CN101177494A - Preparation method of chitosan composite film using glycerin and stearic acid as plasticizer - Google Patents
Preparation method of chitosan composite film using glycerin and stearic acid as plasticizer Download PDFInfo
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- CN101177494A CN101177494A CNA2007100600513A CN200710060051A CN101177494A CN 101177494 A CN101177494 A CN 101177494A CN A2007100600513 A CNA2007100600513 A CN A2007100600513A CN 200710060051 A CN200710060051 A CN 200710060051A CN 101177494 A CN101177494 A CN 101177494A
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 59
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 235000011187 glycerol Nutrition 0.000 title claims abstract description 22
- 235000021355 Stearic acid Nutrition 0.000 title claims abstract description 19
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 title claims abstract description 19
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000008117 stearic acid Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002131 composite material Substances 0.000 title abstract description 7
- 239000004014 plasticizer Substances 0.000 title abstract 4
- 239000007788 liquid Substances 0.000 claims abstract description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 3
- 239000004902 Softening Agent Substances 0.000 claims description 16
- 239000005357 flat glass Substances 0.000 claims description 9
- 239000012528 membrane Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 230000035699 permeability Effects 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 239000011521 glass Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 235000013305 food Nutrition 0.000 description 14
- 238000001035 drying Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- 238000005086 pumping Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 230000006196 deacetylation Effects 0.000 description 4
- 238000003381 deacetylation reaction Methods 0.000 description 4
- 230000000149 penetrating effect Effects 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- 229920002101 Chitin Polymers 0.000 description 2
- 108010054033 Chitin deacetylase Proteins 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009447 edible packaging Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 description 1
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 229920002581 Glucomannan Polymers 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- -1 amino, hydroxyl functional group Chemical group 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000850 deacetylating effect Effects 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 229940046240 glucomannan Drugs 0.000 description 1
- 230000036449 good health Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Landscapes
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
本发明公开了一种壳聚糖复合膜的制备方法，旨在提供一种韧性大、透水透气性小的壳聚糖复合膜的制备方法。包括下述步骤：用稀的醋酸溶液溶解壳聚糖，壳聚糖与醋酸溶液的料液比为1∶40～100(重量/体积)，再加入增塑剂，水浴加热至完全溶解，然后冷却室温，制成膜液；所述增塑剂为占醋酸溶液的体积百分比为0.2～1.0％甘油与占醋酸溶液质量百分比0.3～0.8％的硬脂酸的组合。将上述制备好的膜液过滤，去除杂质，并抽滤脱气半小时，然后倾倒在干净的玻璃板上，在40～80℃下恒温干燥成膜；成膜后，揭膜，得到壳聚糖复合膜。本发明用甘油和硬脂酸作为增塑剂，通过对其用量的选择，制备的复合膜不但具有一定的韧性，还能保持较低的透水透气性。The invention discloses a preparation method of a chitosan composite film, and aims to provide a preparation method of a chitosan composite film with high toughness and low water and air permeability. The method comprises the following steps: dissolving chitosan with dilute acetic acid solution, the ratio of chitosan to acetic acid solution is 1:40-100 (weight/volume), then adding plasticizer, heating in a water bath until completely dissolved, and then Cooling at room temperature to form a film solution; the plasticizer is a combination of 0.2-1.0% glycerol in volume percentage of the acetic acid solution and 0.3-0.8% stearic acid in the mass percentage of the acetic acid solution. Filter the prepared membrane liquid above to remove impurities, and degas it by suction filtration for half an hour, then pour it on a clean glass plate, and dry it at a constant temperature of 40-80°C to form a film; after the film is formed, peel off the film to obtain chitosan Glycocomposite membrane. The present invention uses glycerin and stearic acid as plasticizers, and through the selection of their dosages, the prepared composite film not only has certain toughness, but also maintains relatively low water and gas permeability.
Description
Technical field
The invention belongs to food product pack and preservation technique field, in particular, relating to a kind of is the preparation method of the chitosan complex film of softening agent with glycerine and stearic acid.
Background technology
Chitosan is to be made by the chitin deacetylase base, and chitin extensively is present in the crust of Crustaceans shrimp, crab, the crust of insect, and in cell walls of fungi (yeast, mould) and the cell walls of plant (mushroom), its content on earth is only second to Mierocrystalline cellulose.Studies show that in a large number both at home and abroad, chitin and chitosan are nontoxic, it is foodstuff additive for U.S. food and medical and sanitary control office (FDA) approved, therefore, chitosan is nontoxic and safe natural high moleculer eompound, and is a kind of functional polymer compound, has special amino, hydroxyl functional group on the molecular chain, therefore come compared with many synthetic macromolecular compounds, be more suitable for using in foodstuffs industry.Chitosan mainly contains aspect following three in Application in Food Industry: the first, and the treatment agent of liquid.As reduce total solids content in the liquid, from waste water, reclaim protein, drink water purification, the clarification of beverage and drinks etc.; The second, foodstuff additive.Control as the food configuration shape improves flavours in food products, improves the flowability of food, and the control viscosity increases fibre content etc.; The 3rd, functional materials.As bacteriostasis, preservation agent, diet food, wrapping material or trapped material, also can be used as slow-release material etc.
Present packaging material for food mostly is a plastic membrane product, because plastics film may be harmful, causes " white pollution " after discarding, so many countries are are all competitively researching and developing biodegradable even the edible food packaging material.Along with the develop rapidly of present foodstuffs industry and the people enhancing to environmental protection consciousness, a kind of new packaging material one edible packaging that can solve contradiction between wrapping material and the environment is fully shown one's talent.Edible packaging has obtained extensive concern both domestic and external with its abundant raw material, characteristics such as complete, edible and nuisanceless.Edible packing membrane is also more and more paid attention to as a kind of wrapping material.Edible film can be divided into polyose, protein, lipid and composite membrane class according to film forming material.The polyose edible film has chitosan, starch, sodium alginate, Rhizoma amorphophalli glucomannan and derivative thereof.And chitosan obtains extensive concern as the potential film forming component because of it has good health care function, bacteriostasis property, machinery and penetrating quality.So the edibility chitosan film has very big application prospect in food product pack and fresh-keeping aspect.The research of chitosan film relates to membrane sepn, edible film, biological degradable membrane, medical film, coating-film fresh-keeping, composite membrane etc., and the film-forming properties of chitosan has been applied in industrial circles such as weaving, printing and dyeing, papermaking, medicine, food.Chitosan removes has film-forming properties, also has antibiotic preservative activity and biological degradability, holds out broad prospects aspect Freshkeeping Packaging.
As the edible fresh-keeping packing film, requirement should have the favorable mechanical performance, and good obstruct and penetrating quality are arranged again.Softening agent is the principal element that influences film properties, softening agent add the microstructure that affiliation changes film, thereby influence the machinery and the penetrating quality of film.The adding of softening agent avoids film to produce macropore and crack, and the integrity of film is strengthened.
Only use single softening agent mostly among the at present relevant preparation method of chitosan complex film, promptly glycerine or stearic acid though glycerine can reduce the tensile strength of film, have increased the ventilation property of film; And add the ventilation property that stearic acid can reduce film, but toughness reduces the tensile strength increase.On the 9th phase of the calendar year 2001 Food science magazine, in " research of chitosan film forming characteristics " literary composition that lucky big people such as grade delivers, proposed to make film not only have certain toughness as softening agent and can also keep low water-permeable and air permeable with glycerine and stearic acid combination, but just to the direction of having researched and proposed of film forming characteristics, do not provide suitable glycerine and stearic consumption in this article.Therefore, selecting the consumption of suitable manufacturing methods for use is the key of the chitosan complex film for preparing.
Summary of the invention
The present invention is in order to overcome weak point of the prior art, the preparation method of the chitosan complex film that a kind of toughness is big, water-permeable and air permeable is little to be provided.
The present invention is achieved through the following technical solutions:
The preparation method of chitosan complex film of the present invention is to be film forming material with the chitosan, and it is dissolved in rare acetum, adds glycerine and stearic acid as softening agent, casting film-forming on sheet glass then, solvent evaporated, drying and forming-film, take off from sheet glass, promptly obtain chitosan complex film.Specifically comprise the steps:
A kind of preparation method of chitosan complex film is characterized in that, comprises the steps:
(1) film liquid preparation: with rare acetum dissolving chitosan, the solid-liquid ratio of chitosan and acetum is 1: 40～100 (weight/volume), adds softening agent again, is heated to dissolving fully in 50～70 ℃ of water-baths, cools off room temperature then, makes film liquid; Described softening agent is that the volume percent that accounts for acetum is 0.2～1.0% glycerine and the stearic combination that accounts for acetum mass percent 0.3～0.8%.
(2) film forming: the above-mentioned film liquid for preparing is filtered, remove impurity, and suction filtration outgases half an hour under 0.1～0.5Mpa vacuum tightness, then film liquid is poured on the clean sheet glass, 40～80 ℃ of following freeze-day with constant temperature film forming; After the film forming, take off film, obtain chitosan complex film.
Wherein the volume by volume concentration of dilute acetic acid solution can select 1%～3% for use.
The present invention has following technique effect:
The present invention uses glycerine and stearic acid as softening agent, and by the selection to its consumption, the composite membrane of preparation not only has certain toughness, can also keep lower water-permeable and air permeable.
Can be used as the wrapping material of food by the chitosan complex film of method of the present invention preparation, give full play to the health care and the bacteria resistance function of chitosan.
Embodiment
Below in conjunction with specific embodiment to the detailed description of the invention.
The chitosan, acetic acid, glycerine, the stearic acid that use all are food grade.Be used to prepare the chitosan of film, at first require to be dissolved in diluted acid.Chitosan is made by chitin deacetylase, and deacetylation is little, and chitosan just is insoluble to diluted acid, and the present invention can make the chitosan dissolving just passable to the selection of deacetylating degree of chitosan as long as deacetylation reaches.Generally speaking, deacetylation reaches more than 55%, and chitosan just can be dissolved in the diluted acid.Chitosan in the embodiment of the invention is the product that Jinan Haidebei Marine Organism Engineering Co., Ltd. produces, and its deacetylation is 85.8%.
Embodiment 1
Taking by weighing chitosan 1g, to be dissolved in the 100mL volume by volume concentration be in 1% the acetum, adds 0.2ml glycerine, 0.6g stearic acid, is heated to dissolving fully in 70 ℃ of water-baths, and cool to room temperature is made film liquid.With the above-mentioned film liquid filtered through gauze for preparing, remove impurity, and at 0.1MPa vacuum lower pumping 0.5h, the solution of getting 50ml then is poured on the sheet glass uniformly, and drying and forming-film in 40 ℃ of thermostatic drying chambers is after the film forming, carefully take off film with clean blade, obtain chitosan complex film.
Embodiment 2
Taking by weighing chitosan 1.25g, to be dissolved in the 100mL volume by volume concentration be in 1.5% the acetum, adds 0.4ml glycerine, 0.4g stearic acid, is heated to dissolving fully in 70 ℃ of water-baths, and cool to room temperature is made film liquid.With the above-mentioned film liquid filtered through gauze for preparing, remove impurity, and at 0.1MPa vacuum lower pumping 0.5h, the solution of getting 50ml then is poured on the sheet glass uniformly, and drying and forming-film in 60 ℃ of thermostatic drying chambers is after the film forming, carefully take off film with clean blade, obtain chitosan complex film.
Embodiment 3
Taking by weighing chitosan 1.5g, to be dissolved in the 100mL volume by volume concentration be in 1% the acetum, adds 0.4ml glycerine, 0.5g stearic acid, is heated to dissolving fully in 70 ℃ of water-baths, and cool to room temperature is made film liquid.With the above-mentioned film liquid filtered through gauze for preparing, remove impurity, and at 0.1MPa vacuum lower pumping 0.5h, the solution of getting 50ml then is poured on the sheet glass uniformly, and drying and forming-film in 60 ℃ of thermostatic drying chambers is after the film forming, carefully take off film with clean blade, obtain chitosan complex film.
Embodiment 4
Taking by weighing chitosan 2g, to be dissolved in the 100mL volume by volume concentration be in 2% the acetum, adds 0.2ml glycerine, 0.8g stearic acid, is heated to dissolving fully in 50 ℃ of water-baths, and cool to room temperature is made film liquid.With the above-mentioned film liquid filtered through gauze for preparing, remove impurity, and at 0.3MPa vacuum lower pumping 0.5h, the solution of getting 50ml then is poured on the sheet glass uniformly, and drying and forming-film in 40 ℃ of thermostatic drying chambers is after the film forming, carefully take off film with clean blade, obtain chitosan complex film.
Embodiment 5
Taking by weighing chitosan 2.5g, to be dissolved in the 100mL volume by volume concentration be in 3% the acetum, adds 1.0ml glycerine, 0.3g stearic acid, is heated to dissolving fully in 60 ℃ of water-baths, and cool to room temperature is made film liquid.With the above-mentioned film liquid filtered through gauze for preparing, remove impurity, and at 0.5MPa vacuum lower pumping 0.5h, the solution of getting 50ml then is poured on the sheet glass uniformly, and drying and forming-film in 80 ℃ of thermostatic drying chambers is after the film forming, carefully take off film with clean blade, obtain chitosan complex film.
Above-mentioned chitosan complex film, its machinery and penetrating quality are as shown in table 1 after measured.
Table 1 chitosan complex film performance
| Tensile strength (MPa) | Elongation (%) | Water-permeable (gmm/m 2d mmHg) | Ventilation property (mlm/m 2d kpa) | |
| Embodiment 1 | 11.259 | 6.25 | 0.3626 | 0.0435 |
| Embodiment 2 | 9.832 | 8.75 | 0.3917 | 0.0523 |
| Embodiment 3 | 15.387 | 12.25 | 0.4253 | 0.0972 |
| Embodiment 4 | 13.268 | 5.25 | 0.2394 | 0.0264 |
| Embodiment 5 | 8.362 | 16.75 | 0.5389 | 0.1025 |
| LDEP | 17.8 | 206.5 | 0.011 | 7.4×10 -4 |
| HDEP | 28.7 | 155.4 | 0.007 | 7.4×10 -4 |
As can be seen from the above table, the film properties of the chitosan complex film of method preparation of the present invention is compared with traditional LDEP and HDEP, and tensile strength and LDEP are close, and are lower than the tensile strength of HDEP film; Elongation at break is lower than LDEP film and HDEP film, and water-permeable and air permeable also is higher than LDEP film and HDEP film respectively.In sum, chitosan complex film of the present invention has certain tensile strength and toughness, also has certain water-permeable and air permeable, can be used as the food fresh keeping packing film.
To relate to a kind of be that the preparation method of the chitosan complex film of softening agent has carried out special description with glycerine and stearic acid to disclosed although with reference to embodiment, embodiment described above is illustrative and not restrictive, under the situation that does not break away from the spirit and scope of the present invention, all variations and modification are all within the scope of the present invention.
Claims (2)
1. one kind is the preparation method of the chitosan complex film of softening agent with glycerine and stearic acid, it is characterized in that, comprises the steps:
(1) film liquid preparation: with rare acetum dissolving chitosan, the solid-liquid ratio of chitosan and acetum is 1: 40～100 (weight/volume), adds softening agent again, is heated to dissolving fully in 50～70 ℃ of water-baths, is cooled to room temperature then, makes film liquid; Described softening agent is that the volume percent that accounts for acetum be 0.2～1.0% glycerine with accounting for the acetum mass percent is 0.3～0.8% stearic combination;
(2) film forming: the above-mentioned film liquid for preparing is filtered, remove impurity, and suction filtration outgases half an hour under 0.1～0.5Mpa vacuum tightness, then film liquid is poured on the clean sheet glass, 40～80 ℃ of following freeze-day with constant temperature film forming; After the film forming, take off film, obtain chitosan complex film.
2. according to claim 1 is the preparation method of the chitosan complex film of softening agent with glycerine and stearic acid, it is characterized in that the volume by volume concentration of dilute acetic acid solution is 1%～3%.
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| CN102219090A (en) * | 2011-04-29 | 2011-10-19 | 逯益民 | Edible internal packaging bag and production process thereof |
| CN102249396A (en) * | 2010-05-18 | 2011-11-23 | 中国水利水电科学研究院 | Biologically slow filtering filler and manufacturing method thereof |
| CN102504351A (en) * | 2011-11-03 | 2012-06-20 | 中山火炬职业技术学院 | Chitosan composite preservative film and preparation process thereof |
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2007
- 2007-10-26 CN CNA2007100600513A patent/CN101177494A/en active Pending
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| US20120276185A1 (en) * | 2008-05-30 | 2012-11-01 | Hossainy Syed F A | Soluble coating comprising polyelectrolyte with hydrophobic counterions |
| CN102249396A (en) * | 2010-05-18 | 2011-11-23 | 中国水利水电科学研究院 | Biologically slow filtering filler and manufacturing method thereof |
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