CN115491137A - Portable transparent electric-conduction heat-conduction protective film and preparation method thereof - Google Patents

Portable transparent electric-conduction heat-conduction protective film and preparation method thereof Download PDF

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CN115491137A
CN115491137A CN202211010014.2A CN202211010014A CN115491137A CN 115491137 A CN115491137 A CN 115491137A CN 202211010014 A CN202211010014 A CN 202211010014A CN 115491137 A CN115491137 A CN 115491137A
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film
pvc
transparent
protective film
conduction
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陈界平
徐苏明
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Suzhou Huasu Plastics Co Ltd
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Suzhou Huasu Plastics Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
    • C09J7/24—Plastics; Metallised plastics based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/245—Vinyl resins, e.g. polyvinyl chloride [PVC]
    • 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
    • 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
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • 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
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/044—Forming conductive coatings; Forming coatings having anti-static properties
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24—Electrically-conducting paints
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    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38—Pressure-sensitive adhesives [PSA]
    • C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/385—Acrylic polymers
    • 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
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08J2327/06—Homopolymers or copolymers of vinyl chloride
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    • 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
    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
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    • 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
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
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    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2400/00—Presence of inorganic and organic materials
    • C09J2400/20—Presence of organic materials
    • C09J2400/28—Presence of paper
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2427/00—Presence of halogenated polymer
    • C09J2427/006—Presence of halogenated polymer in the substrate

Abstract

The invention provides a convenient transparent electric-conduction and heat-conduction protective film and a preparation method thereof, wherein the protective film is characterized in that a transparent coating containing water-based nano silver wires is uniformly coated on the surface of a PVC (polyvinyl chloride) calendered film with graphene nano wires inside by using a coating process, a first reticular structure is formed inside, a second reticular structure is formed on the surface, and a space network structure is formed by the first reticular structure and the second reticular structure to obtain a transparent permanent electric-conduction and heat-conduction film, the film material achieves an electric-conduction level effect, heat in the preparation process of electronic components can be effectively transferred to the air, and the damage of core components is avoided.

Description

Portable transparent electric-conduction heat-conduction protective film and preparation method thereof
Technical Field
The invention relates to the technical field of protective films, in particular to a convenient transparent electric-conduction heat-conduction protective film and a preparation method thereof.
Background
In the manufacturing process of electronic components, laser cutting and other processes, such as wafer expanding and cutting processes, are involved, and in these processes, due to the friction, much static electricity is generated, which may break through the wafer and cause damage to the wafer. Therefore, a protective film with an antistatic effect is generally applied to the surface of the wafer to conduct static electricity, thereby preventing damage to the wafer and reducing the defect rate. In addition, a large amount of high temperature and heat can be generated in the wafer cutting process, and if the heat conducting property of the protective film material is poor, the problem that the protective film is seriously shrunk and deformed can be caused, so that the protective film cannot play a full-coverage protection role.
Moreover, inside the computer lab of some high-end accurate electronic equipment after operation a period, can have a large amount of static in the air, if do not derive static in time, can cause electronic equipment's circuit short circuit, damage accurate electronic equipment, bring huge loss. The most common solution at present is to apply antistatic protective films on the walls, floors and ceilings of the machine room to eliminate the static electricity generated by the operation of the equipment.
However, most protective films in related industries only simply apply short-acting antistatic agents to the protective films, the grade of the conductive films cannot be achieved, and the problems of poor conductive effect, heat conduction and the like can occur in the using process, so that static electricity and heat cannot be timely and efficiently conducted out, and equipment and components cannot be effectively protected.
Disclosure of Invention
The invention aims to provide a convenient transparent electric and heat conducting protective film and a preparation method thereof, aiming at the defects of the prior art, the protective film utilizes a coating process to uniformly coat a transparent coating containing water-based nano silver wires on the surface of a PVC calendering film with graphene nano particles inside, a first reticular structure is formed inside, a second reticular structure is formed on the surface, and a transparent permanent electric and heat conducting film with a space network structure is formed by the first reticular structure and the second reticular structure, so that the film material achieves the electric conduction level effect, the heat in the preparation process of an electronic component can be effectively transferred to the air, and the damage of a core component is avoided.
According to a first aspect of the invention, the portable transparent electric conduction and heat conduction protective film comprises a release layer, a transparent pressure-sensitive adhesive layer and a transparent thin film layer, wherein the release layer, the transparent pressure-sensitive adhesive layer and the transparent thin film layer are sequentially and adjacently arranged from bottom to top;
the transparent film layer is a PVC calendered film and comprises the following components in parts by weight: 100 parts of PVC resin; 25-40 parts of a high-molecular polyester plasticizer; 2-4 parts of a powder calcium zinc stabilizer; 0.3-1 part of nano graphene; 1-4 parts of acrylate processing aid;
the nano graphene is uniformly dispersed in the PVC calendered film to form a first reticular structure, and the transparent conductive coating on the surface of the PVC calendered film has a second reticular structure;
the first reticular structure inside the PVC calendering film and the second reticular structure on the surface of the PVC calendering film form an electric and heat conducting space network structure.
Preferably, the thickness of the conductive coating is 10-15 μm, and the conductive coating comprises the following components in percentage by mass: 25-35% of water-based acrylic resin; 50-70% of water-based acrylic emulsion; 4-8% of a defoaming agent; 8-13% of absolute ethyl alcohol; 6-10% of wetting dispersant; 2-5% of nano silver wires.
Preferably, the nano silver wire is a linear nano structure with the diameter of 30-40 nm.
Preferably, the polymerization degree of the PVC resin is 1300, and the high molecular polyester plasticizer is adipate polyester.
Preferably, the carbon content of the nano graphene is not less than 99wt.%, the sheet diameter is 1-10 μm, and the thickness is 2-3nm.
Preferably, the thickness of the transparent pressure-sensitive adhesive layer is 20-30 μm, and the transparent pressure-sensitive adhesive layer is a water-based acrylate pressure-sensitive adhesive and comprises the following components in percentage by mass: 40-70% of water; 30-60% of acrylic polymer; 0.5 to 1.3 percent of ammonium hydroxide; 0.2 to 1.0 percent of triethanolamine.
Preferably, the release layer is silicon-coated release paper, and the gram weight is 120-140g/m 2 。
Preferably, the thickness of the PVC calendered film is 0.07-0.12mm.
According to a second aspect of the present invention, there is provided a method for preparing the portable transparent electrically and thermally conductive protective film, comprising the following steps:
s1, weighing the components in corresponding weight according to the weight parts of the components of the PVC calendered film, and uniformly mixing the nano graphene and the high-molecular polyester plasticizer to obtain a first mixture;
uniformly mixing the first mixture with PVC resin, a powdery calcium zinc stabilizer and an acrylate processing aid to obtain a second mixture;
banburying the second mixture to obtain a preplasticized melt, and then carrying out open milling, extrusion and calendering on the melt to obtain a PVC calendered film with a first network structure inside;
s2, coating the water-based acrylate containing the nano silver wires on one surface of the PVC calendered film obtained in the step S1 in a gravure printing mode by adopting a printing roller with reticular lines, so that a transparent conductive coating with a second reticular structure is formed on the surface of the PVC calendered film;
the first reticular structure inside the PVC calendering film and the second reticular structure on the surface of the PVC calendering film form an electric and heat conducting space network structure;
and S3, coating a transparent pressure-sensitive adhesive layer on the other side of the PVC calendered film obtained in the step S2, and then coating release paper on the transparent pressure-sensitive adhesive layer for lamination.
Preferably, in the step S1, a pneumatic ink stirrer is adopted to fully stir at a speed of 600-800rpm for 8-12min, so as to obtain a first mixture; stirring thoroughly with a high speed stirrer at 1200-1500rpm for 3-5min to obtain a second mixture.
Preferably, in the step S1, the banburying, roll mixing, extruding and rolling process includes:
the banburying conditions are as follows: the rotating speed of the rotor is 50-60rpm, and the loading current of the motor is 200-600A;
the open mill conditions are as follows: the temperature is 155-170 ℃, and the rotating speed is 20-30rpm;
the extrusion conditions were: the temperature is 160-175 ℃, and the single screw rotating speed is 20-28rpm;
the conditions of calendering were: the temperature of the four-roll calender is set as R1 along the feeding to the discharging direction in sequence: 170 ℃ -180 ℃, R2: 170-180 ℃, R3: 175-185 ℃, R4: 155-165 ℃;
the rotating speed of the four-roller calender is set as R1 along the feeding to the discharging direction in sequence: 14-24rpm, R2:18-30rpm, R3, 22-30rpm, R4:35-50rpm.
In step S2, the printing conditions are: printing speed: 40-60m/min, the temperature of the heating blast oven is 30-60 ℃, and the air volume is 2500-4500m 3 And h, drying.
Compared with the prior art, the invention has the beneficial effects that:
1. the portable transparent electric conduction and heat conduction protective film has a spatial network structure, and on one hand, the portable transparent electric conduction and heat conduction protective film is uniformly dispersed in a PVC system by using a special spatial network structure of nano graphene through a blending calendering process to form a PVC film with a good heat conduction and electric conduction spatial structure inside; on the other hand utilizes the netted coating line of hexagon, with transparent nanometer silver line coating through the even coating of this netted line at PVC membrane surface, obtains the electrically conductive heat conduction membrane material that has space network structure, and this membrane material not only the electrically conductive effect is obvious, but also good heat conduction effect, passes through the effectual derivation of space network structure with the high temperature heat that produces in the electronic components preparation process, avoids core component to receive the heat damage.
2. The protective film can achieve the effect of conductive level and can permanently keep the surface resistance of the film at 10 3- 5 The ohm/sq grade can not cause the condition of time-lapse loss, and can be widely applied to the field of electronic components.
3. The coating, the PVC film layer and the pressure-sensitive adhesive layer related to the protective film are transparent, so that the transparency of the film material is higher, the transparency is more than 85%, the film material has low VOC and meets the higher environment-friendly requirement, and meanwhile, the pressure-sensitive adhesive is coated on the bottom of the film material and coated with release paper, so that the protective film is convenient to use, can be used after being torn off, can be cut according to the actual shape requirement and is free from the constraints of the shape and the structure of a specific product, and the film material has the advantages of wider application range, more convenience in use and environmental friendliness.
Drawings
Fig. 1 is a structural diagram of a portable transparent conductive heat-conducting protective film according to the present invention.
Fig. 2 is a distribution and structure diagram of the first mesh structure and the second mesh structure of the present invention.
Fig. 3 is a micro-topography of the silver nanowires of the invention.
FIG. 4 is a grid pattern diagram of a hexagonal spatial network structure formed on the surface of a film by gravure coating printing according to the present invention.
Detailed Description
In order to better understand the technical content of the present invention, specific embodiments are described below with reference to the accompanying drawings.
In this disclosure, aspects of the present invention are described with reference to the accompanying drawings, in which a number of illustrative embodiments are shown. Embodiments of the present disclosure are not necessarily intended to include all aspects of the invention. It should be appreciated that the various concepts and embodiments described above, as well as those described in greater detail below, may be implemented in any of numerous ways.
Related products in the industry at present can only be used as an antistatic film, and cannot reach the grade of a conductive film, and the antistatic film is mainly divided into an organic type and an inorganic type. The organic antistatic film has high surface resistance (generally 10) 8-10 ohm/sq grade) and has the defects of short antistatic effect, failure in time and the like; inorganic products have the defects of opacity, limited application range and the like.
Meanwhile, the heat conduction effect of the antistatic film cannot achieve satisfactory effect aiming at the requirements of the field of electronic components.
Therefore, the invention provides a convenient transparent electric-conduction heat-conduction protective film and a preparation method thereof, wherein a transparent coating containing water-based nano silver wires is uniformly coated on the surface of a PVC calendered film with graphene nano particles inside by using a coating process to form a transparent permanent electric-conduction heat-conduction film with a spatial network shape on the surface, and a transparent pressure-sensitive adhesive is coated on the bottom layer of the film and is covered with release paper to prepare a DIY type product ready to use after being torn, so that the convenience is improved.
With reference to fig. 1, in an exemplary embodiment of the invention, a portable transparent conductive heat-conducting protective film is provided, which includes a release layer 1, a transparent pressure-sensitive adhesive layer 2 and a transparent thin film layer 3, the release layer 1, the transparent pressure-sensitive adhesive layer 2 and the transparent thin film layer 3 are sequentially and adjacently disposed from bottom to top, one surface of the transparent thin film layer 3 is fixedly connected with the transparent pressure-sensitive adhesive layer 2, the other surface of the transparent thin film layer 3 is provided with a transparent conductive coating 4, and the transparent conductive coating 4 is an aqueous acrylate coating containing nano silver wires.
The transparent film layer 3 is a PVC calendered film and comprises the following components in parts by weight: 100 parts of PVC resin; 25-40 parts of a high-molecular polyester plasticizer; 2-4 parts of a powder calcium zinc stabilizer; 0.3-1 part of nano graphene; 1-4 parts of acrylate processing aid.
As shown in fig. 2, the nano-graphene is uniformly dispersed in the PVC rolled film to form a first network structure 31, and the transparent conductive coating on the surface of the PVC rolled film has a second network structure 41.
The first reticular structure inside the PVC calendering film and the second reticular structure on the surface of the PVC calendering film form an electric and heat conducting spatial network structure.
In a preferred embodiment, the thickness of the conductive coating is 10-15 μm, and the conductive coating comprises the following components in percentage by mass: 25-35% of water-based acrylic resin; 50-70% of water-based acrylic emulsion; 4-8% of a defoaming agent; 8-13% of absolute ethyl alcohol; 6-10% of wetting dispersant; 2-5% of nano silver wires.
In a preferred embodiment, the nano silver wire is a linear structure nano material with good heat conduction function and uniform thickness of about 30-40nm, and the microstructure is shown in fig. 3.
The ultraviolet and visible light absorption test is carried out on the nano silver wire solution, the test range is 300nm-650nm, two absorption peaks of the nano silver wire are respectively 350nm and 380nm in an ultraviolet region, wherein the absorption peak at 350nm is determined by the characteristic peak of silver element, and the absorption peak at 380nm is determined by the diameter and the length-diameter ratio of the nano silver wire. In the visible region (between 400nm and 650 nm), the sample does not have an absorption peak, and thus is substantially transparent in the visible region with good transmittance.
The water-based acrylate coating has the characteristics of light color, transparency, excellent light resistance, weather resistance, chemical resistance, excellent construction performance and the like.
In a preferred embodiment, the polymerization degree of the PVC resin is 1300, and the high molecular polyester plasticizer is adipate polyester.
The PVC resin is synthesized by a suspension method, and has the characteristics of high whiteness, high plasticizer absorption rate, high plasticizing speed, concentrated particle size distribution, good transparency and the like.
The adipate polyester plasticizer belongs to a high-molecular polyester plasticizer and has the characteristics of low migration, high system viscosity, excellent gelation property, high molecular weight and the like.
The powder calcium zinc stabilizer has the characteristics of low odor, low VOC, lasting long-term heat resistance, high transparency and the like.
The acrylate processing aid has the characteristics of rapid plasticization, increased compatibility among materials of a system, excellent off-wheel film forming property and the like.
In a preferred embodiment, the carbon content of the nanographene is not less than 99wt.%, the sheet diameter is 1-10 μm, and the thickness is 2-3nm.
The nano graphene has the characteristics of high specific surface area, good electrical and thermal conductivity, easy dispersibility and the like, and is in a honeycomb lattice structure in a microscopic state.
In a preferred embodiment, the thickness of the transparent pressure-sensitive adhesive layer is 20-30 μm, and the transparent pressure-sensitive adhesive layer is a water-based acrylate pressure-sensitive adhesive and comprises the following components in percentage by mass: 40-70% of water; 30-60% of acrylic polymer; 0.5 to 1.3 percent of ammonium hydroxide; 0.2 to 1.0 percent of triethanolamine.
In a preferred embodiment, the release layer is silicon-coated release paper, and the gram weight is 120-140g/m 2 。
In a preferred embodiment, the thickness of the calendered PVC film is from 0.07 to 0.12mm.
The invention also provides an exemplary preparation method of the portable transparent electric-conduction heat-conduction protective film, which comprises the following steps:
s1, weighing the components according to the corresponding weight parts of the components of the PVC calendered film, and uniformly mixing the nano graphene and the high polymer polyester plasticizer to obtain a first mixture.
And uniformly mixing the first mixture with PVC resin, a powdery calcium zinc stabilizer and an acrylate processing aid to obtain a second mixture.
And banburying the second mixture to obtain a preplasticized melt, and then carrying out open milling, extrusion and calendering on the melt to obtain the PVC calendered film with the first network structure inside.
And S2, forming a grid pattern with a hexagonal space network structure on the surface of the film by adopting a printing roller with the grid pattern, wherein as shown in figure 4, the rectangle is a PVC film, and the hexagonal black grid structure is a coating and printing area.
And then coating the water-based acrylate containing the nano silver wires on one surface of the PVC calendered film obtained in the step S1 in a gravure printing mode, so as to form a transparent conductive coating with a second net structure on the surface of the PVC calendered film.
The first reticular structure inside the PVC calendering film and the second reticular structure on the surface of the PVC calendering film form an electric and heat conducting spatial network structure.
And S3, coating a transparent pressure-sensitive adhesive layer on the other side of the PVC calendered film obtained in the step S2, and then coating release paper on the transparent pressure-sensitive adhesive layer for lamination.
In a preferred embodiment, in the step S1, a pneumatic ink agitator is adopted to sufficiently agitate for 8-12min at a speed of 600-800rpm, so as to obtain a first mixture; and fully stirring the mixture for 3 to 5min by adopting a high-speed stirrer at the speed of 1200 to 1500rpm to obtain a second mixture.
In a preferred embodiment, in step S1, the banburying, roll mixing, extruding and rolling process includes:
the banburying conditions are as follows: the rotating speed of the rotor is 50-60rpm, and the loading current of the motor is 200-600A;
the open mill conditions are as follows: the temperature is 155-170 ℃, and the rotating speed is 20-30rpm;
the extrusion conditions were: the temperature is 160-175 ℃, and the single screw rotating speed is 20-28rpm;
the conditions of calendering were: the temperature of the four-roll calender is set as R1 along the feeding to the discharging direction in sequence: 170 ℃ -180 ℃, R2: 170-180 ℃, R3: 175-185 ℃, R4: 155-165 ℃;
the rotating speed of the four-roller calender is set as R1 along the feeding direction to the discharging direction in sequence: 14-24rpm, R2:18-30rpm, R3, 22-30rpm, R4:35-50rpm.
In step S2, the printing conditions are: printing speed: 40-60m/min, the temperature of the heating blast oven is 30-60 ℃, and the air volume is 2500-4500m 3 And h, drying.
In other preferred embodiments, the PVC calendered film is pre-dried at the temperature of 85-90 ℃ for 8-12min, then the film is compounded with release paper while being glued, the glue coating speed of the film is 30-35m/min, and after the glue is coated, the film is cured at the temperature of 60-70 ℃ for 36-48h.
The invention is further illustrated by the following examples. The materials in the examples are prepared according to known methods or are directly commercially available, unless otherwise specified.
The following examples used starting materials including:
the PVC resin is from HS-1300 type PVC resin of Suzhou Huasu plastics Limited company;
the adipate polyester plasticizer is derived from a W-8000 type plasticizer of Zhang Jia hong Di ai Biochemical engineering Co., ltd;
the powder calcium zinc stabilizer is derived from 1921-8 type stabilizer of Dongguan static environment-friendly new material company;
the acrylate processing aid is derived from a Brillouin chemical PA40 type acrylate processing aid;
the nano-graphene is derived from Xianfeng nano 103766 type small-particle-size thin-layer graphene nanosheets;
the conductive coating is derived from the conductive coating of Jiangsu Nayda photoelectric technology limited company; and
transparent water-based acrylate pressure-sensitive adhesive is 3M from 3M company TM Fastbond TM 4224-NF。
The processing equipment used in the following examples included:
a calender: the number of the IHIs is increased,
Figure BDA0003809985180000071
a rubberized fabric machine;
an internal mixer: taishengjing machines industries GmbH, V-IM-0760;
the stirrer: taiwan zhengda iron works, ltd, 300L;
an extrusion filter: a Yangtng mechanical industry Co., ltd,
Figure BDA0003809985180000072
a filter;
an open mill: the Taishengjing industries, inc.,
Figure BDA0003809985180000073
molding;
a middle rolling machine: somatec, ATW-800/2400I;
printing equipment, namely an FR100ELS printing machine (with an electric hot blast drying box) of northern Shanxi; and
coating equipment: shanxi Bei CL150 coater.
Example 1
100 parts of PVC resin; 40 parts of a high-molecular polyester plasticizer; 2 parts of a powder calcium zinc stabilizer; 0.4 part of nano graphene; 2 parts of acrylate processing aid, and under the condition of 40 ℃, the nano-graphene is placed in an adipate polyester plasticizer and is fully stirred for 10min at the speed of 600rpm by a pneumatic ink stirrer, so that the nano-graphene is fully and uniformly dispersed in the plasticizer. Then, the PVC resin, the plasticizer, the stabilizer and the processing aid are fully stirred in a high-speed stirrer at the speed of 1300rpm for 4min to obtain a mixture with uniform components.
And mixing the mixture in an internal mixer for 2min to obtain a preplasticized melt, passing the melt through an open mill, an extruder and a four-roll calender to obtain the PVC film with the thickness of about 0.07 mm.
Wherein, the banburying conditions are as follows: the rotating speed of a rotor is 50rpm, the current is loaded to a motor by 400A, and the mixing time is 2min;
the open mill conditions are as follows: the temperature is 160 ℃, and the rotating speed is 26.2rpm;
the extrusion conditions were: the temperature is 170 ℃, the single screw rotating speed is 25rpm;
the conditions of calendering were: the temperature of the four-roller calender is set as R1 along the feeding to the discharging direction in sequence: 173 ℃, R2: 173 ℃, R3:175 ℃, R4:162 ℃; the rotating speed of the four-roller calender is set as R1 along the feeding direction to the discharging direction in sequence: 19rpm, R2:22.8rpm, R3, R4:43.1rpm.
A printing roller with hexagonal network grains on the surface is prepared by a roller manufacturer in advance through carving, then the conductive coating is coated on the surface of the PVC film in a gravure printing mode, a printing film with hexagonal network grains is formed on the surface of the PVC film, and the nano silver conductive coating is only attached to the hexagonal grains.
Wherein, the printing speed: 60m/min, and the temperature of a rear-section oven is 4000m at 50 DEG C 3 Drying by air flow for h, and finally winding.
Pre-drying the PVC film at 85 ℃ for 8min, then coating glue, wherein the glue coating speed of the film is 35m/min, compounding the film with release paper while coating the glue, curing at 65 ℃ for 36h after coating the glue, and obtaining the self-adhesive PVC film with the glue layer thickness of 20 microns.
Example 2
100 parts of PVC resin; 30 parts of a high-molecular polyester plasticizer; 2.5 parts of powder calcium zinc stabilizer; 1 part of nano graphene; 2.5 parts of acrylate processing aid, and the nano-graphene is placed in an adipate polyester plasticizer and fully stirred for 10min at the speed of 800rpm by a pneumatic ink stirrer at the temperature of 45 ℃ so that the nano-graphene is fully and uniformly dispersed in the plasticizer. Then the PVC resin, the plasticizer, the stabilizer and the processing aid are fully stirred in a high-speed stirrer at 1440rpm for 4.5min to obtain a mixture with uniform components.
And mixing the mixture in an internal mixer for 2.5min to obtain a preplasticized melt, passing the melt through an open mill, an extruder and a four-roll calender to obtain the PVC film with the thickness of about 0.10 mm.
Wherein, the banburying conditions are as follows: the rotating speed of a rotor is 52rpm, the motor loads current 420A, and the mixing time is 2.5min;
the open mill conditions are as follows: the temperature is 163 ℃ and the rotating speed is 26.5rpm;
the extrusion conditions were: the temperature is 172 ℃, and the single screw rotating speed is 27rpm;
the conditions of calendering were: the temperature of the four-roll calender is set as R1 along the feeding to the discharging direction in turn: 176 ℃, R2:177 ℃, R3:180 ℃, R4:165 ℃; the rotating speed of the four-roller calender is set as R1 along the feeding direction to the discharging direction in sequence: 21.2rpm, R2:23.4rpm, R3, 29.1rpm, R4:45.0rpm.
A printing roller with hexagonal network grains on the surface is prepared by a roller manufacturer in advance through carving, then the conductive coating is coated on the surface of the PVC film in a gravure printing mode, a printing film with hexagonal network grains is formed on the surface of the PVC film, and the nano silver conductive coating is only attached to the hexagonal grains.
Wherein, the printing speed: 55m/min, and the temperature of a rear-section oven is 4000m at 57 DEG C 3 Drying by air volume for h, and finally winding.
Pre-drying the PVC film at 88 ℃ for 10min, then coating glue, wherein the glue coating speed of the film is 30m/min, the film is compounded with release paper while coating the glue, and after the glue is coated, curing is carried out at 60 ℃ for 48h, thus obtaining the self-adhesive PVC film with the glue layer thickness of 30 microns.
Example 3
100 parts of PVC resin; 28 parts of a high-molecular polyester plasticizer; 3 parts of a powder calcium zinc stabilizer; 0.6 part of nano graphene; 4 parts of acrylate processing aid, and placing the nano-graphene in an adipate polyester plasticizer at 40 ℃ and fully stirring for 10min at the speed of 700rpm by using a pneumatic ink stirrer so as to fully and uniformly disperse the nano-graphene in the plasticizer. Then, the PVC resin, the plasticizer, the stabilizer and the processing aid were sufficiently stirred in a high-speed stirrer at 1350rpm for 4min to obtain a mixture with uniform components.
And (3) mixing the mixture in an internal mixer for 3.5min to obtain a preplasticized melt, passing the melt through an open mill, an extruder and finally a four-roll calender to obtain the PVC film with the thickness of about 0.12mm.
Wherein, the banburying conditions are as follows: the rotation speed of a rotor is 55rpm, the motor loads current 480A, and the mixing time is 3.5min;
the open mill conditions are as follows: the temperature is 165 ℃, and the rotating speed is 27.2rpm;
the extrusion conditions were: the temperature is 175 ℃, and the single-screw rotating speed is 29rpm;
the conditions of calendering were: the temperature of the four-roller calender is set as R1 along the feeding to the discharging direction in sequence: 178 ℃, R2: 178 ℃, R3:183 ℃, R4:167 deg.C; the rotating speed of the four-roller calender is set as R1 along the feeding direction to the discharging direction in sequence: 18.5rpm, R2:21.4rpm, R3, 26.8rpm, R4:41.2rpm.
The printing roller with hexagonal network grains on the surface is prepared by a roller manufacturer in advance through engraving, then the conductive coating is coated on the surface of the PVC film in a gravure printing mode, a printing film with hexagonal network grains is formed on the surface of the PVC film, and the nano silver conductive coating is only attached to the hexagonal grains.
Wherein, the printing speed: 45m/min, and 4000m at 60 ℃ in a rear-section oven 3 Drying by air volume for h, and finally winding.
Pre-drying the PVC film at the temperature of 90 ℃ for 12min, then coating glue, wherein the glue coating speed of the film is 32m/min, compounding the film with release paper while coating the glue, curing at the temperature of 67 ℃ for 48h after coating the glue, and obtaining the self-adhesive PVC film with the glue layer thickness of 30 microns.
Comparative example 1
PVC protective film in prior art
The raw materials adopted are：
The PVC resin is from HS-1300 type PVC resin of Suzhou Huasu plastics Limited company;
the adipate polyester plasticizer is derived from a W-8000 type plasticizer of Zhang Jia hong Di ai Biochemical engineering Co., ltd;
the powder calcium zinc stabilizer is derived from 1921-8 type stabilizers of Dongguan static environment-friendly new materials Co.Ltd;
the acrylate processing aid is derived from a Brillouin chemical PA40 type acrylate aid;
the surfactant type short-acting antistatic agent is an SAS93 type antistatic agent from Clarian chemical engineering (China) Limited company.
Preparation process
100 parts of PVC resin; 40 parts of a high-molecular polyester plasticizer; 2 parts of a powder calcium zinc stabilizer; 0.5 part of antistatic agent; 2 parts of acrylate processing aid. The PVC resin, the plasticizer, the stabilizer, the antistatic agent and the processing aid are fully stirred in a high-speed stirrer at the speed of 1300rpm for 4min to obtain a mixture with uniform components.
And mixing the mixture in an internal mixer for 2min to obtain a preplasticized melt, passing the melt through an open mill, an extruder and a four-roll calender to obtain the PVC film with the thickness of about 0.07 mm.
Wherein, the banburying conditions are as follows: the rotating speed of a rotor is 50rpm, the current is loaded to a motor by 400A, and the mixing time is 2min;
the open mill conditions are as follows: the temperature is 160 ℃, and the rotating speed is 26.2rpm;
the extrusion conditions were: the temperature is 170 ℃, and the single screw rotating speed is 25rpm;
the conditions of calendering are as follows: the temperature of the four-roller calender is set as R1 along the feeding to the discharging direction in sequence: 173 ℃, R2: 173 ℃, R3:175 ℃, R4:162 ℃; the rotating speed of the four-roller calender is set as R1 along the feeding direction to the discharging direction in sequence: 19rpm, R2:22.8rpm, R3, R4:43.1rpm.
Performance testing
The protective films obtained in example 1 and comparative example 1 were used for transparency, electrical conductivity and thermal conductivity tests, and specific test standards and results are shown in the following table
Figure BDA0003809985180000101
From the above test results, it can be seen that the transparency of the protection of the present invention is better, approaching that of a transparent material (greater than 85% being transparent material).
Excellent conductivity, general surface resistance is more than or equal to 10 11 ohm/sq is insulating material, surface resistance 10 3 -10 5 ohm/sq is conductive material, 10 6 -10 10 ohm/sq is antistatic material, and it can be seen that the protective film of the invention is conductive and has long-lasting conductivity.
The high polymer material has poor heat conducting performance, the heat conducting coefficient is usually less than 0.3 w/(m.K), the heat conducting coefficient is less than 0.2 w/(m.K), the heat insulating material is prepared, and the heat conducting coefficient of the protective film reaches 12 w/(m.K), so that the protective film has excellent heat conducting performance.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, the protection scope of the present invention should be determined by the appended claims.

Claims (11)

1. The convenient transparent electric conduction and heat conduction protective film is characterized by comprising a release layer, a transparent pressure-sensitive adhesive layer and a transparent thin film layer, wherein the release layer, the transparent pressure-sensitive adhesive layer and the transparent thin film layer are sequentially and adjacently arranged from bottom to top;
the transparent film layer is a PVC calendered film and comprises the following components in parts by weight: 100 parts of PVC resin; 25-40 parts of a high-molecular polyester plasticizer; 2-4 parts of a powder calcium zinc stabilizer; 0.3-1 part of nano graphene; 1-4 parts of acrylate processing aid;
the nano graphene is uniformly dispersed in the PVC calendered film to form a first reticular structure, and the transparent conductive coating on the surface of the PVC calendered film has a second reticular structure;
the first reticular structure inside the PVC calendering film and the second reticular structure on the surface of the PVC calendering film form an electric and heat conducting space network structure.
2. The portable transparent electric and thermal conductive protective film according to claim 1, wherein the thickness of the electric conductive coating is 10-15 μm, and the portable transparent electric and thermal conductive protective film comprises the following components in percentage by mass: 25-35% of water-based acrylic resin; 50-70% of water-based acrylic emulsion; 4-8% of a defoaming agent; 8-13% of absolute ethyl alcohol; 6-10% of wetting dispersant; 2-5% of nano silver wires.
3. The portable transparent conductive film according to claim 1, wherein the nanosilver wire is a linear nanostructure with a diameter of 30-40 nm.
4. The portable transparent conductive protective film according to claim 1, wherein the degree of polymerization of the PVC resin is 1300, and the polymer polyester plasticizer is adipate polyester.
5. The portable transparent electric and thermal conductive protective film according to claim 1, wherein the carbon content of the nanographene is not less than 99wt.%, the sheet diameter is 1-10 μm, and the thickness is 2-3nm.
6. The portable transparent electric-conduction heat-conduction protective film according to claim 1, wherein the thickness of the transparent pressure-sensitive adhesive layer is 20-30 μm, and the transparent pressure-sensitive adhesive layer is a water-based acrylate pressure-sensitive adhesive and comprises the following components in percentage by mass: 40-70% of water; 30-60% of acrylic polymer; 0.5 to 1.3 percent of ammonium hydroxide; 0.2 to 1.0 percent of triethanolamine.
7. The portable transparent electric and thermal conductive protective film according to claim 1, wherein the release layer is a silicon-coated release paper with a gram weight of 120-140g/m 2 。
8. The portable transparent conductive protective film according to claim 1, wherein the thickness of the PVC calendered film is 0.07-0.12mm.
9. The preparation method of the portable transparent electric, heat and conductive protective film according to any one of claims 1 to 7, characterized by comprising the following steps:
s1, weighing the components in corresponding weight according to the weight parts of the components of the PVC calendered film, and uniformly mixing the nano graphene and the high-molecular polyester plasticizer to obtain a first mixture;
uniformly mixing the first mixture with PVC resin, a powdery calcium zinc stabilizer and an acrylate processing aid to obtain a second mixture;
banburying the second mixture to obtain a preplasticized melt, and then carrying out open milling, extrusion and calendering on the melt to obtain a PVC calendering film with a first net-shaped structure inside;
s2, coating the water-based acrylate containing the nano silver wires on one surface of the PVC calendered film obtained in the step S1 in a gravure printing mode by adopting a printing roller with reticular lines, so that a transparent conductive coating with a second reticular structure is formed on the surface of the PVC calendered film;
the first reticular structure inside the PVC calendering film and the second reticular structure on the surface of the PVC calendering film form an electric and heat conducting space network structure;
and S3, coating a transparent pressure-sensitive adhesive layer on the other side of the PVC calendered film obtained in the step S2, and then coating release paper on the transparent pressure-sensitive adhesive layer for lamination.
10. The method according to claim 8, wherein in the step S1, a pneumatic ink mixer is used to fully mix the mixture at a speed of 600-800rpm for 8-12min to obtain a first mixture; stirring with high speed stirrer at 1200-1500rpm for 3-5min to obtain second mixture.
11. The production method according to claim 8, wherein in the step S1,
the banburying conditions are as follows: the rotating speed of the rotor is 50-60rpm, and the loading current of the motor is 200-600A;
the open mill conditions are as follows: the temperature is 155-170 ℃, and the rotating speed is 20-30rpm;
the extrusion conditions were: the temperature is 160-175 ℃, and the single screw rotating speed is 20-28rpm;
the conditions of calendering were: the temperature of the four-roll calender is set as R1 along the feeding to the discharging direction in sequence: 170 ℃ -180 ℃, R2: 170-180 ℃, R3: 175-185 ℃, R4: 155-165 ℃;
the rotating speed of the four-roller calender is set as R1 along the feeding direction to the discharging direction in sequence: 14-24rpm, R2:18-30rpm, R3, 22-30rpm, R4:35-50rpm;
in step S2, the printing conditions are: printing speed: 40-60m/min, the temperature of the heating blast oven is 30-60 ℃, and the air volume is 2500-4500m 3 And h, drying.
CN202211010014.2A 2022-08-22 2022-08-22 Portable transparent electric-conduction heat-conduction protective film and preparation method thereof Pending CN115491137A (en)

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Citations (4)

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Publication number Priority date Publication date Assignee Title
CN103642155A (en) * 2013-11-29 2014-03-19 中国科学院金属研究所 Composite conductive film taking graphene as conductive agent and preparation method of composite conductive film
CN106519947A (en) * 2016-12-30 2017-03-22 苏州科立盈胶粘材料有限公司 Transparent antistatic coating on basis of graphene materials, antistatic functional membrane and method for preparing same
CN111161906A (en) * 2020-01-19 2020-05-15 惠州达祺光电科技有限公司 Low-resistance transparent conductive film and preparation method thereof
CN111647366A (en) * 2020-06-03 2020-09-11 江苏久茂精密电子科技有限公司 Anti-static protective film for electronic product packaging and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103642155A (en) * 2013-11-29 2014-03-19 中国科学院金属研究所 Composite conductive film taking graphene as conductive agent and preparation method of composite conductive film
CN106519947A (en) * 2016-12-30 2017-03-22 苏州科立盈胶粘材料有限公司 Transparent antistatic coating on basis of graphene materials, antistatic functional membrane and method for preparing same
CN111161906A (en) * 2020-01-19 2020-05-15 惠州达祺光电科技有限公司 Low-resistance transparent conductive film and preparation method thereof
CN111647366A (en) * 2020-06-03 2020-09-11 江苏久茂精密电子科技有限公司 Anti-static protective film for electronic product packaging and preparation method thereof

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