CN112409856A - Improved preparation method of heat-preservation graphene floor heating film - Google Patents
Improved preparation method of heat-preservation graphene floor heating film Download PDFInfo
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F15/00—Flooring
- E04F15/02—Flooring or floor layers composed of a number of similar elements
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0893—Zinc
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/324—Alkali metal phosphate
Abstract
An improved preparation method of a heat-preservation graphene floor heating film comprises the following steps: s1, after leveling construction ground, coating the ground to form a basement membrane, wherein coating materials of the basement membrane specifically comprise: 25-30 parts of hollow titanium oxide powder and 65-80 parts of base membrane main material; s2, after the base film is coated and before curing, laying a prefabricated graphene floor heating film, wherein the graphene floor heating film comprises a graphene electric heating film and a connecting layer located below the graphene electric heating film, and the graphene electric heating film comprises a metal base material and a graphene film located below the metal base material. According to the invention, the bottom film with the heat preservation and reflection functions is coated on the leveled ground surface, so that the effects of heat insulation and heat preservation can be achieved, the concave-convex ground is filled, a flat construction surface is provided for the graphene floor heating film above the bottom layer, the metal base material is not easy to deform in the construction process, and the floor heating construction quality is improved.
Description
Technical Field
The invention belongs to the technical field of graphene, and particularly relates to a preparation method of an improved heat-preservation graphene floor heating film.
Background
The graphene has excellent mechanical, electrical and thermal properties, and can convert the excellent properties of the monolithic graphene into the properties of macroscopic materials to a certain extent through specific chemical assembly. The graphene film is a typical graphene macroscopic material, and has good electric conductivity and electric heating performance and high electric-heating conversion efficiency. The composite material has wide application prospect in the fields of pipeline anti-freezing, building heating systems and the like, and is expected to replace the existing floor heating and fireplace products. However, most of the graphene electrothermal films reported at present are resistant to double-sided heating, and a part of heat energy is wasted on the back of the graphene electrothermal films due to poor heat insulation performance in application of floor heating and fireplace products to a great extent, so that the applicant provides a preparation method of a heat-insulation type graphene electrothermal film and discloses the preparation method in the Chinese patent application with the application number of 2019105738908.
In the construction operation, when finding that the heat preservation bottom layer at the back of the graphene electrothermal film is laid on the concrete floor slab after construction leveling, because the surface of the concrete floor slab after construction leveling has a large number of concave-convex structures with millimeter sizes, the heat preservation connection layer is laid on the concave-convex structures, in the subsequent construction process, the concave-convex structures extrude the heat preservation connection layer, so that the heat preservation connection layer or the metal base material is deformed, the lamination and the chapping are easy to occur in the subsequent construction, and the heat preservation effect obtained by the original formula still has the space for further promotion.
Disclosure of Invention
In order to overcome the technical defects in the prior art, the invention discloses an improved preparation method of a heat-preservation graphene floor heating film.
The improved preparation method of the heat-preservation graphene floor heating film comprises the following steps:
s1, after leveling construction ground, coating the leveling ground to form a basement membrane, wherein the coating material of the basement membrane comprises the following specific components in parts by mass:
25-30 parts of hollow titanium oxide powder, 65-80 parts of base membrane main material, 0.01-0.5 part of defoaming agent, 0.05-0.5 part of thickening agent, 0.1-0.5 part of film-forming assistant and 1-3 parts of dispersing agent; the particle size of the hollow titanium oxide powder is 1-10 microns, and the wall thickness is 100-2000 nm; the coating amount per square meter of ground is 10-50 g when the wall thickness is coated;
s2, after the base film is coated and before curing, laying a prefabricated graphene floor heating film, wherein the graphene floor heating film comprises a graphene electric heating film and a connecting layer located below the graphene electric heating film, and the graphene electric heating film comprises a metal base material and a graphene film located below the metal base material.
Preferably, the joining layer of the graphene floor heating film is prepared by the following method:
mixing, heating and uniformly mixing the silicone-acrylic emulsion and the water-based fluorocarbon emulsion according to the volume ratio of 1:0.5-5, and mixing according to the ratio of 1: 4-6, introducing the mixture into a high-speed stirrer, stirring for 30-40min, and preparing a film-shaped connecting layer by using a blow molding machine after uniform mixing;
the mixed resin is prepared from the following components in percentage by mass of 3: 0.5-1:0.3-0.6:0.5-1 of zinc powder, cellulose, acrylic resin and conductive epoxy resin.
Further, the base material of the base film is fluorocarbon resin.
Furthermore, the linking layer is connected with the graphene electrothermal film through a high-temperature-resistant conductive adhesive.
Preferably, the metal substrate is a copper foil or an aluminum foil.
Preferably, the preparation method of the hollow titanium oxide powder comprises the following steps:
adding TiCl4 into the ionic liquid and stirring uniformly to form TiCl4 solution with the concentration of 0.8-1.5 mol/L;
slowly adding deionized water, standing for 12-48 hours, and obtaining a solid precipitate after TiCl4 is completely hydrolyzed;
and (3) alternately washing the solid precipitate for multiple times by using deionized water and ethanol, centrifugally separating, drying and roasting to obtain the titanium dioxide hollow spherical powder.
Further, the ionic liquid is imidazole salt ionic liquid.
By adopting the improved preparation method of the heat-preservation graphene floor heating film, the bottom film with the heat-preservation reflection function is coated and formed on the leveled ground surface through process change, so that the heat-preservation and heat-insulation effects can be achieved, the concave-convex ground is filled, a flat construction surface is provided for the graphene floor heating film above the bottom layer, the metal base material is not prone to deformation in the construction process, and the floor heating construction quality is improved.
Drawings
Fig. 1 is a schematic diagram of a specific embodiment of forming a graphene floor heating structure by using the preparation method of the present invention;
FIG. 2 is a photograph of the hollow titanium oxide powder of the present invention under a scanning electron microscope;
the reference numbers in the figures refer to: 1-leveling ground, 2-floor layer, 3-bottom film, 4-joining layer, 5-conductive adhesive, 6-graphene film and 7-metal substrate.
Detailed Description
The following provides a more detailed description of the present invention.
The improved preparation method of the heat-preservation graphene floor heating film comprises the following steps:
s1, after leveling construction ground, coating on the leveling ground 1 to form a basement membrane 3, wherein coating materials of the basement membrane specifically comprise:
25-30 parts of hollow titanium oxide powder, 65-80 parts of base membrane main material, 0.01-0.5 part of defoaming agent, 0.05-0.5 part of thickening agent, 0.1-0.5 part of film-forming assistant and 1-3 parts of dispersing agent; the coating amount of each square meter of ground is 10-30 g when coating;
s2, after the base film is coated and before the base film is solidified, laying a prefabricated graphene floor heating film, wherein the graphene floor heating film comprises a graphene electric heating film and a linking layer 4 positioned below the graphene electric heating film, and the graphene electric heating film comprises a metal base material 7 and a graphene film 6 positioned below the metal base material 7
Firstly, the leveled ground is coated to form a bottom film, the microcosmic uneven plane after ground leveling can be made up through the liquid bottom film in the initial state, the flatness of the upper surface after coating and curing is further improved, and titanium oxide powder and zinc powder have a filling effect on ground pits.
The particle size of the titanium oxide powder particles is usually 1000-10000 nm (1-10 microns), the refractive index is high and is changed along with the change of the wall thickness and the particle size, the temperature of the common household floor heating is usually 22-28 ℃, the wavelength of an infrared band generated by heating the electric heating film is in the range of 200-1800 microns, the refractive index of the room temperature infrared ray of the titanium oxide powder particles with the wall thickness of about 100-2000 nm can reach more than 2.0, and a large amount of hollow titanium oxide powder particles refract the infrared ray for multiple times and can reflect the infrared ray to the upper part of the floor, so that the effects of heat preservation and heat reflection are achieved.
The fluorocarbon resin has good compatibility with titanium oxide powder particles, plays a good role in fixing and adhering the titanium oxide powder particles, and is used as a base membrane main body to be more easily attached to a graphene electrothermal film connecting layer in a solidification process.
And before the bottom film is solidified, covering a prefabricated graphene geothermal film to enable the prefabricated graphene geothermal film to be tightly bonded with fluorocarbon resin on the bottom film.
The film-forming assistant may be benzyl alcohol BA, propylene glycol, etc. The defoaming agent can be polyethylene glycol, sodium dodecyl benzene sulfonate, the thickening agent can be hydroxymethyl cellulose, and the dispersing agent can be sodium phosphate or sodium trimetaphosphate, etc.
The prefabrication of the graphene electrothermal film comprises prefabrication of a connecting layer:
mixing, heating and uniformly mixing the silicone-acrylic emulsion and the water-based fluorocarbon emulsion according to the volume ratio of 1:0.5-5, and mixing according to the ratio of 1: 4-6, introducing the mixture into a high-speed stirrer, stirring for 30-40min, and preparing a film-shaped connecting layer by using a blow molding machine after uniform mixing;
the mixed resin is prepared from the following components in percentage by mass of 3: 0.5-1:0.3-0.6:0.5-1 of zinc powder, cellulose, acrylic resin and conductive epoxy resin.
The zinc powder is added into the connecting layer, the particle size of the zinc powder can be the same as or similar to that of titanium oxide particles, for example, the particle size of the zinc powder particles can be in the range of 1-100 micrometers, and from the physical structure, the connecting layer and the bottom film are provided with particles with similar particle sizes, so that the particles can still easily form a snap fit in the micrometer size, and are not easy to translate on a horizontal plane, and the construction is convenient. The zinc is used as a metal material, has good heat conductivity, and can quickly transfer the heat reflected by the titanium oxide powder upwards.
Zinc powder is added into the connecting layer and is attached to a metal base material of the graphene electrothermal film, the metal base material is generally copper foil or aluminum foil and the like, the potential of the metal zinc is lower in metal, after impurity metal in the metal base material is in electric contact with the zinc, the metal zinc is used as a negative electrode in the corrosion effect of a primary battery caused by connection of metals with different potentials, the corrosion speed of the metal base material can be greatly delayed, and the service life is prolonged.
And uniformly coating high-temperature-resistant conductive adhesive 5 on the obtained heat-preservation joining layer and one side of the graphene electrothermal film, pressing the heat-preservation joining layer and the side of the graphene electrothermal film coated with the high-temperature-resistant conductive adhesive at a relatively high pressure and a high temperature, and cooling to obtain a finished product. The high-temperature-resistant conductive adhesive can be DB2012 copper powder conductive adhesive.
The laminating pressure of the heat-preservation connecting layer and the graphene electrothermal film is 30-45MPa, and the laminating temperature is 90-120 ℃.
The hollow titanium oxide powder used in the present invention can be produced by the following method:
firstly, adding TiCl4 into a proper amount of ionic liquid, uniformly stirring by ultrasonic to form a solution with the concentration of 0.8-1.5 mol/L, then slowly adding deionized water, and initially sealing the lower layer of ionic liquid by water at the upper layer; after a certain period of time, generally standing at normal temperature within 12-48 hours, gradually introducing water into an ionic liquid layer to hydrolyze TiCl4 to obtain a precipitate, wherein the obtained solution still has a layering phenomenon, the upper layer liquid is separated according to colors, the ionic liquid can be recycled, the precipitate is washed by deionized water and ethanol for multiple times, centrifugally separated, dried and baked to obtain titanium dioxide hollow spherical powder with the particle size of about 1-10 microns, and the finally obtained hollow powder can be adjusted by adjusting the concentration of the initially formed ionic liquid TiCl4, so that the particle size is generally increased, the particle size is increased, but is not in a linear relationship.
The film-forming assistant may be benzyl alcohol BA, propylene glycol, etc. The defoaming agent can be polyethylene glycol, sodium dodecyl benzene sulfonate, the thickening agent can be hydroxymethyl cellulose, and the dispersing agent can be sodium phosphate or sodium trimetaphosphate, etc.
Detailed description of the preferred embodiment 1
S1, after leveling construction ground, coating on the leveling ground to form a basement membrane, wherein the specific ratio of coating materials of the basement membrane is as follows:
25 parts of hollow titanium oxide powder, 70 parts of fluorocarbon resin, 0.1 part of polyethylene glycol, 0.05 part of hydroxymethyl cellulose, 0.2 part of benzyl alcohol BA and 1 part of sodium phosphate; coating according to the coating amount of 15 g per square meter of ground when the coating is carried out according to the wall thickness;
and S2, laying the prefabricated graphene floor heating film after the bottom film is coated and before the bottom film is solidified.
After the graphene floor heating film is laid, a floor layer 2 is laid on the graphene floor heating film to complete floor heating construction.
Specific example 2
S1, after leveling construction ground, coating the leveling ground to form a basement membrane, wherein the coating material of the basement membrane comprises the following specific components in parts by mass:
30 parts of hollow titanium oxide powder, 80 parts of fluorocarbon resin, 0.3 part of sodium dodecyl benzene sulfonate serving as a defoaming agent, 0.4 part of thickening agent hydroxymethyl cellulose, 0.3 part of film-forming assistant propylene glycol and 2 parts of dispersant sodium phosphate; the coating amount of each square meter of ground is 35 g when coating;
s2, after the base film is coated and before curing, laying a prefabricated graphene floor heating film, wherein the graphene floor heating film comprises a graphene electric heating film and a connecting layer located below the graphene electric heating film, and the graphene electric heating film comprises a metal base material and a graphene film located below the metal base material.
After the graphene floor heating film is laid, a floor layer is laid on the graphene floor heating film to complete floor heating construction.
In specific embodiments 1 and 2, compared with the manner of directly laying the prefabricated floor heating film described in the reference documents mentioned in the background art, not only is the laying efficiency improved, but also the heating power consumption is respectively reduced by 3.6% and 5.0% for rooms with the same area and the same temperature.
Specific example 3
The graphene floor heating film is prepared by the following method.
The graphene floor heating film is characterized in that a connecting layer of the graphene floor heating film is prepared by the following method:
mixing the silicone-acrylic emulsion and the aqueous fluorocarbon emulsion according to the volume ratio of 1:1, heating and uniformly mixing, and mixing according to the ratio of 1: 5, introducing the mixture into a high-speed stirrer to be stirred for 40min, and preparing a film-shaped connecting layer by using a blow molding machine after uniform mixing;
wherein the mixed resin is prepared from the following components in a mass ratio of 3: 0.5:0.3:0.5 of zinc powder, cellulose, acrylic resin and conductive epoxy resin.
Prefabricating a graphene electrothermal film:
putting a metal base material into an ultrasonic cleaning machine, cleaning the metal base material by using ionized water and ethanol, and then air-drying the metal base material, wherein the metal base material is a copper foil, and an auxiliary cosolvent is added into graphene, and the auxiliary solvent consists of ethylene glycol, glycerol, a cross-linking agent and a cosolvent; the weight ratio of the ethylene glycol to the glycerol to the cross-linking agent to the cosolvent is 3:1:4:6, the mixture is stirred at a constant speed for 30min, then ultrasonic dispersion is carried out for 50min, then mixed resin is added, the mixture is introduced into a high-speed stirrer and stirred for 60min, heating and concentration are carried out, then chemical vapor deposition is carried out to prepare graphene conductive film coating liquid, the graphene conductive film coating liquid is defoamed and then is filled into a spray gun, the graphene conductive film coating liquid is uniformly sprayed on the surface of a metal base material, a hot-pressing roller at 55-65 ℃ is used for rolling and flattening the graphene conductive film coating liquid and carrying out pre-vulcanization, and then vulcanization is carried out in an oven at 90-;
and uniformly coating high-temperature-resistant conductive adhesive on the obtained heat-preservation joining layer and one side of the graphene electrothermal film, wherein the temperature resistance height of the high-temperature-resistant conductive adhesive is more than 200 ℃, pressing the heat-preservation joining layer and the side, coated with the high-temperature-resistant conductive adhesive, of the graphene electrothermal film at a relatively high pressure and a high temperature, cooling to obtain a finished product, and the high-temperature-resistant conductive adhesive can be DB2012 copper powder conductive adhesive. The laminating pressure of the heat-preservation connecting layer and the graphene electrothermal film is 30-45MPa, and the laminating temperature is 110-120 ℃.
Specific example 4
The preparation method of the hollow titanium oxide powder comprises the following steps:
adding TiCl4 into 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid, and uniformly stirring to form TiCl4 solution with the concentration of 1.2 mol/L;
slowly adding deionized water, standing for 30 hours, and obtaining a solid precipitate after TiCl4 is completely hydrolyzed;
washing the solid precipitate with deionized water and ethanol alternately for four times, centrifuging, drying, and roasting to obtain titanium dioxide hollow spherical powder; as shown in FIG. 2, the particle size of the obtained powder was mostly distributed in the range of 3 to 6 μm.
By adopting the improved preparation method of the heat-preservation graphene floor heating film, the bottom film with the heat-preservation reflection function is coated and formed on the leveled ground surface through process change, so that the heat-preservation and heat-insulation effects can be achieved, the concave-convex ground is filled, a flat construction surface is provided for the graphene floor heating film above the bottom layer, the metal base material is not prone to deformation in the construction process, and the floor heating construction quality is improved.
The foregoing is directed to preferred embodiments of the present invention, wherein the preferred embodiments are not obviously contradictory or subject to any particular embodiment, and any combination of the preferred embodiments may be combined in any overlapping manner, and the specific parameters in the embodiments and examples are only for the purpose of clearly illustrating the inventor's invention verification process and are not intended to limit the scope of the invention, which is defined by the claims and the equivalent structural changes made by the description and drawings of the present invention are also intended to be included in the scope of the present invention.
Claims (7)
1. An improved preparation method of a heat-preservation graphene floor heating film is characterized by comprising the following steps:
s1, after leveling construction ground, coating the leveling ground to form a basement membrane, wherein the coating material of the basement membrane comprises the following specific components in parts by mass:
25-30 parts of hollow titanium oxide powder, 65-80 parts of base membrane main material, 0.01-0.5 part of defoaming agent, 0.05-0.5 part of thickening agent, 0.1-0.5 part of film-forming assistant and 1-3 parts of dispersing agent; the particle size of the hollow titanium oxide powder is 1-10 microns, and the wall thickness is 100-2000 nm; the coating amount per square meter of ground is 10-50 g when the wall thickness is coated;
s2, after the base film is coated and before curing, laying a prefabricated graphene floor heating film, wherein the graphene floor heating film comprises a graphene electric heating film and a connecting layer located below the graphene electric heating film, and the graphene electric heating film comprises a metal base material and a graphene film located below the metal base material.
2. The improved heat-preservation graphene floor heating film preparation method according to claim 1, wherein the bonding layer of the graphene floor heating film is prepared by the following method:
mixing, heating and uniformly mixing the silicone-acrylic emulsion and the water-based fluorocarbon emulsion according to the volume ratio of 1:0.5-5, and mixing according to the ratio of 1: 4-6, introducing the mixture into a high-speed stirrer, stirring for 30-40min, and preparing a film-shaped connecting layer by using a blow molding machine after uniform mixing;
the mixed resin is prepared from the following components in percentage by mass of 3: 0.5-1:0.3-0.6:0.5-1 of zinc powder, cellulose, acrylic resin and conductive epoxy resin.
3. The improved heat-preservation graphene floor heating film preparation method according to claim 2, wherein the base film is made of fluorocarbon resin.
4. The improved heat-preservation graphene floor heating film preparation method according to claim 2, wherein the connection layer and the graphene electric heating film are connected through a high-temperature-resistant conductive adhesive.
5. The improved heat-preservation graphene floor heating film as claimed in claim 1, wherein the metal substrate is copper foil or aluminum foil.
6. The improved heat-preservation graphene floor heating film preparation method according to claim 1, wherein the preparation method of the hollow titanium oxide powder comprises the following steps:
adding TiCl4 into the ionic liquid and stirring uniformly to form TiCl4 solution with the concentration of 0.8-1.5 mol/L;
slowly adding deionized water, standing for 12-48 hours, and obtaining a solid precipitate after TiCl4 is completely hydrolyzed;
and (3) alternately washing the solid precipitate for multiple times by using deionized water and ethanol, centrifugally separating, drying and roasting to obtain the titanium dioxide hollow spherical powder.
7. The improved heat-preservation graphene floor heating film preparation method according to claim 6, wherein the ionic liquid is an imidazole salt ionic liquid.
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| CN101580275A (en) * | 2008-05-15 | 2009-11-18 | 中国科学院过程工程研究所 | Method for preparing titanium dioxide hollow spherical powder |
| CN103483944A (en) * | 2013-09-30 | 2014-01-01 | 海南大学 | Light-reflection, heat-insulation and anticorrosion paint and preparation method thereof |
| CN103591632A (en) * | 2013-11-20 | 2014-02-19 | 廖永鸿 | Electric-heating and wood-plastic floor or wall plate |
| CN110324920A (en) * | 2019-06-28 | 2019-10-11 | 乐福之家纳米材料有限责任公司 | A kind of preparation method of thermal-insulating type graphene Electric radiant Heating Film |
-
2020
- 2020-10-20 CN CN202011123559.5A patent/CN112409856A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580275A (en) * | 2008-05-15 | 2009-11-18 | 中国科学院过程工程研究所 | Method for preparing titanium dioxide hollow spherical powder |
| CN103483944A (en) * | 2013-09-30 | 2014-01-01 | 海南大学 | Light-reflection, heat-insulation and anticorrosion paint and preparation method thereof |
| CN103591632A (en) * | 2013-11-20 | 2014-02-19 | 廖永鸿 | Electric-heating and wood-plastic floor or wall plate |
| CN110324920A (en) * | 2019-06-28 | 2019-10-11 | 乐福之家纳米材料有限责任公司 | A kind of preparation method of thermal-insulating type graphene Electric radiant Heating Film |
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