CN113248958A - Heat dissipation electrostatic adsorption powder and preparation method thereof - Google Patents
Heat dissipation electrostatic adsorption powder and preparation method thereof Download PDFInfo
- Publication number
- CN113248958A CN113248958A CN202110665381.5A CN202110665381A CN113248958A CN 113248958 A CN113248958 A CN 113248958A CN 202110665381 A CN202110665381 A CN 202110665381A CN 113248958 A CN113248958 A CN 113248958A
- Authority
- CN
- China
- Prior art keywords
- few
- electrostatic adsorption
- layer graphene
- heat dissipation
- adsorption powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- 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
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/02—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D123/10—Homopolymers or copolymers of propene
- C09D123/12—Polypropene
-
- 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
- C09D127/00—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 a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/04—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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C09D127/06—Homopolymers or copolymers of vinyl chloride
-
- 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
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/10—Homopolymers or copolymers of methacrylic acid esters
- C09D133/12—Homopolymers or copolymers of methyl methacrylate
-
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- 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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/06—Unsaturated polyesters having carbon-to-carbon unsaturation
-
- 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
- C09D177/00—Coating compositions based on polyamides obtained by reactions forming a carboxylic amide link in the main chain; Coating compositions based on derivatives of such polymers
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses heat dissipation electrostatic adsorption powder and a preparation method thereof, when in use, the heat dissipation electrostatic adsorption powder is directly sprayed on the surface of a metal heat dissipation part by adopting an electrostatic spraying process, no solvent is consumed in the whole process, no waste is generated, the operation is simple in the use process, and the environmental protection is high; the coating formed on the surface of the metal radiating component can improve the radiating efficiency of the metal radiating component, improve the corrosion resistance of the metal radiating component and remarkably prolong the service life of the metal radiating component. The invention discloses a preparation method of heat dissipation electrostatic adsorption powder, which utilizes the characteristic of self-assembly of cellulose nanocrystalline into sheets in the freezing process, takes the cellulose nanocrystalline as a carrier to enable few-layer graphene to be self-assembled into sheets, further obtains large-size few-layer graphene through high-temperature carbonization, and then compounds the large-size few-layer graphene, resin powder, inorganic mineral powder and auxiliary agent into the electrostatic adsorption powder with the heat dissipation function, and has simple operation steps.
Description
Technical Field
The invention relates to the technical field of heat dissipation coatings, in particular to heat dissipation electrostatic adsorption powder and a preparation method thereof.
Background
With the rapid development of the high-frequency communication field such as 5G and the like, electronic components generate more heat when working at high frequency, on one hand, the leakage current is increased due to the rise of temperature, the power consumption of the components is increased, and the energy consumption is increased; on the other hand, the increase in temperature leads to a considerable reduction in the service life of the electronic components. According to the arrhenius equation (or formula): the service life of the components is reduced by half when the temperature rises by 10 ℃. Such as the 10 degree law followed in the capacitor industry: the service life of the capacitor is doubled when the working temperature of the capacitor is reduced by 10 degrees, and the service life of the capacitor is doubled when the working temperature of the capacitor is increased by 10 degrees. At present, the cooling method of electronic components is mainly to add metal radiators, and aluminum and copper metal radiators are taken as representatives.
Chinese patent, application No. CN201110031374.6, discloses a heat dissipation material and a method for preparing the same, wherein resin powder and heat conductive powder are physically and chemically treated and then added into an electrophoresis tank, an aluminum alloy radiator is used as an anode, the heat dissipation material is applied to the surface of the aluminum alloy radiator by electrophoresis, and then the heat dissipation material is cleaned by pure water and baked in an oven to cool the radiator. The scheme adopts an electrophoresis mode to generate electrophoresis wastewater, and the electrophoresis wastewater is required to be treated in the later period, otherwise, the environment pollution is generated.
The graphene in the graphite heat conduction material has very good heat conduction performance. Pure defect-free single-layer graphene has a thermal conductivity as high as 5300W/(m.K), and is the carbon material with the highest thermal conductivity up to now. Graphene is a two-dimensional carbon material and is a generic name for single-layer, double-layer, and few-layer graphene. The single-layer graphene is a two-dimensional carbon material consisting of a layer of carbon atoms which are periodically and closely stacked in a benzene ring structure; two layers are "double-layer graphene"; 3-10 layers of the graphene are 'few-layer graphene'. Various outstanding excellent performances of graphene can be embodied only when the quality of graphene is very high, and many excellent performances of graphene are reduced along with the increase of the number of layers and the accumulation of internal defects.
Chemical Vapor Deposition (CVD), which is a method for producing graphene thin films, is currently a more studied method, and the method uses carbon-containing organic gas as a raw material to perform vapor deposition to prepare the graphene thin films. In the later stage of preparation, the chemical vapor deposition method is complex in the transfer process of graphene and low in yield. When the graphene is prepared by using the oxidation-reduction method, the single-layer graphene is very thin and is easy to agglomerate, so that the heat-conducting property and the specific surface area of the graphene are reduced.
Chinese patent, application No. CN200910187298.0, discloses a preparation method of large-size graphene, which comprises the steps of depositing a layer of metal thin film on a solid-phase substrate by using a vacuum evaporation, radio frequency sputtering or electron beam deposition mode, then spin-coating a layer of carbon-containing organic precursor thin film on the surface of the metal thin film, preparing a graphene film through high-temperature carbonization, and removing a metal thin film substrate in an acid corrosion mode to finally obtain the graphene film. According to the scheme, the preparation modes of vacuum evaporation, radio frequency sputtering, electron beam deposition and the like used for preparing the metal film matrix at the early stage have high requirements on equipment, the efficiency is low, batch production is difficult, and the metal film matrix is removed through an acid washing process at the later stage to generate new waste.
Chinese patent, application No. CN201210436521.2, discloses a graphene or graphene oxide composite enhanced heat dissipation coating, which can realize a heat dissipation function by adding a heat dissipation agent, but the formula of the composite enhanced heat dissipation coating contains substances such as solvents and heavy metals, which are also harmful to the environment.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the heat dissipation electrostatic adsorption powder and the preparation method thereof, when the heat dissipation electrostatic adsorption powder is used, the electrostatic spraying process is directly adopted to spray the heat dissipation part on the surface of the metal, the solvent is not required to be consumed in the whole process, no waste is generated, the operation in the use process is simple, and the environmental protection performance is high; the coating formed on the surface of the metal radiating component can improve the radiating efficiency of the metal radiating component, improve the corrosion resistance of the metal radiating component and remarkably prolong the service life of the metal radiating component. The invention discloses a preparation method of heat dissipation electrostatic adsorption powder, which utilizes the characteristic of self-assembly of cellulose nanocrystalline into sheets in the freezing process, takes the cellulose nanocrystalline as a carrier to enable few-layer graphene to be self-assembled into sheets, further obtains large-size few-layer graphene through high-temperature carbonization, and then compounds the large-size few-layer graphene, resin powder, inorganic mineral powder and auxiliary agent into the electrostatic adsorption powder with the heat dissipation function, and has simple operation steps.
In order to achieve the purpose, the technical scheme of the invention is to design the heat dissipation electrostatic adsorption powder which comprises the following components in parts by mass: 2 parts of few-layer graphene sheet-shaped solid, 40-60 parts of high polymer resin, 5-55 parts of inorganic mineral powder and 0.1-5 parts of auxiliary agent; the few-layer graphene sheet solid is prepared by compounding graphene, cellulose nanocrystals, a surfactant and water according to a certain mass ratio, and sequentially carrying out high-pressure homogenization, freeze drying and high-temperature carbonization.
The preferable technical scheme is that the high polymer resin is one or more of polyethylene, polypropylene, polyvinyl chloride, polystyrene, nylon, polycarbonate, polymethyl methacrylate, polybutylene terephthalate/polyethylene terephthalate, unsaturated polyester, epoxy resin and polyimide.
Further preferably, the inorganic mineral powder is one or more of calcium carbonate, talcum powder, barium sulfate, aluminum hydroxide, magnesium hydroxide and titanium dioxide.
Further preferably, the auxiliary agent is one or more of an antioxidant, a heat stabilizer, a light stabilizer, a leveling agent, a crosslinking agent and a coloring agent.
Further preferably, the surfactant is one or more of sodium silicate, sodium tripolyphosphate, sodium hexametaphosphate, sodium pyrophosphate, triethylhexyl phosphoric acid, sodium dodecyl sulfate and fatty acid polyglycol ester.
Further preferably, the mass ratio of the graphene to the cellulose nanocrystal to the surfactant to the water is 5: 10: 0.1: 100.
in order to ensure the smooth preparation of the heat dissipation electrostatic adsorption powder, a method for preparing the heat dissipation electrostatic adsorption powder is provided, which comprises the following steps:
s1: stripping the few-layer graphene, namely, mixing the graphene, the cellulose nanocrystal, the surfactant and water according to a mass ratio of 5: 10: 0.1: 100, compounding in a high-pressure homogenizer, and then performing high-pressure homogenizing circulating reflux treatment to obtain a suspension containing few layers of graphene;
s2: preparing a few-layer graphene sheet solid, namely sequentially carrying out freeze drying and high-temperature carbonization on the suspension containing few-layer graphene prepared in the step S1 to obtain the few-layer graphene sheet solid;
s3: and (2) preparing the heat dissipation electrostatic adsorption powder, namely mixing the few-layer graphene flaky solid prepared in the step (S2) with inorganic mineral powder, high polymer resin and an auxiliary agent according to the mass parts of 2 parts of the few-layer graphene flaky solid, 40-60 parts of high polymer resin, 5-55 parts of inorganic mineral powder and 0.1-5 parts of the auxiliary agent, and sequentially carrying out high-temperature melting, mixing, plasticizing, mechanical crushing and sieving to obtain the heat dissipation electrostatic adsorption powder with the particle size of less than 80 microns.
The invention has the advantages and beneficial effects that:
1. the heat dissipation electrostatic adsorption powder disclosed by the invention is directly sprayed on the surface of a metal heat dissipation part by adopting an electrostatic spraying process when in use, no solvent is consumed in the whole process, no waste is generated, the operation is simple in the use process, and the environmental friendliness is high.
2. The coating formed on the surface of the metal heat dissipation part can improve the heat dissipation efficiency of the metal heat dissipation part, improve the corrosion resistance of the metal heat dissipation part and obviously prolong the service life of the metal heat dissipation part.
3. The invention discloses a preparation method of heat dissipation electrostatic adsorption powder, which utilizes the characteristic of self-assembly of cellulose nanocrystalline into sheets in the freezing process, takes the cellulose nanocrystalline as a carrier to enable few-layer graphene to be self-assembled into sheets, further obtains large-size few-layer graphene through high-temperature carbonization, and then compounds the large-size few-layer graphene, resin powder, inorganic mineral powder and auxiliary agent into the electrostatic adsorption powder with the heat dissipation function, and has simple operation steps.
Drawings
Fig. 1 is an electron microscope scan of few-layer graphene prepared by the high-pressure homogeneous cyclic reflux treatment in step S1 of example 1;
fig. 2 is an electron microscope scan of graphene/cellulose nanocrystalline nanosheets obtained by freeze-drying the suspension containing few-layer graphene in step S2 of example 1;
fig. 3 is an electron microscope scanning image of a few-layer graphene sheet-like solid obtained by freeze-drying and high-temperature carbonization of the suspension containing few-layer graphene in step S3 of example 1 in this order.
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
The heat dissipation electrostatic adsorption powder comprises the following components in parts by mass: 2 parts of few-layer graphene sheet-shaped solid, 40 parts of PVC resin, 55 parts of calcium carbonate and 3 parts of heat stabilizer; the few-layer graphene sheet solid is prepared by compounding graphene, cellulose nanocrystals, a surfactant and water according to a certain mass ratio, and sequentially carrying out high-pressure homogenization, freeze drying and high-temperature carbonization.
Preferably, the PVC resin is SG-5 type, the calcium carbonate is light calcium carbonate, and the heat stabilizer is zinc stearate/calcium stearate.
The preparation method of the heat dissipation electrostatic adsorption powder in the embodiment 1 comprises the following steps:
s1: stripping few-layer graphene, namely putting 50g of graphene, 100g of cellulose nanocrystal and 1g of sodium dodecyl sulfate into 1000g of water, performing circulating reflux for 6 times in a homogenizer under the pressure of 120MPa, and realizing interlayer separation of the graphene by utilizing the high pressure and high shear action of the homogenizer, wherein the sodium dodecyl sulfate enables the layered graphene, the cellulose nanocrystal and the water to form a suspension containing few-layer graphene, so that secondary aggregation and aggregation of the few-layer graphene are avoided;
s2: preparing a few-layer graphene flaky solid, namely freeze-drying the suspension containing few-layer graphene prepared in the step S1 at the temperature of below-30 ℃ for 24h, self-assembling a large-size graphene/cellulose nanocrystalline nanosheet by using hydroxyl existing in cellulose nanocrystals in the freeze-drying process to obtain a large-size graphene/cellulose nanocrystalline nanosheet, namely obtaining a cellulose nanocrystalline ordered layered structure solid containing few-layer graphene, then carbonizing at the high temperature of 800 ℃ for 4 hours under the protection of inert gas nitrogen, and naturally cooling to room temperature to obtain a large-size few-layer graphene flaky solid;
s3: preparing the heat dissipation electrostatic adsorption powder, namely mixing the few-layer graphene flaky solid prepared in the step S2 with inorganic mineral powder, high polymer resin and an auxiliary agent according to the mass parts of 2 parts of the few-layer graphene flaky solid, 40 parts of PVC resin, 55 parts of calcium carbonate and 3 parts of a heat stabilizer, performing melt extrusion in a double-screw extruder at the temperature of 170 ℃, and mechanically crushing, grinding and sieving the plasticized material to obtain the heat dissipation electrostatic adsorption powder with the particle size of less than 80 microns.
An electron microscope scanning image of the few-layer graphene prepared by the high-pressure homogeneous cyclic reflux treatment in step S1 of example 1 is shown in fig. 1;
an electron microscope scanning image of the graphene/cellulose nanocrystalline nanosheet obtained by freeze drying the suspension containing few-layer graphene in step S2 of example 1 is shown in fig. 2;
in step S3 of example 1, an electron microscope scan of a few-layer graphene sheet-like solid obtained by sequentially freeze-drying and carbonizing at a high temperature is shown in fig. 3.
Example 2
The heat dissipation electrostatic adsorption powder comprises the following components in parts by mass: 2 parts of few-layer graphene sheet-shaped solid, 60 parts of PP resin, 35 parts of aluminum hydroxide, 5 parts of titanium dioxide and 0.1 part of antioxidant; the few-layer graphene sheet solid is prepared by compounding graphene, cellulose nanocrystals, a surfactant and water according to a certain mass ratio, and sequentially carrying out high-pressure homogenization, freeze drying and high-temperature carbonization.
Preferably, the model of the PP resin is injection molding grade, the aluminum hydroxide is nano grade, the titanium dioxide is anatase type, and the antioxidant is B215.
The preparation method of the heat dissipation electrostatic adsorption powder in the embodiment 2 comprises the following steps:
s1: stripping few-layer graphene, namely putting 50g of graphene, 100g of cellulose nanocrystal and 0.1g of triethylhexyl phosphoric acid into 1000g of water, performing circulating reflux for 4 times in a homogenizer under the pressure of 130MPa, and realizing interlayer separation of the graphene by utilizing the high pressure and high shear action of the homogenizer, wherein the triethylhexyl phosphoric acid enables the layered graphene, the cellulose nanocrystal and the water to form a suspension containing the few-layer graphene, so that secondary aggregation and aggregation of the few-layer graphene are avoided;
s2: preparing a few-layer graphene flaky solid, namely freeze-drying the suspension containing few-layer graphene prepared in the step S1 at the temperature of below-30 ℃ for 24h, self-assembling a large-size graphene/cellulose nanocrystalline nanosheet by using hydroxyl existing in cellulose nanocrystals in the freeze-drying process to obtain a large-size graphene/cellulose nanocrystalline nanosheet, namely obtaining a cellulose nanocrystalline ordered layered structure solid containing few-layer graphene, then carbonizing at the high temperature of 1000 ℃ for 4 hours under the protection of inert gas nitrogen, and naturally cooling to room temperature to obtain a large-size few-layer graphene flaky solid;
s3: preparing the heat dissipation electrostatic adsorption powder, namely mixing the few-layer graphene sheet-shaped solid prepared in the step S2 with inorganic mineral powder, high polymer resin and an auxiliary agent according to the mass parts of 2 parts of the few-layer graphene sheet-shaped solid, 60 parts of PP resin, 55 parts of aluminum hydroxide, 3 parts of titanium dioxide and 0.1 part of antioxidant, performing melt extrusion in a double-screw extruder at 200 ℃, and mechanically crushing, grinding and sieving the plasticized material to obtain the heat dissipation electrostatic adsorption powder with the particle size of less than 80 microns.
Wherein, an electron microscope scan of the few-layer graphene prepared by the high-pressure homogeneous cyclic refluxing treatment in step S1 of example 2 is the same as an electron microscope scan of the few-layer graphene prepared by the high-pressure homogeneous cyclic refluxing treatment in step S1 of example 1;
an electron microscope scan of the graphene/cellulose nanocrystalline nanosheet obtained by freeze-drying the suspension containing few-layer graphene in step S2 of example 2 is the same as an electron microscope scan of the graphene/cellulose nanocrystalline nanosheet obtained by freeze-drying the suspension containing few-layer graphene in step S2 of example 1;
the scanning electron microscope of the sheet-like solid matter of few-layer graphene obtained by freeze-drying and high-temperature carbonization of the suspension containing few-layer graphene in step S3 of example 2 is the same as the scanning electron microscope of the sheet-like solid matter of few-layer graphene obtained by freeze-drying and high-temperature carbonization of the suspension containing few-layer graphene in step S3 of example 1.
Example 3
The heat dissipation electrostatic adsorption powder comprises the following components in parts by mass: 2 parts of few-layer graphene sheet-shaped solid, 55 parts of unsaturated polyester, 40 parts of barium sulfate and 3 parts of cross-linking agent; the few-layer graphene sheet solid is prepared by compounding graphene, cellulose nanocrystals, a surfactant and water according to a certain mass ratio, and sequentially carrying out high-pressure homogenization, freeze drying and high-temperature carbonization.
Preferably, the unsaturated polyester is ortho-benzene type unsaturated polyester, the barium sulfate is nano precipitated barium sulfate, and the crosslinking agent is triallyl isocyanurate.
The preparation method of the heat dissipation electrostatic adsorption powder in embodiment 3 includes the following steps:
s1: stripping few-layer graphene, namely putting 50g of graphene, 100g of cellulose nanocrystal and 0.1g of sodium dodecyl sulfate into 1000g of water, performing cyclic reflux for 3 times in a homogenizer under the pressure of 150MPa, and realizing interlayer separation of the graphene by utilizing the high pressure and high shear action of the homogenizer, wherein the sodium dodecyl sulfate enables the layered graphene, the cellulose nanocrystal and the water to form a suspension containing few-layer graphene, so that secondary aggregation and aggregation of the few-layer graphene are avoided;
s2: preparing a few-layer graphene flaky solid, namely freeze-drying the suspension containing few-layer graphene prepared in the step S1 at the temperature of below-30 ℃ for 24h, self-assembling a large-size graphene/cellulose nanocrystalline nanosheet by using hydroxyl existing in cellulose nanocrystals in the freeze-drying process to obtain a large-size graphene/cellulose nanocrystalline nanosheet, namely obtaining a cellulose nanocrystalline ordered layered structure solid containing few-layer graphene, then carbonizing at the high temperature of 1200 ℃ for 4 hours under the protection of inert gas nitrogen, and naturally cooling to room temperature to obtain a large-size few-layer graphene flaky solid;
s3: preparing the heat dissipation electrostatic adsorption powder, namely mixing the few-layer graphene flaky solid prepared in the step S2 with inorganic mineral powder, high polymer resin and an auxiliary agent according to the mass parts of 2 parts of the few-layer graphene flaky solid, 55 parts of unsaturated polyester, 40 parts of barium sulfate and 3 parts of a cross-linking agent, performing melt extrusion in a double-screw extruder at 110 ℃, and mechanically crushing, grinding and sieving the plasticized material to obtain the heat dissipation electrostatic adsorption powder with the particle size of less than 80 micrometers.
Wherein, an electron microscope scan of the few-layer graphene prepared by the high-pressure homogeneous cyclic refluxing treatment in step S1 of example 3 is the same as an electron microscope scan of the few-layer graphene prepared by the high-pressure homogeneous cyclic refluxing treatment in step S1 of example 1;
an electron microscope scan of the graphene/cellulose nanocrystalline nanosheet obtained by freeze-drying the suspension containing few-layer graphene in step S2 of example 3 is the same as an electron microscope scan of the graphene/cellulose nanocrystalline nanosheet obtained by freeze-drying the suspension containing few-layer graphene in step S2 of example 1;
the scanning electron microscope of the sheet-like solid matter of few-layer graphene obtained by freeze-drying and high-temperature carbonization of the suspension containing few-layer graphene in step S3 of example 3 is the same as the scanning electron microscope of the sheet-like solid matter of few-layer graphene obtained by freeze-drying and high-temperature carbonization of the suspension containing few-layer graphene in step S3 of example 1.
Example 4
The heat dissipation electrostatic adsorption powder comprises the following components in parts by mass: 2 parts of few-layer graphene sheet-shaped solid, 43 parts of nylon and 55 parts of calcium carbonate; the few-layer graphene sheet solid is prepared by compounding graphene, cellulose nanocrystals, a surfactant and water according to a certain mass ratio, and sequentially carrying out high-pressure homogenization, freeze drying and high-temperature carbonization.
The difference from the heat dissipation electrostatic adsorption powder in the embodiment 1 is that nylon is used for replacing PVC resin, and the toughness of the nylon can be used for improving the cracking resistance of the coating after the heat dissipation electrostatic adsorption powder is sprayed.
Preferably, the calcium carbonate is light calcium carbonate.
The method for preparing the heat dissipating electrostatic adsorption powder in example 4 is the same as the method for preparing the heat dissipating electrostatic adsorption powder in example 1.
Example 5
The heat dissipation electrostatic adsorption powder comprises the following components in parts by mass: 2 parts of few-layer graphene sheet-shaped solid, 45 parts of epoxy resin, 50 parts of aluminum hydroxide, 3 parts of titanium dioxide and 0.1 part of antioxidant; the few-layer graphene sheet solid is prepared by compounding graphene, cellulose nanocrystals, a surfactant and water according to a certain mass ratio, and sequentially carrying out high-pressure homogenization, freeze drying and high-temperature carbonization.
The difference from the heat dissipation electrostatic adsorption powder in the embodiment 2 is that the epoxy resin is used for replacing PP resin, and the adhesion of the coating on the metal matrix after the heat dissipation electrostatic adsorption powder is sprayed can be improved by utilizing the caking property of the epoxy resin.
Preferably, the aluminum hydroxide is in a nanometer level, the titanium dioxide is in an anatase type, and the antioxidant is B215.
The method for preparing the heat dissipating electrostatic adsorption powder in example 5 is the same as the method for preparing the heat dissipating electrostatic adsorption powder in example 2.
Example 6
The heat dissipation electrostatic adsorption powder comprises the following components in parts by mass: 2 parts of few-layer graphene flaky solid, 50 parts of polymethyl methacrylate, 45 parts of barium sulfate and 3 parts of cross-linking agent; the few-layer graphene sheet solid is prepared by compounding graphene, cellulose nanocrystals, a surfactant and water according to a certain mass ratio, and sequentially carrying out high-pressure homogenization, freeze drying and high-temperature carbonization.
The difference from the heat dissipation electrostatic adsorption powder in the embodiment 3 is that the unsaturated polyester in the heat dissipation electrostatic adsorption powder is replaced by polymethyl methacrylate, and the weather resistance of the coating after the heat dissipation electrostatic adsorption powder is sprayed can be improved by utilizing the weather resistance of the polymethyl methacrylate.
The method for preparing the heat dissipating electrostatic adsorption powder in example 6 was the same as that of example 3.
The heat dissipation electrostatic adsorption powder prepared in the embodiments 1 to 6 is respectively sprayed on the surface of the aluminum radiator for the electronic component with the same size and specification by an electrostatic spraying mode, in the embodiment, the specification of the heat dissipation aluminum sheet is selected to be 30mm in diameter and 1.5mm in thickness, the heat dissipation aluminum sheet is treated at a high temperature of 200 ℃ for 20 minutes, after cooling, a heat dissipation coating with a thickness range of 50 to 100 micrometers is formed on the surface of the aluminum radiator, and the performance test shown in table 1 is carried out on the aluminum radiator corresponding to the heat dissipation electrostatic adsorption powder electrostatic spraying in the embodiments 1 to 6, and the test results are shown in table 2:
table 1 test details of electrostatic spraying of heat dissipating electrostatic adsorption powder in examples 1 to 6 corresponding to aluminum heat sink
Table 2 test results of electrostatic spraying of heat dissipating electrostatic adsorption powder corresponding to aluminum heat sink in examples 1 to 6
As can be seen from Table 2: the coating formed by electrostatically spraying the heat dissipation electrostatic adsorption powder on the surface of the aluminum heat radiator in the embodiments 1 to 6 meets the relevant test standards of a gloss test, a film thickness test, a Baige test, a heat dissipation test, a high and low temperature test, an acid resistance test, an alkali resistance test, a salt spray test and a wear resistance test;
in embodiments 1 to 6, the heat dissipation electrostatic adsorption powder prepared by the method of the present invention utilizes the characteristic of self-assembly of cellulose nanocrystals into sheets in the freezing process, uses the cellulose nanocrystals as a carrier to self-assemble a few-layer graphene into sheets, further obtains a large-size few-layer graphene through high-temperature carbonization, and then prepares an electrostatic adsorption powder with a heat dissipation function with resin powder, inorganic mineral powder, and an auxiliary agent, wherein the operation steps are simple; when the heat dissipation electrostatic adsorption powder is used, an electrostatic spraying process is directly adopted, no solvent is consumed in the whole process, no waste is generated, the environment friendliness is high in the using process, and the purpose of the invention is achieved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. The heat dissipation electrostatic adsorption powder is characterized by comprising the following components in parts by mass: 2 parts of few-layer graphene sheet-shaped solid, 40-60 parts of high polymer resin, 5-55 parts of inorganic mineral powder and 0.1-5 parts of auxiliary agent; the few-layer graphene sheet solid is prepared by compounding graphene, cellulose nanocrystals, a surfactant and water according to a certain mass ratio, and sequentially carrying out high-pressure homogenization, freeze drying and high-temperature carbonization.
2. The heat-dissipating electrostatic adsorption powder of claim 1, wherein the polymer resin is one or more of polyethylene, polypropylene, polyvinyl chloride, polystyrene, nylon, polycarbonate, polymethyl methacrylate, polybutylene terephthalate/polyethylene terephthalate, unsaturated polyester, epoxy resin, and polyimide.
3. The heat-dissipating electrostatic adsorption powder according to claim 1, wherein the inorganic mineral powder is one or more of calcium carbonate, talc, barium sulfate, aluminum hydroxide, magnesium hydroxide, and titanium dioxide.
4. The heat-dissipating electrostatic adsorption powder of claim 1, wherein the auxiliary agent is one or more of an antioxidant, a heat stabilizer, a light stabilizer, a leveling agent, a crosslinking agent and a coloring agent.
5. The heat-dissipating electrostatic adsorption powder of claim 1, wherein the surfactant is one or more of sodium silicate, sodium tripolyphosphate, sodium hexametaphosphate, sodium pyrophosphate, triethylhexylphosphoric acid, sodium dodecylsulfate, and fatty acid polyglycol ester.
6. The heat-dissipating electrostatic adsorption powder according to any one of claims 1 to 5, wherein the mass ratio of the graphene to the cellulose nanocrystal to the surfactant to the water is 5: 10: 0.1: 100.
7. the method for preparing the heat-dissipating electrostatic adsorption powder according to claim 6, comprising the steps of:
s1: stripping the few-layer graphene, namely compounding the graphene, the cellulose nanocrystal, the surfactant and the water in a high-pressure homogenizer according to the mass ratio in claim 6, and then performing high-pressure homogenization and circulating reflux treatment to obtain a suspension containing the few-layer graphene;
s2: preparing a few-layer graphene sheet solid, namely sequentially carrying out freeze drying and high-temperature carbonization on the suspension containing few-layer graphene prepared in the step S1 to obtain the few-layer graphene sheet solid;
s3: preparing the heat dissipation electrostatic adsorption powder, namely mixing the few-layer graphene sheet-shaped solid prepared in the step S2, the inorganic mineral powder, the high polymer resin and the auxiliary agent according to the mass part ratio in the claim 1, and sequentially carrying out high-temperature melting, mixing, plasticizing, mechanical crushing and sieving to obtain the heat dissipation electrostatic adsorption powder with the particle size of less than 80 microns.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110665381.5A CN113248958A (en) | 2021-06-16 | 2021-06-16 | Heat dissipation electrostatic adsorption powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110665381.5A CN113248958A (en) | 2021-06-16 | 2021-06-16 | Heat dissipation electrostatic adsorption powder and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113248958A true CN113248958A (en) | 2021-08-13 |
Family
ID=77188212
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110665381.5A Pending CN113248958A (en) | 2021-06-16 | 2021-06-16 | Heat dissipation electrostatic adsorption powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113248958A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116082924A (en) * | 2022-11-07 | 2023-05-09 | 东莞浩川新材料有限公司 | Low-temperature-cured thin-coating insulating powder coating and preparation method thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876215A (en) * | 2015-05-13 | 2015-09-02 | 华中科技大学 | Reduced graphene oxide aqueous dispersion and preparation method thereof |
| CN106867360A (en) * | 2017-01-21 | 2017-06-20 | 江苏华光粉末有限公司 | A kind of radiator graphene powder coating and its preparation technology |
| CN108276615A (en) * | 2017-12-29 | 2018-07-13 | 华中科技大学 | A kind of high heat conduction stratiform graphene composite material and preparation method |
| CN108929624A (en) * | 2018-06-28 | 2018-12-04 | 江苏华光新材料科技有限公司 | Heat conduction and heat radiation powdery paints and preparation method thereof |
| CN109456681A (en) * | 2018-10-26 | 2019-03-12 | 四川大学 | A kind of preparation method of the graphene of anti-corrosive properties/powder thermosetting composite coating |
| CN109705725A (en) * | 2018-12-29 | 2019-05-03 | 六安科瑞达新型材料有限公司 | A kind of heat radiating type polyamide powder coating |
| CN110155985A (en) * | 2019-06-17 | 2019-08-23 | 南京林业大学 | A kind of preparation method of high orientation flaky carbon nanomaterials |
| CN110734689A (en) * | 2019-11-07 | 2020-01-31 | 六安捷通达新材料有限公司 | high-salt-spray-resistant powder coating composition |
| CN110819215A (en) * | 2018-08-14 | 2020-02-21 | 福建宏宇石墨烯新材料有限公司 | Modified graphene antistatic powder coating |
| WO2021031377A1 (en) * | 2019-08-20 | 2021-02-25 | 安徽神剑新材料股份有限公司 | Polyester resin used for graphene-containing powder coating |
-
2021
- 2021-06-16 CN CN202110665381.5A patent/CN113248958A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876215A (en) * | 2015-05-13 | 2015-09-02 | 华中科技大学 | Reduced graphene oxide aqueous dispersion and preparation method thereof |
| CN106867360A (en) * | 2017-01-21 | 2017-06-20 | 江苏华光粉末有限公司 | A kind of radiator graphene powder coating and its preparation technology |
| CN108276615A (en) * | 2017-12-29 | 2018-07-13 | 华中科技大学 | A kind of high heat conduction stratiform graphene composite material and preparation method |
| CN108929624A (en) * | 2018-06-28 | 2018-12-04 | 江苏华光新材料科技有限公司 | Heat conduction and heat radiation powdery paints and preparation method thereof |
| CN110819215A (en) * | 2018-08-14 | 2020-02-21 | 福建宏宇石墨烯新材料有限公司 | Modified graphene antistatic powder coating |
| CN109456681A (en) * | 2018-10-26 | 2019-03-12 | 四川大学 | A kind of preparation method of the graphene of anti-corrosive properties/powder thermosetting composite coating |
| CN109705725A (en) * | 2018-12-29 | 2019-05-03 | 六安科瑞达新型材料有限公司 | A kind of heat radiating type polyamide powder coating |
| CN110155985A (en) * | 2019-06-17 | 2019-08-23 | 南京林业大学 | A kind of preparation method of high orientation flaky carbon nanomaterials |
| WO2021031377A1 (en) * | 2019-08-20 | 2021-02-25 | 安徽神剑新材料股份有限公司 | Polyester resin used for graphene-containing powder coating |
| CN110734689A (en) * | 2019-11-07 | 2020-01-31 | 六安捷通达新材料有限公司 | high-salt-spray-resistant powder coating composition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116082924A (en) * | 2022-11-07 | 2023-05-09 | 东莞浩川新材料有限公司 | Low-temperature-cured thin-coating insulating powder coating and preparation method thereof |
| CN116082924B (en) * | 2022-11-07 | 2023-10-24 | 东莞浩川新材料有限公司 | Low-temperature-cured thin-coating insulating powder coating and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | Sandwich-structured polymers with electrospun boron nitrides layers as high-temperature energy storage dielectrics | |
| Huang et al. | A facile, high‐yield, and freeze‐and‐thaw‐assisted approach to fabricate MXene with plentiful wrinkles and its application in on‐chip micro‐supercapacitors | |
| Thakur et al. | Hybrid polymer composite materials: Applications | |
| US7105108B2 (en) | Graphite intercalation and exfoliation process | |
| US9908996B2 (en) | Catecholamine-flaky graphite based polymer complex for preparation of composite | |
| TWI517774B (en) | Method of producing multilayer graphene-laminated substrate | |
| KR101310520B1 (en) | Electrode material for electrochemical device and composite particle | |
| US20200114622A1 (en) | Process for highly conductive graphitic thick films | |
| Yang et al. | Surface engineering of 2D dielectric polymer films for scalable production of high-energy-density films | |
| KR20150085523A (en) | Film forming composition comprising graphene material and conducting polymer | |
| CN109181654B (en) | Graphene-based composite heat-conducting film and preparation method and application thereof | |
| CN113248958A (en) | Heat dissipation electrostatic adsorption powder and preparation method thereof | |
| WO2019222906A1 (en) | Method for extracting carbon material from plastic and device therefor | |
| CN113429600A (en) | Silver-titanium dioxide filler doped polyvinylidene fluoride dielectric composite film and preparation method thereof | |
| Yuan et al. | Non-covalently modified graphene@ poly (ionic liquid) nanocomposite with high-temperature resistance and enhanced dielectric properties | |
| CN109369930B (en) | Preparation method of graphite-reinforced thermoplastic heat-conducting plastic | |
| Ji et al. | A novel method to fabricate two-dimensional nanomaterial based on electrospinning | |
| WO2020076806A1 (en) | Highly conductive graphitic thick films and method of production | |
| TW201714335A (en) | Manufacturing method of negative electrode plate in secondary battery to deposit the graphene target material on the micro-structure on the copper foil surface for forming the graphene layer to increase the cycle life of the whole graphene negative electrode and the reversible capacity | |
| US20200116443A1 (en) | Highly conductive graphitic thick films and method of production | |
| WO2004108997A2 (en) | Graphite intercalation and exfoliation process | |
| CN108793129B (en) | Heterogeneous graphene film and preparation method thereof | |
| JP6385155B2 (en) | Method for producing thermal conductive paste | |
| CN116014106A (en) | Preparation method and application of carbon/tungsten disulfide intercalation composite material | |
| JP2017052913A (en) | Resin composite material and method for producing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210813 |
|
| RJ01 | Rejection of invention patent application after publication |