CN104097849A - Fresh-keeping packaging material capable of slowly releasing chlorine dioxide disinfectant and preparation method of fresh-keeping packaging material - Google Patents
Fresh-keeping packaging material capable of slowly releasing chlorine dioxide disinfectant and preparation method of fresh-keeping packaging material Download PDFInfo
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- CN104097849A CN104097849A CN201410302768.4A CN201410302768A CN104097849A CN 104097849 A CN104097849 A CN 104097849A CN 201410302768 A CN201410302768 A CN 201410302768A CN 104097849 A CN104097849 A CN 104097849A
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- chlorine dioxide
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- releasing
- keeping packaging
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Abstract
The invention discloses a fresh-keeping packaging material capable of slowly releasing chlorine dioxide disinfectant and a preparation method of the fresh-keeping packaging material, and belongs to the technical field of packaging materials. The fresh-keeping packaging material is a composite membrane made of a high gas permeability plastic polyethylene outer membrane and an ethylene/vinyl acetate copolymer (EVA) modified high gas permeability plastic polyethylene inner membrane by means of a binding agent containing chlorine dioxide releasing agent powder in a dry method in a composite manner. After fruit or vegetable is packaged by a fresh-keeping bag made by the composite membrane, vapour produced by the respiratory action of the fruit or vegetable can induce the membrane to release the low-concentration gas-phase chlorine dioxide disinfectant, the shelf life of the fruit or vegetable is prolonged, and the quality of the fruit or vegetable is improved.
Description
Technical field
The present invention relates to a kind of fresh-keeping packaging material of fresh fruits and vegetables, particularly a kind of preparation method with the Fresh-Keeping Packaging Materials of chlorine dioxide release function, highly-breathable, belongs to field of packaging material.
Background technology
Thereby chlorine dioxide carries out irreversible Oxidative demage effect kill pathogenic bacteria by the running albumen to living cells, be widely used in the fresh-keeping of fruit, vegetables, meat product at home and abroad.The mode of the sterilizing function of chlorine dioxide enforcement at present mainly contains two kinds: powder slowly-releasing, solvent impregnated and slowly-releasing liner mode.
Xinjiang University utilizes the special product Toksun, Xinjiang of acidifying, rich amargosite and sodium chlorite to be mixed with out solid chlorine dioxide powder antistaling agent, and normal temperature was increased to 20 days from 10 days deenergized period.
CN 1439268A discloses a kind of cladded type chlorine dioxide slow-release powder, and it is comprised of sodium chlorite, solid acid and covering; Wherein covering is pressed against alkane ketone, cobalt chloride, water by polyvinyl alcohol, polyethylene arsenic and is formed: sodium chlorite, SODIUM PERCARBONATE are mixed, then covering is coated on to the surface of sodium chlorite and SODIUM PERCARBONATE, make cladded type disinfection agent of chlorine dioxide.
The appendix body of nonwoven fabrics as component usingd in Northcentral University, with the cyclodextrin encapsulated acid combination B of the coated sodium chlorite component A Yong β – of polyvinyl alcohol, in the middle of A, B film, sandwich rate of perviousness and be 33% ± 20% commercially available preservative film, develop the antibacterial liner of chlorine dioxide of slow-release function, when space environment humidity is 85%, chlorine dioxide effectively discharges number of days can reach 17d, and every day, chlorine dioxide effectively discharged quality between 0.15～1.5mg.
Ji'nan University is with the surface upper coating Chitosan-Silver ion antibacterial agent of corn stalk fiber element and be mixed with into film substrate with latex, between two film substrates, press from both sides Annex II chlorine monoxid antiseptic powder and high water absorbent, prepare a kind of cold fresh meat fresh-keeping mat, chlorine dioxide burst size is at 125ppm, and fresh-keeping mat makes cold fresh meat as one-level fresh meat shelf life extension 3～5 days.
Summary of the invention
The present invention relates to a kind of have high oxygen transmitance and high water vapor transmitance, can slowly-releasing chlorine dioxide bactericidal agent laminated film, and can directly be prepared into the form of freshness protection package, this freshness protection package that can slowly-releasing chlorine dioxide bactericidal agent at home and abroad have not been reported.
Freshness protection package involved in the present invention is particularly suitable for fruits and vegetables fresh-keeping of high respiratory rate, and the Fruit and vegetable preserving bag with slowly-releasing chlorine dioxide bactericidal agent function have not been reported at home.
The fresh-keeping packaging material of a kind of slowly-releasing chlorine dioxide bactericidal agent involved in the present invention, it is characterized in that thering is inner membrance, adhesive phase, adventitia three-layer composite structure, wherein in adhesive phase, comprise bactericidal agent, therefore be also bactericidal agent layer, wherein the material of adventitia is linear low density polyethylene resin; Inner membrance is for to be obtained by ethylene-vinyl acetate copolymer (EVA) modifying linear low-density polyethylene resin curtain coating; Adhesive phase is mainly comprised of acrylic resin adhesive and chlorine dioxide releasing agent, wherein chlorine dioxide releasing agent is by sodium chlorite and organic acid composition, wherein organic acid accounts for 40% to 60% of chlorine dioxide releasing agent total mass, and kinds of organic acids comprises one or both or the three kinds of organic acid compounds in sorbic acid, benzoic acid, malic acid.Described solvent is ethyl acetate solvent.Adhesive layer build is 5-10 micron.
Preferably outer film thickness is 15-20 micron, and the OTR oxygen transmission rate of this adventitia is 1 * 10
4to 5 * 10
4ml/m
2.day.atm, the transmitance of aqueous vapor is 10-100g/m
2.day; Inner film thickness is the film of 15-20 micron, and wherein EVA resin accounts for 15% to 50% of inner membrance total mass, and the OTR oxygen transmission rate of inner membrance is 5 * 10
4to 1 * 10
5ml/m
2.day.atm, the transmitance of aqueous vapor is 20-200g/m
2.day.
Adhesive layer is to be that the solvent type acrylic resin adhesives (being dissolution with solvents) of 80000-250000 centipoise, solid content 30%-40% and chlorine dioxide releasing agent powder are mixed with and obtain by viscosity at ambient temperature; Wherein chlorine dioxide releasing agent powder accounts for the 5%-30% of hygrometric state adhesives total mass, chlorine dioxide releasing agent powder is by sodium chlorite and organic acid composition, wherein organic acid accounts for 40% to 60% of chlorine dioxide releasing agent powder total mass, and kinds of organic acids comprises one or both or the three kinds of organic acid compounds in sorbic acid, benzoic acid, malic acid.Described solvent is ethyl acetate solvent.Adhesive layer, the thickness after forming dry film is 5-10 micron.
Preparation method:
The preparation of inner membrance: by after EVA resin and linear low density polyethylene melt blending, be processed into film on casting films former; The preparation of adventitia: directly on casting films former, linear low density polyethylene is processed into film; After solvent type acrylic resin adhesives and chlorine dioxide releasing agent powder are mixed, on dry laminating equipment, binder layer material is evenly placed between adventitia and inner membrance, carries out compoundly, cut, seal.
This bilayer film is adjusted the permeability to air of freshness protection package to adapt to the requirement of different preserving fruit and vegetable utilizings.
What the present invention relates to a kind ofly has a chlorine dioxide slow-release function film, there is three-decker bonding compound in aggregates, be from the different of prior art: 1) existing cladded type slow release powder and existing slowly-releasing liner need to be used in conjunction with outer packaging bag, and packing film involved in the present invention is directly prepared into the form of freshness protection package; 2) existing cladded type slow release powder and existing slowly-releasing liner cannot be realized the control to moisture-vapor transmission and OTR oxygen transmission rate, to be applicable to the requirement of variety classes food fresh keeping; 3) acrylic polymers that packing film involved in the present invention utilizes high molecular weight (adhesive viscosities is higher, its mol wt larger) in adhesive phase is to sodium chlorite and organic acid powder disperses, isolates and coated, obviously different from existing chlorine dioxide slow-release powder covering used; 4) one or more the organic acid compounds in packing film selection sorbic acid acid involved in the present invention, benzoic acid, malic acid are as acidulant, obviously different from the acidulant that prior art adopts; 5) packing film involved in the present invention to the release concentration of chlorine dioxide and periodic Control except with covering kind, outside the Pass resin-coated build has, also relevant with polarity and the thickness of packing inner membrance of the present invention, inner membrance polarity is lower, thickness is larger, barrier to aqueous vapor is higher, release concentration is lower, and deenergized period is longer; 6), when not using, the storage life of packing film involved in the present invention, higher than existing cladded type powder and liner, because there is the protection of inner membrance and adventitia, is added the coating function of acryloid cement resin.
The specific embodiment
Below in conjunction with embodiment, the present invention will be further described, but the present invention is not limited to following examples.The preparation of inner membrance: get after the EVA resin (VA segment quality accounts for 25%-28%, fusion index 15) of 15-50 weight portion and the linear low density polyethylene melt blending of 85-50 part, be processed into the film that thickness is 15-20 micron on casting films former.
The preparation of adventitia: do not add EVA resin, directly linear low density polyethylene is processed into the film that thickness is 15-20 micron on casting films former.
Embodiment 1
The benzoic acid powder suspension of getting 3 weight portions is in the solvent type acrylic resin adhesives (ethyl acetate is as solvent) of 80000-250000 centipoise, solid content 30%-40% in 95 weight portion viscosity, then the sodium chlorite powder with 2 weight portions is also suspended in to above-mentioned solvent type acrylic resin adhesives, after mixing, on dry laminating equipment, the adventitia and the thickness that by thickness, are 20 microns are 15 microns, compound containing the inner membrance of 50%EVA, cut, seal and make freshness protection package 1.
Embodiment 2
Get the malic acid powder suspension of benzoic acid powder+1.5 weight portion of 1.5 weight portions in the above-mentioned solvent type acrylic resin adhesives of 95 weight portion, then the sodium chlorite powder with 2 weight portions is also suspended in to above-mentioned solvent type acrylic resin adhesives, after mixing, on dry laminating equipment, the adventitia and the thickness that by thickness, are 18 microns are 20 microns, compound containing the inner membrance of 30%EVA, cut, seal and make freshness protection package 2.Embodiment 3
Get the malic acid powder suspension of sorbic acid powder+4 weight portion of 5 weight portions in the above-mentioned solvent type acrylic resin adhesives of 85 weight portion, then the sodium chlorite powder with 6 weight portions is also suspended in to above-mentioned solvent type acrylic resin adhesives, after mixing, on dry laminating equipment, the adventitia and the thickness that by thickness, are 16 microns are 20 microns, compound containing the inner membrance of 15%EVA, cut, seal and make freshness protection package 3.
Embodiment 4
Get the benzoic acid powder suspension of sorbic acid powder+10.0 part of 2.0 weight portions in the above-mentioned solvent type acrylic resin adhesives of 70 weight portion, then the sodium chlorite powder with 18 weight portions is also suspended in to above-mentioned solvent type acrylic resin adhesives, after mixing, on dry laminating equipment, the adventitia and the thickness that by thickness, are 15 microns are 15 microns, compound containing the inner membrance of 50%EVA, cut, seal and make freshness protection package 4.
Embodiment 5
Get the sorbic acid powder of 4 weight portions, the malic acid powder suspension of the benzoic acid powder of 4 weight portions, 4 weight portions in the above-mentioned solvent type acrylic resin adhesives of 80 weight portion, then the sodium chlorite powder with 8 weight portions is also suspended in to above-mentioned solvent type acrylic resin adhesives, after mixing, on dry laminating equipment, the adventitia and the thickness that by thickness, are 20 microns are 15 microns, compound containing the inner membrance of 15%EVA, cut, seal and make freshness protection package 5.
Comparative example 1:
The solvent type acrylic resin adhesives (ethyl acetate is as solvent) that use viscosity is 80000-250000 centipoise, solid content 30%-40% is on dry laminating equipment, the adventitia and the thickness that by thickness, are 20 microns are 15 microns, compound containing the inner membrance of 15%EVA, cut, seal and make contrast bag 1.
Comparative example 2:
Use above-mentioned solvent type acrylic resin adhesives, the adventitia and the thickness that by thickness, are 15 microns are 15 microns, compound containing the inner membrance of 50%EVA, cut, seal and make contrast bag 2.
Comparative example 3:
Utilize polyethylene antistaling film and the pallet of commercially available 10 micron thickness to be used in conjunction with, rape is packed, test fresh keeping property (contrast bag 3).
Sample analysis
Gas permeability test
Utilize OTR oxygen transmission rate and the moisture-vapor transmission of oxygen flow, wet instrument test obtains thoroughly material film.The permeability to air data of testing all films are shown in Table 1.The test of moisture-vapor transmission is according to < < GB/T1037-88 plastic sheeting and sheet material water vapor permeability test method > > standard testing.Adopt the water vapor permeation rate tester test of U.S. MOCON company, test and average for three times.OTR oxygen transmission rate is according to standard < < GB/T1038-2000 plastic sheeting and thin slice gas-premeable test method pressure differential method > > test, use the BTY-B1 pressure differential method oxygen flow tester test of Jinan blue streak, test and average for three times.
Freshness protection package discharges chlorine dioxide performance testing
The freshness protection package oad that embodiment 1-5 makes is 250mm * 300mm, and in freshness protection package, inclosure volume is the air of 200 milliliters, encloses 10 grams of rayon balls (containing 5 grams of water) in freshness protection package.Freshness protection package can be to sustained release chlorine dioxide in bag under the initiation of moisture; Chlorine dioxide has higher absorption at 350nm place, utilizes ultraviolet spectrophotometer test freshness protection package to discharge concentration and the deenergized period of chlorine dioxide.First test does not add the absorption value ABS of moisture cotton balls freshness protection package to 350nm ultraviolet light
0, then test every day test and once add the absorption value ABS of freshness protection package to 350nm ultraviolet light after rayon balls
i; (ABS
i-ABS
0) numerical value and freshness protection package in chlorine dioxide concentration be directly proportional.At freshness protection package, discharge chlorine dioxide concentration and chlorine dioxide and reach after balance to overflowing concentration in freshness protection package, in freshness protection package, chlorine dioxide concentration reaches balance, can test out release chlorine dioxide concentration and cycle.
(ABS
i-ABS
0) chlorine dioxide concentration (ppm) corresponding relation adopts following method to obtain in numerical value and freshness protection package: get any one in freshness protection package 1-5, test (ABS
i-ABS
0) after numerical value, with syringe, squeeze into 50 ml deionized water, shake this freshness protection package, allow gas fully contact with water, in gas phase, chlorine dioxide dissolving, in water, then, by the concentration of iodimetric titration test chlorine dioxide, has so just been set up (ABS
i-ABS
0) numerical value and the interior relation that generates chlorine dioxide quality of freshness protection package, obtain gas phase chlorine dioxide concentration numerical value in freshness protection package.
Freshness protection package is fresh-keeping to rape
Get firm harvesting, there is no 6 rapes of mechanical damage, except de-etiolation leaf, put into freshness protection package 1-5 and a contrast bag 1-3, every 1 day, take out one bag of sample, vitamin, the solubility solid content of test rape.
The mensuration of rape soluble solid content (TSS): adopt PR-101 α type hand refractometer to measure, in triplicate, average.
The mensuration of Vit C contents (Vc): with blue basic-dyeable fibre standard solution, to carrying out redox titration containing ascorbic acid leaching solution, dyestuff is reduced to colourless, when arriving titration end-point, unnecessary dyestuff shows as light red in acid medium, the content of reduced form ascorbic acid in dye dosage calculation sample.
Test structure is listed in table 1
From result shown in table 1, can find out, Fruit and vegetable preserving bag involved in the present invention can sustained release chlorine dioxide more than 30 days, according to the adventitia and the inner membrance that need to use different structure, freshness protection package film has different aqueous vapors and OTR oxygen transmission rate, to be applicable to the requirement of different respiratory intensity preserving fruit and vegetable utilizings, discharge between the concentration 10-55ppm of chlorine dioxide, peak concentration is between 20-150ppm.In to the fresh-keeping test of rape, can obviously slow down the changing down of the nutritional labelings such as Vc, solubility solid content, there is excellent fresh-keeping effect.
Those skilled in the art should understand, above preferred embodiment just illustrates of the present invention, is not construed as limiting the invention.Technical scheme of the present invention is carried out to various changes and equivalence replacement, and do not deviate from principle and the scope of technical solution of the present invention, all should be encompassed among the scope of the claims in the present invention.
Claims (6)
1. the fresh-keeping packaging material of a slowly-releasing chlorine dioxide bactericidal agent, it is characterized in that thering is inner membrance, adhesive phase, adventitia three-layer composite structure, wherein in adhesive phase, comprise bactericidal agent, therefore be also bactericidal agent layer, wherein the material of adventitia is linear low density polyethylene resin; Inner membrance is for to be obtained by ethylene-vinyl acetate copolymer (EVA) modifying linear low-density polyethylene resin curtain coating; Adhesive phase is mainly comprised of acrylic resin adhesive and chlorine dioxide releasing agent, wherein chlorine dioxide releasing agent is by sodium chlorite and organic acid composition, wherein organic acid accounts for 40% to 60% of chlorine dioxide releasing agent total mass, and kinds of organic acids comprises one or both or the three kinds of organic acid compounds in sorbic acid, benzoic acid, malic acid.
2. according to the fresh-keeping packaging material of a kind of slowly-releasing chlorine dioxide bactericidal agent of claim 1, it is characterized in that, outer film thickness is 15-20 micron, and the OTR oxygen transmission rate of this adventitia is 1 * 10
4to 5 * 10
4ml/m
2.day.atm, the transmitance of aqueous vapor is 10-100g/m
2.day.
3. according to the fresh-keeping packaging material of a kind of slowly-releasing chlorine dioxide bactericidal agent of claim 1, it is characterized in that, inner film thickness is the film of 15-20 micron, and wherein EVA resin accounts for 15% to 50% of inner membrance total mass, and the OTR oxygen transmission rate of inner membrance is 5 * 10
4to 1 * 10
5ml/m
2.day.atm, the transmitance of aqueous vapor is 20-200g/m
2.day.
4. according to the fresh-keeping packaging material of a kind of slowly-releasing chlorine dioxide bactericidal agent of claim 1, it is characterized in that, adhesive layer is to be that the solvent type acrylic resin adhesives of 80000-250000 centipoise, solid content 30%-40% and chlorine dioxide releasing agent powder are mixed with and obtain by viscosity at ambient temperature; Wherein chlorine dioxide releasing agent powder accounts for the 5%-30% of hygrometric state adhesives total mass, chlorine dioxide releasing agent powder is by sodium chlorite and organic acid composition, wherein organic acid accounts for 40% to 60% of chlorine dioxide releasing agent powder total mass, kinds of organic acids comprises one or both or the three kinds of organic acid compounds in sorbic acid, benzoic acid, malic acid, and described solvent is ethyl acetate solvent.
5. the method for the fresh-keeping packaging material of a kind of slowly-releasing chlorine dioxide bactericidal agent of preparation claim 1, is characterized in that, comprises the following steps:
The preparation of inner membrance: by after EVA resin and linear low density polyethylene melt blending, be processed into film on casting films former; The preparation of adventitia: directly on casting films former, linear low density polyethylene is processed into film; After solvent type acrylic resin adhesives and chlorine dioxide releasing agent powder are mixed, on dry laminating equipment, binder layer material is evenly placed between adventitia and inner membrance, carries out compoundly, cut, seal.
6. the fresh-keeping packaging material of a kind of slowly-releasing chlorine dioxide bactericidal agent of claim 1 is directly used as freshness protection package.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104803078A (en) * | 2015-01-12 | 2015-07-29 | 北京印刷学院 | Multifunctional integrated freshness protection package and preparation method thereof |
| CN105819114A (en) * | 2016-05-17 | 2016-08-03 | 宁波市农业科学研究院 | Fruit parcel packaging method |
| CN106476380A (en) * | 2016-09-30 | 2017-03-08 | 广西大学 | A kind of preparation technology of slow released ClO 2 antibacterial film |
| CN107379703A (en) * | 2017-07-21 | 2017-11-24 | 上海海洋大学 | A kind of control release type active packing film and preparation method thereof |
| CN108025529A (en) * | 2015-09-30 | 2018-05-11 | 陶氏环球技术有限责任公司 | Polyolefins laminar structure with elastic characteristic |
| CN110558372A (en) * | 2019-07-17 | 2019-12-13 | 山东营养源食品科技有限公司 | Fresh-keeping laminate, preparation method and application |
| CN110803395A (en) * | 2019-11-08 | 2020-02-18 | 广东至诚紫光新材料有限公司 | Chlorine dioxide slow-release fresh-keeping packaging material and application thereof |
| CN111011483A (en) * | 2019-12-11 | 2020-04-17 | 严雯熹 | Preparation method and application of chlorine dioxide fruit and vegetable fresh-keeping slow-release agent |
| CN111621141A (en) * | 2020-06-12 | 2020-09-04 | 广西大学 | Slow-release chlorine dioxide-waterborne polyurethane antibacterial film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107379703A (en) * | 2017-07-21 | 2017-11-24 | 上海海洋大学 | A kind of control release type active packing film and preparation method thereof |
| CN107379703B (en) * | 2017-07-21 | 2019-04-19 | 上海海洋大学 | A kind of control release type active packing film and preparation method thereof |
| CN110558372A (en) * | 2019-07-17 | 2019-12-13 | 山东营养源食品科技有限公司 | Fresh-keeping laminate, preparation method and application |
| CN110803395A (en) * | 2019-11-08 | 2020-02-18 | 广东至诚紫光新材料有限公司 | Chlorine dioxide slow-release fresh-keeping packaging material and application thereof |
| CN111011483A (en) * | 2019-12-11 | 2020-04-17 | 严雯熹 | Preparation method and application of chlorine dioxide fruit and vegetable fresh-keeping slow-release agent |
| CN111621141A (en) * | 2020-06-12 | 2020-09-04 | 广西大学 | Slow-release chlorine dioxide-waterborne polyurethane antibacterial film and preparation method thereof |
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