CN111647293B - Infrared radiation insulating coating, coating thereof and preparation method thereof - Google Patents

Infrared radiation insulating coating, coating thereof and preparation method thereof Download PDF

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CN111647293B
CN111647293B CN202010565968.4A CN202010565968A CN111647293B CN 111647293 B CN111647293 B CN 111647293B CN 202010565968 A CN202010565968 A CN 202010565968A CN 111647293 B CN111647293 B CN 111647293B
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王良
方晓
王纪乾
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Tianjin Dancong New Material Technology Co ltd
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Abstract

The invention discloses an infrared radiation insulating coating, a coating thereof and a preparation method thereof, wherein the infrared heating coating mainly comprises 1 weight part of spherical graphene, 0.02-0.12 weight part of graphitizable high-molecular oligomer, 1-4 weight parts of polyaluminosilicate, 0.5-2 weight parts of hyperbranched carbosilane and 0.01-0.1 weight part of peroxide cross-linking agent. The infrared heating coating realizes multistage infrared heating by utilizing the corrugated structure of spherical graphene under the action of the coagulation and combination of high molecules and the insulation of insulating aluminum silicon compounds and the coordination of small-molecule high-radiation inorganic particles. The infrared heating coating greatly improves the heating efficiency, increases the comfort of a human body in the field of infrared radiation heating, and greatly reduces the energy consumption.

Description

Infrared radiation insulating coating, coating thereof and preparation method thereof
Technical Field
The invention belongs to the technical field of new nano materials, and particularly relates to an infrared radiation insulating coating, a coating and a preparation method thereof.
Background
Along with the development of society, the dependence of human beings on energy is higher and higher, but along with the gradual consumption of fossil energy, the cost of energy is higher and higher, and for this reason, the more efficient utilization of energy in human life production activities is urgent. Meanwhile, the quality requirements of people on production and life are higher and higher, and the comfort becomes the first choice under the same energy source condition.
In order to achieve the insulating performance of the existing infrared radiation heating coating, a polymer insulating layer is usually adopted, and due to the limitation of the material of the polymer insulating layer, the thermal conductivity of the existing infrared radiation heating coating is poor (the thermal conductivity is less than 0.1K/mK), the heat transmission speed is slow, and the heat dissipation is serious; on the other hand, the heat resistance is poor, the heat output of high temperature and high power cannot be borne, and the heat-resistant material is not suitable for being used in a large-range heating environment. Furthermore, in such designs, the outer layer needs a black auxiliary heat radiation layer, and the indirect radiation form further causes heat loss, which ultimately results in huge power consumption. Meanwhile, indirect heat radiation has short infrared radiation wavelength and strong energy, easily causes burn of a human body and is poor in comfort.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a multistage infrared heating coating which is coated on the surface of an electric heating material and realizes high-efficiency infrared radiation, wherein an insulating polyaluminosilicate layer is used as a bottom layer, and an insulating silicon carbide layer is used as an intermediate layer, so that the problems of poor heat conduction, low heat dissipation efficiency and poor temperature resistance of the insulating coating, low radiation efficiency, low radiation power and the like of indirect radiation in the prior art are solved. The polyaluminosilicate layer plays a role in isolating the conductive heating material, protects the conductive heating material, isolates the external damage effect and the electric leakage phenomenon and enhances the safety; on the other hand, heat is transferred to the high-emissivity silicon carbide layer. The silicon carbide layer plays an insulating role to protect the conductive heating material, and on the other hand, the silicon carbide layer quickly radiates heat to the outside in a radiation mode.
Another object of the present invention is to overcome the disadvantages of the prior art, and to provide a multi-stage infrared heating coating based on the heat conduction and convection principle, which uses an insulating polyaluminosilicate layer as a bottom layer, an insulating silicon carbide layer as an intermediate layer, a graphitizable polymer layer as an upper layer, and spherical graphene penetrating through the three-layer structure. Spherical graphene has three functions: firstly, heat is guided out from an interface to spherical graphene with a high specific surface area, secondly, the spherical graphene has high radiance and can radiate heat quickly and efficiently, the radiation effect of silicon carbide is greatly enhanced, thirdly, the surface of the spherical graphene has a small number of defect state structures, and moreover, the temperature gradient of the surface of a heating material is enhanced by an external suspension structure, so that the spherical graphene can have a good heat convection effect with gas, and the heating effect of the material interface is further enhanced. The carbonizable nano-film links the spherical graphene and the silicon carbide to function as a rivet.
The size of the spherical graphene is 1-3 um, and the total thickness of a three-layer structure consisting of a bottom layer, a middle layer and an upper layer is not more than 1/4 of the size of the spherical graphene; the thickness of the upper layer is less than 1/10 of the total thickness of the three-layer structure, so as to ensure the stability of the coating and high efficiency infrared radiation.
Further, the graphitizable polymer layer is composed of graphitizable polymer, and the graphitizable polymer is selected from polyimide, asphalt or polyacrylonitrile with a molecular weight of 3000-30000.
Further, the polyaluminosilicate layer is feldspar (K)2O·Al2O3·6SiO2) Layer, mica (K)2O·2Al2O3·6SiO2·2H2O) layer, Kaolin (Al)2O3·2SiO2·22H2O) layer, zeolite (Na)2O·Al2O3·3SiO2·22H2O) layer, garnet(3CaO·Al2O3·3SiO2) And (3) a layer.
The invention also aims to provide a preparation method of the coating, the coating is assembled by a centrifugal spraying mode, materials with different densities are uniformly layered after centrifugal spraying, and a layer-by-layer assembly structure is formed by mixing the coating. Specifically, the method comprises the following steps: carrying out centrifugal spraying and ultraviolet curing on the multistage infrared heating coating, and then heating and shaping to obtain the multistage infrared heating coating, wherein the ultraviolet curing temperature is 60-120 ℃, and the time is 1-6 hours; the multistage infrared heating coating comprises the following raw materials in parts by weight: 1 part by weight of spherical graphene, 0.02-0.12 part by weight of graphitizable high molecular oligomer, 1-4 parts by weight of polyaluminosilicate, 0.5-2 parts by weight of hyperbranched carbosilane and 0.01-0.1 part by weight of peroxide crosslinking agent. The molecular weight of the hyperbranched carbosilane is less than 10000, and the branching degree is 1.1-2. The graphitizable high molecular oligomer is selected from polyimide, asphalt, polyacrylonitrile and the like, and has the molecular weight of 2000-10000. The peroxide crosslinking agents include, but are not limited to: dicumyl peroxide, methyl ethyl ketone peroxide, benzoic acid peroxide, 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane; the polyaluminosilicate is selected from feldspar (K)2O·Al2O3·6SiO2) Mica (K)2O·2Al2O3·6SiO2·2H2O), kaolin (Al)2O3·2SiO2·22H2O), zeolite (Na)2O·Al2O3·3SiO2·22H2O), garnet (3 CaO. Al)2O3·3SiO2)。
Further, the spherical graphene is prepared by spraying graphene oxide solution with the concentration of 0.1-1 mg/mL and carrying out chemical reduction, wherein I of the spherical grapheneD/IGThe value is not higher than 0.05 and its dimension is 0.2-5 μm, the wall thickness is less than 4 atomic layers.
Further, the centrifugal force of the centrifugation is in the range of 2000-10000 rcf.
Further, the specific method for heating and shaping comprises the following steps: at the temperature of 0-250 ℃, the temperature rising speed is less than 5 ℃/min, and the temperature is controlled and preserved for 0.5-2 h; then heating to 500 ℃, wherein the heating speed is less than 5 ℃/min, and keeping the temperature for 1-2 h; then the temperature is quickly raised to 1300 ℃, the temperature raising speed is higher than 50 ℃/min, and the temperature is controlled for 1-5 min.
The invention also aims to provide a coating for preparing the coating, which comprises the following components in parts by weight: 1 part by weight of spherical graphene, 0.02-0.12 part by weight of graphitizable high molecular oligomer, 1-4 parts by weight of polyaluminosilicate, 0.5-2 parts by weight of hyperbranched carbosilane and 0.01-0.1 part by weight of peroxide crosslinking agent. The molecular weight of the hyperbranched carbosilane is less than 10000, and the branching degree is 1.1-2. The graphitizable high molecular oligomer is selected from polyimide, asphalt, polyacrylonitrile and the like, and has the molecular weight of 2000-10000. The organic peroxide crosslinking agents include, but are not limited to: dicumyl peroxide, methyl ethyl ketone peroxide, benzoic acid peroxide, 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane; the polyaluminosilicate is selected from feldspar (K)2O·Al2O3·6SiO2) Mica (K)2O·2Al2O3·6SiO2·2H2O), kaolin (Al)2O3·2SiO2·22H2O), zeolite (Na)2O·Al2O3·3SiO2·22H2O), garnet (3 CaO. Al)2O3·3SiO2)。
Compared with the prior art, the invention has the following beneficial effects:
firstly, the coating realizes that the conversion efficiency of high energy exceeds 80 percent and the radiance reaches 99 percent.
Secondly, the layer-by-layer directional assembly of the coating material is realized by using a centrifugal spraying mode according to different material densities, the operation is simple, and the industrialization degree is high; the coating is tightly combined, the thermal interface is less, and the heat transfer is smooth.
Thirdly, the proportion of the spherical graphene and other auxiliary materials is reasonably regulated and controlled, and the combination of a multi-stage multi-dimensional radiation heating structure is realized. The aluminum silicon layer plays a role in isolating the conductive heating material, on one hand, the conductive heating material is protected, the external damage and electric leakage phenomena are isolated, and the safety is enhanced; on the other hand, heat is transferred to the high-radiation silicon carbide. Silicon carbide plays insulating effect on the one hand, protects the electrically conductive heating material, and on the other hand, with the form of radiation with the heat to outside quick dissipation. The carbonizable nano film links the spherical graphene and the silicon carbide to play a role of a rivet; spherical graphene has three functions: guiding heat out from the interface to spherical graphene with high specific surface area; the spherical graphene has high radiance, quickly and efficiently radiates heat, and the radiation effect of the silicon carbide is greatly enhanced; the spherical graphene surface has a few defect state structures, and moreover, the outer suspension structure enhances the temperature gradient of the surface of the heating material, so that the spherical graphene surface can have a good thermal convection effect with gas, and the material interface heating effect is further enhanced.
Fourthly, the structure of few-layer graphene enables the heat conductivity of the graphene microspheres to maintain the property of graphene, the binding force of the graphene sheet layers in the graphene microspheres is small in the vertical direction, the number of low-frequency sound waves in the vertical direction is increased rapidly relative to graphite, the heat conduction of the graphene microspheres is greatly enhanced, the bottom heat can be rapidly conducted to the whole graphene microspheres, and the heat radiation and the heat conduction efficiency are enhanced under the rapid action of the vertical direction and air.
Fifthly, the materials such as the high-temperature repaired graphene microspheres have excellent air oxygen resistance and can work for a long time at full power within 500 ℃, so that the high-temperature repaired graphene microspheres have good stability.
Drawings
FIG. 1 is a schematic structural view of a multi-stage IR heating coating according to the present invention.
FIG. 2 is a scan of the coating prepared in example 1;
FIG. 3 is a scan of the coating prepared in comparative example 1.
Detailed Description
In order that the objects and effects of the invention will become more apparent, the invention will be further described in detail with reference to the accompanying drawings and specific embodiments.
Example 1
The invention provides a preparation method of a multistage infrared radiation heating coating, which specifically comprises the following steps:
(1) and carrying out spray treatment on the graphene oxide solution with the concentration of 0.1mg/mL at 200 ℃, and reducing for 8h at 80 ℃ through HI to prepare the spherical graphene.
Scanning electron microscope detection proves that the spherical graphene is finally obtained, and Raman detection detects that the spherical graphene has the structure ID/IGThe value is 1.1 and its scale is 1 μm, with a spherical graphene wall thickness of 2 atomic layers.
(2) Uniformly mixing 1 part by weight of spherical graphene, 0.02 part by weight of polyimide with molecular weight of 2000, 4 parts by weight of feldspar nano powder, 0.5 part by weight of hyperbranched carbosilane with molecular weight of 9800 and branching degree of 1.1 and 0.1 part by weight of dicumyl peroxide to obtain the mixed coating.
(3) And (3) centrifugally spraying the mixed coating obtained in the step (2) on a copper substrate, setting the centrifugal force to be 2100rcf, and carrying out ultraviolet curing at the temperature of 60 ℃ for 6 hours. The layer-by-layer assembly structure of the cured structure is observed through a scanning electron microscope, and the spherical graphene penetrates through the three-layer structure. Through EDS analysis, the three-layer structure comprises poly-aluminum silicate, cross-linked carbosilane and polyimide in sequence, which is because materials with different densities are uniformly layered under the action of centrifugal force. Although the density of the folded graphene microspheres obtained by solution spraying is relatively low, the contact area of the substrate is small due to the folded shape, so that the position of the folded graphene microspheres is relatively high in pressure in the centrifugal spraying process, and the folded graphene microspheres can be inserted into the relatively high-density material.
(4) Then adopting a microwave heating and shaping process, namely heating at 250 ℃ at a speed of 4 ℃/min, and keeping the temperature at 250 ℃ for 0.5 h; then heating to 500 ℃, wherein the heating speed is 3 ℃/min, and keeping the temperature for 1 h; and then heating to 1300 ℃, wherein the heating speed is 50 ℃/min, and the temperature is controlled for 1min to obtain the infrared heating coating. The layer-by-layer assembled structure of the sintered structure is observed by a scanning electron microscope, and the spherical graphene penetrates through the three-layer structure, as shown in fig. 2. EDS analysis shows that the three-layer structure sequentially comprises polyaluminium silicate, silicon carbide and polyimide carbide, and is consistent with the structure in the step 3 because easily-decomposed substances volatilize and difficultly-decomposed substances are still fixed in the original layered structure in the sintering process, and the physical structure is not changed in the sintering process.
The infrared heating coating prepared by the method takes a polyaluminosilicate layer as an insulating layer and a heat input layer of a bottom layer; the silicon carbide layer is used as an insulating layer and an infrared radiation layer of the middle layer and is a main radiation layer, the rough surface and the high radiation rate (95%) are added, and the radiation heating efficiency is greatly improved; the polymer layer is used as an upper layer for linking the silicon carbide and the spherical graphene; spherical graphite alkene runs through three layer construction and as outer radiation layer, and its specific surface area is huge, and the radiance reaches 98%, has greatly improved infrared radiation heating, and high specific surface area defect state graphite alkene has fabulous heat-conduction effect simultaneously, can form splendid heat convection interface with external gas, and the reinforcing heating finally forms multistage high-efficient infrared heating coating.
The multi-stage infrared radiation heating coating is heated to 50m by a thermal imager2The temperature of the heat preservation room is 10 ℃ as a reference temperature for heating detection, the temperature of the room rises to 26 ℃ in about 10 minutes, and the temperature difference is 3 ℃; the room temperature of the uncoated material was only 21 degrees with a 7 degree temperature difference after the same power consumption. Therefore, the multistage infrared radiation heating coating can be widely used for high-quality uniform heating of rooms and has the effect of energy conservation. Through the feedback of comfort research, the radiation wavelength of the heating material with the coating is about 8-16um, and the heating material is just the wavelength which is easily absorbed by the human body, so the comfort is enhanced. The heating material without the coating has short radiation wavelength and high energy, and easily burns clothes and even skin, so the body feeling is poor.
Example 2
A preparation method of a multistage infrared radiation heating coating specifically comprises the following steps:
(1) carrying out spray treatment on a graphene oxide solution with the concentration of 1mg/mL at 180 ℃, and reducing for 2h at 100 ℃ through HI to prepare the spherical graphene.
SEM detection proves that spherical high-fold graphene is finally obtained, and Raman detection proves that I of the spherical grapheneD/IGValue of 0.8, and a dimension of 3 μm, spherical graphene wall thicknessIs 4 atomic layers.
(2) Uniformly mixing 1 part by weight of spherical graphene, 0.12 part by weight of asphalt with the molecular weight of 10000, 1 part by weight of mica nano powder, 2 parts by weight of hyperbranched carbosilane with the molecular weight of 8000 and the branching degree of 2 and 0.1 part by weight of peroxybenzoic acid to obtain the mixed coating.
(3) And (3) centrifugally spraying the mixed coating obtained in the step (2) on a copper substrate, setting the centrifugal force to be 10000rcf, and carrying out ultraviolet curing at the temperature of 120 ℃ for 3 h. The layer-by-layer assembly structure of the cured structure is observed through a scanning electron microscope, and the spherical graphene penetrates through the three-layer structure. Through EDS analysis, the three-layer structure comprises poly-aluminum silicate, cross-linked carbon-silicon alkane and asphalt in sequence, and materials with different densities are uniformly layered under the action of centrifugal force.
(4) And then adopting a high-temperature heating and shaping process: heating at 0-250 deg.C at a rate of 4 deg.C/min, and maintaining at 250 deg.C for 2 hr; then heating to 500 ℃, wherein the heating speed is 3 ℃/min, and keeping the temperature for 2 h; and then heating to 1300 ℃, wherein the heating speed is 300 ℃/min, and the temperature is controlled for 5min to obtain the infrared heating coating. The sintered structure is observed to be a layer-by-layer assembled structure through a scanning electron microscope, and the spherical graphene penetrates through the three-layer structure. Through EDS analysis, the three-layer structure sequentially comprises polyaluminium silicate, silicon carbide and carbonized asphalt, and is consistent with the structure in the step 3, because in the sintering process, easily-decomposed substances volatilize, difficultly-decomposed substances are still fixed in the original layered structure, and the physical structure is not changed in the sintering process.
The multi-stage infrared radiation heating coating is heated to 50m by a thermal imaging instrument2The temperature of the heat preservation room is 10 ℃ as a reference temperature for heating detection, the temperature of the room rises to 28 ℃ in about 10 minutes, and the temperature difference is 4 ℃; the room temperature of the material without the coating is only 22 degrees and the temperature difference is 8 degrees after the same power consumption. Therefore, the multistage infrared radiation heating coating can be widely used for high-quality uniform heating of rooms and has the effect of energy conservation. Through the feedback of comfort research, the radiation wavelength of the heating material with the coating is about 8-16um, and the heating material is just the wavelength which is easily absorbed by the human body, so the comfort is enhanced. But not coated heating materialThe material has short radiation wavelength and high energy, and is easy to burn clothes and even skin, so the body feeling is poor.
Example 3
A preparation method of a multistage infrared radiation heating coating specifically comprises the following steps:
(1) carrying out spray treatment on graphene oxide with the concentration of 0.1mg/mL at 220 ℃, and reducing for 4h at 90 ℃ through HI to prepare the spherical graphene.
SEM detection proves that multi-fold spherical graphene is finally obtained, and Raman detection proves that I of the spherical grapheneD/IGThe value is 0.8 and its scale is 2 μm, with a spherical graphene wall thickness of 3 atomic layers.
(2) Uniformly mixing 1 part by weight of spherical graphene, 0.1 part by weight of polyacrylonitrile with the molecular weight of 10000, 2 parts by weight of kaolin nano powder, 1 part by weight of hyperbranched carbosilane with the molecular weight of 8000 and the branching degree of 1.6 and 0.05 part by weight of 2, 5-dimethyl-2, 5 bis (tert-butylperoxy) hexane to obtain the mixed coating.
(3) And (3) centrifugally spraying the mixed coating obtained in the step (2) on a copper substrate, setting the centrifugal force to be 4000, and carrying out ultraviolet curing at the temperature of 120 ℃ for 2 hours. The layer-by-layer assembly structure of the cured structure is observed through a scanning electron microscope, and the spherical graphene penetrates through the three-layer structure. Through EDS analysis, the three-layer structure sequentially comprises polyaluminium silicate, cross-linked carbosilane and polyacrylonitrile, and materials with different densities are uniformly layered under the action of centrifugal force.
(4) And then adopting a high-temperature heating and shaping process: at 250 deg.C, the temperature is raised to 250 deg.C at a rate of 2 deg.C/min. Controlling and preserving heat for 1 h; then heating to 500 ℃, wherein the heating speed is 4.5 ℃/min, and keeping the temperature for 2 hours; and then heating to 1300 ℃, wherein the heating speed is 120 ℃/min, and the temperature is controlled for 2min to obtain the infrared heating coating. The sintered structure is observed to be a layer-by-layer assembled structure through a scanning electron microscope, and the spherical graphene penetrates through the three-layer structure. Through EDS analysis, the three-layer structure sequentially comprises polyaluminium silicate, silicon carbide and polyacrylonitrile carbide, and is consistent with the structure in the step 3, because easily-decomposed substances volatilize in the sintering process, difficultly-decomposed substances are still fixed in the original layered structure, and the physical structure is not changed in the sintering process.
The multi-stage infrared radiation heating coating is heated to 50m by a thermal imaging instrument2The temperature of the heat preservation room is 10 ℃ as a reference temperature for heating detection, the temperature of the room rises to 26 ℃ in about 10 minutes, and the temperature difference is 4 ℃; the room temperature of the material without the coating is only 20 degrees and the temperature difference is 8 degrees after the same power consumption. Therefore, the multistage infrared radiation heating coating can be widely used for high-quality uniform heating of rooms and has the effect of energy conservation. Through the feedback of comfort research, the radiation wavelength of the heating material with the coating is about 8-16um, and the heating material is just the wavelength which is easily absorbed by the human body, so the comfort is enhanced. The heating material without the coating has short radiation wavelength and high energy, and easily burns clothes and even skin, so the body feeling is poor.
Example 4
A preparation method of a multistage infrared radiation heating coating specifically comprises the following steps:
(1) carrying out spray treatment on graphene oxide with the concentration of 0.4mg/mL at 300 ℃, and reducing for 5h at 90 ℃ through HI to prepare the spherical graphene.
SEM detection proves that multi-fold spherical graphene is finally obtained, and Raman detection proves that I of the spherical grapheneD/IGThe value is 0.85, and its scale is 2 μm, with a spherical graphene wall thickness of 3-4 atomic layers.
(2) Uniformly mixing 1 part by weight of spherical graphene, 0.08 part by weight of polyacrylonitrile with the molecular weight of 5000, 1 part by weight of garnet nano powder, 2 parts by weight of hyperbranched carbosilane with the molecular weight of 8000 and the branching degree of 1.8 and 0.006 part by weight of methyl ethyl ketone peroxide to obtain the mixed coating.
(3) And (3) centrifugally spraying the mixed coating obtained in the step (2) on a copper substrate, setting the centrifugal force of the centrifuge to be 6000, and carrying out ultraviolet curing at the temperature of 80 ℃ for 4 hours. The layer-by-layer assembly structure of the cured structure is observed through a scanning electron microscope, and the spherical graphene penetrates through the three-layer structure. Through EDS analysis, the three-layer structure sequentially comprises polyaluminium silicate, cross-linked carbosilane and polyacrylonitrile, and materials with different densities are uniformly layered under the action of centrifugal force.
(4) And then adopting a high-temperature heating and shaping process: at 250 ℃, the temperature rising speed is 4 ℃/min, and the heat preservation is controlled for 1 h; then heating to 500 ℃, wherein the heating speed is 3 ℃/min, and keeping the temperature for 1 h; and then heating to 1300 ℃, wherein the heating speed is 500 ℃/min, and the temperature is controlled for 4min to obtain the infrared heating coating. The sintered structure is observed to be a layer-by-layer assembled structure through a scanning electron microscope, and the spherical graphene penetrates through the three-layer structure. Through EDS analysis, the three-layer structure sequentially comprises polyaluminium silicate, silicon carbide and polyacrylonitrile carbide, and is consistent with the structure in the step 3, because easily-decomposed substances volatilize in the sintering process, difficultly-decomposed substances are still fixed in the original layered structure, and the physical structure is not changed in the sintering process.
The multi-stage infrared radiation heating coating is heated to 50m by a thermal imaging instrument2The temperature of the heat preservation room is 10 ℃ as a reference temperature for heating detection, the temperature of the room rises to 27 ℃ in about 10 minutes, and the temperature difference is 2.8 ℃; the room temperature of the material without the coating was only 21.8 degrees and the temperature difference was 7.2 degrees after the same power consumption. Therefore, the multistage infrared radiation heating coating can be widely used for high-quality uniform heating of rooms and has the effect of energy conservation. Through the feedback of comfort research, the radiation wavelength of the heating material with the coating is about 8-16um, and the heating material is just the wavelength which is easily absorbed by the human body, so the comfort is enhanced. The heating material without the coating has short radiation wavelength and high energy, and easily burns clothes and even skin, so the body feeling is poor.
Comparative example
(1) And uniformly mixing 0.1 part by weight of polyacrylonitrile with the molecular weight of 10000, 2 parts by weight of kaolin nano powder, 1 part by weight of hyperbranched carbosilane with the molecular weight of 8000 and the branching degree of 1.6 and 0.05 part by weight of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane to obtain the mixed coating.
(2) And (2) centrifugally spraying the mixed coating obtained in the step (1), setting the centrifugal force to be 4000, and carrying out ultraviolet curing at the temperature of 120 ℃ for 2 hours.
(3) And then adopting a high-temperature heating and shaping process: at 250 ℃, the temperature rising speed is 2 ℃/min, and the heat preservation is controlled for 1 h; then heating to 500 ℃, wherein the heating speed is 4.5 ℃/min, and keeping the temperature for 2 hours; and then heating to 1300 ℃, wherein the heating speed is 3 ℃/min, and the temperature is controlled for 1h to obtain the infrared heating coating.
The structure of the infrared heating coating prepared by the method has a layer-by-layer assembly structure, as shown in fig. 3. The method specifically comprises the following steps: the polyaluminosilicate layer is used as an insulating layer and a heat input layer of the bottom layer; the silicon carbide layer is used as an insulating layer of the middle layer and an infrared radiation layer, is a main radiation layer, has a rough surface area and a high radiation rate (95%), and greatly improves the radiation heating efficiency; the polymer layer is used as an upper layer for linking the silicon carbide and the gas interface; finally forming the infrared heating coating.
The multi-stage infrared radiation heating coating is heated to 50m by a thermal imaging instrument2The temperature of the heat preservation room is 10 ℃ as a reference temperature for heating detection, the temperature of the room rises to 26 ℃ in about 10 minutes, and the temperature difference is 3 ℃; the room temperature of the material without the coating is only 21 degrees after the same power consumption, and the temperature difference is 7 degrees. Therefore, the multistage infrared radiation heating coating can be widely used for high-quality uniform heating of rooms and has the effect of energy conservation. Through the feedback of comfort research, the radiation wavelength of the heating material with the coating is about 8-16um, and the heating material is just the wavelength which is easily absorbed by the human body, so the comfort is enhanced. The heating material without the coating has short radiation wavelength and high energy, and easily burns clothes and even skin, so the body feeling is poor.

Claims (7)

1. A multi-stage infrared heating coating is characterized in that a polyaluminosilicate layer is used as a bottom layer, a silicon carbide layer is used as a middle layer, a graphitizable high molecular layer is used as an upper layer, and spherical graphene penetrates through the three-layer structure; the size of the spherical graphene is 1-3 mu m, and the total thickness of a three-layer structure consisting of a bottom layer, a middle layer and an upper layer does not exceed 1/4 of the size of the spherical graphene; the thickness of the upper layer is 1/10 less than the total thickness of the three-layer structure; the graphitizable polymer layer is composed of graphitizable polymers, and the graphitizable polymers are selected from polyimide, asphalt or polyacrylonitrile with the molecular weight of 3000-10000.
2. The coating of claim 1, wherein the polyaluminosilicate layer is a feldspar layer, a mica layer, a kaolin layer, a zeolite layer, or a garnet layer.
3. The preparation method of the multistage infrared heating coating of claim 1, characterized in that the multistage infrared heating coating is subjected to centrifugal spraying and ultraviolet curing, and then is heated and shaped to obtain the multistage infrared heating coating, wherein the ultraviolet curing temperature is 60-120 ℃ and the time is 1-6 h; the multistage infrared heating coating comprises the following raw materials in parts by weight: 1 part by weight of spherical graphene, 0.02-0.12 part by weight of graphitizable polymer, 1-4 parts by weight of polyaluminosilicate, 0.5-2 parts by weight of hyperbranched carbosilane and 0.01-0.1 part by weight of peroxide cross-linking agent; the molecular weight of the hyperbranched carbosilane is less than 10000, and the branching degree is 1.1-2; the graphitizable macromolecule is selected from polyimide, asphalt or polyacrylonitrile, and the molecular weight is 3000-10000; the peroxide crosslinking agent is selected from: dicumyl peroxide, methyl ethyl ketone peroxide, benzoic acid peroxide or 2, 5-dimethyl-2, 5 bis (t-butylperoxy) hexane; the polyaluminosilicate is selected from feldspar, mica, kaolin, zeolite or garnet.
4. The preparation method according to claim 3, wherein the spherical graphene is prepared by spraying a graphene oxide solution with a concentration of 0.1mg/mL-1mg/mL and performing chemical reduction, wherein I of the spherical graphene isD/IGThe value is not higher than 0.05 and its dimension is 1-3 μm, the wall thickness is less than 4 atomic layers.
5. The method according to claim 3, wherein the centrifugal force of the centrifugation is in the range of 2000-10000 rcf.
6. The preparation method according to claim 3, wherein the specific method of heat setting is as follows:
heating to 250 deg.C, heating at a speed of less than 5 deg.C/min, and maintaining at 250 deg.C for 0.5-2 h;
heating to 500 deg.C, heating at a speed of less than 5 deg.C/min, and maintaining at 500 deg.C for 1-2 h;
rapidly heating to 1300 deg.C, heating at a speed of more than 50 deg.C/min, and maintaining at 1300 deg.C for 1-5 min.
7. The multistage infrared heating coating is characterized by comprising the following components in parts by weight: 1 part by weight of spherical graphene, 0.02-0.12 part by weight of graphitizable polymer, 1-4 parts by weight of polyaluminosilicate, 0.5-2 parts by weight of hyperbranched carbosilane and 0.01-0.1 part by weight of peroxide cross-linking agent; the molecular weight of the hyperbranched carbosilane is less than 10000, and the branching degree is 1.1-2; the graphitizable macromolecule is selected from polyimide, asphalt or polyacrylonitrile, and the molecular weight is 3000-10000; the peroxide crosslinking agent is selected from: dicumyl peroxide, methyl ethyl ketone peroxide, benzoic acid peroxide or 2, 5-dimethyl-2, 5 bis (t-butylperoxy) hexane; the polyaluminosilicate is selected from feldspar, mica, kaolin, zeolite or garnet.
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