CN116284972A - Preparation method of electromagnetic shielding composite film - Google Patents
Preparation method of electromagnetic shielding composite film Download PDFInfo
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- CN116284972A CN116284972A CN202310469726.9A CN202310469726A CN116284972A CN 116284972 A CN116284972 A CN 116284972A CN 202310469726 A CN202310469726 A CN 202310469726A CN 116284972 A CN116284972 A CN 116284972A
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- composite film
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- silane
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- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 24
- 239000011231 conductive filler Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000001125 extrusion Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 4
- 238000000605 extraction Methods 0.000 claims abstract description 4
- -1 polyethylene Polymers 0.000 claims description 40
- 239000004698 Polyethylene Substances 0.000 claims description 26
- 229920000573 polyethylene Polymers 0.000 claims description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 8
- 239000004014 plasticizer Substances 0.000 claims description 8
- 239000000155 melt Substances 0.000 claims description 7
- 229920005672 polyolefin resin Polymers 0.000 claims description 7
- 229910052723 transition metal Inorganic materials 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000002480 mineral oil Substances 0.000 claims description 4
- 235000010446 mineral oil Nutrition 0.000 claims description 4
- 125000004103 aminoalkyl group Chemical group 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- SLDXSSRFNABVCN-UHFFFAOYSA-N 3-diethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CCO[SiH](OCC)CCCOC(=O)C(C)=C SLDXSSRFNABVCN-UHFFFAOYSA-N 0.000 claims description 2
- BZCWFJMZVXHYQA-UHFFFAOYSA-N 3-dimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[SiH](OC)CCCOC(=O)C(C)=C BZCWFJMZVXHYQA-UHFFFAOYSA-N 0.000 claims description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 229940057995 liquid paraffin Drugs 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Chemical group 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- XQGWAPPLBJZCEV-UHFFFAOYSA-N triethoxy(propyl)silane;urea Chemical compound NC(N)=O.CCC[Si](OCC)(OCC)OCC XQGWAPPLBJZCEV-UHFFFAOYSA-N 0.000 claims description 2
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 8
- 239000000463 material Substances 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 4
- 229920000098 polyolefin Polymers 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 150000001343 alkyl silanes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- 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
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
- B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
- B29C55/14—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/14—Carbides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention aims to provide a preparation method of an electromagnetic shielding composite film, which belongs to the technical field of electromagnetic shielding materials and comprises 5 steps of raw material melt extrusion, sheet longitudinal stretching, sheet transverse stretching, auxiliary agent extraction and secondary transverse stretching, wherein a certain amount of silane coupling agent and conductive filler are added into polyolefin raw materials. The invention combines polyolefin as a matrix and conductive filler, and can prepare the high-performance electromagnetic shielding material with excellent mechanical performance and good flexibility through a biaxial stretching process.
Description
Technical Field
The invention belongs to the technical field of electromagnetic shielding materials, and particularly relates to a preparation method of an electromagnetic shielding composite film.
Background
With the wide application of electronic and electrical equipment, the problems of electromagnetic interference (EMI) and electromagnetic pollution (EMP) are increasingly serious, and the fields of aerospace, civilian use, military use and the like have put higher requirements on electromagnetic shielding materials. The traditional electromagnetic shielding material is a metal material, has high conductivity and high electromagnetic shielding efficiency, but has high density and poor flexibility, and is difficult to meet the requirements of flexibility and wearable electronics.
The conductive polymer composite material prepared from the polymer matrix and the conductive filler is a research hot spot for exploring a flexible electromagnetic shielding material with light weight, thin thickness, high efficiency, high strength and high oxidation resistance. Among the polymer groups, the polyolefin is entirely composed of carbon chain structures and has very excellent mechanical properties, good corrosion resistance and very high thermal stability. MXene, which is a two-dimensional transition metal carbide/nitride, has good hydrophilicity, excellent conductivity and large specific surface area, and is a hot spot material for electromagnetic shielding in recent years.
Disclosure of Invention
The invention aims to provide a preparation method of an electromagnetic shielding composite film, which can solve the problems of high density, poor flexibility and the like of the traditional shielding material.
The invention adopts the following technical scheme:
the preparation method of the electromagnetic shielding composite film comprises the following steps:
first, raw material melt extrusion
Adding polyolefin resin, plasticizer, silane coupling agent and conductive filler into an extruder according to a proportion, heating and shearing to form uniform melt, extruding the melt through a T-shaped die, and cooling to form a composite sheet;
second, stretching the sheet in the machine direction
Longitudinally stretching the composite sheet obtained in the first step by adopting a longitudinal hot roller type stretching method to obtain a longitudinal stretching composite film;
third step, transversely stretching the sheet
Uniformly stretching the composite film obtained in the second step transversely by adopting a chain clamp to obtain a biaxially oriented composite film;
fourth, extracting the auxiliary agent
Immersing the completely stretched composite film obtained in the third step into dichloromethane for multistage extraction, so that the plasticizer in the film body is separated from the film body, and forming the composite film with a uniform micropore structure;
fifth step, the second transverse stretching
And (3) transversely and uniformly stretching the composite film obtained in the fourth step in a transverse drawing machine again to obtain the final composite film.
Further, the polyolefin resin in the first step comprises one or two of polyethylene or polypropylene, the plasticizer comprises organic acid ester, phosphate ester, liquid paraffin or mineral oil, the silane coupling agent comprises one or more of an amino alkyl silane coupling agent, an epoxy alkyl silane coupling agent and a methacryloxy alkyl silane coupling agent, and the conductive filler comprises one or more of a metal-based nano filler, a carbon-based nano filler and an transition metal nitride/carbide MXene.
Further, the polyolefin resin is polyethylene, the weight average molecular weight is 100 ten thousand-500 ten thousand, and the mineral oil is white oil.
Further, the amino alkyl silane coupling agent comprises one or more of amino propyl triethoxy silane, amino propyl trimethoxy silane, amino ethyl amino propyl trimethoxy silane or urea propyl triethoxy silane.
Further, the epoxy hydrocarbon silane coupling agent comprises one or two of 2, 3-glycidoxypropyl trimethoxy silane or 2, 3-glycidoxypropyl triethoxy silane.
Further, the methacryloxyalkyl silane coupling agent comprises one or a mixture of several of methacryloxypropyl trimethoxy silane, methacryloxypropyl diethoxy silane and methacryloxypropyl dimethoxy silane.
Further, the metal-based nanofiller comprises one or a mixture of a plurality of silver, copper, cobalt, nickel and zinc metal oxides.
Further, the carbon-based nano filler comprises one or a mixture of more of carbon black, carbon nano tube and graphene.
Further, the transition metal nitride/carbide MXene has a molecular formula M n+1 X n T x Wherein M is a transition metal element, X represents carbon or nitrogen, n=1, 2 or 3, t x Represents a surface terminal OH, O or F group.
Further, the silane coupling agent is aminopropyl triethoxysilane, and the conductive filler is Ti 3 AlC 2 。
Further, the polyethylene content is 15-25 wt%, the white oil content is 75-85 wt%, the addition amount of the aminopropyl triethoxysilane is 1-5 wt% of the polyethylene mass, and the Ti is 3 AlC 2 The addition amount of (2) is 10-40 wt% of the mass of the polyethylene.
Further, the stretching ratio of the longitudinal stretching in the second step is 3 to 15 times.
Further, the stretching ratio of the transverse stretching in the third step is 3 to 15 times.
The beneficial effects of the invention are as follows:
polyethylene as matrix and Ti 3 AlC 2 MXene is combined to prepare a composite film, and a silane coupling agent is used as polyethylene and Ti 3 AlC 2 Mxene-connected bridge, hydrophilic group of silane coupling agent and Ti 3 AlC 2 The hydrophilic groups on the surface of MXene form hydrogen bonds, the silicon alkoxy groups of the silane coupling agent are tightly connected with polyethylene, and the silane coupling agent plays a role in reticular crosslinking and can crosslink Ti 3 AlC 2 The MXene is uniformly distributed in the polyethylene matrix, and the high-performance electromagnetic shielding material with excellent mechanical performance and good flexibility can be prepared through a biaxial stretching process.
Detailed Description
The invention is further illustrated, but not limited to, by the following examples.
The preparation method of the electromagnetic shielding composite film is carried out according to the following steps, and when the preparation method is concretely implemented, the step (1) is changed, and the steps (2), (3), (4) and (5) are all carried out according to the following steps.
(1) And (3) raw material melt extrusion:
adding a certain amount of polyolefin resin, a plasticizer, a silane coupling agent and a conductive filler into an extruder, heating and shearing to form a uniform melt, extruding the melt through a T-shaped die, and cooling to form a composite sheet;
(2) Stretching the sheet longitudinally:
longitudinally stretching the composite sheet obtained in the step (1) by adopting a longitudinal hot roller type stretching method, wherein the stretching multiple is 3-15 times to obtain a longitudinal stretching composite film;
(3) Sheet transverse stretching:
uniformly stretching the composite film obtained in the step (2) transversely by adopting a chain clamp type, wherein the stretching multiple is 3-15 times, and obtaining a biaxially oriented composite film;
(4) And (3) extracting an auxiliary agent:
immersing the completely stretched composite film obtained in the step (3) into dichloromethane for multistage extraction, so that the plasticizer in the film body is separated from the film body, and the composite film with a uniform micropore structure is formed.
(5) Secondary transverse stretching:
and (3) transversely and uniformly stretching the composite film obtained in the step (4) in a transverse drawing machine again to obtain the final composite film.
Example 1
(1) Melt extrusion of raw materials:
18wt% polyethylene, 82wt% white oil, 10wt% (based on the mass of the polyethylene) Ti 3 AlC 2 Mxene and 1wt% (based on the mass of polyethylene) of aminopropyl triethoxysilane are mixed, the resulting mixture is heated and melted in a twin screw extruder, and the melt is extruded through a T die and cooled to form a cast sheet.
The other steps are carried out according to the steps (2), (3), (4) and (5).
Example 2
(1) Melt extrusion of raw materials:
18wt% polyethylene, 82wt% white oil, 20wt% (based on the mass of the polyethylene) Ti 3 AlC 2 Mxene and 2wt% (based on the mass of the polyethylene) aminopropyl triethoxysilane are mixed, the resulting mixture is heated and melted in a twin screw extruder, and the melt is extruded through a T die and cooled to form a cast sheet.
The other steps are carried out according to the steps (2), (3), (4) and (5).
Example 3
(1) Melt extrusion of raw materials:
18wt% polyethylene, 82wt% white oil, 30wt% (based on the mass of the polyethylene) Ti 3 AlC 2 Mxene and 3wt% (based on the mass of the polyethylene) aminopropyl triethoxysilane are mixed, the resulting mixture is heated and melted in a twin screw extruder, and the melt is extruded through a T die and cooled to form a cast sheet.
The other steps are carried out according to the steps (2), (3), (4) and (5).
Example 4
(1) Melt extrusion of raw materials:
18wt% polyethylene, 82wt% white oil, 40wt% (based on the mass of the polyethylene) Ti 3 AlC 2 Mxene and 5wt% (based on the mass of polyethylene) aminopropyl triethoxysilane are mixed, the resulting mixture is heated and melted in a twin screw extruder, and the melt is extruded through a T die and cooled to form a cast sheet.
The other steps are carried out according to the steps (2), (3), (4) and (5).
The composite film obtained in the above example was subjected to electromagnetic shielding performance and mechanical performance test, and the specific test results are shown in table 1.
Table 1 test data
As can be seen from Table 1, the composite film prepared in each example has a thickness of approximately 16 μm, with Ti 3 AlC 2 The addition amount of Mxene is continuously increased, ti3AlC2 Mxene distributed on the surface of the inner pore structure of the composite film is gradually increased, and the surface density, electromagnetic shielding effectiveness and tensile strength of the composite film are correspondingly improved, but the composite film of example 4 has a tendency of decreasing tensile strength.
The above-described embodiments are merely illustrative of the principles of the present invention and its capabilities, and some of its applications, variations and modifications can be made by those skilled in the art without departing from the inventive concept, which fall within the scope of the present invention.
Claims (10)
1. A preparation method of an electromagnetic shielding composite film is characterized in that: the method comprises the following steps:
first, raw material melt extrusion
Adding polyolefin resin, plasticizer, silane coupling agent and conductive filler into an extruder according to a proportion, heating and shearing to form uniform melt, extruding the melt through a T-shaped die, and cooling to form a composite sheet;
second, stretching the sheet in the machine direction
Longitudinally stretching the composite sheet obtained in the first step by adopting a longitudinal hot roller type stretching method to obtain a longitudinal stretching composite film;
third step, transversely stretching the sheet
Uniformly stretching the composite film obtained in the second step transversely by adopting a chain clamp to obtain a biaxially oriented composite film;
fourth, extracting the auxiliary agent
Immersing the completely stretched composite film obtained in the third step into dichloromethane for multistage extraction, so that the plasticizer in the film body is separated from the film body, and forming the composite film with a uniform micropore structure;
fifth step, the second transverse stretching
And (3) transversely and uniformly stretching the composite film obtained in the fourth step in a transverse drawing machine again to obtain the final composite film.
2. The method for producing an electromagnetic shielding composite film according to claim 1, characterized in that: the polyolefin resin in the first step comprises one or two of polyethylene or polypropylene, the plasticizer comprises organic acid ester, phosphate ester, liquid paraffin or mineral oil, the silane coupling agent comprises one or more of amino hydrocarbon silane coupling agent, epoxy hydrocarbon silane coupling agent and methacryloxyalkyl silane coupling agent, and the conductive filler comprises one or more of metal-based nanofiller, carbon-based nanofiller and transition metal nitride/carbide MXene.
3. The method for producing an electromagnetic shielding composite film according to claim 2, characterized in that: the polyolefin resin is polyethylene, the weight average molecular weight is 100-500 ten thousand, and the mineral oil is white oil.
4. The method for producing an electromagnetic shielding composite film according to claim 2, characterized in that: the amino alkyl silane coupling agent comprises one or more of amino propyl triethoxy silane, amino propyl trimethoxy silane, amino ethyl amino propyl trimethoxy silane or urea propyl triethoxy silane;
the epoxy hydrocarbon silane coupling agent comprises one or two of 2, 3-glycidoxypropyl trimethoxy silane or 2, 3-glycidoxypropyl triethoxy silane;
the methacryloxyalkyl silane coupling agent comprises one or more of methacryloxypropyl trimethoxy silane, methacryloxypropyl diethoxy silane or methacryloxypropyl dimethoxy silane.
5. The method for producing an electromagnetic shielding composite film according to claim 2, characterized in that: the metal-based nano filler comprises one or more of silver, copper, cobalt, nickel and zinc metal oxides;
the carbon-based nano filler comprises one or a mixture of more of carbon black, carbon nano tube and graphene.
6. The method for preparing the electromagnetic shielding composite film according to claim 4, wherein the method comprises the following steps: the molecular formula of the transition metal nitride/carbide MXene is M n+1 X n T x Wherein M is a transition metal element, X represents carbon or nitrogen, n=1, 2 or 3, t x Represents a surface terminal OH, O or F group.
7. The method for producing an electromagnetic shielding composite film according to claim 6, wherein: the silane coupling agent is aminopropyl triethoxy silane, and the conductive filler is Ti 3 AlC 2 。
8. The method for producing an electromagnetic shielding composite film according to claim 7, wherein: the polyethylene content is 15-25 wt%, the white oil content is 75-85 wt%, the addition amount of the aminopropyl triethoxysilane is 1-5 wt% of the polyethylene mass, and Ti 3 AlC 2 The addition amount of (2) is 10-40 wt% of the mass of the polyethylene.
9. The method for producing an electromagnetic shielding composite film according to claim 1, characterized in that: the stretching ratio of the longitudinal stretching in the second step is 3-15 times.
10. The method for producing an electromagnetic shielding composite film according to claim 1, characterized in that: the stretching multiple of the transverse stretching in the third step is 3-15 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202310469726.9A CN116284972A (en) | 2023-04-27 | 2023-04-27 | Preparation method of electromagnetic shielding composite film |
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| CN202310469726.9A CN116284972A (en) | 2023-04-27 | 2023-04-27 | Preparation method of electromagnetic shielding composite film |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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