CN113234392A - High-temperature graphene conductive coating composition, high-temperature graphene conductive coating, preparation method of high-temperature graphene conductive coating, and graphene heating pipe - Google Patents
High-temperature graphene conductive coating composition, high-temperature graphene conductive coating, preparation method of high-temperature graphene conductive coating, and graphene heating pipe Download PDFInfo
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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
- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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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
- 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
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/40—Heating elements having the shape of rods or tubes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention relates to the technical field of graphene heating, and discloses a high-temperature graphene conductive coating composition, a high-temperature graphene conductive coating, a preparation method of the high-temperature graphene conductive coating composition and a graphene heating pipe. The composition comprises graphene, conductive powder, resin, a dispersing agent and a coupling agent; and relative to 100 parts by weight of the high-temperature graphene conductive coating composition, the content of the graphene is 1-4 parts by weight, the content of the conductive powder is 10-18 parts by weight, the content of the resin is 60-85 parts by weight, the content of the dispersant is 2-4 parts by weight, and the content of the coupling agent is 1-4 parts by weight. The graphene heating pipe can be used for a long time at a high temperature without power attenuation.
Description
Technical Field
The invention relates to the technical field of graphene heating, in particular to a high-temperature graphene conductive coating composition, a high-temperature graphene conductive coating, a preparation method of the high-temperature graphene conductive coating composition and a graphene heating pipe.
Background
With the change of science and technology, the application of the graphene conductive coating is more and more extensive, and the types of electric heating products extended by the graphene conductive coating are more and more.
At present, the common graphene conductive coating is basically applied to low environmental temperature, which is mainly limited by the substrate selected by the conductive coating. Some conductive coatings adopt common high polymer materials as coating substrates, and the common high polymer materials are not heat-resistant and can be easily aged after being used for a long time in a high-temperature environment, so that the product fails or safety accidents are caused; some conductive coatings adopt inorganic materials as coating substrates, but the inorganic materials are usually sintered at high temperature for use, and the conductive coatings have the disadvantages of high processing cost, complex process, high energy consumption and great pollution. In addition, since the conductive coating is not resistant to high temperature, it is difficult to prepare an electrothermal conversion device with high power density, and the power of the heating device is generally increased by increasing the tiled area of the conductive coating.
The heating pipe is a relatively effective electric heat conversion device, the heating element of the common heating pipe is a resistance wire, the heating element is usually positioned in the pipe body, the resistance wire is easy to oxidize in a high-temperature environment, the power attenuation is easy to cause after long-time use, and the metal element is not corrosion-resistant and cannot be used as a heating device in a corrosive atmosphere. The carbon fiber can also be used as a heating element of a heating pipe, and needs inert gas to be sealed in the heating pipe, so that the process is complex. The heating element of the heating pipe is positioned inside the pipe body, and the heat dissipation effect is poor.
Therefore, the research and development of the high-temperature graphene conductive coating composition with good temperature resistance are of great significance.
Disclosure of Invention
The invention aims to overcome the defect that the power of a heating pipe can be attenuated when the heating pipe is used at a high temperature for a long time in the prior art, and provides a high-temperature graphene conductive coating composition, a high-temperature graphene conductive coating, a preparation method of the high-temperature graphene conductive coating and a graphene heating pipe.
In order to achieve the above object, a first aspect of the present invention provides a high-temperature graphene conductive coating composition, wherein the composition comprises graphene, a conductive powder, a resin, a dispersant and a coupling agent; and relative to 100 parts by weight of the high-temperature graphene conductive coating composition, the content of the graphene is 1-4 parts by weight, the content of the conductive powder is 10-18 parts by weight, the content of the resin is 60-85 parts by weight, the content of the dispersant is 2-4 parts by weight, and the content of the coupling agent is 1-4 parts by weight.
Preferably, the content of the graphene is 2-4 parts by weight, the content of the conductive powder is 12-15 parts by weight, the content of the resin is 68-72 parts by weight, the content of the dispersant is 3-4 parts by weight, and the content of the coupling agent is 2-4 parts by weight, relative to 100 parts by weight of the high-temperature graphene conductive coating composition.
Preferably, the resin includes a first resin and a second resin, and the dispersant includes a first dispersant and a second dispersant.
Preferably, the weight ratio of the first resin to the first dispersant is (20-35): 1; more preferably (25-30): 1.
preferably, the weight ratio of the second resin to the second dispersant is (10-25): 1; more preferably (15-20): 1.
preferably, the first resin and the second resin are the same or different and are each selected from one or more of silicone resin, phenol resin, urea resin, epoxy resin, polyurethane, and polyimide.
Preferably, the weight ratio of the first resin to the second resin is (1-2): 1, more preferably (1.5-1.9): 1.
preferably, the first dispersant and the second dispersant are the same or different and are each selected from one or more of oleyl aminooleate, sodium salt of polycarboxylic acid, sodium dodecylbenzenesulfonate and polyvinyl alcohol.
Preferably, the weight ratio of the first dispersant to the second dispersant is (0.5-2): 1, preferably (1-1.5): 1.
preferably, the conductive powder is selected from one or more of carbon nanotubes, carbon black, acetylene black, ketjen black, silver nanowires, copper nanopowders and gold nanoparticles.
Preferably, the coupling agent is selected from one or more of a vinyl silane coupling agent, an amino silane coupling agent, and an epoxy silane coupling agent.
Preferably, the composition further comprises an antifoaming agent and a curing accelerator, and the antifoaming agent is present in an amount of 1 to 4 parts by weight and the curing accelerator is present in an amount of 2 to 8 parts by weight, relative to 100 parts by weight of the high-temperature graphene conductive coating composition.
Preferably, the content of the defoaming agent is 2 to 4 parts by weight and the content of the curing accelerator is 5 to 8 parts by weight with respect to 100 parts by weight of the high-temperature graphene conductive coating composition.
The invention provides a method for preparing a high-temperature graphene conductive coating by using the composition, wherein the method comprises the following steps:
(1) in the presence of a first dispersing agent, contacting conductive powder, a first resin and a coupling agent for first mixing to obtain a first mixture;
(2) in the presence of a second dispersing agent, contacting graphene with a second resin for second mixing to obtain a second mixture;
(3) and contacting the first mixture and the second mixture for third mixing to obtain the high-temperature graphene conductive coating.
Preferably, the method further comprises: in the step (3), the first mixture, the second mixture, a defoaming agent and a curing accelerator are contacted to perform fourth mixing, so that the high-temperature graphene conductive coating is obtained.
The third aspect of the invention provides a high-temperature graphene conductive coating prepared by the method.
The invention provides a graphene heating pipe in a fourth aspect, wherein the graphene heating pipe comprises a pipe body and a conductive coating coated on the surface of the pipe body, and the conductive coating is the high-temperature graphene conductive coating.
According to the technical scheme, the high-temperature graphene conductive coating adopts the coupling agent to modify the conductive powder, so that the conductive powder is uniformly dispersed in the resin, and the conductive powder and the graphene are mutually combined in the resin to form the three-dimensional reticular framework conductive structure, so that the high-temperature graphene conductive coating is ensured to have good conductivity, and further, the graphene heating pipe can obtain high power density and can be used for a long time without power attenuation.
Drawings
Fig. 1 is a schematic structural diagram of a graphene heating tube prepared from the high-temperature graphene conductive coating prepared in example 1 of the present invention;
FIG. 2 is a structural sectional view of a graphene heating tube at view A-A;
fig. 3 is a structural sectional view of a graphene heating tube from a B-B view.
Description of the reference numerals
1-a pipe body; 2-a conductive coating layer; 3-a conductive electrode layer; 4-a metal flake;
5-insulating protective layer; 7-connecting lines.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a high-temperature graphene conductive coating composition, wherein the composition comprises graphene, conductive powder, resin, a dispersing agent and a coupling agent; and relative to 100 parts by weight of the high-temperature graphene conductive coating composition, the content of the graphene is 1-4 parts by weight, the content of the conductive powder is 10-18 parts by weight, the content of the resin is 60-85 parts by weight, the content of the dispersant is 2-4 parts by weight, and the content of the coupling agent is 1-4 parts by weight.
The inventors of the present invention found that: the coupling agent is adopted to modify the conductive powder, so that the surface wettability of the conductive powder is improved, the conductive powder can be uniformly dispersed in the resin, the conductive powder is of a zero-dimensional structure, and the conductive powder is in electrical contact with points inside the resin to form a conductive path; the functionalized graphene oxide is of a two-dimensional planar structure and has ultrahigh conductivity and surface area, the conductive powder and the functionalized graphene oxide are combined with each other in the resin, and the conductive path is in point contact from a single point to a point and is in point contact with a surface and surface contact to form a three-dimensional mesh conductive structure, so that the conductive path is increased, and the high-temperature graphene conductive coating disclosed by the invention has good conductivity; in addition, further, by adopting specific components, specific component contents and mutual proportioning, the prepared graphene heating tube can obtain high power density and can be used for a long time without power attenuation.
According to the invention, the high-temperature graphene conductive coating can have better conductivity despite the components and the component contents defined in the foregoing, and the prepared graphene heating tube can obtain high power density and can be used for a long time without power attenuation. However, preferably, the content of the graphene is 2 to 4 parts by weight, the content of the conductive powder is 12 to 15 parts by weight, the content of the resin is 68 to 72 parts by weight, the content of the dispersant is 3 to 4 parts by weight, and the content of the coupling agent is 2 to 4 parts by weight, relative to 100 parts by weight of the high-temperature graphene conductive coating composition, so that the high-temperature graphene conductive coating has better conductivity, and the prepared graphene heating tube can obtain better high power density and can be used for a long time without power attenuation.
According to the present invention, it is further preferable that the content of the graphene is 3 to 3.5 parts by weight, the content of the conductive powder is 12.5 to 13 parts by weight, the content of the resin is 70 to 71 parts by weight, the content of the dispersant is 3 to 3.5 parts by weight, and the content of the coupling agent is 2.5 to 3 parts by weight, relative to 100 parts by weight of the high temperature graphene conductive coating composition, so that the high temperature graphene conductive coating has the best conductivity, and the prepared graphene heating tube can obtain a better high power density and can be used for a long time without power attenuation.
According to the present invention, the resin includes a first resin and a second resin, and the dispersant includes a first dispersant and a second dispersant; preferably, the weight ratio of the first resin to the first dispersant is (20-35): 1, more preferably (25-30): 1, more preferably (26.47-30): 1.
according to the invention, preferably, the weight ratio of the second resin to the second dispersant is (10-25): 1, more preferably (15-20): 1, more preferably (16.67-19.23): 1.
in the present invention, the "weight ratio of the first resin to the first dispersant" and the "weight ratio of the second resin to the second dispersant" are defined within the above ranges, and there is an advantage that the conductive powder is a main conductive filler of the conductive paint, which constitutes a main conductive path inside the paint, and the surface-modified conductive powder reduces the surface energy of the conductive powder and improves the wettability thereof, so that a good dispersion effect is obtained with a smaller amount of dispersant, and the weight ratio of the first resin to the first dispersant is (20-35): experiments show that the proportion can ensure that the conductive powder has good dispersibility, reduce the using amount of the dispersing agent, indirectly improve the content of the conductive powder and improve the conductivity of the coating; since graphene has large surface energy and poor surface wettability, the weight ratio of the second resin to the second dispersant is (10-25): 1, experiments show that in such a ratio, the graphene powder can be uniformly dispersed in the second resin.
According to the invention, the first resin and the second resin are the same or different and are respectively selected from one or more of organic silicon resin, phenolic resin, urea resin, epoxy resin, polyurethane and polyimide; preferably one or more of silicone resin, polyimide and polyurethane, and further preferably polyimide and/or silicone resin; more preferably, the weight ratio of the first resin to the second resin is (1-2): 1, preferably (1.5-1.9): 1, more preferably (1.5-1.8): 1.
according to the invention, the first dispersant and the second dispersant are the same or different and are each selected from one or more of oleyl aminooleate (BYK190), sodium polycarboxylate salts, sodium dodecylbenzenesulfonate and polyvinyl alcohol, preferably oleyl aminooleate; more preferably, the weight ratio of the first dispersant to the second dispersant is (0.5-2): 1, preferably (1-1.5): 1, more preferably (1-1.3): 1.
according to the invention, the conductive powder is selected from one or more of carbon nano tube, carbon black, acetylene black, ketjen black, nano silver wire, copper nano powder and gold nano powder; preferably one or more of carbon nanotubes, ketjen black and copper nano powder, and more preferably copper nano powder.
According to the invention, the coupling agent is selected from one or more of vinyl silane coupling agent, amino silane coupling agent and epoxy silane coupling agent, preferably epoxy silane coupling agent.
According to the invention, the composition further comprises a defoaming agent and a curing accelerator, and the defoaming agent is 1-4 parts by weight and the curing accelerator is 2-8 parts by weight relative to 100 parts by weight of the high-temperature graphene conductive coating composition; preferably, the content of the defoaming agent is 2 to 4 parts by weight and the content of the curing accelerator is 5 to 8 parts by weight, relative to 100 parts by weight of the high-temperature graphene conductive coating composition; preferably, the content of the defoaming agent is 2.5 to 3 parts by weight and the content of the curing accelerator is 6.5 to 7 parts by weight with respect to 100 parts by weight of the high-temperature graphene conductive coating composition.
According to the invention, the defoaming agent is selected from one or more of emulsified silicone oil, higher alcohol fatty acid ester complex, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene amine ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether and polydimethylsiloxane, and is preferably polydimethylsiloxane.
According to the invention, the curing accelerator is selected from one or more of toluene diisocyanate, hydrogenated diphenylmethane diisocyanate, diphenylmethane diisocyanate and hexamethylene diisocyanate, preferably hydrogenated diphenylmethane diisocyanate.
The invention provides a method for preparing a high-temperature graphene conductive coating by using the composition, wherein the method comprises the following steps:
(1) in the presence of a first dispersing agent, contacting conductive powder, a first resin and a coupling agent for first mixing to obtain a first mixture;
(2) in the presence of a second dispersing agent, contacting graphene with a second resin for second mixing to obtain a second mixture;
(3) and contacting the first mixture and the second mixture for third mixing to obtain the high-temperature graphene conductive coating.
According to the invention, in step (1), the conditions of the first mixing comprise: stirring at the stirring speed of 250-350rpm for 30-60min at the room temperature of 20-30 ℃, and slowly adding the mixed conductive powder into the mixed first resin in a stirring state to obtain a first mixture.
According to the invention, in step (2), the conditions of the second mixing comprise: at the room temperature of 20-30 ℃, at the stirring speed of 250-350rpm, the second resin is mixed and stirred uniformly, then the second dispersing agent is added, and the stirring is carried out for 10-30 min; and slowly adding the graphene into the mixed second resin in a stirring state at the stirring speed of 100-200rpm, and stirring for 30-60min to obtain a second mixture.
According to the present invention, in the step (3), the conditions of the third mixing include: and contacting the first mixture and the second mixture at the room temperature of 20-30 ℃ and at the stirring speed of 150-250rpm for third mixing for 30-60min to obtain a third mixture.
According to the present invention, preferably, the method further comprises: in the step (3), the first mixture, the second mixture, a defoaming agent and a curing accelerator are contacted to perform fourth mixing, so that the high-temperature graphene conductive coating is obtained.
According to the invention, the conditions of the fourth mixing are the same as the conditions of the third mixing.
According to a preferred embodiment of the present invention, a method for preparing a high-temperature graphene conductive coating using the composition described above comprises:
(S1) contacting the conductive powder in the first resin with a coupling agent in the presence of a first dispersant to perform a coupling reaction to obtain a first mixture;
(S2) in the presence of a second dispersant, dispersing and mixing graphene and a second resin to obtain a second mixture;
(S3) uniformly mixing the first mixture obtained in the step (S1) and the second mixture obtained in the step (S2) with a curing accelerator and a defoaming agent, and then defoaming in vacuum to obtain the high-temperature graphene conductive coating.
The third aspect of the invention provides a high-temperature graphene conductive coating prepared by the method.
The invention provides a graphene heating pipe in a fourth aspect, wherein the graphene heating pipe comprises a pipe body and a conductive coating coated on the surface of the pipe body, and the conductive coating is the high-temperature graphene conductive coating.
According to the invention, the tube body is selected from one or more of a ceramic tube, a quartz tube, a high silica glass tube, a soda lime glass tube and a silicate glass tube, and is preferably a ceramic tube.
According to the invention, the coating is selected from one or more of spraying, dipping, brushing and printing, preferably dipping.
According to the invention, the dry film thickness of the conductive coating is 50 to 100. mu.m, preferably 55 to 80 μm.
According to a preferred embodiment of the present invention, as shown in fig. 1, the preparation method of the graphene heating tube includes:
(I) coating a high-temperature graphene conductive coating on the surface of a heating pipe 1, drying, and forming a conductive coating layer 2 on the surface of the heating pipe 1;
(II) coating conductive electrode layers 3 on two sides of the heating pipe coated with the high-temperature graphene conductive coating, and drying; covering a metal sheet 4 on the dried conductive electrode layer 3;
(III) connecting and fixing the connecting wire 7 and the metal sheet 4 by connecting the heating pipe in the step (II) in series through a screw, a washer and a nut;
(IV) coating an insulating protective layer 5 on the surface of the heating pipe in the step (III), and drying to obtain the graphene heating pipe.
Fig. 2 is a structural cross-sectional view from a-a perspective of a graphene heating tube, in accordance with the present invention; as can be seen from fig. 2, this part is the part of the heating tube connected to the power supply, and the heating tube comprises a heating tube 1, a conductive coating 2, a conductive electrode layer 3, a metal foil layer 4 and an insulating protective layer 5 in sequence from inside to outside. When the electric heating device is electrified, current is conducted to the conductive electrode layer 3 through the metal sheet layer 4, the conductive electrode layer 3 conducts the current to the conductive coating 2, and therefore the conductive coating 2 is electrified to generate heat. The conductive electrode layer 3 is tightly combined with the conductive coating 2, so that the current can be effectively ensured to be conducted between the conductive electrode layer and the conductive coating; the metal sheet 4 is used as a current sub-carrier and plays a role in connecting the conductive electrode layer 3 with the connecting wire 7; the heating pipe 1 is used as a carrier of the conductive coating, and the insulating protective layer 5 provides insulating protection for the whole heating pipe.
FIG. 3 is a structural cross-sectional view from perspective B-B of a graphene heating tube, in accordance with the present invention; as can be seen from fig. 3, this part is the part of the heating tube for heating operation, and the heating tube is provided with a heating tube 1, a conductive coating 2 and an insulating protective layer 5 in sequence from inside to outside.
The present invention will be described in detail below by way of examples.
In the following examples and comparative examples:
coating thickness was performed according to ASTM D7091-2005;
the square resistor is tested by an RTS-9 double-electric-measurement four-probe tester, Sovium co-generation electronic equipment company;
the surface temperature, the surface temperature difference and the service life are carried out according to JGT 286-2010;
graphene is purchased from Beijing Xu carbon New Material science and technology Limited, and the graphene product specification is as follows: the number of BJ-XTA-1 lamella is 2-10, the oxygen content is 2-3 wt%, and the lamella diameter is 2-10 μm; the measurement method is specifically referred to terms, definitions and codes of T/CGIA 002-.
Example 1
This example illustrates a high-temperature graphene conductive coating and a graphene heating tube prepared by the method of the present invention.
(S1) mixing and stirring the first resin (polyimide and silicone resin) uniformly, adding the first dispersant and the coupling agent, stirring and mixing uniformly at a stirring speed of 300rpm at room temperature of 25 ℃, and slowly adding the mixed conductive powder to the mixed first resin while stirring to obtain a first mixture;
(S2) mixing and stirring the second resin (polyimide and silicone resin) uniformly at a stirring speed of 300rpm, adding the second dispersant, stirring and mixing uniformly at a stirring speed of 150rpm at room temperature of 25 ℃, and slowly adding the graphene to the mixed second resin while stirring to obtain a second mixture;
(S3) mixing the first mixture obtained in the step (S1) and the second mixture obtained in the step (S2), adding a curing accelerator and a defoaming agent, uniformly mixing, and then defoaming in vacuum to obtain a high-temperature graphene conductive coating, wherein the components and the content of the components are shown in Table 1;
(S4) coating the prepared high-temperature graphene conductive coating on the surface of the heating pipe 1, drying, and forming a conductive coating layer 2 on the surface of the heating pipe 1;
(S5) coating conductive electrode layers 3 on two sides of the heating pipe coated with the high-temperature graphene conductive coating, and drying; covering a metal sheet 4 on the dried conductive electrode layer 3;
(S6) connecting and fixing the connecting wire 7 and the metal sheet 4 by connecting the heating pipe in the step (S5) in series through a screw, a washer and a nut;
(S7) coating a layer of insulating protective layer 5 on the surface of the heating pipe in the step (S6), and drying to obtain the graphene heating pipe.
The performance of the prepared graphene heating tube was tested with the results shown in table 2.
Examples 2 to 4
The high-temperature graphene conductive coating and the graphene heating tube were prepared in the same manner as in example 1, except that: the high-temperature graphene conductive coating composition has different components and component contents, and specifically, the components and the component contents are shown in table 1;
the performance of the prepared graphene heating tube was tested with the results shown in table 2.
Examples 5 to 8
The high-temperature graphene conductive coating and the graphene heating tube were prepared in the same manner as in example 1, except that: the components and the component contents are shown in a table 1 (continued table);
results the performance of the prepared graphene heating tube was tested and the results are shown in table 2 (continuation table).
Comparative example 1
The high-temperature graphene conductive coating and the graphene heating tube were prepared in the same manner as in example 1, except that: the resin and the dispersant are fed at one time, that is, the step (S1) and the step (S2) are combined together for feeding, specifically:
(S1-S3) uniformly mixing and stirring resins (polyimide and organic silicon resin), adding a dispersing agent, a coupling agent, conductive powder and graphene, uniformly stirring and mixing at the room temperature of 25 ℃ and the stirring speed of 200rpm, adding a defoaming agent, accelerating curing, uniformly mixing, and defoaming in vacuum to obtain a high-temperature graphene conductive coating, wherein the components and the content of the components are shown in Table 1;
steps (S4) - (S7) are the same as in example 1.
The performance of the prepared graphene heating tube was tested with the results shown in table 2.
Comparative example 2
The high-temperature graphene conductive coating and the graphene heating tube were prepared in the same manner as in example 1, except that: the total weight of the first dispersant and the second dispersant is 5.5 parts by weight;
in addition, no graphene is added;
in addition, the weight ratio of the first resin to the first dispersant was 14.24, the weight ratio of the second resin to the second dispersant was 8.82, and the respective components and component contents were as shown in table 1.
The performance of the prepared graphene heating tube was tested with the results shown in table 2.
Comparative example 3
The high-temperature graphene conductive coating and the graphene heating tube were prepared in the same manner as in example 1, except that: the weight ratio of the first resin to the first dispersant was 39.58, the weight ratio of the second resin to the second dispersant was 27.5, and the respective components and component contents were as shown in table 1.
The performance of the prepared graphene heating tube was tested with the results shown in table 2.
Comparative examples 4 to 5
The high-temperature graphene conductive coating and the graphene heating tube were prepared in the same manner as in example 1, except that: the components and the component contents are shown in a table 1 (continued table);
results the performance of the prepared graphene heating tube was tested and the results are shown in table 2 (continuation table).
TABLE 1
Table 1 (continuation watch)
Remarking:
1. dispersing agent: a represents oleylaminooleate (BYK190), b represents a sodium salt of a polycarboxylic acid, and c represents polyvinyl alcohol;
2. defoaming agent: d represents silicone emulsion, e represents polyoxypropylene glyceryl ether, f represents polyoxypropylene polyoxyethylene glyceryl ether, and g represents polydimethylsiloxane;
3. coupling agent: h represents a vinyl silane coupling agent, i represents an amino silane coupling agent, and j represents an epoxy silane coupling agent;
4. conductive powder: k represents a carbon nanotube, l represents a nano silver wire, and m represents a copper nano powder;
5. curing accelerator: n represents toluene diisocyanate, o represents hydrogenated diphenylmethane diisocyanate, and p represents diphenylmethane diisocyanate.
6. The component contents in examples and comparative examples are expressed in "parts by weight".
TABLE 2
Table 2 (continuation watch)
Remarking: the surface average temperature and the surface temperature difference were measured under the condition of 220V.
The service life is characterized by the time spent by the power to decay by 10% under the voltage of 220V.
It can be seen from the above results that, with examples 1 to 8 of the present invention, the sheet resistance is low, the power density is high, the service life exceeds 30000 hours, the heating temperature is as high as 195 ℃, the surface temperature uniformity is good, and the surface temperature difference is as low as 4.0 ℃, which has significantly better effects.
Comparative example 1 failed to form good network-like conductive paths in the coating due to no addition of graphene, resulting in poor results.
Comparative example 2 has poor results because the surface of the conductive powder and the graphene powder is coated with the dispersant due to an excessively high content of the dispersant, reducing the formation of conductive paths.
Comparative example 3 has poor results because the conductive powder and the graphene powder are difficult to be uniformly dispersed in the resin due to the excessively low content of the dispersant.
Comparative example 4 since the content of the first resin was low, the conductive powder was difficult to be uniformly dispersed in the resin, easily agglomerated in the resin, and the formation of conductive paths in the coating was reduced, resulting in poor results.
Comparative example 5 since the content of the dispersant in the first resin was too low, the conductive powder was difficult to be uniformly dispersed in the resin, easily agglomerated in the resin, and the formation of conductive paths in the coating was reduced, resulting in poor results.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. The high-temperature graphene conductive coating composition is characterized by comprising graphene, conductive powder, resin, a dispersing agent and a coupling agent; and relative to 100 parts by weight of the high-temperature graphene conductive coating composition, the content of the graphene is 1-4 parts by weight, the content of the conductive powder is 10-18 parts by weight, the content of the resin is 60-85 parts by weight, the content of the dispersant is 2-4 parts by weight, and the content of the coupling agent is 1-4 parts by weight.
2. The composition according to claim 1, wherein the content of the graphene is 2 to 4 parts by weight, the content of the conductive powder is 12 to 15 parts by weight, the content of the resin is 68 to 72 parts by weight, the content of the dispersant is 3 to 4 parts by weight, and the content of the coupling agent is 2 to 4 parts by weight, relative to 100 parts by weight of the high temperature graphene conductive coating composition.
3. The composition of claim 1 or 2, wherein the resin comprises a first resin and a second resin, and the dispersant comprises a first dispersant and a second dispersant;
preferably, the weight ratio of the first resin to the first dispersant is (20-35): 1, more preferably (25-30): 1;
preferably, the weight ratio of the second resin to the second dispersant is (10-25): 1, more preferably (15-20): 1.
4. the composition of claim 3, wherein the first resin and the second resin are the same or different and are each selected from one or more of silicone resins, phenolic resins, urea-formaldehyde resins, epoxy resins, polyurethanes, and polyimides;
preferably, the weight ratio of the first resin to the second resin is (1-2): 1, more preferably (1.5-1.9): 1;
preferably, the first dispersant and the second dispersant are the same or different and are each selected from one or more of oleyl aminooleate, sodium salt of polycarboxylic acid, sodium dodecylbenzenesulfonate and polyvinyl alcohol;
preferably, the weight ratio of the first dispersant to the second dispersant is (0.5-2): 1, preferably (1-1.5): 1.
5. the composition of claim 1 or 2, wherein the conductive powder material is selected from one or more of carbon nanotubes, carbon black, acetylene black, ketjen black, silver nanowires, copper nanopowders and gold nanopowders;
preferably, the coupling agent is selected from one or more of a vinyl silane coupling agent, an amino silane coupling agent, and an epoxy silane coupling agent.
6. The composition as claimed in any one of claims 1 to 5, further comprising an antifoaming agent and a curing accelerator, wherein the antifoaming agent is present in an amount of 1 to 4 parts by weight and the curing accelerator is present in an amount of 2 to 8 parts by weight, based on 100 parts by weight of the high temperature graphene conductive coating composition;
preferably, the content of the defoaming agent is 2 to 4 parts by weight and the content of the curing accelerator is 5 to 8 parts by weight with respect to 100 parts by weight of the high-temperature graphene conductive coating composition.
7. A method for preparing a high-temperature graphene conductive coating by using the composition as claimed in any one of claims 1 to 6, wherein the method comprises the following steps:
(1) in the presence of a first dispersing agent, contacting conductive powder, a first resin and a coupling agent for first mixing to obtain a first mixture;
(2) in the presence of a second dispersing agent, contacting graphene with a second resin for second mixing to obtain a second mixture;
(3) and contacting the first mixture and the second mixture for third mixing to obtain the high-temperature graphene conductive coating.
8. The method of claim 7, further comprising: in the step (3), the first mixture, the second mixture, a defoaming agent and a curing accelerator are contacted to perform fourth mixing, so that the high-temperature graphene conductive coating is obtained.
9. A high temperature graphene conductive coating prepared by the method of claim 7 or 8.
10. The graphene heating tube is characterized by comprising a tube body and a conductive coating coated on the surface of the tube body, wherein the conductive coating is the high-temperature graphene conductive coating according to claim 9.
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