CN113681993A - Fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation and preparation method thereof - Google Patents
Fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation and preparation method thereof Download PDFInfo
- Publication number
- CN113681993A CN113681993A CN202110993391.1A CN202110993391A CN113681993A CN 113681993 A CN113681993 A CN 113681993A CN 202110993391 A CN202110993391 A CN 202110993391A CN 113681993 A CN113681993 A CN 113681993A
- Authority
- CN
- China
- Prior art keywords
- film
- bacteriostatic
- breathable
- fresh
- antibacterial
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000012785 packaging film Substances 0.000 title claims abstract description 74
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- 230000003385 bacteriostatic effect Effects 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 54
- 235000012055 fruits and vegetables Nutrition 0.000 title claims abstract description 40
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 89
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- JGUQDUKBUKFFRO-CIIODKQPSA-N dimethylglyoxime Chemical compound O/N=C(/C)\C(\C)=N\O JGUQDUKBUKFFRO-CIIODKQPSA-N 0.000 claims description 8
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Images
Classifications
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- C08K5/47—Thiazoles
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Abstract
The application relates to the technical field of fruit and vegetable packaging materials, in particular to a fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation and a preparation method thereof. The fresh-keeping and bacteriostatic breathable packaging film for ship fruit and vegetable transportation comprises an antibacterial inner film, a polyurethane elastic middle film and an outer protective film, wherein the antibacterial inner film is prepared from the following raw materials: breathable master batch and bacteriostatic master batch; the bacteriostatic master batch consists of low-density polyethylene, 4, 5-dichloro-2-n-octyl-3-isothiazolinone, zeolite powder and nano zinc oxide; the breathable master batch is prepared from the following raw materials in percentage by mass: 8-12% of low density polyethylene, 20-28% of linear low density polyethylene, 14-20% of metallocene linear low density polyethylene and the balance of inorganic filler. The packaging film prepared by the application has good air permeability and antibacterial mildew resistance, can prolong the fresh-keeping time of fruits and vegetables, and meets the fresh-keeping requirement of ocean transportation.
Description
Technical Field
The application relates to the technical field of fruit and vegetable packaging materials, in particular to a fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation and a preparation method thereof.
Background
Ocean shipping is one type of marine transportation and is also an integral part of the entire transportation industry. Due to different climates around the world, different kinds of vegetables, melons and fruits are bred, and the melons, melons and vegetables around the world can not be transported in the ocean. The time for ocean shipping is generally different from 0.5 to 4 months, thereby causing the following problems: the storage and preservation difficulty of the transported fresh fruits and vegetables is high.
Currently, the methods for storing melons, fruits and vegetables for ocean transportation are as follows: firstly, packaging fruits, vegetables and the like in a sealing bag, and then putting the packaged fruits, vegetables and the like into a low-temperature storage chamber, wherein the temperature of the low-temperature storage chamber is controlled to be 0-4 ℃, and the humidity is controlled to be 40-70%. The sealing bags used for packaging are usually PP sealing bags, PVC sealing bags, OPP sealing bags and the like.
Aiming at the method for storing melons, fruits and vegetables in the related art, the inventor finds that the technical scheme has the following defects: due to the fact that the ocean transportation time is relatively long, although the growth and reproduction of microorganisms can be inhibited and the respiration of the melons and fruits can be reduced under the condition of low-temperature storage, a certain amount of water vapor can be generated under the respiration of the melons and fruits, the melons and fruits and vegetables are in a closed environment with water for a long time, the stored melons and fruits and vegetables can go bad, and the quality of the transported melons, fruits and vegetables is reduced.
Disclosure of Invention
In order to solve the problems that the freshness-keeping capacity of fruits and vegetables is relatively poor and the quality of the fruits and vegetables is affected in the prior art, the application provides a fresh-keeping and bacteriostatic breathable packaging film for ship fruit and vegetable transportation and a preparation method thereof.
First aspect, the application provides a fresh-keeping antibacterial ventilative packaging film for boats and ships fruit vegetables transportation, is realized through following technical scheme:
a fresh-keeping bacteriostatic breathable packaging film for shipping fruit and vegetable transportation comprises an antibacterial inner film, a polyurethane elastic intermediate film and an outer protective film, wherein the polyurethane elastic intermediate film is compounded between the antibacterial inner film and the outer protective film; the antibacterial inner membrane is prepared from the following raw materials in parts by weight: 100 parts of breathable master batch and 5-10 parts of antibacterial master batch; the antibacterial mother material consists of low-density polyethylene, 4, 5-dichloro-2-n-octyl-3-isothiazolinone, zeolite powder and nano zinc oxide; the breathable master batch is prepared from the following raw materials in percentage by mass: 8-12% of low density polyethylene, 20-28% of linear low density polyethylene, 14-20% of metallocene linear low density polyethylene and the balance of inorganic filler.
Through adopting above-mentioned technical scheme, the antibacterial ventilative packaging film that keeps fresh that adopts antibiotic inner membrane, polyurethane elasticity intermediate coat and the compound preparation of outer protection film to obtain has better waterproof gas permeability and antibiotic mould proof nature, can be used as the packaging film material of ocean transportation fruit vegetables transportation, effectively prolongs the fresh-keeping time of melon and fruit vegetables, promotes melon and fruit vegetables's quality, brings better economic benefits.
Preferably, the polyurethane elastic intermediate film is composed of two layers of TPU films and a self-healing film compounded between the two layers of TPU films; the TPU film is prepared from TPU master batches, antibacterial fillers and porous breathable fillers; the antibacterial filler is dispersed in the TPU film; the porous breathable filler is embedded in the TPU film; one end of the porous breathable filler is exposed out of the lower surface of the TPU film, and the other end of the porous breathable filler is exposed out of the upper surface of the TPU film.
Through adopting above-mentioned technical scheme, in the packaging film use, be in under 0-4 ℃ of environment through the packaging film, the packaging film is easily receive external impact to take place the damage under low temperature environment, and the polyurethane elasticity intermediate coat that this application adopted self-healing membrane and TPU membrane to combine the preparation has not only guaranteed the waterproof gas permeability and the antibiotic mould proof nature of packaging film, and self mechanical strength is good and self damaged self-healing, can effectively prolong melon and fruit vegetables's fresh-keeping time, guarantees the quality of transportation melon and fruit vegetables.
Preferably, the antibacterial filler is composed of anatase type nano TiO2 and light calcium carbonate; the thickness of the TPU film is 60-100 microns; the porous breathable filler is a 5A molecular sieve; the particle size of the porous breathable filler is 1.05-1.2 times the thickness of the TPU film.
By adopting the technical scheme, the anatase type nano TiO2 has a good sterilization and mildew-proof effect, and the light calcium carbonate plays a role in opening holes in the TPU film during casting processing so as to ensure the water resistance and the air permeability of the TPU film; the 5A molecular sieve is a zeolite material with open pores and is used as a gas flow channel to purify the passing gas, remove harmful microorganisms in the air and further prolong the fresh-keeping time of the fruits and vegetables.
Preferably, the self-healing film is prepared by taking self-healing polyurethane resin as a raw material through tape casting; the self-healing polyurethane resin is prepared from the following raw materials: MDI, 1, 6-hexanediol, polyester polyol, a catalyst, dimethylglyoxime, an organic solvent, an antioxidant and an open-cell filler; the sum of the molar amount of the hydroxyl groups of the 1, 6-hexanediol, the molar amount of the hydroxyl groups of the polyester polyol and the molar amount of the hydroxyl groups of the dimethylglyoxime is 1.01 to 1.05 times of the molar amount of the-NCO in the MDI; the open pore filler is 300-400 mesh barium sulfate.
Through adopting above-mentioned technical scheme, the self-healing membrane of preparation receives external force to strike damaged in this application, can guarantee the gas tightness of the packaging film who prepares in 2 days, effectively prolongs melon and fruit vegetables's fresh-keeping time, reduces the rotten probability of fruit vegetables, guarantees the quality of transportation melon and fruit vegetables.
Preferably, the preparation method of the self-healing film comprises the following steps:
s1, adding accurately measured 1, 6-hexanediol, butanone, polyester polyol and an antioxidant into an organic solvent, and uniformly mixing to obtain a mixed solution;
s2, adding a catalyst with accurate measurement, adding the mixed solution, and adding MDI into the mixed solution for multiple times at the temperature of 70-80 ℃, wherein the reaction time is controlled to be 8 +/-0.5 h;
s3, adding a precisely-measured perforated filler after the reaction is finished, and uniformly stirring to obtain the self-healing polyurethane resin;
s4, extruding and granulating the self-healing polyurethane resin to obtain self-healing resin particles;
and S5, adding the self-healing resin particles into a casting film extruder, and performing casting, stretching and heat setting to obtain the finished self-healing film.
By adopting the technical scheme, the polyurethane elastic intermediate film with the self-healing function can be prepared, the mechanical strength and the air tightness of the packaging film are effectively improved, the preservation time of fruits and vegetables is prolonged, and the quality of the transported fruits and vegetables is ensured.
Preferably, the outer protective film is a PET film; the thickness of the outer protective film is 60-120 microns; the outer protective film is integrally formed with a ventilation hole; the diameter of the air-permeable pore canal is 0.1-0.5 mm; the air-permeable pore channels are distributed in a dot matrix manner; the distance between the circle centers of the adjacent air permeable pore canals is 2.0-3.0 mm.
Through adopting above-mentioned technical scheme, guarantee the gas permeability of the fresh-keeping antibacterial ventilative packaging film who prepares and protect polyurethane elasticity intermediate coat simultaneously to promote holistic mechanical strength, therefore this application has longer life.
Preferably, the inorganic filler is at least one of light calcium carbonate, barium sulfate and titanium dioxide; the grain size of the inorganic filler is less than or equal to 5 microns.
By adopting the technical scheme, the inorganic filler plays a role in opening pores on the antibacterial inner membrane, so that the air permeability of the antibacterial inner membrane is ensured, and the mechanical strength and the chemical resistance stability of the antibacterial inner membrane can be improved.
In a second aspect, the application provides a preparation method of a fresh-keeping, bacteriostatic and breathable packaging film for shipping fruit and vegetable transportation, which is realized by the following technical scheme:
a preparation method of a fresh-keeping bacteriostatic breathable packaging film for shipping fruit and vegetable transportation comprises the following steps:
s1, preparing an antibacterial inner membrane, a polyurethane elastic intermediate membrane and an outer protective membrane;
s2, compounding the antibacterial inner membrane on the upper surface of the polyurethane elastic intermediate membrane in a hot-pressing manner, and compounding the outer protective membrane on the lower surface of the polyurethane elastic intermediate membrane in a hot-pressing manner to obtain a semi-finished product;
and S3, carrying out heat treatment on the semi-finished product to obtain the finished product packaging film.
By adopting the technical scheme, the preparation method is simple, industrial batch production is facilitated, the production cost of the fresh-keeping antibacterial breathable packaging film is reduced, market share is facilitated to be seized, and good economic benefits are obtained.
Preferably, the preparation of the antibacterial inner membrane in S1 comprises the following steps:
s1.1, weighing the breathable master batch and the bacteriostatic master batch according to the proportion, and uniformly mixing;
s1.2, the temperature of the extrusion section, the feeding section and the homogenizing section is 170-220 ℃, and the temperature of the die head is 200-230 ℃;
s1.3, casting, wherein the temperature of a cooling roller is 20-50 ℃;
s1.4, stretching, wherein the stretching multiplying power of the film is 1.08-1.12;
s1.5, performing heat setting, wherein the heat setting temperature of the membrane after stretching is 70 +/-5 ℃, and obtaining the finished antibacterial inner membrane.
By adopting the technical scheme, the antibacterial inner membrane with better waterproof and air permeability and antibacterial and mildewproof effects can be prepared.
Preferably, the heat treatment in S3 is to heat the film to 60-70 ℃ at a heating rate of 1.0-2.0 ℃/min, preserve the heat for 200 and 300 seconds, and naturally cool the film to obtain the finished packaging film.
By adopting the technical scheme, the internal stress of the fresh-keeping and bacteriostatic breathable packaging film can be eliminated, the integral mechanical strength is improved, and the quality of the fresh-keeping and bacteriostatic breathable packaging film is ensured.
In summary, the present application has the following advantages:
1. the fresh-keeping antibacterial breathable packaging film prepared by the application has good air permeability and antibacterial mildew resistance, can prolong the fresh-keeping time of fruits and vegetables, meets the fresh-keeping requirement of ocean transportation, and brings good economic benefits.
2. The preparation method is simple, industrial batch production is facilitated, the production cost of the fresh-keeping bacterium-inhibiting breathable packaging film is reduced, market share is facilitated to be seized, and good economic benefits are obtained.
Drawings
Fig. 1 is a schematic view of the overall structure in embodiment 1 of the present application.
Fig. 2 is a schematic view of the structure of the polyurethane elastic intermediate film in the present application.
In the figure, 1, antibacterial inner membrane; 2. a polyurethane elastic intermediate film; 21. a TPU film; 22. self-healing membrane; 3. An outer protective film; 31. and (4) a ventilation duct.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples.
Raw materials
Table 1 shows the raw materials used in the preparation of the antibacterial inner membrane
Table 2 shows the raw materials used in the preparation of the polyurethane elastic intermediate film
Preparation example
Preparation example 1
The antibacterial inner membrane is prepared from the following raw materials in parts by weight: 100 parts of breathable master batch and 5 parts of antibacterial master batch. The bacteriostatic master batch consists of 800g of low-density polyethylene, 80g of 4, 5-dichloro-2-n-octyl-3-isothiazolinone, 100g of zeolite powder and 20g of nano zinc oxide. Preparing zeolite powder in the antibacterial master batch: the 13x molecular sieve purchased from Zhengzhou Tianxiang inorganic materials Co Ltd is put into a crusher for crushing and screening treatment to obtain zeolite powder with 500-600 meshes. The breathable master batch is prepared from the following raw materials in percentage by mass: 10% of low density polyethylene, 25% of linear low density polyethylene, 15% of metallocene linear low density polyethylene, 25% of light calcium carbonate, 15% of barium sulfate and 10% of titanium dioxide.
Preparing a bacteriostatic master batch: uniformly mixing 800g of low-density polyethylene, 100g of zeolite powder, 80g of 4, 5-dichloro-2-n-octyl-3-isothiazolinone and 20g of nano zinc oxide, adding the mixture into a double-screw extruder, and carrying out extrusion granulation, wherein the temperature of a feeding section of the double-screw extruder is set to be 160 ℃, a homogenizing section is divided into five zones, the temperatures of the five zones are respectively set to be 180 ℃, 190 ℃, 205 ℃, 215 ℃ and 215 ℃, the internal plasticizing temperature is 189.8 ℃, and the die head temperature is 215 ℃, so that the antibacterial master batch with the granularity of 1.8-2.3mm is obtained.
Preparation of breathable master batch: 1000g of low-density polyethylene, 2500g of linear low-density polyethylene, 1500g of metallocene linear low-density polyethylene, 2500g of light calcium carbonate, 1500g of barium sulfate and 1000g of titanium dioxide are added into a double-screw extruder for extrusion granulation, the temperature of a feeding section of the double-screw extruder is set to be 168 ℃, a homogenizing section is divided into five zones, the temperatures of the five zones are respectively set to be 185 ℃, 192 ℃, 208 ℃, 218 ℃ and 218 ℃, the internal plasticizing temperature is 192.8 ℃, and the die head temperature is 218 ℃, so that the breathable master batch with the granularity of 1.8-2.3mm is obtained.
The preparation of the antibacterial inner membrane comprises the following steps:
s1.1, weighing 10.0kg of breathable master batch and 500g of antibacterial master batch according to the proportion, and uniformly mixing to obtain mixed granules;
s1.2, adding the mixed granules in the S1.1 into a casting film extruder, wherein the temperature of a feeding section of the casting film extruder is set to be 170 ℃, a homogenizing section is divided into seven zones, the temperatures of the seven zones are respectively set to be 190 ℃, 195 ℃, 200 ℃, 205 ℃, 210 ℃, 215 ℃ and 215 ℃, the internal plasticizing temperature is 190.5 ℃, and the temperature of a die head is 215 ℃ for extrusion;
s1.3, casting, wherein the temperature of a cooling roller is 25 ℃;
s1.4, adjusting the stretching ratio of a casting film extruder to be 1.08, and stretching to form a film;
s1.5, after the cast film is stretched, placing the cast film at the temperature of 78 ℃ for heat setting for 10min to obtain the antibacterial inner film with the thickness of 50 +/-3 microns.
Preparation example 2
Preparation example 3
Preparation 3 differs from preparation 1 in that: the antibacterial inner membrane is prepared from the following raw materials in parts by weight: 100 parts of breathable master batch and 5 parts of antibacterial master batch. The bacteriostatic master batch consists of low-density polyethylene, 4, 5-dichloro-2-n-octyl-3-isothiazolinone, zeolite powder, silver antibacterial powder and nano zinc oxide.
Preparing a bacteriostatic master batch: 780g of low-density polyethylene, 100g of zeolite powder, 80g of 4, 5-dichloro-2-n-octyl-3-isothiazolinone, 20g of silver antibacterial powder and 20g of nano zinc oxide are added into a double-screw extruder for extrusion granulation, the temperature of a feeding section of the double-screw extruder is set to be 160 ℃, a homogenizing section is divided into five zones, the temperatures of the five zones are respectively set to be 180 ℃, 190 ℃, 205 ℃, 215 ℃, the internal plasticizing temperature is 190.8 ℃, and the die head temperature is 215 ℃, so that the antibacterial master batch with the granularity of 1.8-2.3mm is obtained.
Preparation example 4
Referring to fig. 2, the self-healing polyurethane resin is prepared from the following raw materials: 115.27g of MDI, 5.91g of 1, 6-hexanediol, 600g of polycaprolactone diol with the number average molecular weight of 2000, 0.02g of organic bismuth, 12.15g of dimethylglyoxime, 700g of DMF, 150g of butanone, 1g of antioxidant 1010 and 20g of 325-mesh barium sulfate.
The preparation method of the self-healing film 22 comprises the following steps:
s1, dissolving 12.15g of dimethylglyoxime accurately metered in 100g of DMF to obtain a transparent dimethylglyoxime solution;
s2, adding 600g of DMF and 150g of butanone into a reaction kettle, stirring for 60S at 120rpm, adding 600g of polycaprolactone diol and 5.91g of 1, 6-hexanediol into the reaction kettle, stirring for 200S at 120rpm to dissolve the polycaprolactone diol, adding the transparent dimethylglyoxime solution in S1 into the reaction kettle, stirring for 200S at 120rpm, adding 1g of antioxidant 1010 into the reaction kettle, and stirring for 300S at 120rpm to obtain a mixed solution;
s3, adding 0.01g of catalyst into the mixed solution in the S2, controlling the reaction temperature to be 78 +/-0.5 ℃, adding 115.27g of MDI into the mixed solution in the S2 for multiple times, and controlling the reaction time to be 8.0h at the stirring speed of 300rpm to obtain semi-finished resin;
s4, after the reaction is finished, 20g of 325-mesh barium sulfate is added into the reaction kettle, and the mixture is stirred at 200rpm for 300S to obtain the cured polyurethane resin;
s5, extruding and granulating the self-healing polyurethane resin obtained in the S4 serving as a raw material to obtain self-healing resin particles with the particle size of 1.8-2.3 mm;
s6, adding the self-healing resin particles into a casting film extruder, setting the temperature of a feeding section of the casting film extruder to be 145 ℃, dividing a homogenizing section into seven areas, setting the temperatures of the seven areas to be 165 ℃, 178 ℃, 190 ℃, 195 ℃, 200 ℃ and 200 ℃, setting the internal plasticizing temperature to be 180.3 ℃, extruding at the die head temperature of 200 ℃, casting, setting the temperature of a cooling roller to be 40 ℃, adjusting the stretching ratio of the casting film extruder to be 1.06, stretching to form a film, placing the casting film at the temperature of 75 ℃ after stretching, and carrying out heat setting for 8min to obtain the self-healing film 22 with the thickness of 80 +/-2 microns.
Preparation example 5
Referring to fig. 2, the TPU film 21 is made of TPU master batch and anatase type nano TiO2Light calcium carbonate and 5A molecular sieve. Anatase type nano TiO2And light calcium carbonate is dispersed inside the TPU film 21. The 5A molecular sieve is embedded in the TPU film 21, one end of the 5A molecular sieve is exposed out of the lower surface of the TPU film 21, and the other end of the 5A molecular sieve is exposed out of the upper surface of the TPU film 21.
The TPU film 21 is prepared from 1000g of TPU master batch and 80g of anatase type nano TiO260g of light calcium carbonate and 160g of 5A molecular sieve. Wherein, the granularity of the 5A molecular sieve is crushed and screened, and the granularity of the 5A molecular sieve is controlled to be 180-200 meshes.
A method of making TPU film 21, comprising the steps of:
s1, 1000g of TPU master batch, 80g of anatase type nano TiO2Adding 60g of light calcium carbonate and 160g of 5A molecular sieve into a high-speed dispersion kettle, and stirring and mixing for 5min at 200rpm to obtain mixed granules;
s2, adding the mixed granules obtained in the S1.1 into a casting film extruder, setting the temperature of a feeding section of the casting film extruder to be 170 ℃, dividing a homogenizing section into seven zones, setting the temperatures of the seven zones to be 185 ℃, 190 ℃, 195 ℃, 200 ℃, 205 ℃, 210 ℃ and 210 ℃, setting the internal plasticizing temperature to be 186.3 ℃ and setting the temperature of a die head to be 210 ℃ for extrusion;
s3, casting, wherein the temperature of a cooling roller is 30 ℃;
s4, adjusting the stretching ratio of the casting film extruder to 1.02, and stretching to form a film;
s5, placing the cast film at 75 ℃ after stretching, and carrying out heat setting for 20min to obtain the TPU film 21 with the thickness of 70 +/-1 microns.
Preparation example 6
The preparation method of the polyurethane elastic intermediate film 2 comprises the following steps:
s1, pressing the TPU film 21 on the upper surface and the lower surface of the self-healing film 22 through a composite roller, wherein the TPU film 21 is the TPU film in the preparation example 5, the self-healing film 22 is the self-healing film in the preparation example 4, and the temperature of the composite roller is 30 ℃;
s1, pressing the self-healing films 22 of the TPU films 21 on the upper and lower surfaces, sequentially conveying the self-healing films through a first hot pressing roller, a second hot pressing roller, a third hot pressing roller, a fourth hot pressing roller, a fifth hot pressing roller, a sixth hot pressing roller and a seventh hot pressing roller, wherein the temperature of the first hot pressing roller is 45 ℃, the temperature of the second hot pressing roller is 55 ℃, the temperature of the third hot pressing roller is 65 ℃, the temperature of the fourth hot pressing roller is 80 ℃, the temperature of the fifth hot pressing roller is 110 ℃, the temperature of the sixth hot pressing roller is 80 ℃ and the temperature of the seventh hot pressing roller is 50 ℃, naturally cooling to normal temperature, and rolling to obtain the polyurethane elastic intermediate film 2.
Examples
Example 1
Referring to fig. 1, the fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation disclosed by the application comprises an antibacterial inner film 1, a polyurethane elastic intermediate film 2 and an outer protective film 3, wherein the polyurethane elastic intermediate film 2 is compounded between the antibacterial inner film 1 and the outer protective film 3 in a hot-pressing manner.
Referring to fig. 1, the outer protective film 3 was purchased from PET textured protective film of ohantun new material industry ltd, of fogshan, and the thickness of the PET textured protective film was 100 μm. The outer protective film 3 needs to be post-processed to ensure the overall air permeability. The adopted PET reticulate pattern protective film is punched by a needle plate to form a plurality of air-permeable pore canals 31 distributed in a dot matrix manner, the diameter of each air-permeable pore canal 31 is controlled to be 0.20mm, and the distance between the circle centers of the adjacent air-permeable pore canals 31 is 2.5 mm.
Referring to fig. 2, the polyurethane elastic intermediate film 2 is composed of two TPU films 21 and a self-healing film 22 thermally compressed and laminated between the two TPU films 21. The TPU film 21 used in preparation example 5 was the TPU film 21 having a thickness of 70 ± 1 μm. The self-healing film 22 used in preparation example 4 was the self-healing film 22 having a thickness of 80 ± 2 μm. The antibacterial inner film 1 was the antibacterial inner film prepared in preparation example 1 and having a thickness of 50 ± 3 μm.
A preparation method of a fresh-keeping, bacteriostatic and breathable packaging film for shipping fruit and vegetable transportation comprises the following steps:
s1, preparing an antibacterial inner membrane 1, a polyurethane elastic intermediate membrane 2 and an outer protective membrane 3, wherein the preparation of the antibacterial inner membrane 1 refers to preparation example 1, the preparation of the polyurethane elastic intermediate membrane 2 refers to preparation example 6, and the preparation method of the outer protective membrane 3 comprises the following steps: punching the PET reticulate pattern protective film by using a needle plate to form a plurality of air-permeable pore channels 31 distributed in a dot matrix manner, wherein the diameter of each air-permeable pore channel 31 is controlled to be 0.20mm, and the distance between the circle centers of the adjacent air-permeable pore channels 31 is 2.5 mm;
s2, pressing the antibacterial inner film 1 on the upper surface of the polyurethane elastic intermediate film 2 through a composite roller, and heat-pressing the outer protective film 3 on the lower surface of the polyurethane elastic intermediate film 2, and then sequentially conveying the outer protective film through a first hot-pressing roller, a second hot-pressing roller, a third hot-pressing roller, a fourth hot-pressing roller, a fifth hot-pressing roller, a sixth hot-pressing roller and a seventh hot-pressing roller, wherein the temperature of the first hot-pressing roller is 50 ℃, the temperature of the second hot-pressing roller is 65 ℃, the temperature of the third hot-pressing roller is 80 ℃, the temperature of the fourth hot-pressing roller is 110 ℃, the temperature of the fifth hot-pressing roller is 90 ℃, the temperature of the sixth hot-pressing roller is 60 ℃ and the temperature of the seventh hot-pressing roller is 40 ℃ to obtain a semi-finished product;
and S3, carrying out heat treatment on the semi-finished product, heating to 65 ℃ at a heating speed of 1.5 ℃/min, preserving heat for 300S, naturally cooling, and rolling to obtain the finished product packaging film.
Example 2
Example 2 differs from example 1 in that: the antibacterial inner film 11 used was the antibacterial inner film 11 in preparation example 2.
Example 3
Example 3 differs from example 1 in that: the antibacterial inner film 11 used was the antibacterial inner film 11 in preparation example 3.
Comparative example
Comparative example 1
Comparative example 1 differs from example 1 in that: and (3) compounding the polyurethane elastic intermediate film 2 without compounding, namely compounding the antibacterial inner film 1 and the outer protective film 3 by hot pressing to obtain the packaging film material.
Comparative example 2
Comparative example 2 differs from example 1 in that: the bacteriostatic master batch consists of low-density polyethylene and 4, 5-dichloro-2-n-octyl-3-isothiazolinone.
Preparing a bacteriostatic master batch: adding 800g of low-density polyethylene and 80g of 4, 5-dichloro-2-n-octyl-3-isothiazolinone into a double-screw extruder for extrusion granulation, wherein the temperature of a feeding section of the double-screw extruder is set to be 160 ℃, a homogenizing section is divided into five zones, the temperatures of the five zones are respectively set to be 180 ℃, 190 ℃, 205 ℃, 215 ℃ and 215 ℃, the internal plasticizing temperature is 190.8 ℃, and the temperature of a die head is 215 ℃, so as to obtain the bacteriostatic master batch with the granularity of 1.8-2.3 mm.
Comparative example 3
Comparative example 3 differs from example 1 in that: the bacteriostatic master batch consists of low-density polyethylene, 4, 5-dichloro-2-n-octyl-3-isothiazolinone and nano zinc oxide.
Preparing a bacteriostatic master batch: adding 800g of low-density polyethylene, 80g of 4, 5-dichloro-2-n-octyl-3-isothiazolinone and 20g of nano zinc oxide into a double-screw extruder for extrusion granulation, wherein the temperature of a feeding section of the double-screw extruder is set to be 160 ℃, a homogenizing section is divided into five zones, the temperatures of the five zones are respectively set to be 180 ℃, 190 ℃, 205 ℃, 215 ℃, the internal plasticizing temperature is 190.8 ℃, and the temperature of a die head is 215 ℃, so as to obtain the antibacterial master batch with the granularity of 1.8-2.3 mm.
Comparative example 4
Comparative example 4 differs from example 1 in that: the bacteriostatic master batch consists of low-density polyethylene and nano zinc oxide.
Preparing a bacteriostatic master batch: adding 800g of low-density polyethylene and 20g of nano zinc oxide into a double-screw extruder for extrusion granulation, wherein the temperature of a feeding section of the double-screw extruder is set to be 160 ℃, a homogenizing section is divided into five zones, the temperatures of the five zones are respectively set to be 180 ℃, 190 ℃, 205 ℃, 215 ℃ and 215 ℃, the internal plasticizing temperature is 190.8 ℃, and the temperature of a die head is 215 ℃, so as to obtain the bacteriostatic master batch with the granularity of 1.8-2.3 mm.
Comparative example 5
Comparative example 5 differs from example 1 in that: the bacteriostatic master batch consists of low-density polyethylene and zeolite powder. Preparing the antibacterial master batch: adding 800g of low-density polyethylene and 100g of zeolite powder into a double-screw extruder for extrusion granulation, wherein the temperature of a feeding section of the double-screw extruder is set to be 160 ℃, a homogenizing section is divided into five zones, the temperatures of the five zones are respectively set to be 180 ℃, 190 ℃, 205 ℃, 215 ℃ and 215 ℃, the internal plasticizing temperature is 190.8 ℃, and the temperature of a die head is 215 ℃, so as to obtain the bacteriostatic master batch with the granularity of 1.8-2.3 mm.
Performance test
Detection method/test method
1. And (3) antibacterial testing: the antibacterial properties of the packaging films prepared in examples 1-3 and those of the packaging films prepared in comparative examples 1-5 were tested according to QB/T2591-2003, antibacterial Plastic-antibacterial Property test methods and antibacterial Effect. Antibacterial test objects were antibacterial inner films of the packaging films prepared in examples 1 to 3, and antibacterial inner films of the packaging films prepared in comparative examples 1 to 5. The antibacterial rate is calculated by the formula of R (%) - (B-C)/BX 100; in the formula: r-antibacterial ratio (%); b-average recovery number of bacteria (cfu/patch) for placebo; c-average recovery bacteria count (cfu/piece) of the antibacterial plastic sample;
2. and (3) testing the water vapor transmission coefficient: the antibacterial properties of the packaging films prepared in examples 1-3 and the water vapor transmission coefficients of the packaging films prepared in comparative examples 1-5 were tested in accordance with GB/T1037-1988 Standard test methods for Water vapor Transmission of Plastic films and sheets.
3. Oxygen transmission rate test: GB/T19789-005 packaging Material permeability test Plastic film and sheet oxygen coulometer detection method test the antibacterial properties of the packaging films prepared in examples 1-3 and the oxygen transmission rates of the packaging films prepared in comparative examples 1-5.
4. And (3) testing puncture strength: the antibacterial performance of the packaging films prepared in test examples 1-3 and the puncture strength of the packaging films prepared in comparative examples 1-5 were tested according to the regulations of GB/T10004-2008 > 6.6.13.
5. Testing self-healing performance of the packaging film: the self-healing film in preparation example 4 was used as a test material, 10 pieces of the self-healing film in preparation example 4 with the specification of 80mm by 60mm were cut out as test samples, penetrating wounds with the length of 12mm were scribed at the four corners and the center of each test sample with an art knife, and the healing condition of the penetrating wounds of the test samples was observed every 1 hour, with the self-healing environment of 25-28 ℃ and the humidity of 50-60%. The time to healing throughout the wound was observed and recorded. The through wound healing time (h) (through wound healing time at four corners + through wound healing time at the center position)/5.
6. Testing the preservation performance: test objects: the packaging films of examples 1-3 and comparative examples 1-5 were used to prepare sealed bags of 320mm x 450mm size, labeled test samples 1-3 and comparative test samples 1-5. The test numbers of test samples 1 to 3 and comparative test samples 1 to 5 were 5, respectively. The test method comprises the following steps: taking the same batch of purchased apples as a fresh-keeping storage object, loading the apples into test objects, sealing the test objects, loading 3 apples into each test object, storing the test objects with the apples in an environment at 4.0 ℃, and observing the appearances of the apples and the test objects every 15 days. And (4) storing for 4 months, taking out the apples, and randomly searching three persons to perform taste test on the apples. The mouth feel test was conducted on the apples of examples 1 to 3 and comparative examples 2 to 5 with reference to the apple stored in comparative test sample 1. The taste of the apples stored in the comparative sample 1 was rated 0, and the taste of the apples in the other groups was rated "+" if it was better than the taste of the apples stored in the comparative sample 1, and was rated "-" if it was not.
Data analysis
Table 3 shows the antibacterial test parameters of examples 1 to 3 and comparative examples 1 to 5
Table 4 shows the parameters for measuring the water vapor transmission coefficient, oxygen transmission rate and puncture strength of examples 1 to 3 and comparative examples 1 to 5
Table 5 shows the self-healing property test parameters of the self-healing film in preparation example 4
Table 6 shows the freshness retaining properties of examples 1 to 3 and comparative examples 1 to 5
Table 7 is a mouthfeel test of the stored apples of examples 1-3 and comparative examples 1-5
As can be seen from examples 1 to 3 and comparative examples 1 to 5 in combination with Table 3, the fresh-keeping, bacteriostatic and breathable packaging film prepared in the application has good antibacterial and mildewproof effects, the antibacterial rate can reach 99.99%, the growth and reproduction of bacteria are effectively inhibited, and the quality of transported fruits and vegetables is ensured.
As can be seen by combining examples 1 to 3 and comparative examples 1 to 5 and table 3, the antibacterial rate of the fresh-keeping, bacteriostatic and breathable packaging film prepared in example 1 is greater than that of the fresh-keeping, bacteriostatic and breathable packaging films prepared in comparative examples 2, 4 and 5, and the antibacterial rate of the fresh-keeping, bacteriostatic and breathable packaging film prepared in example 1 is close to that of the fresh-keeping, bacteriostatic and breathable packaging film prepared in comparative example 3, so that the antibacterial inner film prepared from the antibacterial master batch prepared from the low-density polyethylene, 4, 5-dichloro-2-n-octyl-3-isothiazolinone, zeolite powder and nano zinc oxide has a good antibacterial and bacteriostatic effect. In combination with table 4, it can be seen that the addition of zeolite powder can improve the overall water vapor transmission coefficient and oxygen transmission rate of the prepared fresh-keeping bacteriostatic breathable packaging film.
As can be seen by combining examples 1-3 and comparative examples 1-5 and by combining Table 4, the water vapor permeability coefficient of the bacteriostatic and breathable packaging films prepared in examples 1-3 is greater than that of the bacteriostatic and breathable packaging films prepared in comparative examples 2-5, the oxygen permeability of the bacteriostatic and breathable packaging films prepared in examples 1-3 is greater than that of the bacteriostatic and breathable packaging films prepared in comparative examples 2-5, the puncture strength of the bacteriostatic and breathable packaging films prepared in examples 1-3 is greater than that of the bacteriostatic and breathable packaging films prepared in comparative examples 2-5, the water vapor permeability coefficient and the oxygen permeability of the bacteriostatic and breathable packaging films prepared in examples 1-3 are less than that of the bacteriostatic and breathable packaging films prepared in comparative examples 2-5, however, the puncture strength of the fresh-keeping bacteriostatic breathable packaging film prepared in the embodiment 1-3 is greater than that of the fresh-keeping bacteriostatic breathable packaging film prepared in the comparative example 1, so that the fresh-keeping bacteriostatic breathable packaging film prepared in the application has better water vapor permeability coefficient and oxygen permeability and high puncture strength, can effectively keep the freshness of fruits and vegetables in the packaging film, and ensures the quality of the transported fruits and vegetables.
In combination with preparation example 4 and table 5, it can be seen that the self-healing membrane prepared in preparation example 4 has a wound healing time of 34.4h, has taught self-healing performance, and can ensure the quality of transported fruits and vegetables.
By combining the examples 1 to 3 and the comparative examples 1 to 5 and combining the tables 6 to 7, it can be seen that the packaging film prepared in the application has a relatively long-lasting freshness keeping performance, the stored fruits and vegetables have a relatively good taste, the quality of the transported fruits and vegetables can be ensured, and better economic benefits are brought.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The utility model provides a fresh-keeping antibacterial ventilative packaging film for boats and ships fruit vegetables transportation which characterized in that: comprises an antibacterial inner membrane (1), a polyurethane elastic intermediate membrane (2) and an outer protective membrane (3), wherein the polyurethane elastic intermediate membrane (2) is compounded between the antibacterial inner membrane (1) and the outer protective membrane (3); the antibacterial inner membrane (1) is prepared from the following raw materials in parts by weight: 100 parts of breathable master batch and 5-10 parts of antibacterial master batch; the antibacterial master batch consists of low-density polyethylene, 4, 5-dichloro-2-n-octyl-3-isothiazolinone, zeolite powder and nano zinc oxide; the breathable master batch is prepared from the following raw materials in percentage by mass: 8-12% of low density polyethylene, 20-28% of linear low density polyethylene, 14-20% of metallocene linear low density polyethylene and the balance of inorganic filler.
2. The fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation according to claim 1, characterized in that: the polyurethane elastic intermediate film (2) is composed of two layers of TPU films (21) and a self-healing film (22) compounded between the two layers of TPU films (21); the TPU film (21) is prepared from TPU master batches, antibacterial fillers and porous breathable fillers; the antibacterial filler is dispersed inside the TPU film (21); the porous breathable filler is embedded in the TPU film (21); one end of the porous breathable filler is exposed out of the lower surface of the TPU film (21), and the other end of the porous breathable filler is exposed out of the upper surface of the TPU film (21).
3. The fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation according to claim 2, characterized in that: the antibacterial filler is composed of anatase type nano TiO2 and light calcium carbonate; the thickness of the TPU film (21) is 60-100 microns; the porous breathable filler is a 5A molecular sieve; the particle size of the porous breathable filler is 1.05-1.2 times the thickness of the TPU film (21).
4. The fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation according to claim 2, characterized in that: the self-healing film (22) is formed by casting and processing a self-healing polyurethane resin serving as a raw material; the self-healing polyurethane resin is prepared from the following raw materials: MDI, 1, 6-hexanediol, polyester polyol, a catalyst, dimethylglyoxime, an organic solvent, an antioxidant and an open-cell filler; the sum of the molar weight of the hydroxyl groups of the 1, 6-hexanediol, the molar weight of the hydroxyl groups of the polyester polyol and the molar weight of the hydroxyl groups of the dimethylglyoxime is 1.01-1.05 times of the molar weight of the-NCO in the MDI; the open pore filler is barium sulfate with 300-400 meshes.
5. The fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation according to claim 4, characterized in that: the preparation method of the self-healing film (22) comprises the following steps:
s1, adding accurately measured 1, 6-hexanediol, butanone, polyester polyol and an antioxidant into an organic solvent, and uniformly mixing to obtain a mixed solution;
s2, adding a catalyst with accurate measurement, adding the mixed solution, and adding MDI into the mixed solution for multiple times at the temperature of 70-80 ℃, wherein the reaction time is controlled to be 8 +/-0.5 h;
s3, adding a precisely-measured perforated filler after the reaction is finished, and uniformly stirring to obtain the self-healing polyurethane resin;
s4, extruding and granulating the self-healing polyurethane resin to obtain self-healing resin particles;
and S5, adding the self-healing resin particles into a casting film extruder, and performing casting, stretching and heat setting to obtain the finished self-healing film.
6. The fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation according to claim 1, characterized in that: the outer protective film (3) is a PET film; the thickness of the outer protective film (3) is 60-120 microns; the outer protective film (3) is integrally formed with a ventilation pore passage (31); the diameter of the air-permeable pore canal (31) is 0.1-0.5 mm; the air-permeable pore canals (31) are distributed in a dot matrix manner; the distance between the circle centers of the adjacent air permeable pore canals (31) is 2.0-3.0 mm.
7. The fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation according to claim 1, characterized in that: the inorganic filler is at least one of light calcium carbonate, barium sulfate and titanium dioxide; the particle size of the inorganic filler is less than or equal to 5 microns.
8. The preparation method of the fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation according to any one of claims 1 to 7, characterized by comprising the following steps: the method comprises the following steps:
s1, preparing an antibacterial inner membrane (1), a polyurethane elastic middle membrane (2) and an outer protective membrane (3) respectively;
s2, compounding the antibacterial inner membrane (1) on the upper surface of the polyurethane elastic intermediate membrane (2) in a hot-pressing manner, and compounding the outer protective membrane (3) on the lower surface of the polyurethane elastic intermediate membrane (2) in a hot-pressing manner to obtain a semi-finished product;
and S3, carrying out heat treatment on the semi-finished product to obtain the finished product packaging film.
9. The preparation method of the fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation according to claim 8, characterized in that: the preparation of the antibacterial inner membrane (1) in S1 comprises the following steps:
s1.1, weighing the breathable master batch and the bacteriostatic master batch according to the proportion, and uniformly mixing;
s1.2, the temperature of the extrusion section, the feeding section and the homogenizing section is 170-220 ℃, and the temperature of the die head is 200-230 ℃;
s1.3, casting, wherein the temperature of a cooling roller is 20-50 ℃;
s1.4, stretching, wherein the stretching multiplying power of the film is 1.08-1.12;
s1.5, performing heat setting, wherein the heat setting temperature of the membrane after stretching is 70 +/-5 ℃, and obtaining the finished antibacterial inner membrane.
10. The preparation method of the fresh-keeping, bacteriostatic and breathable packaging film for ship fruit and vegetable transportation according to claim 8, characterized in that: the heat treatment in the S3 is to heat up to 60-70 ℃ at a heating speed of 1.0-2.0 ℃/min, preserve the temperature for 200 and 300 seconds, and naturally cool to obtain the finished packaging film.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114379180A (en) * | 2021-12-29 | 2022-04-22 | 和盛包装科技(海宁)股份有限公司 | Composite packaging film with bacteria barrier protection function and preparation method thereof |
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