CN102862361B - 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 multi-layer compound film and preparation method thereof, particularly relate to a kind of Fresh-Keeping Packaging Materials and the preparation method that can discharge 1-methyl cyclopropene.
Background technology
Fruit and vegetable is the requisite non-staple food of people's daily life, is to be only second to the important agricultural product of the second in the world of grain, is also important the processing raw material of food industry simultaneously.Fresh fruit and vegetable is not only for health provides multiple nutrients material.China is fruit big producing country of the world, and fruit industry occupies critical role in national economy.Since the year nineties in last century, China's fruits output and area surely occupy first place in the world always, but fruit and vegetable food moisture content is high, easily rot, present stage China's fresh fruit of vegetables due to gather improper, commercialized treatment after adopting is backward in technique, storing condition is improper and the reason such as saving and processing scarce capacity, the rotten proportion of goods damageds caused, fruit reaches 30%, vegetables reach 30%-40%, and the proportion of goods damageds of developed country are then less than 7%.Fruit rots its shelf phase of supplying is shortened greatly, causes huge economic loss, decreases peasant income, dampened its enthusiasm for production.Therefore, take functional packing material, suppress the vital movement of fruits and vegetables, reduce its metabolism, reduce the loss, extend its storage time, to keep good commercial quality, just seem very important.
In the growth of plant, ethene can promote the after-ripening of crops fruit, flower, blade, aging and come off, and is called by people the hormone that accelerates the ripening.In order to extend the shelf-life of gardening product and keep fresh, suppress the synthesis of endogenous ethylene in plant organ as much as possible or stop ethene to play a role just to seem very important.1-methyl cyclopropene (1-MCP) can irreversibly act on ethylene receptor in plant organ, thus blocks the normal combination of acceptor and ethene, suppresses a series of biochemical reactions relevant to plant or fruit maturation, plays the object of delayed fruit maturation.
2005,1-MCP can be used as the license of the chemicals applied in food, passed the U.S., Britain, Australia, Chile, France, Israel, Mexico, Switzerland, New Zealand, South Africa, Brazil, Honduras etc. are multinational.Commercial 1-MCP antistaling agent product has EthyBlock (ethene blocking agent, the U.S.) to be a kind of white powder, and 1-MCP gas is fixed in dust carrier by absorption; Ansip (An Xipei, taiwan products) is a kind of tablet; These two kinds of 1-MCP antistaling agents all adopt stifling mode to use: the volume first according to handled fruits and vegetables kind and closed container during use, a certain amount of EthyBlock or Ansip is dissolved in cushioning liquid or water, can be deflected and released suddenly out owing to dissolving rear 1-MCP gas, therefore should closed container in time, be strictly on guard against 1-MCP gas leakage.Domestic 1-MCP antistaling agent mostly adopts powder form, also adopts stifling mode to use.
Need airtight space when 1-MCP fumigates, antistaling agent abrupt release, concentration is difficult to control, and generally needs professional person to operate, otherwise is difficult to produce a desired effect, therefore need to develop a kind of can the packaging material of slowly-releasing 1-MCP.
Summary of the invention
The object of the invention is to propose a kind of can the Fresh-keeping Packaging for Fruits and Vegetables multi-layer compound film and preparation method thereof of slowly-releasing 1-MCP.The application relates to and comprises 1-methyl cyclopropene (1-MCP) as active component, it being added in composite dry process binding agent used, is prepared into the copolymer/low density polyethylene (LDPE) with EVA/LDPE(ethylene-vinyl acetate)/modified rubber film is internal layer, conventional polyethylene, polypropylene film or its modified film are the laminated film of adventitia.When fruit or vegetables are loaded into after in freshness protection package prepared by this composite membrane, fruits and vegetables breathe the steam produced can bring out this film slow Co ntrolled release 1-MCP in bag, and 1-MCP is ethylene blocking agent, fruits and vegetables can be suppressed to produce ethene, delay fruits and vegetables maturation, and then extend shelf life and the storage life of packaged fruits and vegetables; And before not loading fruits and vegetables, the water deficient in air is to cause the release of 1-MCP, the fresh-keeping function of this freshness protection package can not be activated.
A kind of Fresh-Keeping Packaging Materials discharging 1-methyl cyclopropene, it is characterized in that, these packaging material are multi-layer compound film, to comprise outermost layer be barrier layer, interlayer bond (or 1-MCP releasing layer) and innermost layer to 1-MCP gas is food contact layer, is also the Co ntrolled release layer of 1-MCP; Skin is 1-MCP barrier layer, based on one or more in low density polyethylene (LDPE) (LDPE), LLDPE (LLDPE), high density polyethylene (HDPE) (HDPE), or based on polypropylene film BOPP(bidirectional stretching polypropylene film), CPP(prolongs polypropylene film), or based on above-mentioned polyethylene and acrylic resin, in main body, add EVA(ethylene-vinyl acetate copolymer) for the film etc. of modifier is as outer; Using EVA modified PE-rubber blend as internal layer; Using 1-methyl cyclopropene (1-MCP) as active component, 1-MCP (is adsorbed on cyclodextrin carrier by 1-MCP/ cyclodextrin, 1-MCP quality accounts for 3-5%) add the drying adhesive layer that obtains in conventional polyurethane or acrylate adhesives to as 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 the outer membrane binding agent that with the addition of above-mentioned 1-MCP are prepared into laminated film by the method for dry type compound, this laminated film is prepared into freshness protection package, after loading fruits and vegetables in freshness protection package, the steam that fruits and vegetables respiration produces can be diffused into adhesive layer by the internal layer with high polarity, when running into the 1-MCP/ cyclodextrin in adhesive layer when hydrone, active force between hydrone and cyclodextrin is higher than the intermolecular forces divided between 1-MCP molecule and cyclodextrin, desorption can be there is in 1-MCP molecule from cyclodextrin carrier, then the internal layer of permeation composite membrane is diffused in packaging bag, packaged fruit is suppressed to produce ethene, preservation is played to fruit.The preferred VAM content of EVA is 16-18wt%.
The preparation method of above-mentioned packaging material, comprise the following steps: by EVA resin melt blending in outer layers body, melt blending on the twin screw extruder, wherein the quality of EVA accounts for the 5-50% of co-mixing system gross mass, prepare EVA modified resin, this modified resin is utilized to be blow molded into EVA-LDPE-rubber membrane, as skin; After EVA resin, LDPE-rubber blend on the twin screw extruder melt blending, this modified resin is utilized to be blow molded into EVA-LDPE-modified rubber film, as internal layer, wherein in LDPE-rubber blend, the content of rubber accounts for 5-40%, and the mass content of EVA resin in EVA-LDPE-modified rubber film is 5-15%; After 1-MCP/ cyclodextrin is mixed with polyurethane or acrylate adhesives, on dry laminating equipment, internal layer and skin are carried out compound, prepares the flexible packaging film with 1-MCP Co ntrolled release function, wherein amount to dry glue, the quality that 1-MCP/ cyclodextrin accounts for intermediate layer is 0.1-5%.
The skin of composite membrane, i.e. 1-MCP barrier layer, can adopt oxygen transmission rate at 1000-5000cc/m
2pure polyethylene (or polypropylene) film between day0.1MPa or their EVA modified film, by EVA melt blending to LDPE(PP) in resin.The quality of EVA accounts for the 5-50% of co-mixing system gross mass.Due to the polarity of EVA resin, comparatively polyethylene and polypropylene are all high, therefore the 1-MCP gas of adventitia to low polarity of EVA modification has higher barrier, the 1-MCP gas of effective prevention intermediate layer release outwardly discharges, and adjusts the oxygen percent of pass of outer membrane to meet the metabolic needs of packaged fruits and vegetables according to packaged fruit respiratory rate.
In the present invention, 1-MCP/ cyclodextrin and binding agent are contained in laminated film intermediate layer, its main component is the dry glue of polyurethane or acrylate adhesives, wherein add a certain amount of 1-MCP/ cyclodextrin, the ratio of 1-MCP/ cyclodextrin shared by the dry glue of binding agent is 0.1-5%(W%), preferred 0.5-2%, binding agent resin added is 3-7 gram/square meter (dry glue), preferred 4-5 gram/square meter.
In the present invention, the internal layer (food contact layer) of compound flexible packaging film is for oxygen transmission rate is at 10000-100000cc/m
2the copolymer of the polyethylene (or polypropylene) between day0.1MPa 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 are on the basis of said components, also add a certain proportion of EVA resin to regulate the polarity of inner membrance in inner membrance.Because polarity EVA adds, make the steam percent of pass of LDPE-rubbery system have raising by a relatively large margin, hydrone makes 1-MCP molecule generation desorption on cyclodextrin carrier, after more hydrone enters middle level, can increase the release concentration of 1-MCP.EVA addition is more, and the polarity of internal layer membrane is higher, and the release concentration of 1-MCP is higher.
By EVA resin melt blending to LDPE, HDPE, LLDPE or their mixture, or in 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 PE or the PP modified film being prepared into different-thickness (10-50 micron) as required makes adventitia, controls the OTR oxygen transmission rate of film at 1000-5000cc/m
2between 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, and therefore adventitia can effectively intercept 1-MCP gas, prevents 1-MCP excessive.
By EVA resin 5-15 part (quality), LDPE-rubber blend 95-85 part (quality) is on the twin screw extruder after melt blending, this modified resin is utilized to be blow molded into the EVA-LDPE-modified rubber film of 15-30 micron thickness, regulate the kind of rubber and content can change the OTR oxygen transmission rate of inner membrance, control the OTR oxygen transmission rate (OTR) of inner membrance at 10000-100000cc/m
2day0.1MPa; Wherein in LDPE-rubber blend, the content of rubber accounts for 5-40%, 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 not have an impact to the gas permeability of whole composite membrane, and has controlled polarity (regulating by EVA) and regulate moisture-vapor transmission, and then reaches and realize the controlled object of 1-MCP concentration.
After the 1-MCP/ cyclodextrin of 0.1-5 part is mixed with 99.9-95.0 part polyurethane (or acrylate) binding agent (amounting to dry glue), on dry laminating equipment, inner membrance and adventitia are carried out compound, prepares the flexible packaging film with 1-MCP Co ntrolled release function.
This composite membrane with 1-MCP Co ntrolled release function adopts conventional dry-lamination process and device fabrication, and preparation technology is simple; The composite membrane of preparation can slow Co ntrolled release 1-MCP, solves the uncontrollable problem of concentration in current preserving fruit and vegetable utilizing employing 1-MCP fumigation process.
The laminated film of this 1-MCP of having release function is prepared into freshness protection package, fruits and vegetables are sealed in sack, the steam that fruits and vegetables respiration produces makes freshness protection package humidity increase, hydrone can be diffused in intermediate layer by the inner membrance with certain polarity, hydrone makes the 1-MCP on the cyclodextrin carrier of intermediate layer desorption occur and discharge, and the polarity of inner membrance is higher, and in freshness protection package, relative humidity is larger, the hydrone then penetrating into middle level is more, and the release concentration of 1-MCP is higher.
Although 1-MCP has applied for many years in preserving fruit and vegetable utilizing field, mostly adopt the stifling technique of 1-MCP to come fresh-keeping, needed whole airtight space, and needed professional to operate just to get a desired effect; For the preserving fruit and vegetable utilizing of small lot, the form generally 1-MCP pharmacy kit being dressed up interior bag (little cartridge bag) is placed in external packing; Also be not prepared into the product form of composite membrane at present.The 1-MCP slowly-releasing flexible packaging film of our invention, there is the structure of ' sandwich ' formula, the gas permeability of composite membrane is adjusted arbitrarily to meet the respiratory needs of variety classes fruits and vegetables according to the needs of packaged fruits and vegetables, directly be prepared into the form of freshness protection package, have easy to use, medicament utilization rate is high, the feature of good refreshing effect.
After fruits and vegetables are enclosed freshness protection package, the steam that fruits and vegetables respiration produces can bring out the gas phase 1-methyl cyclopropene that film produces 0.1-0.5mg/ liter, and 1-methyl cyclopropene can block fruits and vegetables respiration and produce ethene, delays the aging of fruits and vegetables, improve the quality of fruits and vegetables, improve shelf life.Have good fresh-keeping effect to strawberry especially, under can realizing low temperature fresh-keeping 16 days, strawberry quality is good, and decayed fruit rate is lower than 15%.
1-MCP is the fruit and vegetable fresh-keeping agent allowing in the world to use, and working concentration is very low, can not remain on fruits and vegetables.Therefore our packaging material of invention meet food security relevant laws and regulations in the world.
Detailed description of the invention
By following specific embodiment and application example, the invention will be further described.Following specific descriptions are for the ease of understanding the present invention, are not used for limiting the scope of the invention.
1. compound oxygen absorbing film preparation
1.1 raw material
Antistaling film is prepared raw materials and is required as follows: the HDPE of commodity, the resins such as LDPE, LLDPE, PP, POE, EPDM, EVA; 1-MCP/ cyclodextrin; Polyurethane adhesive or acrylate adhesives.
The preparation of 1.2 outer membranes
By W1 part EVA resin and W2 part LDPE, W3 part HDPE, W4 part LLDPE, or after W5 part PP resin physical blending, melt blending at 150-230 DEG C, prepares EVA modified resin, is then prepared into PE or the PP modified film of 10-50 micron as required.
The preparation of 1.3 internal layer membranes
By W6 part EVA resin and W7 part LDPE, W8 part LLDPE, after W9 part POE, W10 part EPDM physical blending, melt blending at 150-230 DEG C, prepares EVA modified rubber polyvinyl resin, is then prepared into the PE modified film of 10-50 micron as required.
1.4 recombination process
On dry laminating equipment, by the internal layer prepared above and outer membrane by polyurethane or acrylate adhesives (containing 1-MCP/ cyclodextrin) compound, the freshness protection package of 300mm × 300mm is made in slaking after 24 hours.The test of 2 pairs of strawberry preservation performances
Take on farm to have no mechanical damage, without courses of infection, hardness at 2.0atm (pressure, atmospheric pressure) more than, the strawberry that volume is identical, medium well, be placed on polypropylene plastics pallet, then load the freshness protection package manufactured by the present invention and contrast in bag, putting the strawberry of about 750 grams in the pallet of each sack, then seal sack, put into 0-3 DEG C of fresh-keeping chamber, within 16 days, test the decayed fruit rate of strawberry, hardness and total sugar content (TSS) afterwards.The structure of comparative example 1 and embodiment 1-5 freshness protection package forms and is shown in Table 1 the fresh-keeping effect of strawberry.
Table 1. preservative film composition and the fresh-keeping effect (0-3 DEG C, after 16 days) to strawberry
Experimental result illustrates, do not add 1-MCP in the adhesive layer of comparative example 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 different with the composition of adventitia and change according to inner membrance, the 1-MCP concentration of release also can regulate according to inner membrance composition difference, freshness protection package prepared by embodiment 1-5 can slowly-releasing 1-MCP, the existence of 1-MCP makes by the rate reduction of fresh-keeping strawberry release ethene, delay the after-ripening of strawberry, improve quality, reduce decayed fruit rate.
Those skilled in the art should understand, above preferred embodiment just illustrates of the present invention, is not construed as limiting the invention.Various variation is carried out to technical scheme of the present invention and equivalence is replaced, and do not deviate from principle and the scope of technical solution of the present invention, among the scope that all should be encompassed in the claims in the present invention.
Claims (9)
1. one kind can discharge the Fresh-Keeping Packaging Materials of 1-methyl cyclopropene, it is characterized in that, these packaging material are multi-layer compound film, comprise the Co ntrolled release layer that outermost layer is barrier layer to 1-MCP gas, interlayer bond, innermost layer are food contact layer 1-MCP; Skin is 1-MCP barrier layer, based on one or more in low density polyethylene (LDPE) (LDPE), high density polyethylene (HDPE) (HDPE), or based on polypropylene film BOPP (bidirectional stretching polypropylene film), CPP (cast polypropylene film), or based on above-mentioned polyethylene and acrylic resin, in main body, add film that EVA (ethylene-vinyl acetate copolymer) is modifier as skin; Using EVA modified PE-rubber blend as internal layer; Using 1-methyl cyclopropene (1-MCP) as active component, 1-MCP/ cyclodextrin is added to the drying adhesive layer that obtains in conventional polyurethane or acrylate adhesives as intermediate layer, 1-MCP/ cyclodextrin is that 1-MCP to be adsorbed on 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 according to claim 1, it is characterized in that, the mass content 5-50% of EVA in skin, the mass ratio of 1-MCP/ cyclodextrin shared by the dry glue of binding agent is 0.1-5%, the dry glue resin added of binding agent is 3-7 gram/square meter, rubber quality content 5-40% in the mass content 5-15% of EVA, PE-rubber blend in internal layer.
3. according to packaging material according to claim 2, it is characterized in that, the mass content 15-25% of EVA in skin, the mass ratio of 1-MCP/ cyclodextrin shared by the dry glue of binding agent is 0.5-2%, the dry glue resin added of binding agent is 4-5 gram/square meter, rubber 15-25% in the mass content 5-15% of EVA, PE-rubber blend in internal layer.
4. according to packaging material according to claim 1, it is characterized in that, outer layer thickness is 10-50 micron, and internal layer thickness is 15-30 micron.
5. according to packaging material according to claim 1, it is characterized in that, in internal layer, PE-rubber blend is that oxygen transmission rate is at 10000-100000cc/m
2polyethylene between day0.1MPa and the blend of rubber resin.
6. according to packaging material according to claim 1, it is characterized in that, the preferred VAM content of EVA is 16-18wt%.
7. according to packaging material according to claim 1, it is characterized in that, skin can be replaced oxygen transmission rate at 1000-5000cc/m
2pure polyethylene between day0.1MPa or polypropylene film.
8. according to packaging material according to claim 1, it is characterized in that, low density polyethylene (LDPE) (LDPE) is LLDPE (LLDPE).
9. a kind of preparation method discharging the Fresh-Keeping Packaging Materials of 1-methyl cyclopropene according to claim 1, it is characterized in that, comprise the following steps: by EVA resin melt blending in outer layers body, melt blending on the twin 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 EVA-LDPE-rubber membrane, as skin; After EVA resin, LDPE-rubber blend on the twin screw extruder melt blending, this modified resin is utilized to be blow molded into EVA-LDPE-modified rubber film, as internal layer, wherein in LDPE-rubber blend, the content of rubber accounts for 5-40%, and the mass content of EVA resin in EVA-LDPE-modified rubber film is 5-15%; After 1-MCP/ cyclodextrin is mixed with polyurethane or acrylate adhesives, on dry laminating equipment, internal layer and skin are carried out compound, prepares the flexible packaging film with 1-MCP Co ntrolled release function, wherein amount to dry glue, the quality that 1-MCP/ cyclodextrin accounts for intermediate layer is 0.1-5%.
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| CN103144845B (en) * | 2013-03-01 | 2017-09-05 | 李东立 | The special paper-plastic composite film of fruit and vegetable normal-temperature fresh-keeping |
| US9394216B2 (en) | 2014-11-10 | 2016-07-19 | Mirtech, Inc. | Complexes of 1-methylcyclopropene with metal coordination polymer networks |
| CN104788781A (en) * | 2015-03-31 | 2015-07-22 | 苏州市鼎立包装有限公司 | Formula and preparation method of LDPE packaging bag |
| JP6935428B2 (en) | 2016-02-19 | 2021-09-15 | ヘイゼル テクノロジーズ， インコーポレイテッド | Composition for controlled release of active ingredient and method for its preparation |
| CN108202517A (en) * | 2016-12-19 | 2018-06-26 | Sabic环球技术有限责任公司 | Multilayer film |
| CN106976646B (en) * | 2017-04-26 | 2019-10-29 | 深圳市裕同包装科技股份有限公司 | A kind of vegetables and fruits packaging material and its preparation process |
| CN109384946B (en) * | 2018-08-09 | 2022-12-06 | 浙江舟山群岛新区紫气东来智能包装材料有限公司 | Fresh-keeping packaging bag, preparation method and application thereof |
| 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 |
| CN112342823B (en) * | 2020-10-23 | 2022-08-16 | 广州市佰润文化创意有限公司 | Method for manufacturing degradable packaging bag |
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Inventor after: Qian Junhao Inventor after: Li Dongli Inventor after: Xu Wencai Inventor after: Xu Weihong Inventor before: Li Dongli Inventor before: Xu Wencai Inventor before: Fu Yabo Inventor before: Qi Yingqun Inventor before: Cao Guorong Inventor before: Liu Quanxiao |
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Effective date of registration: 20160920 Address after: 214000, Wuxi New District, Jiangsu, tian an intelligence city, A1-1205 Patentee after: Jiangsu Fruit Preservation Technology Co., Ltd. Address before: 102600 No. 25 Xinghua North Road, Huangcun village, Beijing, Daxing District Patentee before: Beijing Print College |
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Effective date of registration: 20210406 Address after: 214000 No.37 Lihu business park, Binhu District, Wuxi City, Jiangsu Province Patentee after: Jiangsu Qianye Construction Co., Ltd Address before: 214000 Tian'an smart city a1-1205, Wuxi New District, Jiangsu Province Patentee before: JIANGSU WANGUO FRESH-KEEPING TECHNOLOGY Co.,Ltd. |