CN109705677B - Electrothermal coating based on graphene three-dimensional network structure carbon coating technology and preparation method thereof - Google Patents
Electrothermal coating based on graphene three-dimensional network structure carbon coating technology and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an electrothermal coating based on a graphene three-dimensional network structure carbon coating technology, which is prepared by the following steps: (1) preparing carbon-coated heating particles; (2) preparing carbon-coated heating particles coated with graphene oxide; (3) preparing reduced graphene oxide coated carbon-coated heating particles; (4) and preparing the carbon-coated electrothermal coating with the graphene three-dimensional network structure. The product of the invention has the advantages of fast heating, high heat conversion rate and high far infrared radiation rate.
Description
Technical Field
The invention relates to the technical field of preparation of electrothermal coatings, in particular to an electrothermal coating based on a graphene multi-coating technology.
Background
The electrothermal film product is a film product which can generate heat after being electrified, is prepared by forming a film on electrothermal coating, assisting with conductive leads such as metal current-carrying strips and conductive silver paste and matching with an intelligent control system, has the advantages of no water consumption, energy saving, land saving, material saving, environmental protection, arbitrary switch adjustment, convenience for household metering and the like, and accords with the low-carbon direction. Through the development of many years, the electrothermal film product is widely applied to the fields of industry, agriculture, traffic, household and the like, and particularly has wide development space in the face of the influence of environmental and policy factors such as air pollution, coal-to-electricity and the like.
The key of the electrothermal film product is the electrothermal coating used as a heating body, and the quality of the electrothermal coating directly determines the quality of the product. At present, most of related products in domestic markets have the problems of power attenuation, low heat conversion efficiency and the like no matter traditional heating base materials such as high polymers, printing ink, carbon fibers, metal wires (sheets) and the like are adopted, or heating base materials such as silicon crystals, carbon elements and the like which are raised in recent years are adopted. In view of the disadvantage of low efficiency of the conventional electric heating technology, the development of high performance heating materials with low resistance, high thermal conductivity and high heat resistance stability is becoming a necessary trend in future development.
Graphene is a polymer made of carbon atoms in sp2The hybrid orbit forms a two-dimensional material with hexagonal symmetric lattice and only one carbon atom thickness, and the unique structure endows the graphene with excellent electrical, optical, mechanical and thermal properties, such as: the graphene has the thermal conductivity coefficient of 5300W/m.K, which is higher than that of the carbon nano tube and the diamond, and is an excellent heat dissipation material; the electron mobility at normal temperature exceeds 15000cm2V ∙ s, which is 100 times of silicon; meanwhile, when graphene is heated, carbon atoms are excited and can emit 8-15 μm far-infrared waves. Therefore, the novel electrothermal coating which has the functions of not attenuating power, rapidly increasing temperature, having no electromagnetic radiation, improving human microcirculation, improving human immunity and the like is obtained by means of the graphene technology, and becomes a brand new research field.
Disclosure of Invention
In view of the above problems in the prior art, the applicant of the present invention provides an electrothermal coating containing graphene and a preparation method thereof. The product of the invention has the advantages of fast heating, high heat conversion rate and high far infrared radiation rate.
The technical scheme of the invention is as follows:
an electrothermal coating based on a graphene three-dimensional network structure carbon coating technology is prepared by the following steps:
(1) dispersing the submicron heating particles in an aqueous solution of a water-soluble biomass carbon source, carrying out hydrothermal reaction, and then carrying out solid-liquid separation and drying to obtain carbon-coated heating particles;
(2) uniformly dispersing the carbon-coated heating particles obtained in the step (1) in a graphene oxide aqueous solution, and drying to realize secondary coating of the carbon-coated heating particles obtained in the step (1) by graphene oxide to obtain carbon-coated heating particles coated by graphene oxide;
(3) carrying out thermal reduction treatment on the carbon-coated heating particles coated with the graphene oxide obtained in the step (2) to obtain reduced graphene oxide-coated carbon-coated heating particles;
(4) adding the reduced graphene oxide coated carbon-coated heating particles and conductive graphene powder prepared in the step (3) into base resin, and uniformly dispersing to prepare an electric heating coating slurry; after the slurry is coated on the surface of a base material and dried, the carbon-coated electric heating coating with the graphene three-dimensional network structure can be obtained.
The submicron heating particles in the step (1) are one or more of tourmaline, medical stone, biochar, far infrared ceramic powder, metal oxide, non-metal oxide, carbide, nitride and boride with a porous structure; the submicron heating particles are particles with the three-dimensional direction scale not larger than 1 mu m; the water-soluble biomass carbon source is one or more of glucose, sucrose, chitosan and starch; the concentration of the water solution of the biomass carbon source is 10-200 mg/mL.
The dispersing method in the step (1) is one or more of ultrasonic dispersing, stirring dispersing and high-speed shearing; the mass ratio of the submicron heating particles to the water-soluble biomass carbon source is 50/1-1/50.
The hydrothermal reaction conditions in the step (1) are as follows: and (3) performing heat treatment reaction in a closed container at the temperature of 120-300 ℃ for 0.5-100 h.
The concentration of the graphene oxide aqueous solution in the step (2) is 0.05-10 mg/mL; the mass ratio of carbon to oxygen elements of the graphene oxide is less than 5; the mass ratio of the graphene oxide to the carbon-coated heating particles is 1/2-1/50.
The drying treatment in the step (2) is to obtain a graphene oxide coated product by means of a two-dimensional structure of graphene oxide and a natural shrinkage effect in a drying process of the graphene oxide after materials are uniformly mixed and are subjected to one or more of natural evaporation, spray drying, freeze drying and heat drying.
The thermal reduction treatment in the step (3) is to react for 0.5-100 hours at the temperature of 300-1000 ℃ under the protection of inert and/or reducing atmosphere.
The conductive graphene powder in the step (4) is a graphene powder material with a mass ratio of carbon to oxygen of not less than 10/1 and a conductivity of not less than 10S/cm.
The electrothermal coating slurry in the step (4) comprises the following components in parts by weight:
10-25 parts of reduced graphene oxide coated carbon-coated heating particles
2-10 parts of conductive graphene powder
75-90 parts of base resin.
The base resin in the step (3) comprises the following components in parts by weight:
the resin is one or more of acrylic resin, polyurethane resin and epoxy resin;
the basic solvent is one or more of isopropanol, acetone, dimethylformamide, N-methyl pyrrolidone, butyl acetate, xylene and cyclohexanone.
The electric heating coating coated with the graphene three-dimensional network structure carbon in the step (3) is characterized in that after the electric heating coating slurry is coated on the surface of a base material and dried, the surfaces of submicron heating particles in the coating are respectively coated with a biomass hydrothermal carbonization layer and a graphene oxide thermal reduction coating layer, and the carbon-coated heating particles coated with the reduced graphene oxide and conductive graphene form a three-dimensional cross-linked network structure.
The beneficial technical effects of the invention are as follows:
according to the invention, the heating particles are subjected to hydrothermal carbon coating, so that in-situ carbon coating on the surfaces of the heating particles is realized, the contact resistance among the heating particles is greatly improved, and further, the secondary carbon coating of the heating particles by the graphene oxide is realized by virtue of the two-dimensional structure characteristics of the graphene oxide and the natural coating shrinkage effect of the graphene oxide in the drying process. The secondary carbon coating changes the original point contact of the heating particles into point-to-surface contact, thereby further reducing the contact resistance. Meanwhile, due to the fact that the hydrothermal carbon and the graphene oxide are rich in oxygen-containing functional groups on the surfaces of the hydrothermal carbon and the graphene oxide, the original materials among the materials can be further coated after thermal reduction treatment, the oxygen-containing functional groups perform chemical reaction with each other, and finally the heating particle body is reduced to the chemical coating product of the graphene oxide through hydrothermal carbon coating bridging. By means of the carbon coating technology, the three-dimensional network structure distribution formed by the carbon coating technology and the conductive graphene in the base resin, and the excellent properties of the graphene, such as thermal property, electrical property, mechanical property, optical property and the like, the original point contact structure between heating particles is changed into a stable and effective three-dimensional surface contact structure, so that the performance of the prepared electrothermal coating is improved in the aspects of low resistance, high thermal conductivity, high heat-resistant stability, high thermal conversion rate, excellent far infrared emission and the like, and a key raw material is provided for related products of high-quality electrothermal films.
Drawings
FIG. 1 is a TEM image of hydrothermal carbon-coated heat-generating particles obtained in example 1 of the present invention;
fig. 2 is a transmission electron microscope image of the graphene oxide-coated carbon-coated heating particle obtained in example 1 of the present invention;
FIG. 3 is a transmission electron microscope photograph of the electrothermal coating obtained in example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
An electrothermal coating based on a graphene three-dimensional network structure carbon coating technology is prepared by the following steps:
(1) preparation of carbon-coated exothermic particles
Dissolving 5g of glucose in 500ml of water to obtain 500ml of biomass carbon source aqueous solution with the concentration of 10 mg/ml;
adding 50g of tourmaline powder with the diameter not more than 500nm, 100g of medical stone powder with the diameter not more than 1 mu m and 100g of zinc oxide with the diameter not more than 400nm into the obtained biomass carbon source aqueous solution; dispersing heating particles in a biomass carbon source aqueous solution by ultrasound with stirring;
pouring the mixed solution into a reaction kettle, sealing, carrying out hydrothermal reaction at 300 ℃ for 0.5h, cooling the reaction kettle to room temperature after the reaction is finished, opening the reaction kettle, centrifuging or filtering the material to realize solid-liquid separation of the material, and drying the obtained solid powder material at 80 ℃ for 5h to obtain the hydrothermal carbon-coated heating particles. Fig. 1 shows a transmission electron microscope image of the hydrothermal carbon-coated heat-generating particles, and it is apparent from fig. 1 that the surfaces of the particles are coated with a carbon film.
(2) Preparation of graphene oxide-coated carbon-coated heating particles
Weighing 4mg of graphene oxide powder with a carbon-oxygen ratio of 4, and dispersing the graphene oxide powder in 200ml of water to obtain 200ml of graphene oxide aqueous solution with a concentration of 0.05 mg/ml;
adding a graphene oxide aqueous solution into 0.2g of the carbon-coated heating particles obtained in the step (1), and then performing spray drying on the mixed solution to obtain the carbon-coated heating particles coated by the graphene oxide; the transmission electron microscope image of the particle is shown in fig. 2, and it is obvious from fig. 2 that the surface of the particle is coated with graphene oxide.
(3) Preparation of reduced graphene oxide-coated carbon-coated heating particles
And carrying out thermal reduction reaction on the carbon-coated heating particles coated by the graphene oxide at 1000 ℃ for 0.5h under the protection of nitrogen to obtain reduced graphene oxide-coated carbon-coated heating particle powder.
(4) Preparation of electrothermal coating
Weighing 100mg of the product obtained in the step (3), 20mg of conductive graphene powder (the carbon-oxygen ratio is 10, and the conductivity is more than 10S/cm), and adding the conductive graphene powder into 88mg of base resin (the components of the base resin comprise 50 parts of acrylic resin, 48 parts of acetone, 0.5 part of flatting agent, 0.5 part of defoaming agent, 0.5 part of coupling agent and 0.5 part of dispersing agent); and shearing and dispersing the mixed solution at a high speed for 10min to obtain the electrothermal coating slurry.
Uniformly coating the obtained electrothermal coating slurry on the surface of a PET film, and drying at 90 ℃ to obtain the carbon-coated electrothermal coating with the graphene three-dimensional network structure. As shown in fig. 3, it can be seen from fig. 3 that the surfaces of the submicron heating particles in the coating are respectively coated with a biomass hydrothermal carbonization layer and a graphene oxide thermal reduction coating layer, and the carbon-coated heating particles coated with the reduced graphene oxide and the conductive graphene form a three-dimensional cross-linked network structure. The coating was subjected to a sheet resistance test, and the results of the test were shown in test example 1.
Example 2
An electrothermal coating based on a graphene three-dimensional network structure carbon coating technology is prepared by the following steps:
(1) preparation of carbon-coated exothermic particles
500g of glucose is dissolved in 2500ml of water to obtain 2500ml of biomass carbon source aqueous solution with the concentration of 200 mg/ml;
adding 10g of silicon carbide powder with the diameter not more than 1 mu m into the obtained biomass carbon source aqueous solution; dispersing the heating particles in a biomass carbon source aqueous solution through shearing dispersion;
pouring the mixed solution into a reaction kettle, sealing, carrying out hydrothermal reaction at 120 ℃ for 100 hours, cooling the reaction kettle to room temperature after the reaction is finished, opening the reaction kettle to carry out material centrifugation or suction filtration, realizing solid-liquid separation of the materials, and drying the obtained solid powder material at 100 ℃ for 2 hours to obtain the hydrothermal carbon-coated heating particles.
(2) Preparation of graphene oxide-coated carbon-coated heating particles
Weighing 2g of graphene oxide powder with a carbon-oxygen ratio of 5, and dispersing the graphene oxide powder in 200ml of water to obtain 200ml of graphene oxide aqueous solution with a concentration of 10 mg/ml;
adding a graphene oxide aqueous solution into 4g of the carbon-coated heating particles obtained in the step (1), and then performing spray drying on the mixed solution to obtain carbon-coated heating particles coated with graphene oxide;
(3) preparation of reduced graphene oxide-coated carbon-coated heating particles
And carrying out thermal reduction reaction on the carbon-coated heating particles coated by the graphene oxide at 300 ℃ for 100h under the protection of nitrogen to obtain reduced graphene oxide-coated carbon-coated heating particle powder.
(4) Preparation of electrothermal coating
Respectively weighing 1g of the product obtained in the step (3), 1g of conductive graphene powder (the carbon-oxygen ratio is 20, and the conductivity is more than 100S/cm), and adding 8g of base resin (the components of the base resin comprise 70 parts of acrylic resin, 29 parts of acetone, 0.2 part of flatting agent, 0.2 part of defoaming agent, 0.2 part of coupling agent and 0.4 part of dispersing agent); and shearing and dispersing the mixed solution at a high speed for 30min to obtain the electrothermal coating slurry.
Uniformly coating the obtained electrothermal coating slurry on the surface of the stone, and drying at 100 ℃ to obtain the carbon-coated electrothermal coating with the graphene three-dimensional network structure.
Example 3
An electrothermal coating based on a graphene three-dimensional network structure carbon coating technology is prepared by the following steps:
(1) preparation of carbon-coated exothermic particles
Dissolving 250g of glucose in 2500ml of water to obtain 2500ml of biomass carbon source aqueous solution with the concentration of 100 mg/ml;
adding 3g of far infrared ceramic powder with the diameter not more than 200nm, 3g of silicon carbide powder with the diameter not more than 1 mu m and 4g of zirconium oxide powder with the diameter not more than 500nm into the obtained biomass carbon source aqueous solution; dispersing the heating particles in a biomass carbon source aqueous solution through shearing dispersion;
pouring the mixed solution into a reaction kettle, sealing, carrying out hydrothermal reaction at 180 ℃ for 10 hours, cooling the reaction kettle to room temperature after the reaction is finished, opening the reaction kettle to carry out material centrifugation or suction filtration, realizing solid-liquid separation of the materials, and drying the obtained solid powder material at 120 ℃ for 1 hour to obtain the hydrothermal carbon-coated heating particles.
(2) Preparation of graphene oxide-coated carbon-coated heating particles
Weighing 5g of graphene oxide powder with a carbon-oxygen ratio of 3, and dispersing the graphene oxide powder in 1000ml of water to obtain 1000ml of graphene oxide aqueous solution with a concentration of 5 mg/ml;
adding a graphene oxide aqueous solution into 5g of the carbon-coated heating particles obtained in the step (1), and then performing spray drying on the mixed solution to obtain carbon-coated heating particles coated with graphene oxide;
(3) preparation of reduced graphene oxide-coated carbon-coated heating particles
And carrying out thermal reduction reaction on the carbon-coated heating particles coated by the graphene oxide at 500 ℃ for 10 hours under the protection of nitrogen to obtain reduced graphene oxide-coated carbon-coated heating particle powder.
(4) Preparation of electrothermal coating
Respectively weighing 5g of the product obtained in the step (3), 4g of conductive graphene powder (the carbon-oxygen ratio is 15, and the conductivity is more than 500S/cm), and adding the conductive graphene powder into 90g of base resin (the components of the base resin comprise 60 parts of polyurethane resin, 39 parts of acetone, 0.3 part of flatting agent, 0.3 part of defoaming agent, 0.1 part of coupling agent and 0.3 part of dispersing agent); and shearing and dispersing the mixed solution at a high speed for 60min to obtain the electrothermal coating slurry.
Uniformly coating the obtained electrothermal coating slurry on the surface of the stone, and drying at 100 ℃ to obtain the carbon-coated electrothermal coating with the graphene three-dimensional network structure.
Test example:
the square resistance test of the electrothermal coating obtained in example 1 and the commercially available electrothermal coating is performed, and the test results are shown in table 1, and it is obvious from table 1 that the square resistance of the electrothermal coating obtained in example 1 of the present invention is 9.38 Ω/□ which is much smaller than the square resistance of the commercially available electrothermal coating, 374.2 Ω/□.
TABLE 1
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An electrothermal coating based on a graphene three-dimensional network structure carbon coating technology is characterized by being prepared by the following steps:
(1) dispersing the submicron heating particles in an aqueous solution of a water-soluble biomass carbon source, carrying out hydrothermal reaction, and then carrying out solid-liquid separation and drying to obtain carbon-coated heating particles; the submicron heating particles in the step (1) are one or more of tourmaline, medical stone, biochar, far infrared ceramic powder, metal oxide, non-metal oxide, carbide, nitride and boride with a porous structure; the submicron heating particles are particles with the three-dimensional direction scale not larger than 1 mu m;
(2) uniformly dispersing the carbon-coated heating particles obtained in the step (1) in a graphene oxide aqueous solution, and drying to realize secondary coating of the carbon-coated heating particles obtained in the step (1) by graphene oxide to obtain carbon-coated heating particles coated by graphene oxide;
(3) carrying out thermal reduction treatment on the carbon-coated heating particles coated with the graphene oxide obtained in the step (2) to obtain reduced graphene oxide-coated carbon-coated heating particles;
(4) adding the reduced graphene oxide coated carbon-coated heating particles and conductive graphene powder prepared in the step (3) into base resin, and uniformly dispersing to prepare an electric heating coating slurry; after the slurry is coated on the surface of a base material and dried, the carbon-coated electric heating coating with the graphene three-dimensional network structure can be obtained.
2. The electrothermal coating of claim 1, wherein the water-soluble biomass carbon source is one or more of glucose, sucrose, chitosan, starch; the concentration of the water solution of the biomass carbon source is 10-200 mg/mL.
3. The electrothermal paint according to claim 1, wherein the dispersing method in step (1) is one or more of ultrasonic dispersing, stirring dispersing, and high-speed shearing; the mass ratio of the submicron heating particles to the water-soluble biomass carbon source is 50/1-1/50.
4. The electrothermal paint according to claim 1, wherein the hydrothermal reaction in step (1) is carried out under the following conditions: and (3) performing heat treatment reaction in a closed container at the temperature of 120-300 ℃ for 0.5-100 h.
5. The electrothermal paint of claim 1, wherein the concentration of the graphene oxide aqueous solution in the step (2) is 0.05-10 mg/mL; the mass ratio of carbon to oxygen elements of the graphene oxide is less than 5; the mass ratio of the graphene oxide to the carbon-coated heating particles is 1/2-1/50.
6. The electrothermal coating material according to claim 1, wherein the drying treatment in step (2) is a graphene oxide coated product obtained by means of a two-dimensional structure of graphene oxide and a natural shrinkage effect during drying of the graphene oxide after the materials are uniformly mixed and one or more of natural evaporation, spray drying, freeze drying and heat drying.
7. The electrothermal coating material of claim 1, wherein the thermal reduction treatment in step (3) is carried out at 300-1000 ℃ for 0.5-100 h under the protection of inert and/or reducing atmosphere.
8. The electrothermal paint of claim 1, wherein the conductive graphene powder in the step (4) is a graphene powder material with a mass ratio of carbon to oxygen of not less than 10/1 and an electrical conductivity of not less than 10S/cm.
9. The electrothermal coating of claim 1, wherein the electrothermal coating slurry in the step (4) comprises the following components in parts by weight:
10-25 parts of reduced graphene oxide coated carbon-coated heating particles
2-10 parts of conductive graphene powder
75-90 parts of base resin.
10. The electrothermal paint of claim 1, wherein the base resin in the step (3) comprises the following components in parts by weight:
the resin is one or more of acrylic resin, polyurethane resin and epoxy resin;
the basic solvent is one or more of isopropanol, acetone, dimethylformamide, N-methyl pyrrolidone, butyl acetate, xylene and cyclohexanone.
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