CN112571908A - Electronic crosslinking enhanced PE film and preparation method thereof - Google Patents

Electronic crosslinking enhanced PE film and preparation method thereof Download PDF

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Publication number
CN112571908A
CN112571908A CN202011477975.5A CN202011477975A CN112571908A CN 112571908 A CN112571908 A CN 112571908A CN 202011477975 A CN202011477975 A CN 202011477975A CN 112571908 A CN112571908 A CN 112571908A
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layer
thickness
film
crosslinking
crosslinked
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陈德元
杨伟
刘金花
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Jiangyin Sunrise Packaging Material Co ltd
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Jiangyin Sunrise Packaging Material Co ltd
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Priority to CN202011477975.5A priority Critical patent/CN112571908A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D7/00—Producing flat articles, e.g. films or sheets
    • B29D7/01—Films or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
    • B65D65/38—Packaging materials of special type or form
    • B65D65/40—Applications of laminates for particular packaging purposes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/31—Heat sealable
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/54—Yield strength; Tensile strength
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/558—Impact strength, toughness

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention discloses an electron crosslinking reinforced PE film, which comprises the following components in sequence from top to bottom: the composite layer comprises a heat-resistant layer, a first crosslinking layer, a second crosslinking layer, a third crosslinking layer, a fourth crosslinking layer, a fifth crosslinking layer, a sixth crosslinking layer, a seventh crosslinking layer and a composite layer. The PE film with the enhanced electronic crosslinking has higher heat sealing strength and wider heat sealing temperature range than a non-electronic crosslinking film; the electronic crosslinking enhanced PE film has increased stiffness and surface hardness, and is resistant to surface mechanical scratch; the impact strength of the PE film enhanced by electronic crosslinking is higher than that of a non-electronic crosslinking film.

Description

Electronic crosslinking enhanced PE film and preparation method thereof
Technical Field
The invention belongs to the technical field of packaging films, and particularly relates to an electronic crosslinking enhanced PE film applied to a single recyclable material for thermoformed packaged frozen meat products and a preparation method thereof.
Background
Currently, the packaging films for packaging the frozen meat by thermoforming are BOPA, BOPET and BOPP, and the materials and the polyolefin composite with the heat sealing function do not belong to a single material; at present, olefin polymers such as propylene (PP), ethylene (PE) and the like are common heat-sealing layer materials, PE is suitable for freezing conditions of frozen meat products, and the PP materials become brittle and are easy to crack under the freezing conditions; compared with other materials, the ethylene material is easy to be subjected to electronic crosslinking treatment, and the crosslinking degree is higher.
The patent application with the publication number of CN112009058A discloses a PE film for powder packaging, which belongs to the technical field of PE films, and the PE film is prepared by fusing and co-extruding an inner layer, a middle layer and an outer layer, further discloses the raw material composition of the inner layer, the middle layer and the outer layer, and also provides a preparation method of the PE film. The PE film has high welding seal strength, is not easy to break bags and leak materials, is easy to open, is easy to weld and seal, is antibacterial, is particularly suitable for packaging various powder materials, and reduces the production cost; the middle layer of the composite film is composed of the middle-low density polyethylene, the linear low density polyethylene, the metallocene polyethylene and the fluorine-containing polymer, so that the stiffness of the film can be improved, the appearance of the film is flatter, and the strength of the film can also be improved; the inner layer is used as a welding seal layer, the strength and the welding seal performance of the film are improved by adding metallocene polyethylene, the strength of the film is also improved by adding high-density polyethylene, the freshness retaining property of the film is improved by adding an antibacterial agent, the opening performance in use is improved by adding an anti-caking agent, and the phenomenon that the film adsorbs contents due to static electricity is reduced by adding an antistatic agent.
The patent application with the publication number of CN211441461U discloses a PE film that can be used to freeze packing, including the PE film body, the lower terminal surface complex of PE film body has antibiotic layer, the lower terminal surface complex on antibiotic layer has the active layer, the surface of active layer is provided with miniature shrinkage pool, the inside of miniature shrinkage pool is stained with active ion, the up end complex of PE film body has anti-freeze layer, the up end on anti-freeze layer is provided with tensile layer, the up end complex on tensile layer has the wearing layer. The utility model discloses in, through the setting of antibiotic layer, active layer, the nipagin ester on antibiotic layer can destroy the microorganism cell membrane, makes the characteristic of the protein denaturation in the cell reach good antibacterial effect, and active ion on the active layer acts on and keeps apart back food, makes the cell activity reinforcing of food, can prolong fresh-keeping effect on basic fresh-keeping basis.
Since the above PE films have problems of difficulty in recycling, easy stretching and deformation, etc., it is necessary to develop a PE film having a recyclable material, high strength, and high printing overprinting accuracy.
Disclosure of Invention
The first purpose of the invention is to provide an electronic crosslinking reinforced PE film, the prepared PE film material can be recycled, the printing overprinting precision can be met, the high temperature resistance and easy thermoforming are realized, the problem of inaccurate overprinting caused by easy stretching and deformation of a PE cover film in the printing process is solved, and the problem of seal scalding and melting caused by too low melting point of PE is solved; meanwhile, the problem that the PE base film is easy to puncture and break due to insufficient strength is solved.
The second purpose of the invention is to provide a preparation method of the electron crosslinking reinforced PE film.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the present invention provides an electron cross-linking enhanced PE film, which comprises, from top to bottom: the heat-resistant layer, the first crosslinked layer, the second crosslinked layer, the third crosslinked layer, the fourth crosslinked layer, the fifth crosslinked layer, the sixth crosslinked layer, the seventh crosslinked layer and the composite layer;
the heat-resistant layer is made of HDPE, and the thickness of the layer is 10-30%; the first cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the second crosslinking layer is made of LDPE, and the thickness of the layer is 5-25%; the third cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the fourth cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the fifth cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the sixth cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the seventh cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the composite layer is made of a mixture of LLDPE and LDPE with the mass ratio of 3:2, and the layer thickness is 10-20%.
The above layer thickness means that each layer accounts for the total thickness of the PE film, and for example, the layer thickness of the heat-resistant layer is 10 to 30% means that the heat-resistant layer accounts for 10 to 30% of the thickness of the entire PE film.
Preferably, in the PE film with the enhanced electronic crosslinking, the thickness of the heat-resistant layer is 15-25%; the thickness of the first crosslinking layer is 8-10%; the thickness of the second crosslinking layer is 8-11%; the thickness of the third crosslinking layer is 8-11%; the thickness of the fourth crosslinking layer is 8-11%; the thickness of the fifth crosslinking layer is 7-11%; the thickness of the sixth crosslinking layer is 8-11%; the layer thickness of the seventh crosslinking layer is 8-10%; the layer thickness of the composite layer material is 10-19%.
Most preferably, in the electron crosslinking reinforced PE film, the thickness of the heat-resistant layer is 25%; the thickness of the first crosslinked layer is 10%; the thickness of the second crosslinked layer is 10%; the layer thickness of the third crosslinked layer is 10%; the thickness of the fourth crosslinked layer is 8%; the thickness of the fifth crosslinked layer is 7%; the thickness of the sixth crosslinked layer is 10%; the layer thickness of the seventh crosslinked layer is 10%; the layer thickness of the composite layer material is 10%.
Most preferably, in the electron crosslinking reinforced PE film, the thickness of the heat-resistant layer is 25%; the thickness of the first crosslinked layer is 8%; the thickness of the second crosslinked layer is 8%; the thickness of the third crosslinked layer is 8%; the thickness of the fourth crosslinked layer is 8%; the thickness of the fifth crosslinked layer is 8%; the thickness of the sixth crosslinked layer is 8%; the layer thickness of the seventh crosslinked layer is 8%; the layer thickness of the composite layer material is 19%.
Most preferably, in the electron crosslinking reinforced PE film, the thickness of the heat-resistant layer is 20%; the thickness of the first crosslinked layer is 10%; the thickness of the second crosslinked layer is 10%; the layer thickness of the third crosslinked layer is 10%; the thickness of the fourth crosslinked layer is 10%; the thickness of the fifth crosslinked layer is 10%; the thickness of the sixth crosslinked layer is 10%; the layer thickness of the seventh crosslinked layer is 10%; the layer thickness of the composite layer material is 10%.
Most preferably, in the electron crosslinking reinforced PE film, the thickness of the heat-resistant layer is 15%; the thickness of the first crosslinked layer is 10%; the thickness of the second crosslinked layer is 11%; the thickness of the third crosslinked layer is 11%; the thickness of the fourth crosslinked layer is 11%; the thickness of the fifth crosslinked layer is 11%; the thickness of the sixth crosslinked layer is 11%; the layer thickness of the seventh crosslinked layer is 10%; the layer thickness of the composite layer material is 10%.
The second aspect of the present invention provides a method for preparing the electron crosslinking enhanced PE thin film, comprising the steps of:
firstly, blowing a film on raw materials required by a PE film, then carrying out electronic crosslinking treatment, printing according to needs, and then compounding, curing and cutting to obtain the PE film with enhanced electronic crosslinking;
the film blowing method comprises the following steps:
the first layer is that the raw material HDPE of the heat-resistant layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 2 nd layer, the raw material LDPE of the first crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
a 3 rd layer, adding the LDPE of the second crosslinking layer into a hopper of an extruder, melting at the temperature of 170-200 ℃, and entering a neck mold;
the 4 th layer, the LDPE of the third crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 5 th layer, the LDPE of the fourth crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 6 th layer, the LDPE of the fifth crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 7 th layer, the raw material LDPE of the sixth crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 8 th layer, the raw material of LDPE of the seventh crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
layer 9, mixing the raw materials of the composite layer: adding the mixture of LLDPE and LDPE with the mass ratio of 3:2 into a hopper of an extruder, melting at the temperature of 170-200 ℃, and entering a neck mold;
then, extruding a film bubble of the multilayer co-extruded film through a die orifice, cooling a sizing cage on the outer side of the film bubble above the die orifice through an air ring to determine the diameter of the film bubble, and supporting the floating of the film bubble by air flow sprayed by a plurality of air cushion rollers above the sizing cage; the sizing cage and the air cushion roller cool the film bubble, so that the film bubble has certain structural strength, and the fixed diameter and the fixed thickness of the film bubble are determined; meanwhile, the film bubble is supported and floated by the air flow of the air cushion roller and the sizing cage: sizing and cooling the film bubble, cutting the film bubble into a sheet-shaped film, and rolling the film bubble to obtain a film product;
the electronic crosslinking treatment comprises the following steps:
and (3) putting the PE film roll obtained after the film blowing in the previous step into an offline EB machine through an unreeling device, carrying out high-energy ray scanning irradiation for crosslinking treatment under different irradiation doses, wherein the treatment voltage is 0.1-100 Mv, the treatment dose is 8-22 Mrad, cooling through a cooling roller, and then rolling to obtain the PE film subjected to electronic crosslinking treatment, namely the EPE film.
The treatment voltage of the electron crosslinking treatment is 0.5Mv, and the treatment dose is 12 Mrad.
The different irradiation doses have different influences on the crosslinking degree of the PE film, and the dose is controlled by equipment parameters, and the specific relation is as follows:
D＝(K*N*I)/V
v: linear velocity; k: a K value constant; n: the number of quenching treatment layers; i: beam current; d: and (4) dosage.
The compounding is solvent-free compounding, the gluing amount is 1.3-2.0g, the PE surface needs to be subjected to online corona treatment in the PE compounding process, the power is 3000w, and the dyne value is more than or equal to 38;
compounding the EPE film obtained in the last step with a PE film, wherein the amount of the EPE film accounts for 50% of the mass of the electron crosslinking enhanced PE film, the amount of the PE film accounts for 50% of the mass of the electron crosslinking enhanced PE film, gluing the EPE film, and compounding the EPE film and the PE film in a compounding machine.
The parameters of the composite process are as follows: the temperature of a glue barrel is 40 ℃, the temperature of a coating roller is 45 ℃, the tension of B5 is 30-40N, the taper is 20%, the temperature of a pipeline is 40 ℃, the temperature of a composite roller is 50 ℃, the tension of LY3 is 90-110N, the gluing amount is 1.2-1.4 g/square meter, the temperature of a metering roller is 45 ℃, the tension of B1 is 60-70N, the initial tension of B20 is 100 plus 120N, and the compounding speed is less than or equal to 200 m/min.
The printing is carried out according to the requirement, and the parameters of the printing process are as follows: the viscosity is 14 +/-2 s, the temperature is 55 +/-15 ℃, the scraper pressure is 0.3 +/-0.15 MPa, the compression roller pressure is 0.2 +/-0.15 MPa, the unreeling tension is 0.1-0.3N, the incoming tension is 0.2-0.4N, the printing-out tension is 0.2-0.4N, the reeling initial tension is 20 +/-5% N, the reeling finishing tension is 15 +/-5% N, and the printing speed is less than or equal to 150 m/min.
The curing is to cure the composite film for 1 to 96 hours at the temperature of 30 to 40 ℃; preferably 35 ℃ for 72 h.
And the cutting is carried out according to the normal product requirement.
Due to the adoption of the technical scheme, the invention has the following advantages and beneficial effects:
according to the preparation method of the PE film enhanced by electronic crosslinking, the prepared PE film is applied to thermoforming packaging, is used as a cover film surface layer printing composite base material film, is applied to freezing storage of packaged frozen meat, is improved in tensile strength, barrier property, puncture resistance, tension stability and thermal stability after being subjected to electronic crosslinking treatment, and can meet the requirements of stretching and heat sealing of thermoforming packaging.
The raw materials adopted by the invention are single materials which can be recycled, can meet the requirement of printing overprinting precision, are high-temperature resistant and easy to thermally form, and solve the problems of inaccurate overprinting caused by easy stretching and deformation of a PE (polyethylene) cover film in the printing process and seal scalding and melting caused by too low melting point of PE; meanwhile, the problem that the PE base film is easy to puncture and break due to insufficient strength is solved.
The electronic crosslinking enhanced PE film improves the melting point, the tensile strength and the puncture resistance of the PE film through electronic crosslinking. Under the irradiation of high-energy electron beams, a large amount of energy is introduced to break C-H bonds, and formed free radicals between molecules are combined into stable bonds, so that the linear structure of the PE is converted into a net structure, and the performance of a product is changed. Due to the selectivity of the PE material, different varieties of PE resins and different degrees of crosslinking cause the film to exhibit different physical and mechanical properties.
The PE film with the enhanced electronic crosslinking has higher heat sealing strength and wider heat sealing temperature range than a non-electronic crosslinking film; the electronic crosslinking enhanced PE film has increased stiffness and surface hardness, and is resistant to surface mechanical scratch; the impact strength of the PE film enhanced by electronic crosslinking is higher than that of a non-electronic crosslinking film.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
The raw materials used in the examples of the present invention and the comparative examples are abbreviated as follows:
LDPE is low density polyethylene available from Kataler, Inc. under the designation FD0270, with a melt index of 2.4g/10min (190 deg.C, 2.16kg), and a density of 0.923g/cm3。
LLDPE is a linear low density polyethylene available from Exxon Mobil under the trade designation 1002AY, having a melt index of 2g/10min (190 ℃, 2.16kg), and a density of 0.918g/cm3。
HDPE is a high density polyethylene available from Dadaler under the trade designation F920A, has a melt index of 1g/10min (190 ℃, 2.16kg), and a density of 0.956g/cm3。
Example 1
A preparation method of an electron crosslinking reinforced PE film comprises the following steps:
film blowing → electronic crosslinking → (printing) → compounding → curing → slitting
Firstly, blowing a film on raw materials required by the PE film, then carrying out electronic crosslinking treatment, printing according to the requirement, and then compounding, curing and cutting to obtain the PE film with enhanced electronic crosslinking.
Film blowing: controlling the thickness uniformity of the PE film: the average deviation is less than or equal to 3 percent, and the limit deviation is less than or equal to 5 percent.
The film blowing method comprises the following steps:
the first layer is that the raw material HDPE of the heat-resistant layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 2 nd layer, the raw material LDPE of the first crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
a 3 rd layer, adding the LDPE of the second crosslinking layer into a hopper of an extruder, melting at the temperature of 170-200 ℃, and entering a neck mold;
the 4 th layer, the LDPE of the third crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 5 th layer, the LDPE of the fourth crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 6 th layer, the LDPE of the fifth crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 7 th layer, the raw material LDPE of the sixth crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 8 th layer, the raw material of LDPE of the seventh crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
layer 9, mixing the raw materials of the composite layer: adding the mixture of LLDPE and LDPE with the mass ratio of 3:2 into a hopper of an extruder, melting at the temperature of 170-200 ℃, and entering a neck mold;
then, extruding a film bubble of the multilayer co-extruded film through a die orifice, cooling a sizing cage on the outer side of the film bubble above the die orifice through an air ring to determine the diameter of the film bubble, and supporting the floating of the film bubble by air flow sprayed by a plurality of air cushion rollers above the sizing cage; the sizing cage and the air cushion roller cool the film bubble, so that the film bubble has certain structural strength, and the fixed diameter and the fixed thickness of the film bubble are determined; simultaneously, the bubble is supported by the air current of air cushion roller and sizing cage and is floated, can not produce the friction with the bubble, avoids the bubble surface to produce phenomenons such as wire drawing, ensures the best quality on membrane limit: and (5) sizing and cooling the film bubble, cutting the film bubble into a sheet-shaped film, and rolling to obtain a film product.
The electron crosslinking treatment is to change the PE film into the EPE film through electron crosslinking treatment, and the specific method comprises the following steps:
and (3) putting the PE film roll obtained after the film blowing in the previous step into an offline EB machine through an unreeling device, carrying out high-energy ray scanning irradiation under different irradiation doses for carrying out crosslinking treatment, wherein the treatment voltage is 0.5Mv, the treatment dose is 12Mrad, cooling through a cooling roller, and then rolling to obtain the PE film subjected to electronic crosslinking treatment, namely the EPE film.
Production equipment: offline EB machine, purchased from ito, ippa radiation technologies, inc.
The different irradiation doses have different influences on the crosslinking degree of the PE film, and the dose is controlled by equipment parameters, and the specific relation is as follows:
D＝(K*N*I)/V
v: linear velocity (10-40 m/min, preferably 30 m/min); k: k value constant (2.2-2.7, chosen here as 2.3); n: the number of quenching treatment layers is (1-5, wherein 5 is selected); i: beam (< 55mA, here selected to be 30 mA); d (unit Mrad): dosage (according to process requirements).
Samples 1-6 are six samples of the electron cross-linked reinforced PE film prepared in this example, irradiated with different doses of radiation, as shown in table 1:
TABLE 1
50um Voltage Mv Value of K Number of quenching treatment layers N I beam current mA V line speed m/min Dose Mrad
Sample 1 0.5 2.3 4.5 30 38.8 8
Sample 2 0.5 2.3 4.5 30 31.1 10
Sample 3 0.5 2.3 4.5 30 25.9 12
Sample No. 4 0.5 2.3 4.5 30 22.2 14
Sample No. 5 0.5 2.3 4.5 30 19.4 16
Sample No. 6 0.5 2.3 4.5 30 17.3 18
The compounding is solvent-free compounding, the gluing amount is 1.3-2.0g, and the PE surface needs to be subjected to online corona treatment in the PE compounding process (the power is 3000w, and the dyne value is more than or equal to 38). The method comprises the following specific steps: compounding the EPE film obtained in the last step with a PE film, wherein the amount of the EPE film accounts for 50% of the mass of the electron crosslinking enhanced PE film, the amount of the PE film accounts for 50% of the mass of the electron crosslinking enhanced PE film, gluing the EPE film, and compounding the EPE film and the PE film in a compounding machine. The thickness of the EPE film can be matched according to the customer requirements at will, and the EPE film can meet the tension requirement of a printing composite process and the temperature resistance during hot forming sealing. Typically (30, 40, 50, 60 um).
The parameters of the compounding process are shown in table 2:
TABLE 2
Temperature of the glue barrel/. degree.C 40 Temperature of pipeline/. degree.C 40 Metering roll temperature/. degree.C 45
Coating roll temperature/. degree.C 45 Composite roll temperature/. degree.C 50 B1 tension/N 60-70
B5 tension/N 30-40 LY3 tension/N 90-110 B20 initial tension/N 100-120
Taper of taper 20％ Gluing quantity/g/square meter 1.2-1.4 Composite velocity/m/min ≤200
The printing is carried out according to the requirement, the step can be selectively added or not added, and the parameters of the printing process are shown in a table 3:
TABLE 3
Figure BDA0002836271480000081
In table 3, the unit of viscosity is s, the unit of doctor blade pressure and platen pressure is MPa, the unit of unwinding tension, introducing tension, printing-out tension, winding start tension, and winding end tension is N, and the printing speed is m/min.
The curing is to cure the composite film for 72 hours at the temperature of 35 ℃;
and the cutting is carried out according to the normal product requirement.
The electron crosslinking reinforced PE film prepared by the invention comprises the following components in sequence from top to bottom: the heat-resistant layer, the first crosslinked layer, the second crosslinked layer, the third crosslinked layer, the fourth crosslinked layer, the fifth crosslinked layer, the sixth crosslinked layer, the seventh crosslinked layer and the composite layer;
the heat-resistant layer is made of HDPE, and the thickness of the layer is 25%; the first cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the second crosslinking layer is made of LDPE, and the thickness of the layer is 10%; the third cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the fourth cross-linked layer is made of LDPE, and the thickness of the layer is 8%; the fifth cross-linked layer is made of LDPE, and the thickness of the layer is 7%; the sixth cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the seventh cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the composite layer is made of a mixture of LLDPE and LDPE with the mass ratio of 3:2, and the layer thickness is 10%.
The above layer thickness means that each layer accounts for the total thickness of the PE film, and for example, a layer thickness of the heat-resistant layer of 25% means that the heat-resistant layer accounts for 25% of the thickness of the entire PE film.
Table 4 presents data on the tensile properties and puncture resistance of the films of the PE reinforced with electronic crosslinking prepared in example 1 according to the invention:
TABLE 4
Figure BDA0002836271480000082
Figure BDA0002836271480000091
As can be seen from the data in Table 4, the samples 1 to 6 after the crosslinking treatment all have better mechanical properties than the samples without the crosslinking treatment, wherein the mechanical property of the sample 3 is the best. After the PE film with the enhanced electronic crosslinking is subjected to proper crosslinking treatment, the tensile strength, the deformability, the heat resistance and the puncture resistance of the PE film are improved. The requirements of the printing composite process can be met, the quality of the product is more convenient to control, and the yield is improved; meanwhile, the film can be used as the outer layer of the cover film of the thermal forming package to realize the functions of heat sealing and no adhesion.
Under the irradiation of high-energy electron beams, a large amount of energy is introduced to break C-H bonds, and formed free radicals between molecules are combined into stable bonds, so that the linear structure of the PE is converted into a net structure, and the performance of a product is changed. Due to the selectivity of the PE material, different varieties of PE resins and different degrees of crosslinking cause the film to exhibit different physical and mechanical properties.
The main body of the electron cross-linking reinforced PE film prepared in the embodiment 1 of the invention is not changed, and the film is still an ethylene copolymer, only the molecular chain structure is changed, and the film can be melted, granulated and blown again for use; the printing overprinting precision can be met, the common PE film is easy to deform under the action of tension during printing and compounding, so that the phenomenon of inaccurate overprinting is caused, the strength of the PE film is improved after electronic crosslinking treatment, the PE film is not easy to deform, and the printing and compounding are facilitated; the high-temperature-resistant heat-sealing film is easy to thermally form, the common PE film can have the problem of adhesion to a heating plate at about 130 ℃, after electronic crosslinking treatment, the molecular chains are combined with each other by the dispersing branched chains to form a net shape, so that the common PE film is more stable at high temperature, needs more heat, and forms a certain temperature difference with a heat-sealing layer, so that the adhesion condition can not occur during sealing.
Example 2
An electron crosslinking reinforced PE film comprises the following components in sequence from top to bottom: the heat-resistant layer, the first crosslinked layer, the second crosslinked layer, the third crosslinked layer, the fourth crosslinked layer, the fifth crosslinked layer, the sixth crosslinked layer, the seventh crosslinked layer and the composite layer;
the heat-resistant layer is made of HDPE, and the thickness of the layer is 25%; the first cross-linked layer is made of LDPE, and the thickness of the layer is 8%; the second crosslinking layer is made of LDPE, and the thickness of the layer is 8%; the third cross-linked layer is made of LDPE, and the thickness of the layer is 8%; the fourth cross-linked layer is made of LDPE, and the thickness of the layer is 8%; the fifth cross-linked layer is made of LDPE, and the thickness of the layer is 8%; the sixth cross-linked layer is made of LDPE, and the thickness of the layer is 8%; the seventh cross-linked layer is made of LDPE, and the thickness of the layer is 8%; the composite layer is made of a mixture of LLDPE and LDPE with the mass ratio of 3:2, and the layer thickness is 19%.
The preparation method is the same as that of example 1.
Example 3
An electron crosslinking reinforced PE film comprises the following components in sequence from top to bottom: the heat-resistant layer, the first crosslinked layer, the second crosslinked layer, the third crosslinked layer, the fourth crosslinked layer, the fifth crosslinked layer, the sixth crosslinked layer, the seventh crosslinked layer and the composite layer;
the heat-resistant layer is made of HDPE, and the thickness of the layer is 20%; the first cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the second crosslinking layer is made of LDPE, and the thickness of the layer is 10%; the third cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the fourth cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the fifth cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the sixth cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the seventh cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the composite layer is made of a mixture of LLDPE and LDPE with the mass ratio of 3:2, and the layer thickness is 10%.
The preparation method is the same as that of example 1.
Example 4
An electron crosslinking reinforced PE film comprises the following components in sequence from top to bottom: the heat-resistant layer, the first crosslinked layer, the second crosslinked layer, the third crosslinked layer, the fourth crosslinked layer, the fifth crosslinked layer, the sixth crosslinked layer, the seventh crosslinked layer and the composite layer;
the heat-resistant layer is made of HDPE, and the thickness of the layer is 15%; the first cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the second crosslinking layer is made of LDPE, and the thickness of the layer is 11%; the third cross-linked layer is made of LDPE, and the thickness of the layer is 11%; the fourth cross-linked layer is made of LDPE, and the thickness of the layer is 11%; the fifth cross-linked layer is made of LDPE, and the thickness of the layer is 11%; the sixth cross-linked layer is made of LDPE, and the thickness of the layer is 11%; the seventh cross-linked layer is made of LDPE, and the thickness of the layer is 10%; the composite layer is made of a mixture of LLDPE and LDPE with the mass ratio of 3:2, and the layer thickness is 10%.
The preparation method is the same as that of example 1.
Table 5 shows the performance test data for the E-crosslinked PE films of examples 2-4:
TABLE 5
Figure BDA0002836271480000101
Comparative example 1
Uncrosslinked film:
the layer A is a surface layer: the material is LLDPE + LDPE, 1002AY + FD0270 ═ 60/40, 1002AY, Exxon Mobil; FD0270, catal, layer thickness 15%;
the B layer is a first crosslinking layer: the material is LLDPE + LDPE, 1002AY + FD0270 ═ 60/40, 1002AY, Exxon Mobil; FD0270, catal, layer thickness 10%;
layer C is a second crosslinked layer: the material is LLDPE + LDPE, 1002AY + FD0270 ═ 60/40, 1002AY, Exxon Mobil; FD0270, catal, layer thickness 10%;
layer D is a third crosslinked layer: the material is LLDPE + LDPE, 1002AY + FD0270 ═ 60/40, 1002AY, Exxon Mobil; FD0270, catal, layer thickness 10%;
layer E is a fourth crosslinked layer: the material is LLDPE + LDPE, 1002AY + FD0270 ═ 60/40, 1002AY, Exxon Mobil; FD0270, catal, layer thickness 10%;
layer F is a fifth crosslinked layer: the material is LLDPE + LDPE, 1002AY + FD0270 ═ 60/40, 1002AY, Exxon Mobil; FD0270, catal, layer thickness 10%;
the G layer is a sixth crosslinked layer: the material is LLDPE + LDPE, 1002AY + FD0270 ═ 60/40, 1002AY, Exxon Mobil; FD0270, catal, layer thickness 10%;
layer H is a seventh crosslinked layer: the material is LLDPE + LDPE, 1002AY + FD0270 ═ 60/40, 1002AY, Exxon Mobil; FD0270, catal, layer thickness 10%;
the layer I is a composite layer: the material is LLDPE + LDPE, 1002AY/FD0270 ═ 60/40, 1002AY, Exxon Mobil; FD0270, catal, layer thickness 15%.
Properties of the product of comparative example 1: the heat resistance, tensile property and puncture property were all inferior to those of the electronically crosslinked reinforced PE film prepared in example 1.
TABLE 6
Figure BDA0002836271480000111
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The utility model provides an electron cross-linking reinforcing PE film which characterized in that from last to down in proper order: the heat-resistant layer, the first crosslinked layer, the second crosslinked layer, the third crosslinked layer, the fourth crosslinked layer, the fifth crosslinked layer, the sixth crosslinked layer, the seventh crosslinked layer and the composite layer;
the heat-resistant layer is made of HDPE, and the thickness of the layer is 10-30%; the first cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the second crosslinking layer is made of LDPE, and the thickness of the layer is 5-25%; the third cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the fourth cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the fifth cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the sixth cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the seventh cross-linked layer is made of LDPE, and the thickness of the layer is 5-25%; the composite layer is made of a mixture of LLDPE and LDPE with the mass ratio of 3:2, and the layer thickness is 10-20%.
2. The PE film with enhanced electronic crosslinking as claimed in claim 1, wherein the layer thickness of the heat-resistant layer is 15-25%; the thickness of the first crosslinking layer is 8-10%; the thickness of the second crosslinking layer is 8-11%; the thickness of the third crosslinking layer is 8-11%; the thickness of the fourth crosslinking layer is 8-11%; the thickness of the fifth crosslinking layer is 7-11%; the thickness of the sixth crosslinking layer is 8-11%; the layer thickness of the seventh crosslinking layer is 8-10%; the layer thickness of the composite layer material is 10-19%.
3. The PE film with enhanced electronic crosslinking as claimed in claim 2, wherein the layer thickness of the heat-resistant layer is 25%; the thickness of the first crosslinked layer is 10%; the thickness of the second crosslinked layer is 10%; the layer thickness of the third crosslinked layer is 10%; the thickness of the fourth crosslinked layer is 8%; the thickness of the fifth crosslinked layer is 7%; the thickness of the sixth crosslinked layer is 10%; the layer thickness of the seventh crosslinked layer is 10%; the layer thickness of the composite layer material is 10%.
4. The PE film with enhanced electronic crosslinking as claimed in claim 2, wherein the layer thickness of the heat-resistant layer is 25%; the thickness of the first crosslinked layer is 8%; the thickness of the second crosslinked layer is 8%; the thickness of the third crosslinked layer is 8%; the thickness of the fourth crosslinked layer is 8%; the thickness of the fifth crosslinked layer is 8%; the thickness of the sixth crosslinked layer is 8%; the layer thickness of the seventh crosslinked layer is 8%; the layer thickness of the composite layer material is 19%.
5. The PE film with enhanced electronic crosslinking as claimed in claim 2, wherein the layer thickness of the heat-resistant layer is 20%; the thickness of the first crosslinked layer is 10%; the thickness of the second crosslinked layer is 10%; the layer thickness of the third crosslinked layer is 10%; the thickness of the fourth crosslinked layer is 10%; the thickness of the fifth crosslinked layer is 10%; the thickness of the sixth crosslinked layer is 10%; the layer thickness of the seventh crosslinked layer is 10%; the layer thickness of the composite layer material is 10%.
6. The PE film with enhanced electronic crosslinking as claimed in claim 2, wherein the layer thickness of the heat-resistant layer is 15%; the thickness of the first crosslinked layer is 10%; the thickness of the second crosslinked layer is 11%; the thickness of the third crosslinked layer is 11%; the thickness of the fourth crosslinked layer is 11%; the thickness of the fifth crosslinked layer is 11%; the thickness of the sixth crosslinked layer is 11%; the layer thickness of the seventh crosslinked layer is 10%; the layer thickness of the composite layer material is 10%.
7. A method for preparing an electron cross-linking reinforced PE film according to any one of claims 1 to 6, comprising the steps of:
firstly, blowing a film on raw materials required by a PE film, then carrying out electronic crosslinking treatment, printing according to needs, and then compounding, curing and cutting to obtain the PE film with enhanced electronic crosslinking;
the film blowing method comprises the following steps:
the first layer is that the raw material HDPE of the heat-resistant layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 2 nd layer, the raw material LDPE of the first crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
a 3 rd layer, adding the LDPE of the second crosslinking layer into a hopper of an extruder, melting at the temperature of 170-200 ℃, and entering a neck mold;
the 4 th layer, the LDPE of the third crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 5 th layer, the LDPE of the fourth crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 6 th layer, the LDPE of the fifth crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 7 th layer, the raw material LDPE of the sixth crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
the 8 th layer, the raw material of LDPE of the seventh crosslinking layer is added into a hopper of an extruder, melted at the temperature of 170-200 ℃ and enters a neck mold;
layer 9, mixing the raw materials of the composite layer: adding the mixture of LLDPE and LDPE with the mass ratio of 3:2 into a hopper of an extruder, melting at the temperature of 170-200 ℃, and entering a neck mold;
then, extruding a film bubble of the multilayer co-extruded film through a die orifice, cooling a sizing cage on the outer side of the film bubble above the die orifice through an air ring to determine the diameter of the film bubble, and supporting the floating of the film bubble by air flow sprayed by a plurality of air cushion rollers above the sizing cage; the sizing cage and the air cushion roller cool the film bubble, so that the film bubble has certain structural strength, and the fixed diameter and the fixed thickness of the film bubble are determined; meanwhile, the film bubble is supported and floated by the air flow of the air cushion roller and the sizing cage: sizing and cooling the film bubble, cutting the film bubble into a sheet-shaped film, and rolling the film bubble to obtain a film product;
the electronic crosslinking treatment comprises the following steps:
and (3) putting the PE film roll obtained after the film blowing in the previous step into an offline EB machine through an unreeling device, carrying out high-energy ray scanning irradiation for crosslinking treatment under different irradiation doses, wherein the treatment voltage is 0.1-100 Mv, the treatment dose is 8-22 Mrad, cooling through a cooling roller, and then rolling to obtain the PE film subjected to electronic crosslinking treatment, namely the EPE film.
8. The method for preparing an electron crosslinking-reinforced PE film according to claim 7, wherein the treatment voltage of the electron crosslinking treatment is 0.5Mv, and the treatment dose is 12 Mrad;
the different irradiation doses have different influences on the crosslinking degree of the PE film, and the dose is controlled by equipment parameters, and the specific relation is as follows:
D＝(K*N*I)/V
v: linear velocity; k: a K value constant; n: the number of quenching treatment layers; i: beam current; d: and (4) dosage.
9. The method for preparing the PE film with the enhanced electronic crosslinking as claimed in claim 7, wherein the compounding is solvent-free compounding, the gluing amount is 1.3-2.0g, the PE surface needs to be subjected to online corona treatment in the PE compounding process, the power is 3000w, and the dyne value is more than or equal to 38;
compounding the EPE film obtained in the last step with a PE film, wherein the amount of the EPE film accounts for 50% of the mass of the electron crosslinking enhanced PE film, the amount of the PE film accounts for 50% of the mass of the electron crosslinking enhanced PE film, gluing the EPE film, and compounding the EPE film and the PE film in a compounding machine.
10. The method for preparing an electron cross-linking reinforced PE film according to claim 7, wherein the printing is performed according to the requirement, and the parameters of the printing process are as follows: the viscosity is 14 +/-2 s, the temperature is 55 +/-15 ℃, the scraper pressure is 0.3 +/-0.15 MPa, the compression roller pressure is 0.2 +/-0.15 MPa, the unreeling tension is 0.1-0.3N, the incoming tension is 0.2-0.4N, the printing tension is 0.2-0.4N, the reeling initial tension is 20 +/-5% N, the reeling finishing tension is 15 +/-5% N, and the printing speed is less than or equal to 150 m/min;
the curing is to cure the composite film for 1-96 hours at the temperature of 30-40 ℃.
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