiy chitosan |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1460687A true CN1460687A (en) | 2003-12-10 |
| CN1217957C CN1217957C (en) | 2005-09-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03127930 Expired - Fee Related CN1217957C (en) | 2003-04-24 | 2003-04-24 | Method for preparing high-qualtiy chitosan |
Country Status (1)
| Country | Link |
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| CN (1) | CN1217957C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235101B (en) * | 2008-03-13 | 2010-06-02 | 华东师范大学 | Preparation method for water-soluble low molecular weight chitosan |
| CN104693318A (en) * | 2015-03-24 | 2015-06-10 | 中国科学院海洋研究所 | Beta-chitosan preparation method |
| CN104788584A (en) * | 2014-01-17 | 2015-07-22 | 厦门大学 | New technology for clean production of chitosan and carboxymethyl chitosan by using crustacean shell raw materials |
| CN105111331A (en) * | 2015-09-29 | 2015-12-02 | 天津科技大学 | Method for preparing chitosan by using high boiling solvent-NaOH system |
| CN105794948A (en) * | 2016-03-25 | 2016-07-27 | 浙江海洋学院 | Squid bone antimicrobial agent used for frozen cooked mussels and preparation method thereof |
| CN105903024A (en) * | 2015-12-14 | 2016-08-31 | 威海百合生物技术股份有限公司 | Use method of chitosan as disintegrating agent in tablet |
| CN106008748A (en) * | 2016-07-01 | 2016-10-12 | 浙江金壳药业有限公司 | Energy-saving and environment-friendly production method of chitosan and by-product |
| CN107573442A (en) * | 2017-10-16 | 2018-01-12 | 南通大学 | A kind of method that chitosan is prepared using supercritical carbon dioxide reaction technology |
-
2003
- 2003-04-24 CN CN 03127930 patent/CN1217957C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235101B (en) * | 2008-03-13 | 2010-06-02 | 华东师范大学 | Preparation method for water-soluble low molecular weight chitosan |
| CN104788584A (en) * | 2014-01-17 | 2015-07-22 | 厦门大学 | New technology for clean production of chitosan and carboxymethyl chitosan by using crustacean shell raw materials |
| CN104788584B (en) * | 2014-01-17 | 2021-08-10 | 厦门大学 | Novel process for cleanly producing chitosan and carboxymethyl chitosan by using crustacean raw materials |
| CN104693318A (en) * | 2015-03-24 | 2015-06-10 | 中国科学院海洋研究所 | Beta-chitosan preparation method |
| CN105111331A (en) * | 2015-09-29 | 2015-12-02 | 天津科技大学 | Method for preparing chitosan by using high boiling solvent-NaOH system |
| CN105903024A (en) * | 2015-12-14 | 2016-08-31 | 威海百合生物技术股份有限公司 | Use method of chitosan as disintegrating agent in tablet |
| CN105794948A (en) * | 2016-03-25 | 2016-07-27 | 浙江海洋学院 | Squid bone antimicrobial agent used for frozen cooked mussels and preparation method thereof |
| CN106008748A (en) * | 2016-07-01 | 2016-10-12 | 浙江金壳药业有限公司 | Energy-saving and environment-friendly production method of chitosan and by-product |
| CN107573442A (en) * | 2017-10-16 | 2018-01-12 | 南通大学 | A kind of method that chitosan is prepared using supercritical carbon dioxide reaction technology |
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| Publication number | Publication date |
|---|---|
| CN1217957C (en) | 2005-09-07 |
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