CN102862361A - Fruit and vegetable freshness retaining packaging material capable of releasing 1-methyl cyclopropene and preparation method thereof - Google Patents
Fruit and vegetable freshness retaining packaging material capable of releasing 1-methyl cyclopropene and preparation method thereof Download PDFInfo
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Abstract
The invention provides a fruit and vegetable freshness retaining packaging material capable of releasing 1-methyl cyclopropene and a preparation method thereof, belonging to the technical field of a packaging material. The 1-methyl cyclopropene (1-MCP) is used as an active component and is added into a binding agent used by a dry method composite technique, so as to prepare a composite thin film using EVA/LDPE (Ethylene-Vinyl Acetate copolymer/ Low-Density Polyethylene)/rubber modified film as an inner layer and using normally used polyethylene and polyethylene and or modified thin film thereof as an outer layer. When fruits or vegetables are filled into a freshness retaining bag prepared by the composite film, water gas generated by breath of the fruits or the vegetables induces the thin film to slowly release the 1-MCP in the bag; the 1-MCP is an ethylene stopping agent, and the fruits and the vegetables can be prevented from generating ethylene; the maturity of the fruits or the vegetables can be slowed, so that the goods self period and the storage period of the packaged fruits or vegetables can be prolonged; and before the fruits or vegetables are filled, water in air is not enough to release the 1-MCP. The freshness retaining function of the freshness retaining bag is not opened.
Description
Technical field
The invention belongs to field of packaging material, relate to a kind of Fresh-keeping Packaging for Fruits and Vegetables with multi-layer compound film and preparation method thereof, relate in particular to a kind of Fresh-Keeping Packaging Materials and preparation method that can discharge the 1-methyl cyclopropene.
Background technology
Fruit and vegetable is the requisite non-staple food of people's daily life, is the important agricultural product of the second in the world that are only second to grain, also is important the processing raw material of food industry simultaneously.Fresh fruit and vegetable not only provides the multiple nutrients material for health.China is world fruit big producing country, and the fruit industry is occupied critical role in national economy.Since the year nineties in last century, China's fruits output and area are sure to occupy first place, the world always, but the fruit and vegetable food moisture content is high, rot easily, present stage China's fresh fruit of vegetables improper owing to gathering, adopt that rear commercialization treatment technology falls behind, the storing condition is improper and the reason such as storage working ability deficiency, the rotten proportion of goods damageds that cause, fruit reaches 30%, vegetables reach 30%-40%, and the proportion of goods damageds of developed country are then less than 7%.Fruit rots to make its shelf supply phase greatly to shorten, and causes huge economic loss, has reduced peasant income, has dampened its enthusiasm for production.Therefore, take functional packing material, suppress the vital movement of fruits and vegetables, reduce its metabolism, reduce the loss, prolong its storage time, to keep good commercial quality, just seem very important.
In the growth of plant, ethene can promote after-ripening, the aging of crops fruit, flower, blade and come off, is called the hormone that accelerates the ripening by people.For the shelf-life that prolongs gardening product and keep fresh, suppress as much as possible the synthetic of endogenous ethylene in the plant organ or stop ethene to play a role just to seem very important.1-methyl cyclopropene (1-MCP) can irreversibly act on ethylene receptor in the plant organ, thus the normal combination of blocking-up acceptor and ethene, and a series of biochemical reactions that inhibition is relevant with plant or fruit maturation play the purpose of delayed fruit maturation.
2005,1-MCP can be used as the license of the chemicals of using in food, multinational passing such as the U.S., Britain, Australia, Chile, France, Israel, Mexico, Switzerland, New Zealand, South Africa, Brazil, Honduras.EthyBlock (ethene blocking agent, the U.S.) is arranged is a kind of white powder to commercial 1-MCP antistaling agent product, and 1-MCP gas is absorbed and is fixed in the dust carrier; Ansip (An Xipei, taiwan products) is a kind of tablet; These two kinds of 1-MCP antistaling agents all adopt stifling mode to use: elder generation is according to the volume of handled fruits and vegetables kind and closed container during use, a certain amount of EthyBlock or Ansip are dissolved in cushioning liquid or the water, because 1-MCP gas can be discharged immediately after the dissolving, therefore timely closed container is strictly on guard against the 1-MCP gas leakage.Domestic 1-MCP antistaling agent mostly adopts powder form, also adopts stifling mode to use.
Need to the space is airtight when 1-MCP is stifling, the antistaling agent abrupt release, concentration is difficult to control, generally needs the professional person to operate, otherwise is difficult to produce a desired effect, and therefore needs a kind of packaging material that can slowly-releasing 1-MCP of exploitation.
Summary of the invention
The objective of the invention is to propose a kind of Fresh-keeping Packaging for Fruits and Vegetables that can slowly-releasing 1-MCP with multi-layer compound film and preparation method thereof.The application relates to and comprises 1-methyl cyclopropene (1-MCP) as active component, it is added in the used binding agent of composite dry process, is prepared into take the copolymer/low density polyethylene (LDPE) of EVA/LDPE(ethylene-vinyl acetate)/laminated film of modified rubber film as internal layer, polyethylene, polypropylene film or its modified film commonly used as adventitia.After fruit or vegetables are loaded in the freshness protection package of this composite membrane preparation, the steam that the fruits and vegetables breathing produces can bring out this film and slowly control release 1-MCP in bag, and 1-MCP is the ethene blocking agent, can suppress fruits and vegetables and produce ethene, delay the fruits and vegetables maturation, and then prolong shelf life and the storage life of packaged fruits and vegetables; And before not loading fruits and vegetables, airborne water deficient is to cause the release of 1-MCP, and the fresh-keeping function of this freshness protection package can not be activated.
A kind of Fresh-Keeping Packaging Materials that discharges the 1-methyl cyclopropene, it is characterized in that, these packaging material are multi-layer compound film, comprising that outermost layer is that barrier layer, intermediate layer binding agent (or 1-MCP releasing layer) and innermost layer to 1-MCP gas is the Food Contact layer, also is the control releasing layer of 1-MCP; Skin is the 1-MCP barrier layer, that in low density polyethylene (LDPE) (LDPE), LLDPE (LLDPE), the high density polyethylene (HDPE) (HDPE) one or more are as main body, perhaps take polypropylene film BOPP(bidirectional stretching polypropylene film), CPP(prolongs polypropylene film) as main body, perhaps take above-mentioned polyethylene and acrylic resin as main body, in main body, add the EVA(ethylene-vinyl acetate copolymer) be that the film etc. of modifier is as skin; With EVA modified PE-rubber blend as internal layer; With 1-methyl cyclopropene (1-MCP) as active component, the 1-MCP/ cyclodextrin (is adsorbed on 1-MCP on the cyclodextrin carrier, the 1-MCP quality accounts for 3-5%) add the drying adhesive layer that obtains in polyurethane commonly used or the acrylate adhesives to as the intermediate layer, outer field polarity is higher than the polarity of internal layer, and outer field barrier is higher than the barrier of internal layer.Above-mentioned internal layer and outer membrane are prepared into laminated film with the binding agent that has added above-mentioned 1-MCP by the compound method of dry type, this laminated film is prepared into freshness protection package, behind filling fruits and vegetables in the freshness protection package, the steam that the fruits and vegetables respiration produces can be diffused into adhesive layer by the internal layer with high polarity, when hydrone runs into 1-MCP/ cyclodextrin in the adhesive layer, active force between hydrone and the cyclodextrin be higher than between 1-MCP molecule and cyclodextrin minute between active force, desorption can occur from the cyclodextrin carrier in the 1-MCP molecule, then the internal layer of permeation composite membrane is diffused in the packaging bag, suppress packaged fruit and produce ethene, fruit is played preservation.The preferred VAM content of EVA is 16-18wt%.
The preparation method of above-mentioned packaging material, may further comprise the steps: the EVA resin melting is blended in the outer layer main body, melt blending on double screw extruder, wherein the quality of EVA accounts for the 5-50% of co-mixing system gross mass, prepare EVA modified resin, utilize this modified resin to be blow molded into the EVA-LDPE-rubber membrane, as skin; With EVA resin, LDPE-rubber blend behind melt blending on the double screw extruder, utilize this modified resin to be blow molded into EVA-LDPE-modified rubber film, as internal layer, wherein the content of rubber accounts for 5-40% in the LDPE-rubber blend, and the mass content of EVA resin in EVA-LDPE-modified rubber film is 5-15%; With the 1-MCP/ cyclodextrin with after polyurethane or acrylate adhesives mix, on dry laminating equipment, internal layer and skin are carried out compound, prepare the flexible packaging film with 1-MCP control release function, wherein amount to dried glue, the quality that the 1-MCP/ cyclodextrin accounts for the intermediate layer is 0.1-5%.
The skin of composite membrane, namely the 1-MCP barrier layer can adopt oxygen transmission rate at 1000-5000cc/m
2Pure polyethylene (or polypropylene) film between the day0.1MPa or their EVA modified film, with the EVA melt blending to LDPE(PP) in the resin.The quality of EVA accounts for the 5-50% of co-mixing system gross mass.Because the polarity of EVA resin is all high than polyethylene and polypropylene, therefore the adventitia of EVA modification has higher barrier to the 1-MCP gas of low polarity, the 1-MCP gas that effectively stops the intermediate layer to discharge discharges to the external world, adjusts the oxygen percent of pass of outer membrane to satisfy the metabolic needs of packaged fruits and vegetables according to packaged fruit respiratory rate.
1-MCP/ cyclodextrin and binding agent are contained in the laminated film intermediate layer among the present invention, its main component is the dried glue of polyurethane or acrylate adhesives, wherein add a certain amount of 1-MCP/ cyclodextrin, 1-MCP/ cyclodextrin shared ratio in the dried glue of binding agent is 0.1-5%(W%), preferred 0.5-2%, the binding agent resin added is 3-7 gram/square meter (dried glue), preferred 4-5 gram/square meter.
The internal layer of compound flexible packaging film among the present invention (Food Contact layer) is that oxygen transmission rate is at 10000-100000cc/m
2The copolymer of the polyethylene between the day0.1MPa (or polypropylene) and rubber resin, rubber resin comprises ethylene propylene diene rubber (EPDM), POE(ethylene-octene copolymer) etc., in order to regulate the moisture-vapor transmission of inner membrance, we also add a certain proportion of EVA resin to regulate the polarity of inner membrance in inner membrance on the basis of said components.Because polarity EVA adds, make the steam percent of pass of LDPE-rubbery system that by a relatively large margin raising be arranged, hydrone is so that 1-MCP molecule generation desorption on the cyclodextrin carrier after more hydrone enters the middle level, can increase the release concentration of 1-MCP.The EVA addition is more, and the polarity of internal layer membrane is higher, and the release concentration of 1-MCP is higher.
The EVA resin melting is blended into LDPE, HDPE, LLDPE or their mixture, or in the PP resin, wherein the quality of EVA accounts for the 5-50% of co-mixing system gross mass, preferred 15-25%, prepare EVA modified resin, then the PE or the PP modified film that are prepared into as required different-thickness (10-50 micron) are made adventitia, and the OTR oxygen transmission rate of control film is at 1000-5000cc/m
2Between the day0.1MPa, the polarity of adventitia is higher than the polarity of inner membrance, and the barrier of adventitia is higher than the barrier of inner membrance, so adventitia can effectively intercept 1-MCP gas, prevents that 1-MCP is excessive.
With EVA resin 5-15 part (quality), LDPE-rubber blend 95-85 part (quality) is behind melt blending on the double screw extruder, utilize this modified resin to be blow molded into the EVA-LDPE-modified rubber film of 15-30 micron thickness, regulate the kind of rubber and the OTR oxygen transmission rate that content can change inner membrance, the OTR oxygen transmission rate (OTR) of control inner membrance is at 10000-100000cc/m
2Day0.1MPa; Wherein the content of rubber accounts for 5-40% in the LDPE-rubber blend, preferred 15-25%, and the kind of optional rubber comprises EPDM, POE etc.The OTR oxygen transmission rate of this inner membrance is high, can the gas permeability of whole composite membrane not exerted an influence, and has controlled polarity (regulating by EVA) and regulate moisture-vapor transmission, and then reach and realize the controlled purpose of 1-MCP concentration.
With the 1-MCP/ cyclodextrin of 0.1-5 part with after 99.9-95.0 part polyurethane (or acrylate) binding agent (amounting to dried glue) mixes, on dry laminating equipment, inner membrance and adventitia are carried out compound, prepare the flexible packaging film with 1-MCP control release function.
This composite membrane with 1-MCP control release function adopts conventional dry-lamination process and device fabrication, and preparation technology is simple; The composite membrane of preparation can slowly be controlled and discharge 1-MCP, has solved present preserving fruit and vegetable utilizing and has adopted the uncontrollable problem of concentration in the 1-MCP fumigation process process.
The laminated film of this 1-MCP of having release function is prepared into freshness protection package, fruits and vegetables are sealed in the sack, the steam that the fruits and vegetables respiration produces makes humidity increase in the freshness protection package, hydrone can be diffused into by the inner membrance with certain polarity in the intermediate layer, hydrone so that in the intermediate layer 1-MCP on the cyclodextrin carrier desorption occurs and discharge, the polarity of inner membrance is higher, relative humidity is larger in the freshness protection package, the hydrone that then is penetrated into the middle level is more, and the release concentration of 1-MCP is higher.
Although 1-MCP has used for many years in the preserving fruit and vegetable utilizing field, it is fresh-keeping mostly to adopt the stifling technique of 1-MCP, need to whole space is airtight, and need the professional to operate just to get a desired effect; For the preserving fruit and vegetable utilizing of small lot, the form of generally the 1-MCP pharmacy kit being dressed up interior bag (little cartridge bag) places in the external packing; Also be not prepared at present the product form of composite membrane.The 1-MCP slowly-releasing flexible packaging film of our invention, structure with ' sandwich ' formula, according to the needs of packaged fruits and vegetables and the gas permeability of adjusting arbitrarily composite membrane to satisfy the respiratory needs of variety classes fruits and vegetables, directly be prepared into the form of freshness protection package, have easy to use, the medicament utilization rate is high, the characteristics of good refreshing effect.
After fruits and vegetables are enclosed freshness protection package, the steam that the fruits and vegetables respiration produces can bring out film and produce the gas phase 1-methyl cyclopropene that 0.1-0.5mg/ rises, and the 1-methyl cyclopropene can be blocked the fruits and vegetables respiration and produce ethene, delays the aging of fruits and vegetables, improve the quality of fruits and vegetables, improve shelf life.Especially strawberry is had preferably fresh-keeping effect, can realize under the low temperature that the strawberry quality was good fresh-keeping 16 days, the decayed fruit rate is lower than 15%.
1-MCP allows the fruit and vegetable fresh-keeping agent that uses in the world, and working concentration is very low, can be not residual on fruits and vegetables.Therefore our packaging material of invention meet in the world food security relevant laws and regulations.
The specific embodiment
The invention will be further described by following specific embodiment and application example.Following specific descriptions are for the ease of understanding the present invention, not being used for limiting protection scope of the present invention.
1. compound oxygen absorbing film preparation
1.1 raw material
Antistaling film prepares raw materials and requires as follows: the HDPE of commodity, LDPE, LLDPE, PP, POE, EPDM, the resins such as EVA; The 1-MCP/ cyclodextrin; Polyurethane adhesive or acrylate adhesives.
1.2 the preparation of outer membrane
With W1 part EVA resin and W2 part LDPE, W3 part HDPE, W4 part LLDPE, or behind W5 part PP resin physical blending, at 150-230 ℃ of lower melt blending, prepare EVA modified resin, then be prepared into as required PE or the PP modified film of 10-50 micron.
1.3 the preparation of internal layer membrane
With W6 part EVA resin and W7 part LDPE, W8 part LLDPE, W9 part POE behind W10 part EPDM physical blending, at 150-230 ℃ of lower melt blending, prepares EVA modified rubber polyvinyl resin, then is prepared into as required the PE modified film of 10-50 micron.
1.4 recombination process
On dry laminating equipment, the internal layer and the outer membrane that prepare above is compound by polyurethane or acrylate adhesives (containing the 1-MCP/ cyclodextrin), and the freshness protection package of 300mm * 300mm is made in slaking after 24 hours.2 pairs of strawberry preservation performance tests
Take to have no mechanical damage on the farm, without germ infect, hardness is at 2.0atm (pressure, atmospheric pressure) more than, the strawberry that volume is identical, medium well, be placed on the polypropylene plastics pallet, then pack in the freshness protection package and contrast bag of manufacturing of the present invention, put the strawberry about 750 grams in the pallet of each sack, then seal sack, put into 0-3 ℃ of fresh-keeping chamber, tested afterwards decayed fruit rate, hardness and the total sugar content (TSS) of strawberry in 16 days.The structure of Comparative Examples 1 and embodiment 1-5 freshness protection package forms and the fresh-keeping effect of strawberry is shown in Table 1.
Table 1. preservative film forms the fresh-keeping effect (0-3 ℃, after 16 days) that reaches strawberry
1-MCP is not added in the experimental result explanation in the adhesive layer of Comparative Examples 1, prepared freshness protection package can not discharge 1-MCP, and packaged strawberry 70% occurs to rot, and loses edibility; And embodiment 1-5, the gas permeability of prepared freshness protection package can be according to different variation of composition of inner membrance and adventitia, the 1-MCP concentration that discharges also can form different the adjusting according to inner membrance, because the prepared freshness protection package of embodiment 1-5 can slowly-releasing 1-MCP, the existence of 1-MCP is so that discharged the rate reduction of ethene by fresh-keeping strawberry, delay the after-ripening of strawberry, improved quality, reduced the decayed fruit rate.
Those skilled in the art should understand that above preferred embodiment just specifies of the present invention, is not construed as limiting the invention.Technical scheme of the present invention is carried out 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 claim of the present invention.
Claims (8)
1. Fresh-Keeping Packaging Materials that can discharge the 1-methyl cyclopropene, it is characterized in that, these packaging material are multi-layer compound film, comprise that outermost layer is barrier layer, intermediate layer binding agent or the 1-MCP releasing layer to 1-MCP gas, the control releasing layer that innermost layer is Food Contact layer or 1-MCP; Skin is the 1-MCP barrier layer, that in low density polyethylene (LDPE) (LDPE), LLDPE (LLDPE), the high density polyethylene (HDPE) (HDPE) one or more are as main body, perhaps take polypropylene film BOPP(bidirectional stretching polypropylene film), CPP(prolongs polypropylene film) as main body, perhaps take above-mentioned polyethylene and acrylic resin as main body, in main body, add the EVA(ethylene-vinyl acetate copolymer) be that the film etc. of modifier is as skin; With EVA modified PE-rubber blend as internal layer; With 1-methyl cyclopropene (1-MCP) as active component, add the 1-MCP/ cyclodextrin to obtain in polyurethane commonly used or the acrylate adhesives drying adhesive layer as the intermediate layer, the 1-MCP/ cyclodextrin is that 1-MCP is adsorbed on the cyclodextrin carrier and 1-MCP mass content 3-5%, outer field polarity is higher than the polarity of internal layer, and outer field barrier is higher than the barrier of internal layer.
2. according to packaging material claimed in claim 1, it is characterized in that, the mass content 5-50% of EVA in the skin, 1-MCP/ cyclodextrin shared mass ratio in the dried glue of binding agent is 0.1-5%, the dried glue resin added of binding agent is 3-7 gram/square meter, the mass content 5-15% of EVA in the internal layer, rubber quality content 5-40% in the PE-rubber blend.
3. according to packaging material claimed in claim 2, it is characterized in that, the mass content 15-25% of EVA in the skin, 1-MCP/ cyclodextrin shared mass ratio in the dried glue of binding agent is 0.5-2%, the dried glue resin added of binding agent is 4-5 gram/square meter, the mass content 5-15% of EVA in the internal layer, rubber 15-25% in the PE-rubber blend.
4. according to packaging material claimed in claim 1, it is characterized in that outer layer thickness is the 10-50 micron, internal layer thickness is the 15-30 micron.
5. according to packaging material claimed in claim 1, it is characterized in that the PE-rubber blend is that oxygen transmission rate is at 10000-100000cc/m in the internal layer
2The copolymer of the polyethylene between the day0.1MPa or polypropylene and rubber resin.
6. according to packaging material claimed in claim 1, it is characterized in that the preferred VAM content of EVA is 16-18wt%.
7. according to packaging material claimed in claim 1, it is characterized in that skin is replaceable to be that oxygen transmission rate is at 1000-5000cc/m
2Pure polyethylene or polypropylene film between the day0.1MPa.
8. a kind of preparation method who discharges the Fresh-Keeping Packaging Materials of 1-methyl cyclopropene claimed in claim 1, it is characterized in that, may further comprise the steps: the EVA resin melting is blended in the outer layer main body, melt blending on double screw extruder, wherein the quality of EVA accounts for the 5-50% of co-mixing system gross mass, prepare EVA modified resin, utilize this modified resin to be blow molded into the EVA-LDPE-rubber membrane, as skin; With EVA resin, LDPE-rubber blend behind melt blending on the double screw extruder, utilize this modified resin to be blow molded into EVA-LDPE-modified rubber film, as internal layer, wherein the content of rubber accounts for 5-40% in the LDPE-rubber blend, and the mass content of EVA resin in EVA-LDPE-modified rubber film is 5-15%; With the 1-MCP/ cyclodextrin with after polyurethane or acrylate adhesives mix, on dry laminating equipment, internal layer and skin are carried out compound, prepare the flexible packaging film with 1-MCP control release function, wherein amount to dried glue, the quality that the 1-MCP/ cyclodextrin accounts for the intermediate layer is 0.1-5%.
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| CN109880527A (en) * | 2019-02-01 | 2019-06-14 | 西安泰鲜生物科技有限公司 | Increase the method for one layer of preservative film on packaging material and articles |
| CN112342823A (en) * | 2020-10-23 | 2021-02-09 | 广州市佰润文化创意有限公司 | Method for manufacturing degradable packaging bag |
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