CN1256370C - Process for preparing water-soluble chitosan packing film - Google Patents
Process for preparing water-soluble chitosan packing film Download PDFInfo
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- CN1256370C CN1256370C CN 200410025384 CN200410025384A CN1256370C CN 1256370 C CN1256370 C CN 1256370C CN 200410025384 CN200410025384 CN 200410025384 CN 200410025384 A CN200410025384 A CN 200410025384A CN 1256370 C CN1256370 C CN 1256370C
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Abstract
The present invention discloses a preparation method of water soluble chitosan packaging films. Through making use of the water solubility of chitosan with a deacetylation degree of 50% and respectively using water, water and ethanol or water and propanone as solvent, after chitosan with a deacetylation degree of 50% is dissolved, the chitosan is cast into a film under the condition of neutral pH value. Meanwhile, eatable ingredients, such as starch and sugar, and water soluble ingredients, such as polyvinyl alcohol, can be added before the film is cast. The preparation method has the characteristics of short preparation time, neutrality of the film and no requirement of post-treatment. The prepared chitosan film with water solubility and edibility can be used as an inner lining film or a packaging film of products.
Description
Technical field
The present invention relates to a kind of preparation method of water-soluble chitosan packing film, this chitosan film has water-soluble and characteristics edibility, can be used as commodity inner lining film or packing film and uses.
Background technology
Chitin is that N-ethanoyl-D-glucose passes through the straight-chain polysaccharide that β (1 → 4) glycosidic link links to each other, extensively is present in crustacean and the arthropods heart bacteria cell wall, and be one of organic compound that is only second on the earth cellulosic most abundant.Chitin is through taking off product---the chitosan that acetyl is handled, owing to contain the higher free amine group of a large amount of activity in the molecular structure, therefore have some unique physico-chemical property and physiological functions, have broad application prospects at medicine, food, makeup, agricultural and environmental protection aspects, particularly have many effects to the human body beneficial with this chitosan biological health-care product of making, by European and American countries be described as dewater, the sixth-largest vital principle of needed by human body outside protein, carbohydrate, Mierocrystalline cellulose and the mineral substance.Chitosan is used also increasingly extensive owing to have excellent biodegradability, film-forming properties and certain restraining and sterilizing bacteria effect in the research in a plurality of fields such as medicine, preparation and food fresh keeping.
In " chitosan " (Chemical Industry Press that Jiang Tingda writes, 2001, the 170th page) in the general preparation method of the chitosan film recorded and narrated be: chitosan is dissolved in 2% acetic acid aqueous solution, be made into concentration and be 0.1~2% solution, filter and remove impurity, filtrate is poured into casting film-forming on culture dish, sheet glass, polyethylene film or the rigid plastics, solvent evaporated at room temperature, place alkali lye to soak then, wash lixiviating with water after solidifying well, carefully peel off, natural airing or oven dry, a chitosan film.This preparation method's time is longer, because of the chitosan solution of preparing is acid, needs to use in the alkali lye after the film forming and the acid in the chitosan film, is washed to neutrality then.Preparation technology is relatively complicated thus.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of water-soluble chitosan packing film is provided, it is shorter to have preparation time, it is neutral that film is, do not need the characteristics of aftertreatment, the chitosan film that makes has water-soluble and characteristics edibility, can be used as commodity inner lining film or packing film and uses.
For achieving the above object; in the technical scheme of the present invention; utilize the water dissolution performance of 50% deacetylation chitosan; under the acetic acid aqueous solution homogeneous phase condition, prepare 50% deacetylation chitosan by the chitosan with high deacetylation degree raw material with the diacetyl oxide acetylization reaction; Yi Shui, water and ethanol or water and acetone are solvent respectively then; under the pH neutrallty condition; after the dissolving of 50% deacetylation chitosan; casting film; can add simultaneously edibility composition such as starch, sugar, make film after also can adding water soluble component such as polyvinyl alcohol.
The concrete steps of the inventive method are as follows:
20g chitosan raw material (deacetylation is 94%) is dissolved in the 1L 2wt% acetic acid aqueous solution, drip the 25.4g diacetyl oxide under the stirring at room, behind the stirring reaction 1h, mixed solution is added dropwise in the 1L 0.5mol/l potassium hydroxide-ethanol solution, obtain flocks, filter out precipitation, to neutral, drying obtains 50% deacetylation chitosan product with washing with alcohol.
With the water-soluble solution of 50% deacetylation chitosan, volume percent is that 1~50% aqueous ethanolic solution or volume percent are in 1~50% the aqueous acetone solution, be made into the solution that chitosan concentration is 0.1~2.5wt%, solution is poured into casting film-forming on culture dish, sheet glass, polyethylene film or the rigid plastics, at room temperature solvent evaporated behind the freezing film, is carefully peeled off, nature airing or oven dry, chitosan film.
The present invention can be after being made into the solution that concentration is 0.1~2.5wt% with 50% deacetylation chitosan, adds 0.5g/100ml edibility composition such as starch and sweeting agent, makes film after also can adding 0.5g/100ml water soluble component such as polyvinyl alcohol.
The present invention can be by adopting the different size mould, or the different chitosan dosage of same size mould adjust the thickness of film, and it is water-soluble that the film of different thickness all is, but the elevated temperature accelerate dissolution.
The present invention utilizes the water dissolution performance of 50% deacetylation chitosan, and Yi Shui, water and ethanol or water and acetone are solvent, casting film under the pH neutrallty condition, need not pass through the alkali neutralizing treatment, can directly obtain neutral chitosan film, it is shorter to have a preparation time, does not need the characteristics of aftertreatment.Because 50% deacetylation chitosan can dissolve in the pH of broad scope, has improved the restriction of film forming pH condition, the chitosan film that makes has water-soluble and characteristics edibility, can be used as commodity inner lining film or packing film and uses.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is further described.
Embodiment 1:
20g chitosan raw material (deacetylation is 94%) is dissolved in the 1L 2wt% acetic acid aqueous solution, drip the 25.4g diacetyl oxide under the stirring at room, behind the stirring reaction 1h, mixed solution is added dropwise in the 1L 0.5mol/l potassium hydroxide-ethanol solution, obtain flocks, filter out precipitation, to neutral, drying obtains 50% deacetylation chitosan product with washing with alcohol.
1g 50% deacetylation chitosan is dissolved in the 100ml aqueous solution, is made into the solution that chitosan concentration is 1.0wt%, solution is poured into casting film-forming on the polyethylene film, at room temperature solvent evaporated behind the freezing film, is carefully peeled off, nature airing or oven dry, chitosan film.
Implementation result: chitosan film is neutrality, when the thickness of control chitosan film is 0.05mm, and i.e. dissolving in 1 minute in 20 ℃ of water, dissolving is accelerated in 80 ℃ of water, when the adjustment film thickness is 0.1mm, dissolving in 2 minutes in 20 ℃ of water.
Embodiment 2:
Same method makes 50% deacetylation chitosan product among the employing embodiment 1.
1g 50% deacetylation chitosan is added in the 50ml water, stirring makes dissolving form clear solution, add the 50ml dehydrated alcohol, stir evenly, be made into the solution that chitosan concentration is 1.1wt%, solution is poured into casting film-forming on the polyethylene film, at room temperature solvent evaporated behind the freezing film, is carefully peeled off, nature airing or oven dry, chitosan film.
Implementation result: film forming behind the chitosan film drying at room temperature 4h, chitosan film are neutral, when the thickness of control chitosan film is 0.05mm, i.e. dissolving in 1 minute in 20 ℃ of water, dissolving is accelerated in 80 ℃ of water, when the adjustment film thickness is 0.1mm, and dissolving in 2 minutes in 20 ℃ of water.
Embodiment 3:
Make 50% deacetylation chitosan product with method same among the embodiment 1.
1g 50% deacetylation chitosan is added in the 50ml water, stirring makes dissolving form clear solution, add 50ml acetone, stir, be made into the solution that chitosan concentration is 1.1wt%, solution is poured into casting film-forming on the polyethylene film, at room temperature solvent evaporated behind the freezing film, is carefully peeled off, nature airing or oven dry, chitosan film.
Implementation result: film forming behind the chitosan film drying at room temperature 4h, chitosan film are neutral, when the thickness of control chitosan film is 0.05mm, i.e. dissolving in 1 minute in 20 ℃ of water, dissolving is accelerated in 80 ℃ of water, when the adjustment film thickness is 0.1mm, and dissolving in 2 minutes in 20 ℃ of water.
Embodiment 4:
Make 50% deacetylation chitosan product with method same among the embodiment 1.
1g 50% deacetylation chitosan is dissolved in the 100ml aqueous solution, be made into the solution that chitosan concentration is 1.0wt%, with 0.5g edibility composition---starch and sugar add solution, stirring disperses dissolving, and mixture is poured into casting film-forming on the culture dish, at room temperature solvent evaporated, behind the freezing film, carefully peel off, natural airing or oven dry, chitosan film.
Implementation result: chitosan film is direct-edible.
Embodiment 5:
Make 50% deacetylation chitosan product with method same among the embodiment 1.
1g 50% deacetylation chitosan is dissolved in the 100ml aqueous solution, be made into the solution that chitosan concentration is 1.0wt%, add the 0.5g water soluble component---stir behind the polyvinyl alcohol and make it dissolving, then solution is poured into casting film-forming on the sheet glass, at room temperature solvent evaporated behind the freezing film, is carefully peeled off, nature airing or oven dry, chitosan film.
Implementation result: chitosan film is good water-solubility.
Claims (2)
1, a kind of preparation method of water-soluble chitosan packing film, it is characterized in that at first being that 94% chitosan material dissolution is in 1L 2wt% acetic acid aqueous solution with the 20g deacetylation, drip the 25.4g diacetyl oxide under the stirring at room, behind the stirring reaction 1 hour, mixed solution is added dropwise in the 1L 0.5mol/l potassium hydroxide-ethanol solution, obtain flocks, filter out precipitation, extremely neutral with washing with alcohol, drying obtains 50% deacetylation chitosan product, then with the water-soluble solution of 50% deacetylation chitosan, volume percent is that 1~50% aqueous ethanolic solution or volume percent are in 1~50% the aqueous acetone solution, be made into the solution that chitosan concentration is 0.1~2.5wt%, solution is poured into culture dish, sheet glass, casting film-forming on polyethylene film or the rigid plastics, solvent evaporated at room temperature, peel off behind the freezing film, natural airing or oven dry, chitosan film.
2, the preparation method of water-soluble chitosan packing film as claimed in claim 1, after it is characterized in that 50% deacetylation chitosan is made into the solution that concentration is 0.1~2.5wt%, add 0.5g/100ml edibility composition, make film after perhaps adding the 0.5g/100ml water soluble component.
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CN 200410025384 CN1256370C (en) | 2004-06-24 | 2004-06-24 | Process for preparing water-soluble chitosan packing film |
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CN 200410025384 CN1256370C (en) | 2004-06-24 | 2004-06-24 | Process for preparing water-soluble chitosan packing film |
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CN1256370C true CN1256370C (en) | 2006-05-17 |
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Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
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JP4866173B2 (en) * | 2006-01-25 | 2012-02-01 | 大日精化工業株式会社 | Hydroxyalkylated chitosan solution |
US20080110370A1 (en) * | 2006-11-13 | 2008-05-15 | Verrall Andrew P | Water-soluble film |
CN101215383B (en) * | 2008-01-14 | 2010-06-09 | 浙江大学 | Method for preparing acid and base amphiprotic dissoluble chitosan |
CN101704956B (en) * | 2009-11-19 | 2011-11-09 | 浙江理工大学 | Preparation method for oxygen permeable degradable wrapping film |
CN102619143B (en) * | 2012-04-13 | 2014-07-23 | 东华大学 | Flocculent fiber film felt and preparation method thereof |
CN102691230B (en) * | 2012-05-18 | 2014-08-13 | 东华大学 | Macromolecule flocculating suspension liquid and preparation method thereof |
CN102691229B (en) * | 2012-05-18 | 2014-02-26 | 东华大学 | Chitosan film and preparation method thereof |
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