CN111688316A - Graphene multilayer composite heat insulation film and preparation method and application thereof - Google Patents

Graphene multilayer composite heat insulation film and preparation method and application thereof Download PDF

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CN111688316A
CN111688316A CN202010722957.2A CN202010722957A CN111688316A CN 111688316 A CN111688316 A CN 111688316A CN 202010722957 A CN202010722957 A CN 202010722957A CN 111688316 A CN111688316 A CN 111688316A
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graphene
multilayer composite
layer
heat insulation
film
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常海欣
李刚辉
郭辉
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Wuhan Lianwei New Materials Technology Co ltd
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Wuhan Lianwei New Materials Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
    • 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
    • B32B27/322—Layered products comprising a layer of synthetic resin comprising polyolefins comprising halogenated polyolefins, e.g. PTFE
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/40—Layered products comprising a layer of synthetic resin comprising polyurethanes
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    • 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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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
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    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/164—Drying
    • 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
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09D133/04—Homopolymers or copolymers of esters
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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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
    • E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
    • E04B1/62—Insulation or other protection; Elements or use of specified material therefor
    • E04B1/74—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
    • E04B1/76—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to heat only
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F15/00—Flooring
    • E04F15/18—Separately-laid insulating layers; Other additional insulating measures; Floating floors
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/24—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer not being coherent before laminating, e.g. made up from granular material sprinkled onto a substrate
    • B32B2037/243—Coating
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/20—Inorganic coating
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/26—Polymeric coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/304—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/718—Weight, e.g. weight per square meter

Abstract

The invention discloses a graphene multilayer composite heat insulation film and a preparation method and application thereof, and belongs to the technical field of heat insulation films or heating films. The graphene multilayer composite heat insulation film comprises a graphene layer, a flexible polymer film layer, a silica sol layer and a glass fiber reinforced silica aerogel layer which are sequentially arranged from top to bottom. According to the invention, graphene slurry prepared from graphene is organically combined with the existing glass fiber reinforced silica aerogel heat insulation material, and the excellent thermal and mechanical properties of graphene are used for enhancing the external heat insulation and the strength of the heat insulation film, so that the advantages of the two materials are exerted to the maximum extent. In addition, the left and right ends of the graphene layer in the graphene multilayer composite heat-insulating film can be used as a graphene electrothermal film after being connected with copper sheet electrodes, and the obtained electrothermal film has uniform heating, low use voltage and good electrothermal performance, and can be widely applied to living fields of heating floors, building heating, far infrared health care and medical treatment and the like.

Description

Graphene multilayer composite heat insulation film and preparation method and application thereof
Technical Field
The invention belongs to the technical field of heat insulation films or heating films, and particularly relates to a graphene multilayer composite heat insulation film and a preparation method and application thereof.
Background
The domestic economy is rapidly increased, and various constructions obtain huge achievements and simultaneously have the problems of energy waste, low energy use efficiency and the like. The energy consumption of the building (including air-conditioning heating, refrigerating, living energy consumption, construction energy consumption and the like) accounts for 1/3 of the total energy consumption of China, and the energy consumption of the air-conditioning refrigerating and heating accounts for 20% of the total energy consumption. Besides the reasons of the equipment, the energy-saving design scheme is not adopted by the building and the energy consumption is increased due to the poor performance of the heat insulation material.
Although there are many heat-insulating and heat-preserving building materials on the market at present, the materials with better heat-insulating, flame-retardant and fireproof performances are expensive, and some manufacturers seek to save cost, so that the produced heat-insulating building materials have poorer heat-insulating, flame-retardant, fireproof, mechanical and other performances.
In recent years, graphene has been greatly developed due to its excellent optical, electrical, thermal, mechanical and other properties, and the production cost thereof is continuously reduced, so that it is necessary to develop a graphene thermal insulation material with relatively low price and good performance.
The electric heating film is used as a heating material with infinite potential, is widely applied to living fields such as building heating, heating floors, far infrared health care rooms and the like, and industrial fields such as paint baking rooms, drying rooms and the like, and the electric heating body used by the current electric heating material basically adopts metal wires or powder materials such as graphite, carbon powder, conductive carbon black, carbon fiber and the like, so that the electric heating conversion efficiency is low; for a large number of used metal wire heating bodies, due to the oxidation effect of the metal wires at high temperature, the phenomena of oxidation corrosion, energy consumption increase and the like are easily generated, the service life is short, and unsafe problems of electric leakage, combustion and the like are easily generated when 220V alternating current is used in the field of home.
The present application has been made for the above reasons.
Disclosure of Invention
The invention aims to overcome the defects or shortcomings of thermal insulation films in the prior art in the aspects of mechanical strength, fire resistance, water resistance, moisture resistance and the like, and provides a graphene multilayer composite thermal insulation film and a preparation method and application thereof. The graphene multilayer composite heat-insulating film is a multilayer structure constructed by utilizing the existing raw materials and graphene layers, and has the functions of high-performance heating, heat insulation and heat preservation.
The left end and the right end of the graphene layer in the graphene multilayer composite film are provided with the conductive electrodes, so that the graphene electrothermal film can be obtained. The graphene electrothermal film reduces heat loss while realizing a heating function, greatly improves the use efficiency of the electric heating, is safe and effective, saves energy and protects environment, and can be widely applied to living fields such as heating floors, building heating, far infrared health care and medical treatment and the like.
In order to achieve the first object of the present invention, the present invention adopts the following technical solutions:
the utility model provides a compound thermal-insulated membrane of graphite alkene multilayer, includes from last to down graphite alkene layer, flexible polymer membrane layer, silica sol layer and the glass fiber reinforcing silica aerogel layer that sets gradually.
Further, according to the technical scheme, the thickness of the graphene layer is 10-100 μm, and preferably 30-100 μm.
Further, according to the technical scheme, the thickness of the flexible polymer film layer is 80-120 microns, the thickness of the silica sol layer is 5-10 microns, and the thickness of the glass fiber reinforced silica aerogel layer is 0.2-0.5 cm.
Further, in the above technical scheme, the flexible polymer film layer is made of a composite material of any one or more of Polyimide (PI), polyethylene terephthalate (PET), polyvinyl chloride (PVC), Polyamide (PA) and Polyurethane (PU).
The second objective of the present invention is to provide a method for preparing the graphene multilayer composite thermal insulation film, which specifically comprises the following steps:
(1) uniformly mixing graphene powder, water-soluble resin, a defoaming agent, a flatting agent and a film-forming assistant according to a ratio to obtain graphene slurry for later use;
(2) coating the graphene slurry obtained in the step (1) on the surface of a flexible polymer film, and then drying to form a graphene layer;
(3) and (3) bonding the flexible polymer film with the graphene layer coated on the surface, which is obtained in the step (2), with glass fiber reinforced silica aerogel by using a silica sol binder, and drying to obtain the graphene multilayer composite heat insulation film.
Further, according to the technical scheme, the mass of the graphene powder in the step (1) is 0.5-13% of the mass of the water-soluble resin.
Further, in the above technical solution, the water-soluble resin in the step (1) is used as a binder, so as to adhere graphene in the graphene slurry to the surface of the flexible polymer film. The water-soluble resin is one or more of water-based acrylic resin, water-based epoxy resin, water-based acrylic modified epoxy resin, water-based polyurethane, water-based amino resin and water-soluble phenolic resin.
Further, in the above technical solution, the defoaming agent in the step (1) functions to suppress the generation of foam or eliminate foam already generated by reducing the surface tension. The defoaming agent is an organosiloxane defoaming agent. For example, the defoamer can be BYK024, TEGO Airex902W, and the like.
Further, according to the technical scheme, the mass of the defoaming agent in the step (1) is 0.3-1% of the mass of the water-soluble resin.
Further, according to the technical scheme, the leveling agent in the step (1) has the function of promoting the slurry to form a uniform, flat and smooth film layer in the drying and film forming process. The leveling agent is an organic silicon leveling agent. For example, the leveling agent may be polydimethylsiloxane, polymethylphenylsiloxane, or the like.
Further, according to the technical scheme, the mass of the leveling agent in the step (1) is 0.5-1.5% of the mass of the water-soluble resin.
Further, in the above technical solution, the film forming aid in the step (1) plays a role of plasticization in the film forming process. The film-forming assistant is any one of benzyl alcohol, ethylene glycol butyl ether, dodecyl alcohol ester, propylene glycol phenyl ether and the like.
Further, according to the technical scheme, the mass of the film-forming assistant in the step (1) is 0.5-1% of that of the water-soluble resin.
Further, in the above technical solution, the coating manner in the step (2) is preferably spray coating or roll coating. The invention has no special requirements on the specific implementation modes of the spraying and the rolling, and the technology well known by the technical personnel in the field is adopted to realize the uniform distribution of the graphene slurry on the surface of the flexible polymer film.
Further, in the above technical scheme, the drying manner in the step (2) is not particularly limited, so that the graphene coating can be completely dried to form a uniformly dispersed single graphene layer. For example, the drying method may be any of vacuum drying, infrared drying, freeze drying, and the like.
Further, in the above technical solution, the drying manner in the step (3) is not particularly limited, so as to achieve complete drying and curing of the silica sol coating. For example, the drying method may be any of vacuum drying, infrared drying, and freeze drying.
The third purpose of the invention is to provide the application of the graphene multilayer composite heat insulation film, which can be used for preparing a graphene electrothermal film.
The utility model provides a graphite alkene electric heat membrane, includes above-mentioned graphite alkene multilayer composite heat insulating film and conductive electrode, conductive electrode sets up graphite alkene multilayer composite heat insulating film's both ends of layer of graphite alkene.
Compared with the prior art, the invention has the following beneficial effects:
(1) compared with the traditional heat insulation film, the graphene multilayer composite heat insulation film disclosed by the invention has the advantages of being light and thin in material, capable of being provided with back glue, simple and convenient to install, non-toxic and odorless, and meanwhile, the problems that the traditional heat insulation film is not damp-proof, waterproof, fireproof, tensile and poor in supporting performance, is easy to generate light pollution and the like are greatly improved.
(2) According to the invention, graphene slurry prepared from graphene is organically combined with the existing glass fiber reinforced silica aerogel heat insulation material, and the excellent thermal and mechanical properties of graphene are used for enhancing the external heat insulation and the strength of the heat insulation film, so that the advantages of the two materials are exerted to the maximum extent.
(3) The preparation method is green and environment-friendly, the equipment and the process are simple and feasible, and the industrial production is easy to realize.
(4) The graphene electrothermal film can be used after copper sheet electrodes are respectively connected with the left end and the right end of the graphene layer (conducting layer) of the graphene multilayer composite heat insulation film, and the obtained electrothermal film has uniform heating, low use voltage and good electrothermal performance.
(5) The graphene electrothermal film prepared by the invention is simple to prepare and easy to process, and can be widely applied to living fields of heating floors, building heating, far infrared health care and medical treatment and the like.
Drawings
Fig. 1 is a schematic structural view of a graphene multilayer composite thermal insulation film according to the present invention; wherein: 1 is a glass fiber reinforced silica aerogel layer; 2 is a silica sol layer; 3 is a flexible polymer film layer; and 4 is a graphene layer.
FIG. 2 is a schematic view of the experimental apparatus for grilling.
Fig. 3 is a stress-strain curve of the graphene multilayer composite thermal insulation film prepared in example 1 of the present invention;
fig. 4 is a stress-strain curve of the graphene multilayer composite thermal insulation film prepared in example 2 of the present invention;
fig. 5 is a stress-strain curve of the graphene multilayer composite thermal insulation film prepared in example 3 of the present invention;
fig. 6 is a stress-strain curve of the graphene multilayer composite thermal insulation film prepared in example 4 of the present invention.
Detailed Description
The present invention will be described in further detail below with reference to examples. The present invention is implemented on the premise of the technology of the present invention, and the detailed embodiments and specific procedures are given to illustrate the inventive aspects of the present invention, but the scope of the present invention is not limited to the following embodiments.
Various modifications to the precise description of the invention will be readily apparent to those skilled in the art from the information contained herein without departing from the spirit and scope of the appended claims. It is to be understood that the scope of the invention is not limited to the procedures, properties, or components defined, as these embodiments, as well as others described, are intended to be merely illustrative of particular aspects of the invention. Indeed, various modifications of the embodiments of the invention which are obvious to those skilled in the art or related fields are intended to be covered by the scope of the appended claims.
For a better understanding of the invention, and not as a limitation on the scope thereof, all numbers expressing quantities, percentages, and other numerical values used in this application are to be understood as being modified in all instances by the term "about". At the very least, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
The test methods used in the following examples are all conventional methods unless otherwise specified; the raw materials and reagents used are, unless otherwise specified, those commercially available from ordinary commercial sources. Wherein: the glass fiber reinforced silica aerogel is purchased from Shenzhen Zhongji science and technology Limited.
Example 1
The graphene multilayer composite heat insulation film comprises a graphene layer, a flexible polymer film layer, a silica sol layer and a glass fiber reinforced silica aerogel layer which are sequentially arranged from top to bottom; wherein:
the flexible polymer film is a PET film;
the thickness of graphite alkene layer is 30 μm, the thickness of flexible polymer membranous layer is 80 μm, the silica sol layer thickness is 5 μm, the thickness of glass fiber reinforced silica aerogel layer is 0.2 cm.
The graphene multilayer composite heat insulation film is prepared by the following method, and the method comprises the following steps:
(1) 0.2g of graphene powder was added to 40g of aqueous acrylic resin and mechanically stirred at 1200 rpm for 30 minutes. After uniformly mixing the graphene and the water-based acrylic resin, sequentially adding 0.12g of TEGOAirex902W (Germany Digao auxiliary agent) defoaming agent, 0.2g of polymethyl phenyl siloxane flatting agent and 0.2g of film-forming auxiliary agent ethylene glycol butyl ether into the obtained mixed solution, and then stirring for 1-2 hours again to uniformly mix the components to obtain the graphene slurry.
(2) And (2) spraying the graphene slurry obtained in the step (1) to the surface of a PET film with the thickness of 80 microns by using a pneumatic spray gun, transferring the PET film with the graphene slurry sprayed on the surface into an oven, and baking for 2 hours at the constant temperature of 100 ℃ to obtain a graphene layer with the thickness of 30 microns.
(3) And (3) bonding the PET film coated with the graphene layer on the surface obtained in the step (2) with glass fiber reinforced silica aerogel by using a silica sol binder, and then drying for 2h at the temperature of 80 ℃ to obtain the graphene multilayer composite heat insulation film.
Example 2
The graphene multilayer composite heat insulation film comprises a graphene layer, a flexible polymer film layer, a silica sol layer and a glass fiber reinforced silica aerogel layer which are sequentially arranged from top to bottom; wherein:
the flexible polymer film adopts a PI film;
the thickness of graphite alkene layer is 50 μm, the thickness of flexible polymer membranous layer is 100 μm, the silica sol layer thickness is 8 μm, the thickness of glass fiber reinforced silica aerogel layer is 0.4 cm.
The graphene multilayer composite heat insulation film is prepared by the following method, and the method comprises the following steps:
(1) 5.2g of graphene powder was added to 40g of aqueous epoxy resin and mechanically stirred at 1200 rpm for 30 minutes. After graphene and water-based epoxy resin are uniformly mixed, 0.4g of defoaming agent BYK-024 (Germany Bikk chemical, belonging to organosilicone defoaming agent), 0.6g of polydimethylsiloxane leveling agent and 0.4g of film-forming aid benzyl alcohol are sequentially added into the obtained mixed solution, and the mixture is stirred for 1-2 hours again to uniformly mix the components to obtain graphene slurry.
(2) Spraying the graphene slurry obtained in the step (1) to the surface of a PI film with the thickness of 100 microns by using a pneumatic spray gun, transferring the PI film with the graphene slurry sprayed on the surface into an oven, and baking for 2 hours at the constant temperature of 100 ℃ to obtain a graphene layer with the thickness of 50 microns.
(3) And (3) bonding the PI film coated with the graphene layer on the surface and obtained in the step (2) with glass fiber reinforced silica aerogel by using a silica sol binder, and then drying at 80 ℃ for 2h to obtain the graphene multilayer composite heat insulation film.
Example 3
The graphene multilayer composite heat insulation film comprises a graphene layer, a flexible polymer film layer, a silica sol layer and a glass fiber reinforced silica aerogel layer which are sequentially arranged from top to bottom; wherein:
the flexible polymer film is a PVC film;
the thickness of graphene layer is 70 μm, the thickness of flexible polymer membrane layer is 100 μm, the thickness of silica sol layer is 10 μm, the thickness of glass fiber reinforced silica aerogel layer is 0.5 cm.
The graphene multilayer composite heat insulation film is prepared by the following method, and the method comprises the following steps:
(1) 2g of graphene powder is added into 40g of waterborne polyurethane and mechanically stirred for 30 minutes at the speed of 1200 rpm. After graphene and waterborne polyurethane are uniformly mixed, 0.16g of defoaming agent BYK-024 (Germany Bikk chemical, belonging to organosilicone defoaming agent), 0.32g of polydimethylsiloxane leveling agent and 0.28g of film-forming aid dodecyl alcohol ester are sequentially added into the obtained mixed solution, and the mixture is stirred for 1-2 hours again to uniformly mix the components to obtain graphene slurry.
(2) And (2) spraying the graphene slurry obtained in the step (1) to the surface of a PVC film with the thickness of 100 microns by using a pneumatic spray gun, transferring the PVC film with the graphene slurry sprayed on the surface into an oven, and baking for 2 hours at the constant temperature of 100 ℃ to obtain a graphene layer with the thickness of 70 microns.
(3) And (3) bonding the PVC film coated with the graphene layer on the surface and obtained in the step (2) with glass fiber reinforced silica aerogel by using a silica sol binder, and then drying for 2h at the temperature of 80 ℃ to obtain the graphene multilayer composite heat insulation film.
Example 4
The graphene multilayer composite heat insulation film comprises a graphene layer, a flexible polymer film layer, a silica sol layer and a glass fiber reinforced silica aerogel layer which are sequentially arranged from bottom to top; wherein:
the flexible polymer film is a PU film;
the thickness of the graphene layer is 100 micrometers, the thickness of the flexible polymer film layer is 120 micrometers, the thickness of the silica sol layer is 10 micrometers, and the thickness of the glass fiber reinforced silica aerogel layer is 0.5 cm.
The graphene multilayer composite heat insulation film is prepared by the following method, and the method comprises the following steps:
(1) 3.2g of graphene powder is added into 40g of water-soluble phenolic resin and mechanically stirred for 30 minutes at the speed of 1200 rpm. After graphene and water-soluble phenolic resin are uniformly mixed, 0.28g of TEGOAirex902W (Germany Di high auxiliary agent) defoaming agent, 0.4g of polymethyl phenyl siloxane flatting agent and 0.36g of film forming auxiliary agent propylene glycol phenyl ether are sequentially added into the obtained mixed solution, and then the mixture is stirred for 1-2 hours again, so that the components are uniformly mixed, and graphene slurry is obtained.
(2) And (2) spraying the graphene slurry obtained in the step (1) to the surface of a PU film with the thickness of 120 microns by using a pneumatic spray gun, transferring the PU film with the graphene slurry sprayed on the surface into an oven, and baking for 2 hours at the constant temperature of 100 ℃ to obtain the graphene layer with the thickness of 100 microns.
(3) And (3) bonding the PU film coated with the graphene layer on the surface obtained in the step (2) with glass fiber reinforced silica aerogel by using a silica sol binder, and then drying for 2h at the temperature of 80 ℃ to obtain the graphene multilayer composite heat insulation film.
Hydrophobic Performance test
Contact angle test: the method adopts an OCA15EC type video optical contact angle measuring instrument for measurement, and comprises the following steps:
dripping water drops on the surface of the graphene multilayer composite heat insulation film sample prepared in the embodiment 1-4, adjusting light, the focal length of a camera and the visual range, automatically calculating the contact angle value through an analyzer, and testing results are shown in table 1.
As can be seen from table 1, the contact angles of the graphene multilayer composite heat insulation films prepared in examples 1 to 4 are all greater than 90 °, which shows that the graphene multilayer composite heat insulation film material of the present invention has obvious hydrophobicity, i.e., has good waterproof and moistureproof properties.
Tensile Strength test
An AG-X plus type universal testing machine is adopted to carry out mechanical property test according to GB/T8489-.
As can be seen from fig. 3 to 6 and table 1, when the graphene multilayer composite thermal insulation films prepared in examples 1 to 4 are deformed by 10%, the stress thereof is 79.9 to 81.2MPa, which indicates that the graphene multilayer composite thermal insulation film material of the present invention has high tensile strength, strong tensile strength, and excellent mechanical properties.
Test for fire resistance
Roasting experiment: the fire resistance and safety of the graphene multilayer composite heat insulation film prepared in examples 1 to 4 were examined by an alcohol burner broil method. The method comprises the following specific steps: placing the heat insulation film in the air and roasting the heat insulation film on an alcohol lamp with the outer flame temperature of 500-600 ℃ for 30-60 minutes, wherein: the graphene layer faces the flame and is marked as the front; the silica aerogel layer was facing away from the flame and was reported as the back side and the test results are shown in table 1.
As can be seen from table 1, the back temperature of the graphene multilayer composite heat insulation films prepared in examples 1 to 4 is 40.5 to 45.7 ℃ in the whole roasting process, and the roasting back temperature is low, which indicates that the graphene multilayer composite heat insulation film material of the present invention has good heat insulation performance and good safety.
Table 1 is a comparison table of performance test results of graphene multilayer composite heat insulation films prepared in embodiments 1 to 4 of the present invention
Item Example 1 Example 2 Example 3 Example 4
Contact Angle/° 137 136 138 135
10% deformation/MPa 79.9 80.1 80.7 81.2
Roast back temperature/. degree.C 45.7 42.0 40.5 37.8
Note 1: the contact angle is characterized by hydrophobicity, and the larger the contact angle, the better the hydrophobicity, i.e. the better the moisture resistance.
Note 2: the 10% deformation is characterized by tensile strength, the higher the value, the stronger the tensile resistance.
Note 3: the roasting experiment represents the heat insulation and fire resistance of the material, and the lower the roasting back temperature is, the better the heat insulation performance of the material is and the better the safety is.
Application example 1
The copper sheet electrodes are connected to the left and right ends of the graphene layer in the graphene multilayer composite heat insulation film prepared in embodiment 1 of the invention, so that the graphene electrothermal film is prepared. The temperature rise time and the electrothermal radiation conversion efficiency of the graphene electrothermal film are tested according to the test standards of JG/T286-. The test results are shown in table 2.
Table 2 is a comparison table of the test results of the electric heating performance of the graphene electric heating film and the national standard electric heating film
Time of temperature rise Electric-thermal radiation conversion efficiency Service life test
National standard ＜10min >55％ >3 ten thousand hours
The invention ＜1min 75％ >6 ten thousand hours

Claims (10)

1. The utility model provides a compound thermal-insulated membrane of graphite alkene multilayer which characterized in that: comprises a graphene layer, a flexible polymer film layer, a silica sol layer and a glass fiber reinforced silica aerogel layer which are sequentially arranged from top to bottom.
2. The graphene multilayer composite thermal barrier film according to claim 1, wherein: the thickness of the graphene layer is 10-100 mu m.
3. The graphene multilayer composite thermal barrier film according to claim 1, wherein: the thickness of the flexible polymer film layer is 80-120 mu m, the thickness of the silica sol layer is 5-10 mu m, and the thickness of the glass fiber reinforced silica aerogel layer is 0.2-0.5 cm.
4. The graphene multilayer composite thermal barrier film according to claim 1, wherein: the flexible polymer film layer is made of one or more of polyimide, polyethylene terephthalate, polyvinyl chloride, polyamide and polyurethane.
5. The method for preparing the graphene multilayer composite heat insulation film according to claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
(1) uniformly mixing graphene powder, water-soluble resin, a defoaming agent, a flatting agent and a film-forming assistant according to a ratio to obtain graphene slurry for later use;
(2) coating the graphene slurry obtained in the step (1) on the surface of a flexible polymer film, and then drying to form a graphene layer;
(3) and (3) bonding the flexible polymer film with the graphene layer coated on the surface, which is obtained in the step (2), with glass fiber reinforced silica aerogel by using a silica sol binder, and drying to obtain the graphene multilayer composite heat insulation film.
6. The method for preparing the graphene multilayer composite heat insulation film according to claim 5, wherein: in the step (1), the mass of the graphene powder is 0.5-13% of the mass of the water-soluble resin, the mass of the defoaming agent is 0.3-1% of the mass of the water-soluble resin, the mass of the leveling agent is 0.5-1.5% of the mass of the water-soluble resin, and the mass of the film-forming assistant is 0.5-1% of the mass of the water-soluble resin.
7. The method for preparing the graphene multilayer composite heat insulation film according to claim 5, wherein: the water-soluble resin is one or more of water-based acrylic resin, water-based epoxy resin, water-based acrylic modified epoxy resin, water-based polyurethane, water-based amino resin and water-soluble phenolic resin.
8. The method for preparing the graphene multilayer composite heat insulation film according to claim 5, wherein: the film-forming assistant in the step (1) is any one of benzyl alcohol, ethylene glycol butyl ether, dodecyl alcohol ester and propylene glycol phenyl ether.
9. The application of the graphene multilayer composite heat insulation film as defined in claims 1-4 or the graphene multilayer composite heat insulation film prepared by the method as defined in claims 5-8 in preparing a graphene electrothermal film.
10. A graphite alkene electric heat membrane which characterized in that: the graphene multilayer composite thermal insulation film comprises the graphene multilayer composite thermal insulation film of claims 1 to 4 or the graphene multilayer composite thermal insulation film prepared by the method of claims 5 to 8 and conductive electrodes, wherein the conductive electrodes are arranged at two ends of a graphene layer in the graphene multilayer composite thermal insulation film.
CN202010722957.2A 2020-07-24 2020-07-24 Graphene multilayer composite heat insulation film and preparation method and application thereof Pending CN111688316A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110224376A1 (en) * 2010-03-15 2011-09-15 University Of Central Florida Research Foundation, Inc. Carbon nanotube or graphene-based aerogels
CN107097478A (en) * 2017-04-10 2017-08-29 佛山欧神诺陶瓷股份有限公司 A kind of Ceramic Tiles with heating function and preparation method thereof
GB201802899D0 (en) * 2018-02-22 2018-04-11 Graphene Composites Ltd Composite structure and method of manufacture
CN110603147A (en) * 2017-02-23 2019-12-20 格拉芬康普西斯有限公司 Composite structure and method of manufacture

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110224376A1 (en) * 2010-03-15 2011-09-15 University Of Central Florida Research Foundation, Inc. Carbon nanotube or graphene-based aerogels
CN110603147A (en) * 2017-02-23 2019-12-20 格拉芬康普西斯有限公司 Composite structure and method of manufacture
CN107097478A (en) * 2017-04-10 2017-08-29 佛山欧神诺陶瓷股份有限公司 A kind of Ceramic Tiles with heating function and preparation method thereof
GB201802899D0 (en) * 2018-02-22 2018-04-11 Graphene Composites Ltd Composite structure and method of manufacture

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Application publication date: 20200922