CN1165552C - Process for preparing non-derivative low deacetylation water soluble chitin - Google Patents
Process for preparing non-derivative low deacetylation water soluble chitin Download PDFInfo
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- CN1165552C CN1165552C CNB021354863A CN02135486A CN1165552C CN 1165552 C CN1165552 C CN 1165552C CN B021354863 A CNB021354863 A CN B021354863A CN 02135486 A CN02135486 A CN 02135486A CN 1165552 C CN1165552 C CN 1165552C
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- chitin
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- gel
- water soluble
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Abstract
The present invention relates to a method for preparing non-derivative water-solubility chitin with low deacetylation. The method is characterized in that the method comprises the following steps: (1) chitin is processed by alkaline solution; (2) a substance for destroying hydrogen bonds is added to the prepared suspension liquid, water is added to the suspension liquid at the temperature of 0 to 25 DEG C, and then the suspension liquid is dissolved into solution; (3) the pH valve of the solution is adjusted to 8 to 10 by an acid substance; (4) chitin gel is aged, and heated for 10 to 50 minutes at the temperature of 90 to 100 DEG C; (5) the chitin gel is cooled, and the pH valve is adjusted to 5.0 to 7.0 by the acid substance; (6) the ultrafiltration and the desalting are carried out; (7) an organic precipitant is added to the desalted chitin water solution; (8) the chitin water solution is centrifugated to obtain precipitate, and then the precipitate is depressurized and dried. The method destroys the hydrogen bonds in the chitin molecules and among the chitin molecules, and has no need of chemical derivatization to prepare water-solubility chitin with low deacetylation, and the natural activity of the chitin is maintained. The prepared and produced product is in a state of water solution, but not in a state of water-solubility gel.
Description
Technical field
The present invention relates to a kind of chitin, particularly relate to a kind of method for preparing non-derivative low deacetylation water soluble chitin.
Background technology
Chitin is that occurring in nature is only second to cellulosic natural biologic material, it is active substance important in the Living marine resources, it is the macromolecular compound that is made of acetylglucosamine, have different physiological roles such as antitumor, hypotensive, antibiotic, reducing blood-fat, can be used for fields such as industry, agricultural, medical science simultaneously as novel biomaterial.Chitin can not dissolve in the water equal solvent, but at hexafluoroisopropanol or contain in the N,N-DIMETHYLACETAMIDE of lithium chloride and can dissolve.Chitin in water and organic solvent all undissolvable property effect Applications of Chitosan and exploitation.So many people are trying every possible means to make the chitin can be water-soluble.Existing bibliographical information, chitinous deacetylation reaches 50%, just can be water-soluble.But the chitin of 50% deacetylation is to need just to obtain through acetylize through the chitosan that takes off acetyl or height is taken off acetyl.This method is difficult to keep chitinous natural radioactivity strongly because of chemical reaction.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing non-derivative low deacetylation water soluble chitin, it can overcome the above-mentioned shortcoming of prior art.
The method for preparing non-derivative low deacetylation water soluble chitin of the present invention is characterized in that comprising the following steps: that (1) handle chitin with basic solution; (2) in the suspension of gained, add the material that destroys hydrogen bond, and under temperature 0-25 ℃ condition, be dissolved in water into solution; (3) this solution is transferred pH to 8-10 with acidic substance; (4) the chitin gel is aging, heating is 10-50 minute under 90-100 ℃ of condition; (5) cooling is regulated pH to 5.0-7.0 with acidic substance; (6) ultrafiltration desalination; (7) to adding organic precipitant through in the chitin aqueous solution of desalination; (8) the centrifugal precipitation that obtains, drying under reduced pressure, described basic solution is sodium hydroxide, potassium hydroxide or aqua calcis, concentration range is 5-50%, and its consumption is chitinous 5-20 times, and the treatment time is 8-28 hour, the chemical substance of described destruction hydrogen bond has urea, lithium chloride, its concentration expressed in percentage by weight in chitin solution is 1-5%, and described organic precipitant is ethanol or acetone, and consumption is 3-5 a times of chitin solution.
The present invention obtains the water soluble chitin of low deacetylation by destroying in the chitin molecule and intermolecular hydrogen bond without chemical derivatization, kept chitinous natural radioactivity.Preparation is not to be water miscible gel state with the product of producing, but is the state of the aqueous solution.
Embodiment
The pulverous chitin of 1.0Kg is joined in 12000ml 20% aqueous sodium hydroxide solution, kept 24 hours, under agitation condition, add 240g urea, under 5 ℃ of conditions, add the chitin solution of entry 37000ml preparation 2%.PH to 8.0 with concentrated hydrochloric acid adjusting chitin solution forms gel.The chitin gel was worn out 2 hours, and 95 ℃ of heating made the chitin depolymerization in 30 minutes, and cooling is regulated the pH to 6.0 of gel with dilute hydrochloric acid, and formed transparent solution.Chitin solution is filtered, with the ultra-filtration membrane ultrafiltration desalination of molecular weight cut-off 30,000.Volume after the ultrafiltration is 50 liters, adds 150 liters acetone, makes the water soluble chitin precipitation.Centrifugation goes out throw out, and drying under reduced pressure is pulverized the product that promptly obtains non-derivative low deacetylation water soluble chitin, and weight is 950g.This product is as raw materials such as preparation antibacterial fiber, operating sutures, artificial skin, foodstuff additive, ecological agricultural chemical, chitin oligose, parting materials.
Among the present invention the 1st used basic solution of step is strong alkali solutions such as sodium hydroxide, potassium hydroxide or calcium hydroxide, and concentration range is 5-50%, and its consumption is chitinous 5-20 times, and the treatment time is 8-28 hour.The chemical substance of the destruction hydrogen bond in the 2nd step has urea, lithium chloride etc., and its concentration expressed in percentage by weight in chitin solution is 1-5%.Acidic substance in the 3rd step can be strong acid such as hydrochloric acid, sulfuric acid and phosphoric acid.The chitin gel that forms in the 4th step needs through overaging, increasing its intensity, and makes the chitin depolymerization under 90-100 ℃ condition.The cooling of the 5th step is regulated chitin solution with acidic substance, obtains vitreous state, if be muddy and the white precipitate appearance, then is difficult to obtain water miscible chitin.The ultra-filtration membrane of molecular weight cut-off as 1-5 ten thousand used in ultrafiltration desalination in the 6th step, removes the chemical substance of salt and destruction hydrogen bond.Used organic precipitant can be ethanol or acetone in the 7th step, and consumption is 3-5 a times of chitin solution.
Claims (1)
1, a kind of method for preparing non-derivative low deacetylation water soluble chitin is characterized in that comprising the following steps: that (1) handle chitin with basic solution; (2) in the suspension of gained, add the material that destroys hydrogen bond, and under temperature 0-25 ℃ condition, be dissolved in water into solution; (3) this solution is transferred pH to 8-10 with acidic substance; (4) the chitin gel is aging, heating is 10-50 minute under 90-100 ℃ of condition; (5) cooling is regulated pH to 5.0-7.0 with acidic substance; (6) ultrafiltration desalination; (7) to adding organic precipitant through in the chitin aqueous solution of desalination; (8) the centrifugal precipitation that obtains, drying under reduced pressure, described basic solution is sodium hydroxide, potassium hydroxide or aqua calcis, concentration range is 5-50%, and its consumption is chitinous 5-20 times, and the treatment time is 8-28 hour, the chemical substance of described destruction hydrogen bond has urea, lithium chloride, its concentration expressed in percentage by weight in chitin solution is 1-5%, and described organic precipitant is ethanol or acetone, and consumption is 3-5 a times of chitin solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021354863A CN1165552C (en) | 2002-09-19 | 2002-09-19 | Process for preparing non-derivative low deacetylation water soluble chitin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021354863A CN1165552C (en) | 2002-09-19 | 2002-09-19 | Process for preparing non-derivative low deacetylation water soluble chitin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1408729A CN1408729A (en) | 2003-04-09 |
| CN1165552C true CN1165552C (en) | 2004-09-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021354863A Expired - Fee Related CN1165552C (en) | 2002-09-19 | 2002-09-19 | Process for preparing non-derivative low deacetylation water soluble chitin |
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| CN (1) | CN1165552C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059320B (en) * | 2013-01-29 | 2015-02-18 | 武汉大学 | Solvent composition for dissolving chitin |
| CN103059319B (en) * | 2013-01-30 | 2015-03-04 | 武汉大学 | Preparation method of chitin nano fiber |
| CN105732842B (en) * | 2016-02-23 | 2018-01-23 | 李海洋 | A kind of high bioactivity chitin and preparation method thereof |
| CN105622780B (en) * | 2016-03-15 | 2017-11-28 | 武汉大学 | A kind of homogeneous preparation method of quaternized chitin |
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2002
- 2002-09-19 CN CNB021354863A patent/CN1165552C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1408729A (en) | 2003-04-09 |
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Granted publication date: 20040908 Termination date: 20130919 |