CN117227292B - High-barrier biaxially oriented polyethylene film and preparation method and application thereof - Google Patents
High-barrier biaxially oriented polyethylene film and preparation method and application thereof Download PDFInfo
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 11
- PLDLPVSQYMQDBL-UHFFFAOYSA-N 2-[[3-(oxiran-2-ylmethoxy)-2,2-bis(oxiran-2-ylmethoxymethyl)propoxy]methyl]oxirane Chemical compound C1OC1COCC(COCC1OC1)(COCC1OC1)COCC1CO1 PLDLPVSQYMQDBL-UHFFFAOYSA-N 0.000 claims description 10
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 9
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- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 8
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
The invention relates to the technical field of polyethylene films, and particularly discloses a high-barrier biaxially-oriented polyethylene film, a preparation method and application thereof, wherein the high-barrier biaxially-oriented polyethylene film is prepared by three layers of coextrusion and biaxially-oriented, and sequentially comprises, by mass, 55-70 parts of low-density polyethylene, 20-35 parts of metallocene polyethylene and 0.5-1 part of compatilizer, the raw materials of the base material layer comprise 50-65 parts of modified polyethylene terephthalate, 25-45 parts of high-density polyethylene and 1-2 parts of anti-adhesive, and the raw materials of the penetration-resistant layer comprise 40-55 parts of low-density polyethylene, 30-45 parts of elastomer and 25-42 parts of nylon resin. The polyethylene film prepared by biaxial stretching has excellent tensile elastic modulus, puncture resistance and bending life, improves heat resistance, cold resistance, transparency, glossiness and gas barrier property, can effectively block the entry of external water vapor and the like, is not easy to crack, and has strong tensile force and puncture resistance.
Description
Technical Field
The invention relates to the technical field of polyethylene films, in particular to a high-barrier biaxially oriented polyethylene film and a preparation method and application thereof.
Background
Biaxial stretching is an orientation processing method widely applied, and the mechanical property, optical property, heat resistance, gas barrier property and the like of the biaxially stretched material are improved to different degrees. Biaxially Oriented Polyethylene (BOPE) film is a novel packaging material emerging in the film industry in recent years, has the characteristics of stable chemical property, good water resistance, good moisture resistance and the like, is a main polyolefin film material in the field of flexible packaging, and has wide application in the fields of food packaging, industrial product packaging and the like.
Chinese patent CN104589749B discloses a high-barrier biaxially oriented polyethylene film and a method for preparing the same, comprising a polyethylene structure layer, an ethylene-vinyl alcohol copolymer barrier layer, and an adhesive resin layer interposed between the polyethylene structure layer and the ethylene-vinyl alcohol copolymer barrier layer, wherein the film is formed by coextrusion biaxially oriented, and has excellent barrier properties and mechanical properties, high mechanical strength and stiffness, but poor puncture resistance, easy puncture by sharp objects, resulting in deterioration of packaged materials, poor high temperature resistance, difficulty in being used as a printing surface layer, and easy dimensional shrinkage deformation at a higher temperature. Chinese patent CN102774110B discloses a biaxially oriented polyethylene shrink film and a process for producing the same, the film is prepared from low density polyethylene, metallocene polyethylene, linear low density polyethylene, antistatic agent, anti-blocking agent and slipping agent, and has the advantage of thin thickness, and can reduce the amount of raw materials when applied to flexible packaging of composite plastics, thereby reducing the cost, and meanwhile the biaxially oriented polyethylene shrink film has the advantages of high stiffness, high strength, high heat sealing temperature and high transverse shrinkage, but the barrier property of the polyethylene shrink film is general, especially the gas barrier property.
Therefore, development of a biaxially oriented polyethylene film which is puncture resistant, heat resistant and high barrier is desired.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-barrier biaxially oriented polyethylene film, and a preparation method and application thereof, and solves the problems of poor puncture resistance, poor heat resistance and general barrier property of the biaxially oriented polyethylene film.
In order to achieve the above purpose, the invention discloses a high-barrier biaxially oriented polyethylene film which is prepared by biaxially stretching after three layers are co-extruded and sequentially comprises a substrate layer, a barrier layer and a penetration-resistant layer; the substrate layer raw materials comprise the following components in parts by weight: 55-70 parts of low-density polyethylene, 20-35 parts of metallocene polyethylene and 0.5-1 part of compatilizer; the barrier layer comprises the following raw materials in parts by weight: 50-65 parts of modified polyethylene terephthalate, 25-45 parts of high-density polyethylene and 1-2 parts of anti-adhesive; the penetration-resistant layer raw material comprises the following components in parts by weight: 40-55 parts of low-density polyethylene, 30-45 parts of elastomer and 25-42 parts of nylon resin.
Preferably, the compatibilizing agent in the substrate layer comprises maleic anhydride grafted polyethylene.
Further, the anti-caking agent comprises one of silicon dioxide and talcum powder.
Further, the thickness of the high-barrier biaxially oriented polyethylene film is 15-60 mu m.
Preferably, the modified polyethylene terephthalate in the barrier layer is prepared by the following steps:
firstly, ultrasonically dispersing nano titanium dioxide into absolute ethyl alcohol, adding gamma-methacryloxypropyl trimethoxy silane after uniform dispersion, mixing, reacting, cooling, filtering, washing with ethanol, and drying at 80 ℃ for 12 hours to obtain alkenyl modified titanium dioxide;
dispersing alkenyl modified titanium dioxide into deionized water by ultrasonic, adding acrylic acid and an initiator after uniform dispersion, mixing, reacting, cooling, filtering, washing by using ethanol, and vacuum drying at 60 ℃ for 6 hours to obtain carboxyl modified titanium dioxide;
and thirdly, vacuum drying the polyethylene terephthalate at 130 ℃ for 24 hours, uniformly mixing the polyethylene terephthalate with carboxyl modified titanium dioxide and pentaerythritol glycidyl ether, adding the mixture into a rheometer, and carrying out melt blending reaction to obtain the modified polyethylene terephthalate.
Preferably, the initiator in the second step comprises any one of tert-butyl peroxybenzoate, benzoyl peroxide and ammonium persulfate.
Preferably, in the third step, the mass ratio of polyethylene terephthalate, carboxyl modified titanium dioxide and pentaerythritol glycidyl ether is 100: (15-35): (42-60).
Further, in the first step, the mass ratio of the nano titanium dioxide to the anhydrous ethanol to the gamma-methacryloxypropyl trimethoxysilane is 100: (2500-3000): (108-135).
Further, the temperature of the reaction in the first step is 65-75 ℃, and the reaction time is 12-14h.
Further, in the step two, the mass ratio of the alkenyl modified titanium dioxide to the deionized water to the acrylic acid to the initiator is 100: (1800-2500): (85-125): (4-7).
Further, the reaction temperature in the second step is 60-70 ℃, and the reaction time is 5-8h.
Further, the temperature of the melt blending in the third step is 250-270 ℃, and the time of the melt blending is 5-7min.
Preferably, the elastomer in the penetration-resistant layer includes any one of polyurethane elastomer and polyolefin thermoplastic elastomer.
Further, the polyolefin thermoplastic elastomer is POE polyolefin.
Preferably, the preparation method of the high-barrier biaxially oriented polyethylene film comprises the following steps:
s1, respectively preparing, mixing and drying raw materials of a base material layer, a barrier layer and a penetration resistant layer according to the raw material formulation of the base material layer, the barrier layer and the penetration resistant layer;
s2, respectively heating a substrate layer raw material, a barrier layer raw material and a penetration-resistant layer raw material in an extruder barrel, processing into a plasticized and homogenized substrate layer melt, a barrier layer melt and a penetration-resistant layer melt, respectively carrying out pipeline transmission and filter filtration on the substrate layer melt, the barrier layer melt and the penetration-resistant layer melt, extruding into sheet-shaped fluid by a three-layer co-extrusion composite die head, and cooling by a chilling roller to form a casting sheet;
and S3, carrying out biaxial stretching on the cast sheet, after stretching, drawing to rolling, carrying out corona treatment, rolling and slitting to obtain the high-barrier biaxially-oriented polyethylene film.
Preferably, the specific step of S2 is as follows: heating the base material layer raw material, the barrier layer raw material and the penetration-resistant layer raw material in an extruder barrel respectively, processing into a plasticized and homogenized base material layer melt, a barrier layer melt and a penetration-resistant layer melt, wherein the heating temperature of the base material layer raw material, the barrier layer raw material and the penetration-resistant layer raw material is 190-205 ℃, 255-260 ℃ and 215-230 ℃, respectively, and after the obtained base material layer melt, barrier layer melt and penetration-resistant layer melt are respectively conveyed by a pipeline and filtered by a filter, extruding into sheet-shaped fluid by a three-layer co-extrusion composite die head, and cooling by a chilling roller, thereby forming a casting sheet.
Further, the temperature of the chilling roller in the step S2 is 30-40 ℃.
Preferably, in the biaxial stretching process in S3, the cast sheet is subjected to preheating, stretching and heat treatment setting in the longitudinal stretching unit in sequence to finish longitudinal stretching, wherein the preheating temperature is 90-105 ℃, the longitudinal stretching ratio is 4-6 times, the temperature in the longitudinal stretching process is controlled at 165-175 ℃, and the heat treatment setting temperature is 210-220 ℃; the longitudinal stretching is completed after preheating, stretching, heat treatment shaping and cooling in a transverse stretching machine, wherein the preheating temperature is 115-125 ℃, the transverse stretching ratio is 5-9 times, the temperature in the transverse stretching process is controlled at 185-195 ℃, and the heat treatment shaping temperature is 220-230 ℃.
Further, the strength of the corona treatment in the step S3 is 40-42mN/m.
Preferably, the high-barrier biaxially oriented polyethylene film is applied to liquid packaging and soft packaging.
According to the invention, the raw material formulas of the base material layer, the barrier layer and the penetration-resistant layer are subjected to burdening, mixing and drying pretreatment, and then the base material layer melt, the barrier layer melt and the penetration-resistant layer melt which are formed by heating are subjected to three-layer coextrusion outflow, and then are subjected to biaxial stretching treatment, so that the high-barrier biaxial stretching polyethylene film is obtained. The low-density polyethylene has the characteristics of good impact strength, cold resistance, low temperature resistance and higher temperature resistance, has better moisture resistance, but has poor barrier property, good air permeability and easy aging, and the metallocene polyethylene has the characteristics of high heat resistance, simultaneously has excellent chemical stability and mechanical property, can strengthen the firmness of a matrix, and can be uniformly dispersed under the action of a compatilizer to form a substrate layer.
The polyethylene terephthalate has better crystallinity, rigidity and strength, high barrier property to nonpolar gas, good creep resistance and dimensional stability, small linear expansion coefficient, the excellent characteristics of the polyethylene terephthalate are that the polyethylene terephthalate is extremely suitable for packaging materials, gamma-methacryloxypropyl trimethoxysilane is firstly used for modifying the nano titanium dioxide, carbon-carbon double bonds are introduced into the surface of the nano titanium dioxide to obtain alkenyl modified titanium dioxide, the alkenyl modified titanium dioxide and acrylic acid are polymerized under the action of an initiator to obtain carboxyl modified titanium dioxide, pentaerythritol glycidyl ether is used as a cross-linking agent to crosslink the polyethylene terephthalate and the titanium dioxide, and epoxy on carboxyl groups on the polyethylene terephthalate and the titanium dioxide and pentaerythritol glycidyl ether are subjected to ring-opening reaction to obtain modified polyethylene terephthalate, the introduction of polyacrylic acid further improves the barrier property of the film material, has ultrahigh barrier property, and simultaneously has very strong tensile strength and excellent denaturation, has better barrier property to water vapor and gas, and the modified polyethylene terephthalate and the high-density polyethylene terephthalate are mixed to obtain the barrier layer under the action of an anti-adhesive.
The elastomer used in the invention can effectively improve the puncture resistance and flexibility of the film, and the nylon resin is added into the film material, so that the nylon resin has the characteristics of good transparency, good glossiness, high tensile strength and tensile strength, and the like, and simultaneously has excellent heat resistance, cold resistance, wear resistance and puncture resistance. The low density polyethylene, the elastomer and the nylon resin are mixed to obtain the penetration-resistant layer.
Compared with the prior art, the invention has the beneficial effects that: the polyethylene film prepared by biaxial stretching has excellent tensile elastic modulus and puncture resistance, and improves heat resistance, cold resistance, transparency, glossiness and gas barrier property of the polyethylene film. The three-layer coextrusion avoids the problems of crystallization, rupture, uneven thickness, incapability of forming films and the like, and the prepared biaxially oriented polyethylene film has excellent puncture resistance, heat resistance and high barrier property, can effectively block external water vapor and the like from entering, and meanwhile, the film material is easy to stretch, difficult to rupture, and has strong tensile force and puncture resistance.
Drawings
FIG. 1 is a flow chart of the process of preparing a high barrier biaxially oriented polyethylene film of the invention;
FIG. 2 is a flow chart of the process for preparing the modified polyethylene terephthalate according to the invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
Example 1
The preparation method of the high-barrier biaxially oriented polyethylene film comprises the following steps:
s1, according to a raw material formula, 55 parts of low-density polyethylene, 20 parts of metallocene polyethylene, 0.5 part of compatilizer maleic anhydride grafted polyethylene, 50 parts of modified polyethylene terephthalate, 25 parts of high-density polyethylene, 1 part of anti-adhesive talcum powder and 25 parts of penetration-resistant layer, wherein the raw materials comprise 40 parts of low-density polyethylene, 30 parts of elastomer POE polyolefin and 25 parts of nylon resin, and the raw materials are respectively subjected to burdening, mixing and drying pretreatment;
s2, respectively heating a substrate layer raw material, a barrier layer raw material and a penetration-resistant layer raw material in an extruder barrel, processing into a plasticized and homogenized substrate layer melt, a barrier layer melt and a penetration-resistant layer melt, wherein the heating temperature of the substrate layer raw material, the barrier layer raw material and the penetration-resistant layer raw material is 190 ℃, 255 ℃, 215 ℃, respectively transmitting the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a pipeline, filtering by a filter, extruding the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt by a three-layer co-extrusion composite die head into sheet fluid, and discharging the sheet fluid, wherein the temperature of the composite die head is 240 ℃, cooling the sheet fluid by a chilling roller, and the temperature of the chilling roller is 30 ℃ to form a casting sheet;
s3, carrying out biaxial stretching on the cast sheet, wherein in the biaxial stretching process, the cast sheet is subjected to preheating, stretching and heat treatment shaping in sequence in a longitudinal stretching unit to finish longitudinal stretching, wherein the preheating temperature is 90 ℃, the longitudinal stretching ratio is 4 times, the temperature in the longitudinal stretching process is controlled at 165 ℃, and the heat treatment shaping temperature is 210 ℃; and (3) sequentially preheating, stretching, heat treatment shaping and cooling in a transverse stretching machine to finish longitudinal stretching, wherein the preheating temperature is 115 ℃, the transverse stretching ratio is 5 times, the temperature in the transverse stretching process is 185 ℃, the heat treatment shaping temperature is 220 ℃, after the stretching is finished, the stretching is pulled to rolling, corona treatment is carried out, the strength of the corona treatment is 40mN/m, and the high-barrier biaxially oriented polyethylene film is obtained through rolling and slitting.
Wherein, the modified polyethylene glycol terephthalate in the barrier layer is prepared by the following steps:
step one, ultrasonically dispersing nano titanium dioxide into absolute ethyl alcohol, after uniformly dispersing, adding gamma-methacryloxypropyl trimethoxy silane, wherein the mass ratio of the added nano titanium dioxide to the absolute ethyl alcohol to the gamma-methacryloxypropyl trimethoxy silane is 100:2500:108, mixing, reacting for 12 hours at 65 ℃, cooling, filtering, washing with ethanol, and drying for 12 hours at 80 ℃ to obtain alkenyl modified titanium dioxide;
secondly, ultrasonically dispersing alkenyl modified titanium dioxide into deionized water, after uniformly dispersing, adding acrylic acid and initiator tert-butyl peroxybenzoate, wherein the mass ratio of the added alkenyl modified titanium dioxide to the deionized water to the acrylic acid to the initiator tert-butyl peroxybenzoate is 100:1800:85:4, mixing, reacting for 5 hours at 60 ℃, cooling, filtering, washing with ethanol, and vacuum drying for 6 hours at 60 ℃ to obtain carboxyl modified titanium dioxide;
step three, vacuum drying polyethylene terephthalate at 130 ℃ for 24 hours, and uniformly mixing the polyethylene terephthalate with carboxyl modified titanium dioxide and pentaerythritol glycidyl ether, wherein the mass ratio of the added polyethylene terephthalate to the carboxyl modified titanium dioxide to the pentaerythritol glycidyl ether is 100:15:42, adding the mixture into a rheometer, carrying out melt blending reaction, wherein the melt blending temperature is 250 ℃, the melt blending time is 5 minutes, and obtaining the modified polyethylene terephthalate after the reaction.
Example 2
The preparation method of the high-barrier biaxially oriented polyethylene film comprises the following steps:
s1, according to a raw material formula of 58 parts of low-density polyethylene, 24 parts of metallocene polyethylene and 0.6 part of compatilizer maleic anhydride grafted polyethylene serving as a base material layer, 54 parts of modified polyethylene terephthalate serving as a barrier layer, 30 parts of high-density polyethylene, 1.2 parts of anti-adhesive talcum powder and 44 parts of low-density polyethylene serving as a penetration-resistant layer, 34 parts of elastomer POE polyolefin and 30 parts of nylon resin serving as raw materials, respectively carrying out burdening, mixing and drying pretreatment on the raw materials;
s2, respectively heating a substrate layer raw material, a barrier layer raw material and a penetration-resistant layer raw material in an extruder barrel, processing into a plasticized and homogenized substrate layer melt, a barrier layer melt and a penetration-resistant layer melt, wherein the heating temperature of the substrate layer raw material, the barrier layer raw material and the penetration-resistant layer raw material is 195 ℃, 258 ℃ and 220 ℃, respectively transmitting the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a pipeline and filtering the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a filter, extruding the substrate layer melt, barrier layer melt and penetration-resistant layer melt through a three-layer co-extrusion composite die head into sheet fluid, and discharging the sheet fluid, wherein the temperature of the composite die head is 245 ℃, cooling the sheet fluid through a chilling roller, and the temperature of the chilling roller is 35 ℃ to form a casting sheet; s3, carrying out biaxial stretching on the cast sheet, wherein in the biaxial stretching process, the cast sheet is subjected to preheating, stretching and heat treatment shaping in sequence in a longitudinal stretching unit to finish longitudinal stretching, wherein the preheating temperature is 95 ℃, the longitudinal stretching ratio is 5 times, the temperature in the longitudinal stretching process is controlled at 170 ℃, and the heat treatment shaping temperature is 215 ℃; and (3) sequentially preheating, stretching, heat treatment shaping and cooling in a transverse stretching machine to finish longitudinal stretching, wherein the preheating temperature is 120 ℃, the transverse stretching ratio is 7 times, the temperature in the transverse stretching process is controlled at 190 ℃, the heat treatment shaping temperature is 225 ℃, after the stretching is finished, the stretching is pulled to rolling, corona treatment is carried out, the strength of the corona treatment is 41mN/m, and the rolling and slitting are carried out, so that the high-barrier biaxially oriented polyethylene film is obtained.
Wherein, the modified polyethylene glycol terephthalate in the barrier layer is prepared by the following steps:
step one, ultrasonically dispersing nano titanium dioxide into absolute ethyl alcohol, after uniformly dispersing, adding gamma-methacryloxypropyl trimethoxy silane, wherein the mass ratio of the added nano titanium dioxide to the absolute ethyl alcohol to the gamma-methacryloxypropyl trimethoxy silane is 100:2800:120, mixing, reacting at 70 ℃ for 13 hours, cooling, filtering, washing with ethanol, and drying at 80 ℃ for 12 hours to obtain alkenyl modified titanium dioxide;
secondly, ultrasonically dispersing alkenyl modified titanium dioxide into deionized water, after uniformly dispersing, adding acrylic acid and initiator tert-butyl peroxybenzoate, wherein the mass ratio of the added alkenyl modified titanium dioxide to the deionized water to the acrylic acid to the initiator tert-butyl peroxybenzoate is 100:2200:105:6, mixing, reacting for 7 hours at 65 ℃, cooling, filtering, washing with ethanol, and vacuum drying for 6 hours at 60 ℃ to obtain carboxyl modified titanium dioxide;
step three, vacuum drying polyethylene terephthalate at 130 ℃ for 24 hours, and uniformly mixing the polyethylene terephthalate with carboxyl modified titanium dioxide and pentaerythritol glycidyl ether, wherein the mass ratio of the added polyethylene terephthalate to the carboxyl modified titanium dioxide to the pentaerythritol glycidyl ether is 100:25:52, adding the mixture into a rheometer, carrying out melt blending reaction, wherein the melt blending temperature is 260 ℃, the melt blending time is 6min, and obtaining the modified polyethylene terephthalate after the reaction.
Example 3
The preparation method of the high-barrier biaxially oriented polyethylene film comprises the following steps:
s1, according to a raw material formula, wherein the raw materials of a base material layer comprise 63 parts of low-density polyethylene, 28 parts of metallocene polyethylene and 0.7 part of compatilizer maleic anhydride grafted polyethylene, the raw materials of a barrier layer comprise 58 parts of modified polyethylene terephthalate, 35 parts of high-density polyethylene, 1.5 parts of anti-adhesive talcum powder and 35 parts of penetration-resistant layer comprise 48 parts of low-density polyethylene, 38 parts of elastomer POE polyolefin and 35 parts of nylon resin, and the raw materials are respectively subjected to burdening, mixing and drying pretreatment;
s2, respectively heating a substrate layer raw material, a barrier layer raw material and a penetration-resistant layer raw material in an extruder barrel, processing into a plasticized and homogenized substrate layer melt, a barrier layer melt and a penetration-resistant layer melt, wherein the heating temperatures of the substrate layer raw material, the barrier layer raw material and the penetration-resistant layer raw material are respectively 200 ℃, 258 ℃ and 225 ℃, respectively transmitting the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a pipeline and filtering the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a filter, extruding the substrate layer melt, barrier layer melt and penetration-resistant layer melt through a three-layer co-extrusion composite die head into sheet fluid, and discharging the sheet fluid, wherein the temperature of the composite die head is 250 ℃, cooling the sheet fluid through a chilling roller, and the temperature of the chilling roller is 35 ℃ to form a casting sheet;
s3, carrying out biaxial stretching on the cast sheet, wherein in the biaxial stretching process, the cast sheet is subjected to preheating, stretching and heat treatment shaping in sequence in a longitudinal stretching unit to finish longitudinal stretching, wherein the preheating temperature is 100 ℃, the longitudinal stretching ratio is 5 times, the temperature in the longitudinal stretching process is controlled at 170 ℃, and the heat treatment shaping temperature is 215 ℃; and (3) sequentially preheating, stretching, heat treatment shaping and cooling in a transverse stretching machine to finish longitudinal stretching, wherein the preheating temperature is 120 ℃, the transverse stretching ratio is 7 times, the temperature in the transverse stretching process is controlled at 190 ℃, the heat treatment shaping temperature is 225 ℃, after the stretching is finished, the stretching is pulled to rolling, corona treatment is carried out, the strength of the corona treatment is 41mN/m, and the rolling and slitting are carried out, so that the high-barrier biaxially oriented polyethylene film is obtained.
Wherein the preparation method of the modified polyethylene terephthalate in the barrier layer is the same as in example 2.
Example 4
The preparation method of the high-barrier biaxially oriented polyethylene film comprises the following steps:
s1, according to a raw material formula, wherein 68 parts of low-density polyethylene, 32 parts of metallocene polyethylene and 0.9 part of compatilizer maleic anhydride grafted polyethylene are used as raw materials of a base material layer, 62 parts of modified polyethylene terephthalate, 40 parts of high-density polyethylene, 1.8 parts of anti-adhesive talcum powder and 52 parts of low-density polyethylene, 42 parts of elastomer POE polyolefin and 40 parts of nylon resin are used as raw materials of a barrier layer, and the raw materials are respectively subjected to burdening, mixing and drying pretreatment;
s2, respectively heating a substrate layer raw material, a barrier layer raw material and a penetration-resistant layer raw material in an extruder barrel, processing into a plasticized and homogenized substrate layer melt, a barrier layer melt and a penetration-resistant layer melt, wherein the heating temperatures of the substrate layer raw material, the barrier layer raw material and the penetration-resistant layer raw material are respectively 200 ℃, 260 ℃ and 225 ℃, respectively transmitting the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a pipeline and filtering the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a filter, extruding the substrate layer melt, barrier layer melt and penetration-resistant layer melt through a three-layer co-extrusion composite die head into sheet fluid, and discharging the sheet fluid, wherein the temperature of the composite die head is 250 ℃, cooling the sheet fluid through a chilling roller, and the temperature of the chilling roller is 35 ℃ to form a casting sheet; s3, carrying out biaxial stretching on the cast sheet, wherein in the biaxial stretching process, the cast sheet is subjected to preheating, stretching and heat treatment shaping in sequence in a longitudinal stretching unit to finish longitudinal stretching, wherein the preheating temperature is 100 ℃, the longitudinal stretching ratio is 5 times, the temperature in the longitudinal stretching process is controlled at 170 ℃, and the heat treatment shaping temperature is 215 ℃; and (3) sequentially preheating, stretching, heat treatment shaping and cooling in a transverse stretching machine to finish longitudinal stretching, wherein the preheating temperature is 120 ℃, the transverse stretching ratio is 7 times, the temperature in the transverse stretching process is controlled at 190 ℃, the heat treatment shaping temperature is 225 ℃, after the stretching is finished, the stretching is pulled to rolling, corona treatment is carried out, the strength of the corona treatment is 41mN/m, and the rolling and slitting are carried out, so that the high-barrier biaxially oriented polyethylene film is obtained.
Wherein the preparation method of the modified polyethylene terephthalate in the barrier layer is the same as in example 2.
Example 5
The preparation method of the high-barrier biaxially oriented polyethylene film comprises the following steps:
s1, according to a raw material formula, wherein the raw materials of a base material layer comprise 70 parts of low-density polyethylene, 35 parts of metallocene polyethylene and 1 part of compatilizer maleic anhydride grafted polyethylene, the raw materials of a barrier layer comprise 65 parts of modified polyethylene terephthalate, 45 parts of high-density polyethylene, 2 parts of anti-adhesive talcum powder and 55 parts of penetration-resistant layer raw materials, 45 parts of elastomer POE polyolefin and 42 parts of nylon resin, and the raw materials are respectively subjected to burdening, mixing and drying pretreatment;
s2, respectively heating a substrate layer raw material, a barrier layer raw material and a penetration-resistant layer raw material in an extruder barrel, processing into a plasticized and homogenized substrate layer melt, a barrier layer melt and a penetration-resistant layer melt, wherein the heating temperatures of the substrate layer raw material, the barrier layer raw material and the penetration-resistant layer raw material are 205 ℃, 260 ℃ and 230 ℃, respectively transmitting the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a pipeline and filtering the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a filter, extruding the substrate layer melt, the barrier layer melt and the penetration-resistant layer melt into sheet-shaped fluid by a three-layer co-extrusion composite die head, cooling the sheet-shaped fluid by a chilling roll, wherein the temperature of the composite die head is 255 ℃, and the temperature of the chilling roll is 40 ℃ to form a casting sheet;
s3, carrying out biaxial stretching on the cast sheet, wherein in the biaxial stretching process, the cast sheet is subjected to preheating, stretching and heat treatment shaping in sequence in a longitudinal stretching unit to finish longitudinal stretching, wherein the preheating temperature is 105 ℃, the longitudinal stretching ratio is 6 times, the temperature in the longitudinal stretching process is controlled at 175 ℃, and the heat treatment shaping temperature is 220 ℃; and (3) sequentially preheating, stretching, heat treatment shaping and cooling in a transverse stretching machine to finish longitudinal stretching, wherein the preheating temperature is 125 ℃, the transverse stretching ratio is 9 times, the temperature in the transverse stretching process is controlled to be 195 ℃, the heat treatment shaping temperature is 230 ℃, after the stretching is finished, the stretching is pulled to a winding, and the corona treatment is carried out, wherein the strength of the corona treatment is 42mN/m, the winding and the slitting are carried out, so that the high-barrier biaxially oriented polyethylene film is obtained.
Wherein the preparation method of the modified polyethylene terephthalate in the barrier layer is the same as in example 2.
Comparative example 1
The preparation method of the biaxially oriented polyethylene film comprises the following steps:
s1, according to a raw material formula, wherein 68 parts of low-density polyethylene, 32 parts of metallocene polyethylene and 0.9 part of compatilizer maleic anhydride grafted polyethylene are used as raw materials of a base material layer, 62 parts of polyethylene terephthalate, 40 parts of high-density polyethylene, 1.8 parts of anti-adhesive talcum powder and 52 parts of low-density polyethylene, 42 parts of elastomer POE polyolefin and 40 parts of nylon resin are used as raw materials of a barrier layer, and the raw materials are respectively subjected to burdening, mixing and drying pretreatment;
s2, respectively heating a substrate layer raw material, a barrier layer raw material and a penetration-resistant layer raw material in an extruder barrel, processing into a plasticized and homogenized substrate layer melt, a barrier layer melt and a penetration-resistant layer melt, wherein the heating temperatures of the substrate layer raw material, the barrier layer raw material and the penetration-resistant layer raw material are respectively 200 ℃, 260 ℃ and 225 ℃, respectively transmitting the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a pipeline and filtering the obtained substrate layer melt, barrier layer melt and penetration-resistant layer melt through a filter, extruding the substrate layer melt, barrier layer melt and penetration-resistant layer melt through a three-layer co-extrusion composite die head into sheet fluid, and discharging the sheet fluid, wherein the temperature of the composite die head is 250 ℃, cooling the sheet fluid through a chilling roller, and the temperature of the chilling roller is 35 ℃ to form a casting sheet;
s3, carrying out biaxial stretching on the cast sheet, wherein in the biaxial stretching process, the cast sheet is subjected to preheating, stretching and heat treatment shaping in sequence in a longitudinal stretching unit to finish longitudinal stretching, wherein the preheating temperature is 100 ℃, the longitudinal stretching ratio is 5 times, the temperature in the longitudinal stretching process is controlled at 170 ℃, and the heat treatment shaping temperature is 215 ℃; and (3) sequentially preheating, stretching, heat treatment shaping and cooling in a transverse stretching machine to finish longitudinal stretching, wherein the preheating temperature is 120 ℃, the transverse stretching ratio is 7 times, the temperature in the transverse stretching process is controlled at 190 ℃, the heat treatment shaping temperature is 225 ℃, after the stretching is finished, the stretching is pulled to rolling, corona treatment is carried out, the strength of the corona treatment is 41mN/m, and the rolling and slitting are carried out to obtain the biaxially oriented polyethylene film.
The low density polyethylene used in the examples and comparative examples of the present invention was purchased from petrochemical company, model 2426K; metallocene polyethylene was purchased from Dongguan Ming Yuan Plastic Co., ltd., brand: ceramic, trade name NG5401B; the nano titanium dioxide is purchased from Xuancheng Jinrui new material Co., ltd, the model is JR05, and the average grain diameter is 5nm; the high-density polyethylene is purchased from Dongguan chemical industry Co., ltd, and the brand is LH606; polyethylene terephthalate was purchased from Dongguan City right friend plastic materials Co., ltd, under the product number CR-8816; the elastomeric POE polyolefin is a thermoplastic elastomeric ethylene-octene-copolymer available from exkesen mobil, usa under model 9361; the nylon resin is PA6 resin, which is purchased from engineering plastics Co., aoxen, suzhou, and has the product number YH3400, and other raw materials and reagents are all sold in the market.
The biaxially oriented polyethylene films of examples 1 to 5 and comparative example 1 were used as samples for performance test, and the samples were prepared into polyethylene films having a thickness of 25. Mu.m, and the polyethylene films were subjected to the following performance test using the test standard of GB/T6672-2001 mechanical measurement for thickness determination of Plastic films and sheets:
(1) The test standard GB/T4456-2008 polyethylene blown film for packaging is adopted to test the barrier property of the sample, and the water vapor transmittance (g/m) 2 24 h), the puncture strength (N) of the sample is tested by using a GB/T10004-2008 test standard of packaging plastic composite film, bag Dry method composite and extrusion composite, and the test results are shown in Table 1:
as can be seen from the test results of Table 1, the three-layer coextrusion according to the present invention prevents crystallization, cracking and thicknessThe biaxially oriented polyethylene film prepared by the method has excellent puncture resistance and high barrier property, and can effectively block the entry of external water vapor and the like, wherein the water vapor transmittance corresponding to the embodiment 5 is 3.0g/m 2 24h, the puncture resistance can reach 7.0N;
(2) Determination of Plastic tensile Properties using GB/T1040.3-2006 section 3: test criteria of test conditions for films and sheets tensile strength (MPa) and elongation at break (%) were tested on the samples, and the test results are shown in table 2:
as can be seen from the test results in Table 2, the biaxially oriented polyethylene film of the invention has excellent mechanical properties, the film material is easy to stretch and break, has strong tensile force and puncture resistance, and has excellent tensile strength in both the transverse direction and the longitudinal direction and high elongation at break;
(3) The samples were subjected to a transverse and longitudinal heat shrinkage (%) test using the test standard of GB/T13519-2016 polyethylene heat shrink film for packaging, and the test results are shown in Table 3:
as can be seen from the test results of Table 3, the biaxially oriented polyethylene film of the present invention has excellent heat resistance and small heat shrinkage in the transverse and longitudinal directions, wherein example 5 corresponds to a heat shrinkage in the transverse direction of 3.6% and a heat shrinkage in the longitudinal direction of 6.2%.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made hereto without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. The high-barrier biaxially oriented polyethylene film is characterized by being prepared by biaxially stretching after three layers of coextrusion and sequentially comprising a substrate layer, a barrier layer and a penetration-resistant layer;
the substrate layer raw materials comprise the following components in parts by weight: 55-70 parts of low-density polyethylene, 20-35 parts of metallocene polyethylene and 0.5-1 part of compatilizer;
the barrier layer comprises the following raw materials in parts by weight: 50-65 parts of modified polyethylene terephthalate, 25-45 parts of high-density polyethylene and 1-2 parts of anti-adhesive;
the modified polyethylene terephthalate is prepared by the following steps: uniformly mixing the polyethylene terephthalate subjected to drying treatment with carboxyl modified titanium dioxide and pentaerythritol glycidyl ether, and carrying out melt blending reaction to obtain modified polyethylene terephthalate after the reaction;
wherein the mass ratio of the polyethylene glycol terephthalate to the carboxyl modified titanium dioxide to the pentaerythritol glycidyl ether is 100 (15-35) (42-60);
the carboxyl modified titanium dioxide is prepared by the following steps:
firstly, ultrasonically dispersing nano titanium dioxide into absolute ethyl alcohol, adding gamma-methacryloxypropyl trimethoxy silane after uniform dispersion, mixing, reacting, cooling, filtering, washing with ethanol, and drying to obtain alkenyl modified titanium dioxide;
dispersing alkenyl modified titanium dioxide into deionized water by ultrasonic, adding acrylic acid and an initiator after uniform dispersion, mixing, reacting, cooling, filtering, washing by using ethanol, and drying to obtain carboxyl modified titanium dioxide;
wherein the mass ratio of the alkenyl modified titanium dioxide to the deionized water to the acrylic acid to the initiator is 100 (1800-2500): 85-125): 4-7; the reaction temperature is 60-70 ℃ and the reaction time is 5-8h;
the penetration-resistant layer raw material comprises the following components in parts by weight: 40-55 parts of low-density polyethylene, 30-45 parts of elastomer and 25-42 parts of nylon resin.
2. The high barrier biaxially oriented polyethylene film of claim 1, wherein the compatibilizing agent in the substrate layer comprises maleic anhydride grafted polyethylene.
3. The high barrier biaxially oriented polyethylene film according to claim 1, wherein the initiator in the second step comprises any one of t-butyl peroxybenzoate, benzoyl peroxide and ammonium persulfate when preparing the carboxyl-modified titanium dioxide.
4. The high barrier biaxially oriented polyethylene film of claim 1, wherein the elastomer in the puncture-resistant layer comprises any one of a polyurethane-based elastomer and a polyolefin-based thermoplastic elastomer.
5. A method of producing a high barrier biaxially oriented polyethylene film according to any one of claims 1 to 4, comprising the steps of:
s1, respectively preparing, mixing and drying raw materials of a base material layer, a barrier layer and a penetration resistant layer according to the raw material formulation of the base material layer, the barrier layer and the penetration resistant layer;
s2, respectively heating a substrate layer raw material, a barrier layer raw material and a penetration-resistant layer raw material in an extruder barrel, processing into a plasticized and homogenized substrate layer melt, a barrier layer melt and a penetration-resistant layer melt, respectively carrying out pipeline transmission and filter filtration on the substrate layer melt, the barrier layer melt and the penetration-resistant layer melt, extruding into sheet-shaped fluid by a three-layer co-extrusion composite die head, and cooling by a chilling roller to form a casting sheet;
and S3, carrying out biaxial stretching on the cast sheet, after stretching, drawing to a winding device, carrying out corona treatment, winding and slitting to obtain the high-barrier biaxially-oriented polyethylene film.
6. The method for preparing a high-barrier biaxially oriented polyethylene film according to claim 5, wherein the specific steps of S2 are as follows: heating the base material layer raw material, the barrier layer raw material and the penetration-resistant layer raw material in an extruder barrel respectively, processing into a plasticized and homogenized base material layer melt, a barrier layer melt and a penetration-resistant layer melt, wherein the heating temperature of the base material layer raw material, the barrier layer raw material and the penetration-resistant layer raw material is 190-205 ℃, 255-260 ℃ and 215-230 ℃, respectively, and after the obtained base material layer melt, barrier layer melt and penetration-resistant layer melt are respectively conveyed by a pipeline and filtered by a filter, extruding into sheet-shaped fluid by a three-layer co-extrusion composite die head, and cooling by a chilling roller, thereby forming a casting sheet.
7. The method for preparing a biaxially oriented polyethylene film with high barrier according to claim 5, wherein in the biaxially oriented process in step S3, the cast sheet is subjected to preheating, stretching and heat treatment setting in the longitudinal stretching unit in this order, and then longitudinal stretching is completed, wherein the preheating temperature is 90-105 ℃, the longitudinal stretching ratio is 4-6 times, the temperature in the longitudinal stretching process is controlled at 165-175 ℃, and the heat treatment setting temperature is 210-220 ℃; the longitudinal stretching is completed after preheating, stretching, heat treatment shaping and cooling in a transverse stretching machine, wherein the preheating temperature is 115-125 ℃, the transverse stretching ratio is 5-9 times, the temperature in the transverse stretching process is controlled at 185-195 ℃, and the heat treatment shaping temperature is 220-230 ℃.
8. Use of the high-barrier biaxially oriented polyethylene film according to any one of claims 1 to 4 in liquid packaging, soft packaging.
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| CN108608696A (en) * | 2018-04-28 | 2018-10-02 | 青岛方大包装有限公司 | A kind of puncture-resistant, high-barrier composite plastic film and packaging bag |
| CN116554801A (en) * | 2023-05-29 | 2023-08-08 | 奎达高分子材料科技(宜兴)有限公司 | PVB photovoltaic adhesive film resistant to mechanical impact and preparation method thereof |
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| CN108608696A (en) * | 2018-04-28 | 2018-10-02 | 青岛方大包装有限公司 | A kind of puncture-resistant, high-barrier composite plastic film and packaging bag |
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