CN104371127A - Juicy food packaging biodegradable chitosan film preparation method - Google Patents
Juicy food packaging biodegradable chitosan film preparation method Download PDFInfo
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- CN104371127A CN104371127A CN201410701701.8A CN201410701701A CN104371127A CN 104371127 A CN104371127 A CN 104371127A CN 201410701701 A CN201410701701 A CN 201410701701A CN 104371127 A CN104371127 A CN 104371127A
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Abstract
The invention discloses a juicy food packaging biodegradable chitosan film preparation method. The method includes dissolving chitosan powder into acetic acid solution, then adding alkylated nano cellulose, mixing completely, filtering and purifying, and obtaining alkylated nano cellulose/chitosan solution through ultrasound treatment; dissolving gallic acid or gallic acid ester substances into ethanol, adding 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and N-hydroxysuccinimide reagent for full reaction, adding the mixture into the alkylated nano cellulose/chitosan solution, stirring at low temperature, placing at room temperature, performing ultrasonic dispersion and vacuum deaeration treatment, drying, and obtaining the film; soaking with alkali solution, flushing and treating through water till neutral, drying at room temperature, and obtaining the product. The method has the advantages that the chitosan is modified through the nano cellulose and gallic acid, and the tensile strength, oxidation resistance and antibacterial properties of the chitosan film are improved greatly.
Description
Technical field
That the present invention relates to is the preparation method of the food packaging degradable chitosan film of a kind of juicy, this film is composited primarily of chitosan, alkylation nano-cellulose and gallic acid, have that intensity is high, resistance of oxidation and the advantage such as antibacterial ability is strong, and belong to can be degradable biomass composite.
Background technology
" do not use and do not produce objectionable impurities yet, utilize the friendly chemical of renewable resources synthetic environment " and become International Technology Disciplinary Frontiers.Renewable resources mainly refers to the native biopolymer materials such as occurring in nature animals and plants and microorganism, and they are easily become water, carbonic acid gas and inorganic molecules by the microbial decomposition of occurring in nature after a procedure, belong to real environmental friendliness shaped material.Along with the development of current nanotechnology and perfect, native biopolymer can be prepared to various functional materials more and more, and they probably become main Chemicals replacing synthetic plastics in the future, are applied in the middle of daily life.In recent years, this kind of focus material of people's research mainly concentrates on Mierocrystalline cellulose, xylogen, starch, chitin, chitosan, other polysaccharide, protein and natural rubber etc., and makes some progress.
Chitosan (Chitosan); normally from chitin extraction (Chitin) the shell or fungal cell wall of shrimp, crab, insect; 100 ~ 180 DEG C, heterogeneous deacetylate obtains in the sodium hydroxide solution of 40 ~ 60%; chemical name is (Isosorbide-5-Nitrae)-2-acetylaminohydroxyphenylarsonic acid 2-deoxidation-callose.As a kind of native biopolymer material, why chitosan can have good application prospect at packaging field, and major cause is: 1. wide material sources, is only second to the cellulosic content of occurring in nature; 2. belong to degradation material, be easy to degraded under the effect of soil microorganisms and generate carbonic acid gas and water etc., problem of environmental pollution can be solved well; 3. nontoxic, self there is good biocompatibility and germ resistance; 4. good film-forming properties.But, compare and apply more Plastic Packaging Materials at present, chitosan but receives the restriction of the shortcomings such as physical strength is low, fragility is large, resistance of oxidation is weak, moisture-proof acid resistance difference in actual applications, and thus suitable application area is relatively little, needs further modification.
Summary of the invention
The preparation method of the degradable chitosan film that what the present invention proposed the is juicy of a kind of high strength, high anti-oxidation ability and high anti-microbial property is food packaging, its object is to overcome chitosan physical strength is low in actual applications, fragility is large, resistance of oxidation is weak, moisture-proof acid resistance difference and the shortcoming such as bacteriostasis is not strong.
Technical solution of the present invention: the preparation method of the food packaging degradable chitosan film of a kind of juicy, comprises the steps:
(1) joined by acetum and be dispersed with in the ethanolic soln of nano-cellulose, regulate pH value to 4 ~ 5, then add silane coupling agent, stirs 40 ~ 60 minutes, eccentric cleaning is neutral postlyophilization extremely, namely obtains alkylating nano-cellulose;
(2) getting Chitosan powder is dissolved in acetic acid or other weakly acidic aqueous solutions, being heated to 40 ~ 60 DEG C and uniform stirring makes chitosan dissolve completely in 15 ~ 20 minutes, then in this solution, add the alkylation nano-cellulose of step (1) gained, fully stir 30 ~ 45 minutes at 45 ~ 55 DEG C, after suction filtration removal of impurities, then within 10 ~ 20 minutes, be nano-cellulose/chitosan solution through supersound process;
(3) gallic acid is dissolved in ethanol, and in gallic acid ethanolic soln, add 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxy-succinamide reagent respectively, it is made fully to react, then this solution is added in the made alkylation nano-cellulose/chitosan solution of step (2), or directly gallic acid or gallate ester material are directly added in the made alkylation nano-cellulose/chitosan solution of step (2);
(4) gallic acid/nano-cellulose/chitosan solution prepared by step (3) is placed in low temperature environment to stir 20 ~ 40 minutes, and at room temperature place 6 ~ 12 hours, carry out vacuum defoamation process through supersound process after 10 ~ 20 minutes again, finally at 40 ~ 60 DEG C, dry film forming; Be that the basic solution of 0.05 ~ 0.2mol/L soaks 20 ~ 35 minutes by the composite membrane concentration of dry gained, rinse process to neutral with water, at room temperature dry and obtain degradable chitosan film product.
The present invention comparatively prior art tool has the following advantages:
1) chitosan is owing to having nontoxic, biocompatibility, biological degradability and the easy feature such as film-forming properties, has been widely used in the fresh-keeping of fruits and vegetables, meat, Poultry and Eggs, fish etc. using it as auxiliary agent or the laminated film after being modified.
2) but the research of alkylating nano-cellulose and chitosan blend be have not been reported, especially still report is had no by the research of gallic acid modification again after nano-cellulose and chitosan blend.
3) appear in the newspapers with the research of nano-cellulose or nano-cellulose whisker reinforcement chitosan film, but also there are some problems to need to improve, because Mierocrystalline cellulose is that its molecular formula is (C by numerous β-D-glucopyranosyls each other with the linear polymer that (1-4)-β-glycosidic bond is formed by connecting
6h
10o
5) n, and each glucosyl residue ring is all containing three alcoholic extract hydroxyl groups, i.e. C(2), C(3) position secondary hydroxyl group and C(6) primary hydroxyl group on position, the existence of these hydroxyls makes nano-cellulose polarity strengthen, and is very easily formed and reunites and disperse uneven in chitosan solution.
4) in the present invention, nano-cellulose, after alkylation process, improves the nonpolar of nano-cellulose, and nano-cellulose is disperseed in chitosan solution more even, mechanics reinforced effects is more obvious.On the other hand, gallic acid is a kind of natural Phenolic Antioxidant extracted from plant, there is the O-H bond rupture enthalpy that trihydroxy-group on higher reducing power and phenyl ring is lower,-the OH of hydroxy-acid group in its molecular structure easily and on chitosan molecule and nano-cellulose reacts and is combined into gallic acid-derivate, thus the ability such as oxidation-resistance, germ resistance of raising chitosan film.
Embodiment
A preparation method for the food packaging degradable chitosan film of juicy, comprises the steps:
(1) joined by acetum and be dispersed with in the ethanolic soln of nano-cellulose, regulate pH value to 4 ~ 5, then add silane coupling agent, stirs 40 ~ 60 minutes, eccentric cleaning is neutral postlyophilization extremely, namely obtains alkylating nano-cellulose;
(2) getting Chitosan powder is dissolved in acetic acid or other weakly acidic aqueous solutions, being heated to 40 ~ 60 DEG C and uniform stirring makes chitosan dissolve completely in 15 ~ 20 minutes, then in this solution, add the alkylation nano-cellulose of step (1) gained, fully stir 30 ~ 45 minutes at 45 ~ 55 DEG C, after suction filtration removal of impurities, then within 10 ~ 20 minutes, be nano-cellulose/chitosan solution through supersound process;
(3) gallic acid is dissolved in ethanol, and in gallic acid ethanolic soln, add 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxy-succinamide reagent respectively, it is made fully to react, then this solution is added in the made alkylation nano-cellulose/chitosan solution of step (2), or directly gallic acid or gallate ester material are directly added in the made alkylation nano-cellulose/chitosan solution of step (2);
(4) gallic acid/nano-cellulose/chitosan solution prepared by step (3) is placed in low temperature environment to stir 20 ~ 40 minutes, and at room temperature place 6 ~ 12 hours, carry out vacuum defoamation process through supersound process after 10 ~ 20 minutes again, finally at 40 ~ 60 DEG C, dry film forming; Be that the basic solution of 0.05 ~ 0.2mol/L soaks 20 ~ 35 minutes by the composite membrane concentration of dry gained, rinse process to neutral with water, at room temperature dry and obtain degradable chitosan film product.
Acetum mass concentration in described step (1) is 1 ~ 5%, and the mass volume ratio of nano-cellulose and ethanol is 1g:100ml, and the mass ratio of silane coupling agent and nano-cellulose is 0.3 ~ 1.5%:1.
The massfraction of the acetum in described step (2) is 0.5 ~ 2%, and the massfraction of alkylation nanofiber cellulose solution is 1 ~ 5%, and nano-cellulose and chitosan mass are than 3 ~ 15%:1, and ultrasonic generator power is 800W.
The mass ratio of the gallic acid in described step (3) and 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride is 1:1, the mass ratio of gallic acid and N-hydroxy-succinamide is 1:1, and gallic acid or gallate ester material are 2 ~ 12%:1 with nano-cellulose/chitosan mass ratio.
The reaction conditions of described gallic acid and 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride reacts 20 ~ 30 minutes at normal temperatures, the reaction conditions of gallic acid and N-hydroxy-succinamide reacts 40 ~ 60 minutes in ice-water bath, reacts the stirring that all remains a constant speed.
Embodiment
(1) be that 5% acetic acid slowly instills 100ml and is dispersed with in the ethanolic soln of nano-cellulose by massfraction, regulate PH to 4.5, then the silane coupler solution that 10ml massfraction is 10g/L is added, stir 60 minutes, eccentric cleaning, to neutral postlyophilization, namely obtains alkylating nano-cellulose.
(2) 0.5g Chitosan powder being dissolved in 100ml concentration of volume percent is in the aqueous acetic acid of 1%, being heated to 50 DEG C and uniform stirring makes chitosan dissolve completely in 20 minutes, then in chitosan solution, add the alkylation nano-cellulose 0.05g of step (1) gained, fully stir 40 minutes at 45 DEG C, after suction filtration removal of impurities, then within 15 minutes, be nano-cellulose/chitosan solution through supersound process.
(3) 0.04g gallic acid is dissolved in 5ml ethanol, uniform stirring 5 minutes, and in gallic acid ethanolic soln, add 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride of 0.04g respectively, react 10 minutes at normal temperatures, then the N-hydroxy-succinamide of 0.04g is added, react 40 minutes in ice-water bath, whole process adopts magnetic stirring apparatus at the uniform velocity to stir, then is added by this solution in the made nano-cellulose/chitosan solution of step (2).
(4) gallic acid/nano-cellulose/chitosan solution prepared by step (3) is placed in ice-water bath to stir 30 minutes, and at room temperature place 12 hours, vacuum defoamation process is carried out after 15 minutes again through supersound process, when seeing that in solution, bubble-free produces, then this mixing solutions is dried film forming at 50 DEG C.The NaOH solution being 0.1mol/L by the composite membrane concentration of dry gained soaks 30 minutes, rinses to neutral, at room temperature dry and be products obtained therefrom with water.
(5) 0.5g Chitosan powder being dissolved in 100ml concentration of volume percent is in the aqueous acetic acid of 1%, be heated to after 50 DEG C and uniform stirring make chitosan dissolve completely in 20 minutes, vacuum defoamation process is carried out after 15 minutes again through supersound process, when seeing that in solution, bubble-free produces, then chitosan solution is dried film forming at 50 DEG C.The basic solution being 0.1mol/L by the composite membrane concentration of dry gained soaks 30 minutes, rinses to neutral, at room temperature dry and be pure chistosan film with water.
Performance Detection:
The tensile strength of pure chistosan film is 45.3MPa, and gallic acid/nano-cellulose/chitosan complex film tensile strength is 78.6MPa, improves about 65.7%; After process 100min, compare pure chistosan film and composite membrane discovery, water-intake rate drops to 23.4% by 62%; The permeability coefficient of pure chistosan film is 1.63 × 10
-9cm
2s
-1, the permeability coefficient of composite membrane drops to 1.06 × 10 gradually
-9cm
2s
-1.
Resistance of oxidation is passed judgment on respectively by the Scavenging activity of film to hydroxyl radical free radical, DPPH free radical and ultra-oxygen anion free radical.The Scavenging activity of pure chistosan film to hydroxyl radical free radical, DPPH free radical and ultra-oxygen anion free radical is respectively: 2.13%, 1.08% and 3.46%, and the Scavenging activity of composite membrane to three is respectively: 75%, 83.4% and 62.3%; Pure chitosan (A) and this experiment gained composite membrane (B) have obvious inhibition zone to occur to around colibacillary bacteriostasis display composite membrane, and the surrounding of pure chistosan film does not almost have inhibition zone to occur, illustrate that composite membrane has good antibacterial ability.
Claims (5)
1. a preparation method for the food packaging degradable chitosan film of juicy, is characterized in that the method comprises the steps:
(1) joined by acetum and be dispersed with in the ethanolic soln of nano-cellulose, regulate pH value to 4 ~ 5, then add silane coupling agent, stirs 40 ~ 60 minutes, eccentric cleaning is neutral postlyophilization extremely, namely obtains alkylating nano-cellulose;
(2) getting Chitosan powder is dissolved in acetic acid or other weakly acidic aqueous solutions, being heated to 40 ~ 60 DEG C and uniform stirring makes chitosan dissolve completely in 15 ~ 20 minutes, then in this solution, add the alkylation nano-cellulose of step (1) gained, fully stir 30 ~ 45 minutes at 45 ~ 55 DEG C, after suction filtration removal of impurities, then within 10 ~ 20 minutes, be nano-cellulose/chitosan solution through supersound process;
(3) gallic acid is dissolved in ethanol, and in gallic acid ethanolic soln, add 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxy-succinamide reagent respectively, it is made fully to react, then this solution is added in the made alkylation nano-cellulose/chitosan solution of step (2), or directly gallic acid or gallate ester material are directly added in the made alkylation nano-cellulose/chitosan solution of step (2);
(4) gallic acid/nano-cellulose/chitosan solution prepared by step (3) is placed in low temperature environment to stir 20 ~ 40 minutes, and at room temperature place 6 ~ 12 hours, carry out vacuum defoamation process through supersound process after 10 ~ 20 minutes again, finally at 40 ~ 60 DEG C, dry film forming; Be that the basic solution of 0.05 ~ 0.2mol/L soaks 20 ~ 35 minutes by the composite membrane concentration of dry gained, rinse process to neutral with water, at room temperature dry and obtain degradable chitosan film product.
2. the preparation method of the food packaging degradable chitosan film of a kind of juicy according to claim 1, it is characterized in that the acetum mass concentration in described step (1) is 1 ~ 5%, the mass volume ratio of nano-cellulose and ethanol is 1g:100ml, and the mass ratio of silane coupling agent and nano-cellulose is 0.3 ~ 1.5%:1.
3. the preparation method of the food packaging degradable chitosan film of a kind of juicy according to claim 1, the massfraction that it is characterized in that the acetum in described step (2) is 0.5 ~ 2%, the massfraction of alkylation nanofiber cellulose solution is 1 ~ 5%, nano-cellulose and chitosan mass are than 3 ~ 15%:1, and ultrasonic generator power is 800W.
4. the preparation method of the food packaging degradable chitosan film of a kind of juicy according to claim 1, the mass ratio that it is characterized in that gallic acid in described step (3) and 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride is 1:1, the mass ratio of gallic acid and N-hydroxy-succinamide is 1:1, and gallic acid or gallate ester material are 2 ~ 12%:1 with nano-cellulose/chitosan mass ratio.
5. the preparation method of the food packaging degradable chitosan film of a kind of juicy according to claim 4, the reaction conditions that it is characterized in that described gallic acid and 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride reacts 20 ~ 30 minutes at normal temperatures, the reaction conditions of gallic acid and N-hydroxy-succinamide reacts 40 ~ 60 minutes in ice-water bath, reacts the stirring that all remains a constant speed.
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Cited By (9)
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| CN104744905A (en) * | 2015-03-31 | 2015-07-01 | 苏州维泰生物技术有限公司 | Polycaprolactone-cellulose acetate medical composite film and preparation method thereof |
| CN106220876A (en) * | 2016-08-12 | 2016-12-14 | 扬州大学 | A kind of preparation method of chitosan protocatechuic acid graft copolymer membrane |
| CN106977622A (en) * | 2016-01-15 | 2017-07-25 | 扬州大学 | A kind of preparation method of phenolic acid modification of chitosan coating liquid for edible fungus fresh-keeping |
| CN108264743A (en) * | 2018-02-08 | 2018-07-10 | 福建农林大学 | A kind of preparation method of plant polyphenol/nano-cellulose polymer composite based on multiple hydrogen bonding effect |
| CN108440798A (en) * | 2018-04-20 | 2018-08-24 | 常州市蒽盗钟情生物科技有限公司 | A kind of preparation method of fruit freshness preserving film |
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| CN112552416A (en) * | 2020-12-14 | 2021-03-26 | 江南大学 | Preparation method of multifunctional nano-cellulose |
| CN113881276A (en) * | 2021-10-19 | 2022-01-04 | 湖北中烟工业有限责任公司 | Water-based edible antibacterial ink and preparation method thereof |
| CN113980407A (en) * | 2021-12-03 | 2022-01-28 | 广东爱丽斯包装有限公司 | Degradable antifogging zipper food bag and preparation process thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744905A (en) * | 2015-03-31 | 2015-07-01 | 苏州维泰生物技术有限公司 | Polycaprolactone-cellulose acetate medical composite film and preparation method thereof |
| CN106977622A (en) * | 2016-01-15 | 2017-07-25 | 扬州大学 | A kind of preparation method of phenolic acid modification of chitosan coating liquid for edible fungus fresh-keeping |
| CN106220876A (en) * | 2016-08-12 | 2016-12-14 | 扬州大学 | A kind of preparation method of chitosan protocatechuic acid graft copolymer membrane |
| CN108264743A (en) * | 2018-02-08 | 2018-07-10 | 福建农林大学 | A kind of preparation method of plant polyphenol/nano-cellulose polymer composite based on multiple hydrogen bonding effect |
| CN108440798A (en) * | 2018-04-20 | 2018-08-24 | 常州市蒽盗钟情生物科技有限公司 | A kind of preparation method of fruit freshness preserving film |
| CN110951119A (en) * | 2019-11-23 | 2020-04-03 | 清远高新华园科技协同创新研究院有限公司 | Preparation method and equipment of degradable environment-friendly packaging material for food contact |
| CN112552416A (en) * | 2020-12-14 | 2021-03-26 | 江南大学 | Preparation method of multifunctional nano-cellulose |
| CN113881276A (en) * | 2021-10-19 | 2022-01-04 | 湖北中烟工业有限责任公司 | Water-based edible antibacterial ink and preparation method thereof |
| CN113980407A (en) * | 2021-12-03 | 2022-01-28 | 广东爱丽斯包装有限公司 | Degradable antifogging zipper food bag and preparation process thereof |
| CN113980407B (en) * | 2021-12-03 | 2023-01-20 | 广东爱丽斯包装有限公司 | Degradable antifog zipper food bag and preparation process thereof |
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Application publication date: 20150225 |