CN117021722A - Flexible substrate film for flexible electronic device and preparation method thereof - Google Patents
Flexible substrate film for flexible electronic device and preparation method thereof Download PDFInfo
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- CN117021722A CN117021722A CN202311049481.0A CN202311049481A CN117021722A CN 117021722 A CN117021722 A CN 117021722A CN 202311049481 A CN202311049481 A CN 202311049481A CN 117021722 A CN117021722 A CN 117021722A
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- lldpe
- flexible substrate
- substrate film
- electronic device
- agent
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- 239000000758 substrate Substances 0.000 title claims abstract description 48
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- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 claims description 3
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Classifications
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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
- B32B27/327—Layered products comprising a layer of synthetic resin comprising polyolefins comprising polyolefins obtained by a metallocene or single-site catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
- B29C48/08—Flat, e.g. panels flexible, e.g. films
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- 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
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- 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
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- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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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
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
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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
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
- B32B3/266—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by an apertured layer, the apertures going through the whole thickness of the layer, e.g. expanded metal, perforated layer, slit layer regular cells B32B3/12
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
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- 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
- B32B2307/582—Tearability
- B32B2307/5825—Tear resistant
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a flexible substrate film for a flexible electronic device and a preparation method thereof, wherein the flexible substrate film comprises a core layer and two surface layers positioned on the upper surface and the lower surface of the core layer, and the core layer comprises the following raw materials in percentage by weight: 45-55% of first LLDPE, 45-55% of second LLDPE, 0.05-0.2% of antistatic agent, 0.1-0.2% of antibacterial agent, 0.1-0.15% of antioxidant and 0.05-0.2% of UV inhibitor; the surface layer comprises the following raw materials in percentage by weight: 5-10% of PBE elastomer, 30-45% of first LLDPE, 30-45% of second LLDPE, 3.5-5.5% of modified sepiolite, 0.05-0.2% of antistatic agent, 0.05-0.2% of antibacterial agent, 0.05-0.1% of antioxidant, 0.05-0.1% of anti-caking agent and 0.05-0.1% of UV inhibitor. According to the invention, through the cooperation of the first LLDPE and the second LLDPE, the tearing strength and the tensile modulus of the film can be greatly improved while the film has air permeability, the film thickness is reduced, the air permeability can be further improved through the use of the modified sepiolite, and finally the prepared finished product can be perfectly suitable for the flexible substrate film for the flexible electronic device, so that the economic benefit is huge.
Description
Technical Field
The invention belongs to the field of flexible electronic device production, and particularly relates to a flexible substrate film for a flexible electronic device and a preparation method thereof.
Background
Because the flexible electronic device has the advantages of light weight, low energy consumption, good biocompatibility, mechanical property and the like, along with the development of science and technology, the flexible electronic device has important application prospects in the fields of biomedicine, precision industry, robots and the like, and particularly has the basis of wearable intelligent products.
However, since the wearable product needs to be attached to the skin of the human body for a long period of time without affecting the daily activities of people, for this reason, it is required that the flexible electronic device has superior breathability, that is, that the flexible substrate film used for the flexible electronic device has superior breathability, and, as a wearable smart product, the flexible electronic device often needs to be subjected to a large strain during operation, so that the flexible substrate film used for the flexible electronic device has superior tensile properties. In order to obtain an increasingly better user experience, efforts have been made to develop flexible electronic devices that are excellent in performance, while at the same time, efforts have been made to develop flexible substrates for the preparation of flexible electronic devices that are excellent in performance.
Polyethylene is a thermoplastic resin produced by polymerizing ethylene. Polyethylene is odorless, nontoxic, wax-like in hand feeling, excellent in low-temperature resistance, good in chemical stability and resistant to most of acid and alkali corrosion. Is insoluble in common solvents at normal temperature, has small water absorption and excellent electrical insulation. The polyethylenes currently available on the market are high density polyethylene (hdpe, also known as low pressure polyethylene), medium density polyethylene (mdpe), low density polyethylene (ldpe), linear low density polyethylene (lldpe).
Metallocene polyethylene is a novel thermoplastic plastic, is the most important technical development of polyolefin industry in the 90 th year, and is an important innovation following LLDPE production technology. Since it is a polyethylene produced using Metallocene (MAO) as a polymerization catalyst, it is significantly different in performance from PE polymerized by conventional Ziegler-Natta catalysts. Metallocene polyethylene was first produced commercially by the U.S. Exxon company. The metallocene polyethylene can set the molecular size, has narrow molecular weight distribution and density of 0.9-0.93, and has good processability, but still can not directly manufacture the flexible substrate for the flexible electronic device, and the formula for manufacturing the flexible substrate for the flexible electronic device needs to be further improved.
Disclosure of Invention
The invention aims to provide a flexible substrate film for a flexible electronic device, which has excellent air permeability and stretching characteristics, and a preparation method thereof.
The invention is realized by the following technical scheme:
the flexible substrate film for the flexible electronic device comprises a core layer and two surface layers positioned on the upper surface and the lower surface of the core layer, wherein the surface layers are formed by the following mass ratio: core layer: skin = 1: (2.5-3.5): 1, a step of;
the core layer comprises the following raw materials in percentage by weight: 45-55% of first LLDPE, 45-55% of second LLDPE, 0.05-0.2% of antistatic agent, 0.1-0.2% of antibacterial agent, 0.1-0.15% of antioxidant and 0.05-0.2% of UV inhibitor;
the surface layer comprises the following raw materials in percentage by weight: 5-10% of PBE elastomer, 30-45% of first LLDPE, 30-45% of second LLDPE, 3.5-5.5% of modified sepiolite, 0.05-0.2% of antistatic agent, 0.05-0.2% of antibacterial agent, 0.05-0.1% of antioxidant, 0.05-0.1% of anti-caking agent and 0.05-0.1% of UV inhibitor;
the first LLDPE has a molecular weight distribution (Mw/Mn) of from 2.0 to 4.0, from 0.900 to 0.920 g/cm 3 And a density of 1-3.0dg/min I 2 LLDPE of (C); the second partLLDPE has a molecular weight distribution (Mw/Mn) of 2.0 to 6.0, 0.915 to 0.927 g/cm 3 And a density of 2-8.0dg/min I 2 LLDPE of (C); the density of the second LLDPE is at least 0.002 g/cm greater than the density of the first LLDPE 3 The method comprises the steps of carrying out a first treatment on the surface of the The first LLDPE and the second LLDPE are metallocene linear low density polyethylene mLLDPE prepared through metallocene catalytic reaction.
Compared with the conventional process of preparing a breathable polyethylene film by adopting calcium carbonate as a filler, separating filler particles from a polymer matrix to form mutually communicated micro-tunnels, wherein the addition of calcium carbonate easily leads to the increase of matrix resin viscosity, and the poor fluidity in the processing process makes the filler difficult to uniformly disperse in the matrix, and is unfavorable for the formation of the micro-tunnels under the action of stretching, the modified sepiolite is adopted as the raw material of a surface layer, firstly, the sepiolite is a chain layered silicate mineral, after modification treatment, the interlayer structure is effectively widened, interlayer acting force is weakened, and under the action of a silane coupling agent, the silicon hydroxyl groups in the master batch can be well dispersed in the preparation process of the master batch, and the silicon hydroxyl groups on the surface of the silane coupling agent are mutually dehydrated to form silicon-oxygen bonds, and under the action of tensile force, the organic chain segments of the silane coupling agent and the polymer are mutually wound, so that the excellent interlayer structure of the sepiolite is widened, thereby forming the micro-tunnels between the layers, and the sepiolite of a single layer is still well combined with the polyethylene matrix, so that the mechanical property of the product is effectively maintained, and the breathability is also exerted; moreover, the sepiolite has good rheological property and high-viscosity suspension stability, a stably dispersed suspension system can be formed in a resin system after the hydrophilic surface of the sepiolite is improved by a coupling agent, and good rheological property is exerted in the processing process, so that a filler can be well and stably dispersed in the resin system in the processing process, thereby being beneficial to uniform distribution of a microporous structure in the resin, further improving the air permeability of a product, and further improving the quality of the product by the assistance of additives such as an antistatic agent, an antibacterial agent, an antioxidant, an anti-caking agent and a UV inhibitor.
Preferably, the metallocene linear low density polyethylene mLLDPE is polyethylene prepared by adopting a single active site catalyst-metallocene catalyst system, and can be obtained by copolymerizing ethylene with butene-1 and hexene-1, and can also be obtained by homopolymerizing ethylene.
Preferably, the surface layer comprises the following components in percentage by mass: core layer: skin = 1:3:1.
preferably, the core layer further comprises the following raw materials in percentage by weight: 2-3.5% of high-temperature antifogging agent and 2-2.5% of low-temperature antifogging agent; preferably, the surface layer further comprises the following raw materials in percentage by weight: 1-2.5% of high-temperature antifogging agent, 1.5-2% of low-temperature antifogging agent and 1.0-2% of superfine diatomite; the high-temperature antifogging agent is oleic acid diethanolamide, and the low-temperature antifogging agent is polyethylene oxide glycerol trioleate. The film has high and low temperature antifogging performance simultaneously by adding a certain proportion of high and low temperature compound antifogging agent into the surface layer and the core layer. By adding a certain amount of superfine diatomite into the surface layer, the adsorption function of the diatomite can be utilized, precipitation of auxiliary agents such as antifogging agents and the like can be delayed, the antifogging time of the film can be prolonged, the air permeability of the film can be improved by utilizing the granularity of the diatomite, on the other hand, the strength of the film can be improved by the inorganic material diatomite, and the problem of the reduction of the film strength caused by the addition of the auxiliary agents such as antifogging agents and the like is solved; the PBE elastomer with a certain proportion is added in the surface layer, and the PBE elastomer has a tackifying effect, so that the problem of reduced heat sealing strength of the film caused by the increase of auxiliary agents such as antifogging agents and the like can be solved.
Preferably, the flexible substrate film includes a plurality of micro ventilation holes having a pore size in a range of 5nm to 1000 nm.
Preferably, the thickness of the flexible substrate film is 20um-150um.
Preferably, the modification process of the modified sepiolite comprises the following steps: sepiolite and water are mixed according to the mass ratio of 1:1 to 1:1.5, adding the mixture into a hydrothermal kettle, heating, pressurizing, stirring, reacting for 50-55 min, and carrying out suction filtration to obtain a filter cake, and then mixing the filter cake with 10-12% hydrochloric acid according to the mass ratio of 1:10 to 1:13, carrying out constant-temperature ultrasonic reaction for 3 hours, filtering, washing, drying and roasting to obtain pretreated sepiolite, sequentially taking 70-75 parts of pretreated sepiolite, 85-90 parts of water, 25-28 parts of silane coupling agent KH-560 and 65-75 parts of absolute ethyl alcohol according to parts by weight, firstly mixing the silane coupling agent KH-560 and the absolute ethyl alcohol, then mixing the pretreated sepiolite with water, regulating the pH value to 4.0-4.2, carrying out constant-temperature stirring reaction for 3 hours, filtering, washing and drying to obtain the modified sepiolite.
Preferably, the first linear LLDPE and the second linear LLDPE are both subjected to compounding modification by adding a compounding auxiliary agent before use so as to improve the melt strength of the metallocene polyethylene, and the weight of the metallocene linear low-density polyethylene mLLDPE in the compounding raw materials is hundred percent, and the compounding raw materials comprise: 100 percent of mLLDPE, 0.2 to 0.3 percent of compound crosslinking auxiliary agent, 0.015 to 0.020 percent of dibenzoyl peroxide BPO, 0.1 to 0.2 percent of heat stabilizer and 0.1 to 0.2 percent of antioxidant; the compound cross-linking auxiliary agent is formed by compounding 1, 1-dimethyl ethyl-hydrogen peroxide TB and tert-butyl peroxyacetate TBPA, and the mixing weight ratio of the TB to the TBPA is 10:1-4:3.
More preferably, the heat stabilizer is one of stearates, such as zinc stearate, calcium stearate and the like; the antioxidant is one of phenol, hindered amine and phosphite antioxidants.
More preferably, the specific steps of the compounding modification of the first linear LLDPE and the second linear LLDPE are as follows:
1) Firstly, mixing two crosslinking auxiliary agents in proportion, adding a solvent, then mixing with mLLDPE, a heat stabilizer and an antioxidant which account for 5-10% of the total mass at a high speed for 3-5 min, preparing a premixed master batch, and adding the premixed master batch into an extruder through a feed inlet;
2) Adding the residual mLLDPE into an extruder from a feed inlet, wherein the reaction time is 1.5-2.5 min, and the reaction temperature is 170-200 ℃;
3) Preparing solution by BPO and solvent, dripping the solution into a plasticizing section of an extruder, controlling the residence time of the BPO in the extruder to be less than 20 seconds, controlling the reaction temperature to be not more than 220 ℃, and then extruding, cooling and granulating.
Further, the solvent added in the compound crosslinking auxiliary agent and the BPO is toluene, dimethylbenzene, acetone and the like, and the addition amount of the solvent is 2-5 times of the weight of the compound crosslinking auxiliary agent or the BPO.
Further, the first linear LLDPE and the second linear LLDPE compounding modification are carried out in an internal mixer, kneader or screw extruder, most preferably in a twin screw extruder.
In the process of compounding and modifying the first linear LLDPE and the second linear LLDPE, on one hand, a compound crosslinking system composed of peroxides with low activity and higher activity is selected to carry out a crosslinking reaction on the base resin, so that the crosslinking rate and the crosslinking degree of the resin can be effectively controlled, a micro-crosslinking structure is realized, the melt strength of the resin can be moderately improved, the processability of the resin is improved, and the problems that the dosage is too large or the safety, the environmental protection, the modification cost and the like are not facilitated due to the single use of one peroxide are avoided. On the other hand, on the basis of the resin with the pre-crosslinked structure, a small amount of high-activity organic peroxide is added again, and through reactive extrusion, a micro-crosslinking reaction is carried out again, so that the melt strength of the base resin is further improved. The synergistic effect ensures that the cross-linked structure of the composition is amplified stepwise and gradually, thus realizing a large number of micro-cross-linked structures instead of body-type cross-linked structures. Thus, the melt strength of the composition can be improved by more than 2 times compared with that of mLLDPE, the problem that a wide film cannot be blown by the mLLDPE is solved, and the appearance of a film product is uniform and attractive, so that the excellent physical properties of the mLLDPE can be fully exerted in the aspect of film use.
The compound modification method enables the crosslinking structure of the base resin mLLDPE to be amplified step by step, realizes the controllability of crosslinking degree, prevents gel from occurring, and can greatly improve the melt strength. The method has the advantages of short flow, simple process, low development cost, short development period, small fluctuation of product quality and the like.
Alternatively, preferably, the first linear LLDPE and the second linear LLDPE are modified before use by adding small amounts of ultra-high molecular weight polyethylene and polyolefin elastomer POE to increase the melt strength of the metallocene polyethylene, the modified mixture comprises 82-90% of metallocene polyethylene resin and 7-10% of ultra-high molecular weight polyethylene UHMWPE, the ultra-high molecular weight polyethylene UHMWPE being calculated as weight percentThe polyethylene has a viscosity average molecular weight of 150 ten thousand or more and a density of 0.936-0.964 g/cm 3 The melting point range is 130-156 ℃; 3 to 4 percent of polyolefin elastomer POE, wherein the polyolefin elastomer POE is a saturated ethylene-octene copolymer, has very narrow molecular weight distribution and has the density ranging from 0.852 g/cm to 0.880g/cm and is produced by an in-situ polymerization technology of ethylene and octene 3 The melting point ranges from 50 to 70 ℃.
The modifying step comprises the following steps: melting UHMWPE at 220-240 ℃, cooling to 155-165 ℃, adding polyolefin elastomer POE, banburying to obtain blended UHMWPE/POE, and finally blending the blended UHMWPE/POE with metallocene polyethylene to obtain the metallocene polyethylene resin composition with high melt strength.
The best method for modifying comprises the following specific steps:
(1) Adding an antioxidant into UHMWPE, melting in an internal mixer for 10-15 minutes at 220-240 ℃, and then cooling to 155-165 ℃;
(2) Adding polyolefin elastomer POE into an internal mixer according to the weight ratio, carrying out internal mixing for 6-8 minutes at the rotation speed of 40-50 r/min at the temperature of 155-165 ℃, and then granulating to obtain a mixed material UHMWPE/POE;
(3) Weighing mixed UHMWPE/POE and metallocene polyethylene after banburying and granulating according to the weight ratio, and uniformly mixing at room temperature;
(4) Extruding and granulating the mixed materials in a double-screw extruder, wherein the rotating speed of the screw is 120-180 rpm, and the temperature is 190-220 ℃.
(5) Drying at 80-90 deg.c to obtain high melt strength metallocene polyethylene resin composition.
The melt strength is based on the degree of molecular chain entanglement in the molten state of the polymer, and the degree of molecular chain entanglement is high, so that the melt strength is high. By modifying, the incorporation of ultra-high molecular weight polyethylene enhances the degree of molecular chain entanglement of the metallocene polyethylene composition and thereby increases its melt strength. However, because the ultra-high molecular weight polyethylene and the metallocene polyethylene have large melt property difference and are difficult to fully mix, the ultra-high molecular weight polyethylene is firstly subjected to flow modification by using polyolefin POE during preparation, and the characteristics of low molecular weight and containing branches with a certain length of polyolefin elastomer are utilized to prepare an UHMWPE/POE blend with partially entangled molecular chains in a program feeding mode, and then the metallocene polyethylene composition with high melt strength is obtained through melt blending.
By modification, the obtained mixture has high melt strength compared with the metallocene polyethylene, and the physical and mechanical properties of the mixture are not lost, while the physical and mechanical properties of the metallocene polyethylene can be reduced by the method for improving the melt strength of the metallocene polyethylene by using general polyethylene resins such as low-density polyethylene and the like in the prior art.
The invention also discloses a preparation method of the flexible substrate film, which comprises the following steps: firstly, respectively mixing and granulating the raw materials of each layer to obtain a core layer master batch and a surface layer master batch; and then drying the two types of master batches, and carrying out coextrusion and stretching to obtain the flexible substrate film.
Preferably, when the flexible substrate film is prepared by coextrusion and stretching, the extrusion temperature is 230-330 ℃; in the stretching process, firstly, stretching an unoriented film 1.5-3.5 times in the longitudinal direction and stretching 5-9 times in the transverse direction; the biaxially oriented film is then separated.
The beneficial effects of the invention are as follows:
according to the flexible substrate film for the flexible electronic device, the first LLDPE and the second LLDPE are matched in the core layer and the two surface layers positioned on the upper surface and the lower surface of the core layer, so that the tearing strength and the tensile modulus of the film can be greatly improved while the film has air permeability, the film thickness is reduced, the production cost is reduced, the air permeability can be further improved through the use of modified sepiolite, and finally the finished product can be perfectly suitable for the flexible substrate film for the flexible electronic device, and the economic benefit is huge.
Drawings
For ease of illustration, the invention is described in detail by the following specific examples and figures.
Fig. 1 is a schematic structural view of a flexible substrate film of the present invention.
Detailed Description
Example 1
The flexible substrate film for the flexible electronic device shown in fig. 1 comprises a core layer 1 and two surface layers 2 positioned on the upper surface and the lower surface of the core layer 1, wherein the surface layers are formed by the following mass ratio: core layer: skin = 1:3:1, a step of;
the core layer comprises the following raw materials in percentage by weight: 50% of a first LLDPE, 49.4% of a second LLDPE, 0.2% of an antistatic agent, 0.2% of an antibacterial agent, 0.1% of an antioxidant and 0.1% of a UV inhibitor;
the surface layer comprises the following raw materials in percentage by weight: 8% of PBE elastomer, 45% of first LLDPE, 43% of second LLDPE, 3.5% of modified sepiolite, 0.2% of antistatic agent, 0.1% of antibacterial agent, 0.1% of antioxidant, 0.05% of anti-caking agent and 0.05% of UV inhibitor;
the first LLDPE has a molecular weight distribution (Mw/Mn) of from 2.0 to 4.0, from 0.900 to 0.920 g/cm 3 And a density of 1-3.0dg/min I 2 LLDPE of (C); the second LLDPE has a molecular weight distribution (Mw/Mn) of from 2.0 to 6.0, from 0.915 to 0.927 g/cm 3 And a density of 2-8.0dg/min I 2 LLDPE of (C); the density of the second LLDPE is at least 0.002 g/cm greater than the density of the first LLDPE 3 The method comprises the steps of carrying out a first treatment on the surface of the The first LLDPE and the second LLDPE are metallocene linear low density polyethylene mLLDPE prepared through metallocene catalytic reaction.
The metallocene linear low-density polyethylene mLLDPE is polyethylene prepared by adopting a single-site catalyst-metallocene catalyst system, can be obtained by copolymerizing ethylene with butene-1 and hexene-1, and can also be obtained by homopolymerizing ethylene.
The modification process of the modified sepiolite comprises the following steps: sepiolite and water are mixed according to the mass ratio of 1:1 to 1:1.5, adding the mixture into a hydrothermal kettle, heating, pressurizing, stirring, reacting for 50-55 min, and carrying out suction filtration to obtain a filter cake, and then mixing the filter cake with 10-12% hydrochloric acid according to the mass ratio of 1:10 to 1:13, carrying out constant-temperature ultrasonic reaction for 3 hours, filtering, washing, drying and roasting to obtain pretreated sepiolite, sequentially taking 70-75 parts of pretreated sepiolite, 85-90 parts of water, 25-28 parts of silane coupling agent KH-560 and 65-75 parts of absolute ethyl alcohol according to parts by weight, firstly mixing the silane coupling agent KH-560 and the absolute ethyl alcohol, then mixing the pretreated sepiolite with water, regulating the pH value to 4.0-4.2, carrying out constant-temperature stirring reaction for 3 hours, filtering, washing and drying to obtain the modified sepiolite.
The preparation method of the flexible substrate film comprises the following steps: firstly, respectively mixing and granulating the raw materials of each layer to obtain a core layer master batch and a surface layer master batch; and drying the two masterbatches, and then carrying out coextrusion and stretching to obtain the flexible substrate film.
When the flexible substrate film is prepared by coextrusion and stretching, the extrusion temperature is 230-330 ℃; in the stretching process, the unoriented film is stretched 3.5 times in the machine direction and 8 times in the transverse direction; the biaxially oriented film is then separated.
The flexible substrate film includes a plurality of micro-ventilation holes having a pore size in a range of 5nm to 1000 nm.
The thickness of the flexible substrate film is 20um-150um.
Example 2
Other characteristics of the flexible substrate film for flexible electronic devices are the same as in example 1, and the flexible substrate film comprises, in mass ratio, the surface layer: core layer: skin = 1:2.5:1, a step of;
the core layer comprises the following raw materials in percentage by weight: 45% of a first LLDPE, 54.6% of a second LLDPE, 0.1% of an antistatic agent, 0.1% of an antibacterial agent, 0.15% of an antioxidant and 0.05% of a UV inhibitor;
the surface layer comprises the following raw materials in percentage by weight: 10% of PBE elastomer, 30% of first LLDPE, 44% of second LLDPE, 3.5% of modified sepiolite, 0.1% of antistatic agent, 0.2% of antibacterial agent, 0.05% of antioxidant, 0.1% of anti-caking agent and 0.05% of UV inhibitor.
Example 3
Other characteristics of the flexible substrate film for flexible electronic devices are the same as in example 1, and the flexible substrate film comprises, in mass ratio, the surface layer: core layer: skin = 1:3.5:1, a step of;
the core layer comprises the following raw materials in percentage by weight: 54% of a first LLDPE, 45.5% of a second LLDPE, 0.15% of an antistatic agent, 0.1% of an antibacterial agent, 0.1% of an antioxidant and 0.15% of a UV inhibitor;
the surface layer comprises the following raw materials in percentage by weight: 8% of PBE elastomer, 44% of first LLDPE, 42% of second LLDPE, 5.5% of modified sepiolite, 0.2% of antistatic agent, 0.05% of antibacterial agent, 0.1% of antioxidant, 0.05% of anti-caking agent and 0.1% of UV inhibitor.
Example 4
The flexible substrate film for flexible electronic device has the same other characteristics as those of embodiment 1, and the core layer further comprises the following raw materials in percentage by weight: 3.2% of high-temperature antifogging agent and 2.2% of low-temperature antifogging agent; the surface layer also comprises the following raw materials in percentage by weight: 2% of high-temperature antifogging agent, 1.5% of low-temperature antifogging agent and 2% of superfine diatomite; the high-temperature antifogging agent is oleic acid diethanolamide, and the low-temperature antifogging agent is polyethylene oxide glycerol trioleate. The film has high and low temperature antifogging performance simultaneously by adding a certain proportion of high and low temperature compound antifogging agent into the surface layer and the core layer.
Example 5
The flexible substrate film for flexible electronic device is characterized in that, except for the embodiment 1, the first linear LLDPE and the second linear LLDPE are both subjected to compounding modification by adding a compounding auxiliary agent before use so as to improve the melt strength of metallocene polyethylene, and in the compounding raw materials, the weight of the metallocene linear low density polyethylene mLLDPE is hundred percent, and the method comprises the following steps: 100% of mLLDPE, 0.2% of a compound crosslinking auxiliary agent, 0.020% of dibenzoyl peroxide BPO, 0.2% of a heat stabilizer and 0.2% of an antioxidant; the compound cross-linking auxiliary agent is formed by compounding 1, 1-dimethyl ethyl-hydrogen peroxide TB and tert-butyl peroxyacetate TBPA, and the mixing weight ratio of the TB to the TBPA is 5:1.
The heat stabilizer is zinc stearate; the antioxidant is phosphite antioxidant.
The specific steps of the compound modification of the first linear LLDPE and the second linear LLDPE are as follows:
1) Firstly, mixing two crosslinking auxiliary agents in proportion, adding a solvent, then mixing with mLLDPE, a heat stabilizer and an antioxidant which account for 8% of the total mass at a high speed for 4min, preparing a premix master batch, and adding the premix master batch into an extruder through a feed inlet;
2) Adding the residual mLLDPE into an extruder from a charging port, wherein the reaction time is 2min, and the reaction temperature is 180 ℃;
3) Preparing solution by BPO and solvent, dripping the solution into a plasticizing section of an extruder, controlling the residence time of the BPO in the extruder to be less than 20 seconds, controlling the reaction temperature to be not more than 220 ℃, and then extruding, cooling and granulating.
And the solvent added into the compound crosslinking auxiliary agent and the BPO is toluene, and the addition amount of the solvent is 3 times of the weight of the compound crosslinking auxiliary agent or the BPO.
The first linear LLDPE and the second linear LLDPE are compounded and modified in a double-screw extruder.
Example 6
A flexible substrate film for flexible electronic devices, characterized in that the first linear LLDPE and the second linear LLDPE are modified before use by adding a small amount of ultra-high molecular weight polyethylene and polyolefin elastomer POE to improve the melt strength of metallocene polyethylene, wherein the modified mixture comprises 88% of metallocene polyethylene resin and 8% of ultra-high molecular weight polyethylene UHMWPE, which is polyethylene with a viscosity average molecular weight of more than 150 ten thousand and has a density of 0.936-0.964 g/cm, by weight percent 3 The melting point range is 130-156 ℃;4% of polyolefin elastomer POE which is a saturated ethylene-octene copolymer and has very narrow molecular weight distribution and density ranging from 0.852 to 0.880g/cm and is produced by an in-situ polymerization technology of ethylene and octene 3 The melting point ranges from 50 to 70 ℃.
The modifying step comprises the following steps: melting UHMWPE at 230 ℃, cooling to 155-165 ℃, adding polyolefin elastomer POE, banburying to obtain blended UHMWPE/POE, and finally blending the blended UHMWPE/POE with metallocene polyethylene to obtain the metallocene polyethylene resin composition with high melt strength.
The best method for modifying comprises the following specific steps:
(1) Adding an antioxidant into ultra-high molecular weight polyethylene UHMWPE, melting in an internal mixer for 10-15 minutes at 230 ℃, and then cooling to 155-165 ℃;
(2) Adding polyolefin elastomer POE into an internal mixer according to the weight ratio, carrying out internal mixing for 6-8 minutes at the rotation speed of 40-50 r/min at the temperature of 155-165 ℃, and then granulating to obtain a mixed material UHMWPE/POE;
(3) Weighing mixed UHMWPE/POE and metallocene polyethylene after banburying and granulating according to the weight ratio, and uniformly mixing at room temperature;
(4) Extruding and granulating the mixed materials in a double-screw extruder, wherein the rotating speed of a screw is 120-180 rpm, and the temperature is 190-220 ℃;
(5) Drying at 80-90 deg.c to obtain high melt strength metallocene polyethylene resin composition.
Performance test: the flexible substrate films obtained in examples 1 to 6 were subjected to performance test, and the results were as follows
From this, it is clear that the flexible substrate film obtained by the present invention has excellent air permeability and tensile properties.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any changes or substitutions that do not undergo the inventive effort should be construed as falling within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope defined by the claims.
Claims (9)
1. The flexible substrate film for the flexible electronic device comprises a core layer and two surface layers positioned on the upper surface and the lower surface of the core layer, wherein the surface layers are formed by the following mass ratio: core layer: skin = 1: (2.5-3.5): 1, characterized in that,
the core layer comprises the following raw materials in percentage by weight: 45-55% of first LLDPE, 45-55% of second LLDPE, 0.05-0.2% of antistatic agent, 0.1-0.2% of antibacterial agent, 0.1-0.15% of antioxidant and 0.05-0.2% of UV inhibitor;
the surface layer comprises the following raw materials in percentage by weight: 5-10% of PBE elastomer, 30-45% of first LLDPE, 30-45% of second LLDPE, 3.5-5.5% of modified sepiolite, 0.05-0.2% of antistatic agent, 0.05-0.2% of antibacterial agent, 0.05-0.1% of antioxidant, 0.05-0.1% of anti-caking agent and 0.05-0.1% of UV inhibitor;
the first LLDPE has a molecular weight distribution (Mw/Mn) of from 2.0 to 4.0, from 0.900 to 0.920 g/cm 3 And a density of 1-3dg/min I 2 LLDPE of (C); the second LLDPE has a molecular weight distribution (Mw/Mn) of from 2.0 to 6.0, from 0.915 to 0.927 g/cm 3 And a density of 2-8.0dg/min I 2 LLDPE of (C); the density of the second LLDPE is at least 0.002 g/cm greater than the density of the first LLDPE 3 The method comprises the steps of carrying out a first treatment on the surface of the The first LLDPE and the second LLDPE are metallocene linear low density polyethylene mLLDPE prepared through metallocene catalytic reaction.
2. The flexible substrate film for flexible electronic device according to claim 1, wherein the metallocene linear low density polyethylene mLLDPE is a polyethylene prepared by using a single site catalyst-metallocene catalyst system, is obtained by copolymerizing ethylene with butene-1, hexene-1, or is obtained by homopolymerizing ethylene.
3. The flexible substrate film for flexible electronic device according to claim 1, wherein the core layer further comprises the following raw materials in percentage by weight: 2-3.5% of high-temperature antifogging agent and 2-2.5% of low-temperature antifogging agent; the surface layer also comprises the following raw materials in percentage by weight: 1 to 2.5 percent of high-temperature antifogging agent, 1.5 to 2 percent of low-temperature antifogging agent and 1.0 to 2.0 percent of superfine diatomite; the high-temperature antifogging agent is oleic acid diethanolamide, and the low-temperature antifogging agent is polyethylene oxide glycerol trioleate.
4. The flexible substrate film for a flexible electronic device according to claim 1, wherein the flexible substrate film comprises a plurality of micro ventilation holes having a pore size in a range of 5nm to 1000 nm.
5. The flexible substrate film for flexible electronic device according to claim 1, wherein the first linear LLDPE and the second linear LLDPE are each modified by adding a compounding aid before use, and the weight of metallocene linear low density polyethylene mLLDPE in the compounding raw materials is hundred percent, comprising: 100 percent of mLLDPE, 0.2 to 0.3 percent of compound crosslinking auxiliary agent, 0.015 to 0.020 percent of dibenzoyl peroxide BPO, 0.1 to 0.2 percent of heat stabilizer and 0.1 to 0.2 percent of antioxidant; the compound cross-linking auxiliary agent is formed by compounding 1, 1-dimethyl ethyl-hydrogen peroxide TB and tert-butyl peroxyacetate TBPA, and the mixing weight ratio of the TB to the TBPA is 10:1-4:3.
6. The flexible substrate film for flexible electronic device according to claim 5, wherein the specific steps of compounding and modifying the first linear LLDPE and the second linear LLDPE are as follows:
1) Firstly, mixing two crosslinking auxiliary agents in proportion, adding a solvent, then mixing with mLLDPE, a heat stabilizer and an antioxidant which account for 5-10% of the total mass at a high speed for 3-5 min, preparing a premixed master batch, and adding the premixed master batch into an extruder through a feed inlet;
2) Adding the residual mLLDPE into an extruder from a feed inlet, wherein the reaction time is 1.5-2.5 min, and the reaction temperature is 170-200 ℃;
3) Preparing solution by BPO and solvent, dripping the solution into a plasticizing section of an extruder, controlling the residence time of the BPO in the extruder to be less than 20 seconds, controlling the reaction temperature to be not more than 220 ℃, and then extruding, cooling and granulating.
7. The flexible substrate film for flexible electronic device according to claim 1, wherein the first linear LLDPE and the second linear LLDPE are each modified by adding a small amount of ultra-high molecular weight polyethylene and polyolefin elastomer POE before use, and the modified mixture contains 82 to 90% by weight of a metallocene polyethylene resin, 7 to 10% by weight of ultra-high molecular weight polyethylene UHMWPE which is polyethylene having a viscosity average molecular weight of 150 ten thousand or more and has a density in the range of 0.936 to 0.964g/cm 3 The melting point range is 130-156 ℃; 3 to 4 percent of polyolefin elastomer POE, wherein the polyolefin elastomer POE is saturated ethylene-octene copolymer, and the density range is 0.852 to 0.880g/cm 3 The melting point ranges from 50 to 70 ℃.
8. The method for producing a flexible substrate film for a flexible electronic device according to any one of claims 1 to 7, wherein the raw materials of the respective layers are mixed and granulated to obtain a core layer master batch and a surface layer master batch, respectively; and then drying the two types of master batches, and carrying out coextrusion and stretching to obtain the flexible substrate film.
9. The method for producing a flexible substrate film for a flexible electronic device according to claim 8, wherein when the flexible substrate film is produced by coextrusion and stretching, the extrusion temperature is 230 to 330 ℃; in the stretching process, firstly, stretching an unoriented film 1.5-3.5 times in the longitudinal direction and stretching 5-9 times in the transverse direction; the biaxially oriented film is then separated.
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Citations (6)
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| CN102408601A (en) * | 2010-09-21 | 2012-04-11 | 中国石油天然气股份有限公司 | Ultra-wide metallocene polyethylene greenhouse film resin composition and preparation method thereof |
| CN102408600A (en) * | 2010-09-21 | 2012-04-11 | 中国石油天然气股份有限公司 | High-strength ultra-wide metallocene polyethylene greenhouse film resin composition and preparation method thereof |
| CN103374171A (en) * | 2012-04-13 | 2013-10-30 | 中国石油天然气股份有限公司 | metallocene polyethylene resin composition with high melt strength and preparation method thereof |
| CN107283976A (en) * | 2017-06-30 | 2017-10-24 | 永新股份（黄山）包装有限公司 | A kind of microporous polyethylene breathable films and preparation method thereof |
| CN108976574A (en) * | 2018-05-25 | 2018-12-11 | 黄智慧 | A kind of breathable polyethylene film |
| CN110948974A (en) * | 2019-10-31 | 2020-04-03 | 福建师范大学福清分校 | High-low temperature antifogging breathable polyethylene heat-sealing film for fruit and vegetable packaging and preparation method thereof |
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- 2023-08-21 CN CN202311049481.0A patent/CN117021722A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102408601A (en) * | 2010-09-21 | 2012-04-11 | 中国石油天然气股份有限公司 | Ultra-wide metallocene polyethylene greenhouse film resin composition and preparation method thereof |
| CN102408600A (en) * | 2010-09-21 | 2012-04-11 | 中国石油天然气股份有限公司 | High-strength ultra-wide metallocene polyethylene greenhouse film resin composition and preparation method thereof |
| CN103374171A (en) * | 2012-04-13 | 2013-10-30 | 中国石油天然气股份有限公司 | metallocene polyethylene resin composition with high melt strength and preparation method thereof |
| CN107283976A (en) * | 2017-06-30 | 2017-10-24 | 永新股份（黄山）包装有限公司 | A kind of microporous polyethylene breathable films and preparation method thereof |
| CN108976574A (en) * | 2018-05-25 | 2018-12-11 | 黄智慧 | A kind of breathable polyethylene film |
| CN110948974A (en) * | 2019-10-31 | 2020-04-03 | 福建师范大学福清分校 | High-low temperature antifogging breathable polyethylene heat-sealing film for fruit and vegetable packaging and preparation method thereof |
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