CN115175385A - Water-soluble high-temperature-resistant infrared carbon-based heating slurry and preparation method thereof - Google Patents

Water-soluble high-temperature-resistant infrared carbon-based heating slurry and preparation method thereof Download PDF

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CN115175385A
CN115175385A CN202210899979.5A CN202210899979A CN115175385A CN 115175385 A CN115175385 A CN 115175385A CN 202210899979 A CN202210899979 A CN 202210899979A CN 115175385 A CN115175385 A CN 115175385A
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water
temperature
carbon
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杨佳
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Wuxi Chenhai New Material Technology Co ltd
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Wuxi Chenhai New Material Technology Co ltd
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/10Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/145Carbon only, e.g. carbon black, graphite
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02BCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B30/00Energy efficient heating, ventilation or air conditioning [HVAC]

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Abstract

The invention belongs to the technical field of electric heating of materials, and particularly provides water-soluble high-temperature-resistant infrared carbon-based heating slurry and a preparation method thereof, wherein the heating slurry comprises water and a slurry matrix, and the slurry matrix is prepared by mixing the following components in parts by weight: 15-20 parts of 40-50wt% phosphate solution or the amount of phosphate equivalent to the phosphate solution; 2-14 parts of glass powder; 1-40 parts of carbon-based conductive powder; 5-10 parts of inorganic filler powder; 1-3 parts of tetrabutyl titanate; 1-5 parts of high-temperature resistant oxidant; 0.1-5 parts of a dispersant; 1-20 parts of a film forming agent; 0.1-3 parts of a leveling agent; 0.1-3 parts of anti-settling agent; 0.01-3 parts of a defoaming agent; 0.01-3 parts of thickening agent; 10-100 parts of water. With such a configuration, a water-soluble high-temperature-resistant infrared carbon-based heating slurry which is particularly suitable for high-temperature fields such as household appliances, industrial baking, boiler heating, and the like can be obtained.

Description

Water-soluble high-temperature-resistant infrared carbon-based heating slurry and preparation method thereof
Technical Field
The invention relates to the technical field of electric heating materials, in particular to water-soluble high-temperature-resistant infrared carbon-based heating slurry and a preparation method thereof.
Background
The nano carbon material represented by graphene is used as a novel material, and has excellent performances in the aspects of conductivity, infrared radiation performance and the like, so that the nano carbon material has great application potential in the field of electric heating. A product form that adopts this novel material of graphite alkene is graphite alkene heating film, and at present, the comparatively common application mode of graphite alkene heating film is with the low temperature scene of the form reply within 100 ℃ of heating film warms up, and application field is very limited. In view of the excellent properties of graphene, how to develop a graphene electro-thermal paste with the advantages of high working temperature, low cost, convenient construction method and the like is a common demand in the field. Such as:
chinese patent application (CN 112521796A) discloses a graphene heating ink and a preparation method and application thereof, wherein the graphene heating ink comprises a resin matrix, a conductive filler, an auxiliary agent and a solvent, the conductive filler comprises graphene, and the resin matrix is prepared by mixing an organic polymer and polysilazane according to a mass ratio of 1:0.08-1.5, and the preparation method comprises the following steps: graphene adopts graphene powder in a powder form, polysilazane adopts a polysilazane solution in a solution form, the graphene powder and the polysilazane solution are firstly stirred and dispersed to be fully mixed, and after the graphene powder and the polysilazane solution are uniformly mixed, the rest raw materials are added under stirring to prepare the graphene-polysilazane composite material.
However, in this document, the polysilazane is expensive, and therefore the graphene heat-generating ink obtained has a drawback of being expensive.
Chinese patent application (CN 112996153A) discloses a graphene heating plate and a preparation method and application thereof, wherein the preparation method of the graphene heating plate comprises the following steps: s1, coating graphene on the surface of glass micro powder to generate graphene coated glass powder; s2, mixing the graphene-coated glass powder, an organic carrier and a silane coupling agent according to a preset weight ratio (1 part of graphene-coated glass powder, 0.2-0.5 part of glass powder, 10 parts of organic carrier and 0.5-1.5 parts of silane coupling agent) to obtain graphene conductive slurry; s3, laying the graphene conductive slurry on a substrate, and then baking and curing to form a graphene conductive heating layer; and S4, carrying out wiring and insulating treatment on the graphene conductive heating layer to generate the graphene heating plate.
However, in the document, since the operating temperature of the glass frit is low, the prepared graphene heating plate has a defect of low stable operating temperature.
Accordingly, there is a need in the art for a new solution to the above-mentioned problems.
Disclosure of Invention
Technical problem
The present invention has been made to solve at least the above-mentioned problems to some extent.
Technical scheme
In view of the above, the first aspect of the present invention provides a water-soluble high temperature resistant infrared carbon-based heating slurry, which comprises water and a slurry matrix, wherein the slurry matrix is prepared by mixing the following components in parts by weight: 15-20 parts of 40-50wt% phosphate solution or the amount of phosphate equivalent to the phosphate solution; 2-14 parts of glass powder; 1-40 parts of carbon-based conductive powder; 5-10 parts of inorganic filler powder; 1-3 parts of tetrabutyl titanate; 1-5 parts of high-temperature resistant oxidant; 0.1-5 parts of a dispersant; 1-20 parts of a film forming agent; 0.1-3 parts of a leveling agent; 0.1-3 parts of anti-settling agent; 0.01-3 parts of a defoaming agent; 0.01-3 parts of thickening agent.
Through the structure, a structure mode of the water-soluble high-temperature-resistant infrared carbon-based heating slurry is provided.
In particular, the phosphate solution therein is used as a binder. Compared with organic binders, the organic binder has better heat resistance and weather resistance, namely: the phosphate solution mainly plays a role of bonding, and can resist high temperature while playing a role of bonding. The carbon-based conductive powder plays a role in conducting electricity, heating when being electrified and playing a role in infrared radiation. The inorganic filler can be selected from corresponding functional materials, and has the effects of enhancing radiation, adjusting resistance temperature coefficient, enhancing heat conduction, enhancing insulation and the like. The tetrabutyl titanate is used as a coupling agent, so that the combination between phosphates is tighter. The glass powder can realize high-temperature secondary film formation, and has the hole sealing protection effect at high temperature, so that the prepared heating film can stably work for a long time in a high-temperature environment. The addition of the high-temperature resistant oxidant has a good antioxidation protection effect on the carbon-based powder in a temperature environment within 750 ℃.
It should be noted that the amount equivalent to 15 to 20 parts of phosphate of a 40 to 50wt% phosphate solution should be interpreted as: assuming that the mass percentage of phosphate solution in the commercially available phosphate solution is adjusted or the phosphate solution can be obtained in a home-made manner, the net phosphate content should be approximately the same.
For the water-soluble high-temperature-resistant infrared carbon-based heating slurry, in a possible implementation mode, the slurry matrix further comprises the following components mixed according to the following weight ratio: 8-12 parts of inorganic sol; and/or 0.1-10 parts of oxygen absorbent.
With this constitution, a preferable constitution of the water-soluble high-temperature-resistant infrared carbon-based heating paste is given.
For the above water-soluble high temperature resistant infrared carbon-based heating slurry, in one possible embodiment, the inorganic sol comprises an aluminum-based sol; and/or the oxygen absorbent is simple substance boron powder and/or metal boride.
The aluminum-based sol can greatly improve the bonding performance of the bonding agent such as aluminum dihydrogen phosphate and the like, participates in film formation, and has a great promotion effect on the bonding strength and the thermal shock resistance at high temperature, so that the effect of complementing performance advantages can be achieved by matching the aluminum dihydrogen phosphate and the aluminum-based sol as the bonding agent.
For the above water-soluble high temperature resistant infrared carbon-based heating slurry, in one possible embodiment, the aluminum-based sol has the following properties: the pH is 5-7; the particle size of colloidal particles of the sol is 20-80nm.
For the above water-soluble high temperature resistant infrared carbon-based heating slurry, in one possible embodiment, the solute of the phosphate solution comprises aluminum dihydrogen phosphate, aluminum chromium phosphate; and/or the glass powder is one or more of silicate glass, borate glass, borosilicate glass and phosphate glass; and/or the carbon-based conductive powder is one or more of graphene, nano graphite sheets, conductive carbon black, carbon fibers and carbon nano tubes; and/or the inorganic filler comprises heat-conducting powder, insulating powder and a TCR (temperature coefficient of resistance) regulator; and/or the high-temperature-resistant oxidizing agent is one or more of phosphoric acid, zinc phosphate, triammonium phosphate and boric acid.
For the above water-soluble high temperature resistant infrared carbon-based heating slurry, in one possible embodiment, the phosphate solution includes a curing agent.
Aluminum dihydrogen phosphate, aluminum chromium phosphate and the like which are matched with the curing agent can have more excellent temperature resistance, bonding property and low-temperature film forming property.
For the above water-soluble high temperature resistant infrared carbon-based heating slurry, in one possible embodiment, the curing agent comprises oxides and/or hydroxides of magnesium, copper, zinc, zirconium, and/or aluminum; and/or the content of the curing agent is 2-10wt% of the solute of the phosphate solution.
By such a constitution, possible forms and specific contents of the curing agent are given.
For the water-soluble high-temperature-resistant infrared carbon-based heating slurry, in one possible embodiment, the heat-conducting powder is one or more of inert ceramic powder, cordierite-based infrared radiation powder, transition metal oxide infrared radiation powder and boron nitride; and/or the insulating powder is mica and/or kaolin; and/or the TCR modulator is one or more of ruthenium oxide, modified barium titanate, eucryptite and zirconium phosphate.
For the water-soluble high-temperature-resistant infrared carbon-based heating slurry, in one possible embodiment, the oxygen absorbent is elemental boron powder and/or metal boride.
In conclusion, the water-soluble high-temperature graphene heating slurry with the component/weight ratio has excellent high-temperature oxidation resistance and aging resistance after film formation, so that the water-soluble high-temperature graphene heating slurry can reliably and stably work for a long time in a high-temperature environment. In addition, the material has extremely high infrared emissivity at high temperature, and can realize a larger energy-saving effect. In addition, the heating of the slurry also has the advantage of lower cost due to the lower cost of the raw materials used. Therefore, the method can be widely applied to the high-temperature application fields of household appliances, industrial baking, boiler heating and the like.
In the water-soluble high-temperature-resistant infrared carbon-based heating slurry, the carbon material without the glass powder and the high-temperature-resistant oxidant is oxidized in the air at the temperature of more than 400 ℃, which is the root cause of the power attenuation of the carbon-based electric heating slurry. Generally, the highest electrothermal working temperature requires that the construction temperature is higher than 200 ℃, and the carbon-based material is rapidly oxidized at the high temperature of 600-800 ℃, so that the inhibition of the oxidation of the material is a core way for improving the high-temperature working performance of the material, and the oxidation of the carbon material in the high-temperature construction and working processes can be effectively relieved by performing the treatments of coating, packaging, hole plugging and the like on the material, so that the service life of the electrothermal film is prolonged. Phosphate and borate contained in the heating slurry can be coated on the surface of the carbon material at low temperature, so that the effect of blocking air is achieved; the simple substance boron powder and boride have the function of absorbing oxygen in the air, so that the carbon material is effectively protected in the construction process, and the oxidation degree of the carbon material is reduced. And finally, the pores among the materials of the heating slurry are filled up through the combined action of the glass powder and the high-temperature-resistant oxygen absorbent, so that the working stability of the heating slurry at high temperature is further ensured.
The invention provides a preparation method of water-soluble high-temperature-resistant infrared carbon-based heating slurry, which comprises the following steps of; s101, at least uniformly mixing a phosphate solution, a high-temperature-resistant oxidant and water at the temperature of 40-80 ℃ to prepare a first mixed solution; s103, at least adding glass powder, carbon-based conductive powder and inorganic filler powder into the first mixed solution, dispersing for 0.5-1h, and cooling to obtain a second mixed solution; s105, adding tetrabutyl titanate into the second mixed solution, and stirring at the rotating speed of 500-2000r/min for 1-4h to prepare a third mixed solution; s107, rolling the third mixed solution to a set thickness to obtain the water-soluble high-temperature-resistant infrared carbon-based heating slurry.
For the above method for preparing water-soluble high-temperature resistant infrared carbon-based heating slurry, in a possible embodiment, the S101 includes: uniformly mixing phosphate solution, high-temperature-resistant oxidant, aluminum-based sol and water to prepare first mixed solution; and/or said S103 comprises: adding glass powder, carbon-based conductive powder, an oxygen absorbent and inorganic filler powder into the first mixed solution, dispersing for 0.5-1h, and cooling to prepare a second mixed solution; the S105 includes: adding tetrabutyl titanate into the second mixed solution, and stirring for the first time at the rotating speed of 500-2000r/min under the temperature condition of 40-80 ℃; after cooling, adding a dispersing agent, a film forming agent, a flatting agent, an anti-settling agent, a defoaming agent and a thickening agent, and stirring for the second time at the rotating speed of 500-2000 r/min.
It can be understood that the preparation method of the water-soluble high-temperature-resistant infrared carbon-based heating slurry at least has all the technical effects of any one of the water-soluble high-temperature-resistant infrared carbon-based heating slurries, and details are not repeated herein.
Drawings
The water-soluble high temperature resistant infrared carbon-based heating slurry and the preparation method thereof according to the present invention will be described with reference to examples. In the drawings:
fig. 1 shows a schematic flow diagram of a preparation method of a water-soluble high-temperature-resistant infrared carbon-based heating slurry according to an embodiment of the invention.
Detailed Description
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and are not intended to limit the scope of the present invention.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better understanding of the present invention, and it will be apparent to one skilled in the art that the present invention may be practiced without some of the specific details. In some instances, slurry preparation processes and the like well known to those skilled in the art have not been described in detail in order to highlight the gist of the present invention.
The invention provides a water-soluble high-temperature-resistant infrared carbon-based heating slurry, which can be used as a water-soluble high-temperature carbon-based electric heating coating and the like. In one possible embodiment, the heating slurry comprises water and a slurry matrix, and the components of the slurry matrix are mixed according to the following weight ratio: 15-20 parts of 40-50wt% phosphate solution or an amount equivalent to the phosphate content (this example takes 15-20 parts of 40-50wt% phosphate solution as an example); 2-14 parts of glass powder; 1-40 parts of carbon-based conductive powder; 5-10 parts of inorganic filler powder; 1-3 parts of tetrabutyl titanate; 1-5 parts of high-temperature resistant oxidant; 0.1-5 parts of a dispersant; 1-20 parts of a film forming agent; 0.1-3 parts of a leveling agent; 0.1-3 parts of anti-settling agent; 0.01-3 parts of a defoaming agent; 0.01-3 parts of thickening agent.
In one possible embodiment, the phosphate solution is selected from aluminum dihydrogen phosphate and aluminum chromium phosphate which are commercially available. And oxides or hydroxides of magnesium, copper, zinc, zirconium, and aluminum are compounded as a curing agent contained in the phosphate solution, for example, the curing agent is usually 2 to 10wt% of the solid content of the phosphate solution.
In one possible embodiment, the glass powder is selected from one or more of silicate, borate, borosilicate and phosphate glasses having acid resistance and a total melting temperature of 300-1050 ℃.
In one possible embodiment, the carbon-based conductive powder is selected from one or more of graphene, graphite nanoplatelets, conductive carbon black, carbon fibers and carbon nanotubes.
In one possible embodiment, the inorganic filler mainly comprises (high) thermal conductive powder, insulating powder and TCR regulator, wherein the (high) thermal conductive powder is selected from one or more of inert ceramic powder, cordierite-based infrared radiation powder, transition metal oxide infrared radiation powder, boron nitride and the like, the insulating powder is selected from one or more of mica, kaolin and the like, and the TCR regulator is selected from one or more of ruthenium oxide, modified barium titanate, eucryptite, zirconium phosphate and the like.
In one possible embodiment, the high temperature resistant oxidizing agent is one or more selected from phosphoric acid, zinc phosphate, triammonium phosphate or boric acid.
Preferably, the slurry matrix further comprises the following components mixed according to the following weight ratio: 8-12 parts of inorganic sol; 0.1-10 parts of oxygen absorbent.
Wherein, the main function of the inorganic sol is to improve the high-temperature stability of the slurry. The boron oxygen absorbent can be continuously oxidized in the air at 600-850 ℃, has the function of taking oxygen on the surface of the conductive phase to protect the conductive material from being oxidized, can also form a high-thick-state and low-melting-point glass phase, plays a role in blocking a gap remained by curing and shrinking phosphate, and is fused with surrounding glass powder to form the borosilicate glass with better performance.
It is understood that the skilled person can add an appropriate amount of water to form the slurry according to actual needs, for example, the slurry contains 10-100 parts of water (not containing water as a solvent in the phosphate solution).
In one possible embodiment, the inorganic sol comprises an aluminum-based sol, which is a highly transparent viscous colloid having a pH of 5 to 7 and a colloidal particle diameter of 20 to 80nm, and is dehydrated at a high temperature to produce activated alumina or high-purity alumina. Optionally, the aluminum-based sol may further include other inorganic sols such as nano zirconium sol, nano titanium sol, nano yttrium sol, and nano silicon sol.
In one possible embodiment, the oxygen-absorbing agent may be elemental boron powder, a metal boride, or the like.
Referring to fig. 1, fig. 1 shows a schematic flow chart of a preparation method of a water-soluble high-temperature-resistant infrared carbon-based heating slurry according to an embodiment of the invention. As shown in fig. 1, in one possible embodiment, the preparation method mainly comprises the following steps:
s101, uniformly mixing the aluminum-based sol, the phosphate solution, the high-temperature-resistant oxidant and water at the temperature of 40-80 ℃ to prepare a first mixed solution.
S103, adding glass powder, carbon-based conductive powder, an oxygen absorbent and inorganic filler powder into the first mixed solution, and dispersing at a high speed for 0.5-1h to prepare a second mixed solution.
And S105, adding tetrabutyl titanate into the second mixed solution, stirring for the first time at the rotating speed of 500-2000r/min at the temperature of 40-80 ℃ for 1-4h, cooling (for example, cooling to the room temperature approximately), adding an auxiliary agent (comprising the dispersing agent, the film forming agent, the leveling agent, the anti-settling agent, the defoaming agent and the thickening agent), and stirring for the second time at the rotating speed of 500-2000r/min at the room temperature for 1-4h to prepare a third mixed solution.
S107, rolling the third mixed solution to a corresponding thickness (the thickness is mainly used for controlling the solid content of the slurry, such as 10 mu m) by adopting equipment such as a three-roll mill and the like, and thus obtaining the water-soluble high-temperature-resistant infrared carbon-based heating slurry.
Based on this, the water-soluble high temperature resistant infrared carbon-based heating slurry and the preparation method thereof of the present invention are further described below with reference to four specific examples.
Example 1:
in the embodiment, the components of the heated slurry are mixed according to the following weight ratio:
8 parts of aluminum-based sol; 20 parts of aluminum dihydrogen phosphate; 8 parts of low-melting-point glass powder; 10 parts of nano graphite sheet; 10 parts of alumina powder; 3 parts of tetrabutyl titanate; 3 parts of high-temperature resistant oxidant; 5 parts of an oxygen absorbent; 5 parts of a dispersing agent; 10 parts of a film forming agent; 2 parts of a leveling agent; 0.5 part of anti-settling agent; 0.5 part of a defoaming agent; 0.1 part of thickening agent and 50 parts of water.
Correspondingly, the preparation method of the heating slurry comprises the following steps:
uniformly mixing the aluminum-based sol, aluminum dihydrogen phosphate, a high-temperature-resistant oxidant and water at the temperature of 60-80 ℃ to form a first mixed solution;
adding glass powder, carbon-based conductive powder, an oxygen absorbent and alumina powder into the first mixed solution, and dispersing at a high speed for 0.5h to obtain a second mixed solution;
adding tetrabutyl titanate into the second mixed solution, and stirring at the temperature of 60-80 ℃ and the rotating speed of 1500-2000r/min for about 3h (first stirring);
cooling to room temperature, adding the auxiliary agent, and stirring at the rotating speed of 500-1000r/min for about 1h (stirring for the second time) to obtain a third mixed solution;
and rolling the third mixed solution to 10 mu m by using a three-roller rolling mill to obtain the water-soluble high-temperature graphene heating slurry.
The prepared heating slurry is prepared into an electric heating element through screen printing, the thickness of the obtained electric heating element is 30 mu m, the sheet resistance is 43 omega cm, the TCR value is-800 ppm/DEG C, and the electric heating element can realize the heating function of 450 ℃ by electrifying 220V.
Example 2:
in the embodiment, the components of the heated slurry are mixed according to the following weight ratio:
12 parts of aluminum-based sol; 20 parts of aluminum dihydrogen phosphate; 8 parts of low-melting-point glass powder; 2 parts of few-layer graphene; 4 parts of modified cordierite powder; 2 parts of ruthenium oxide powder; synthesizing 3 parts of mica powder; 3 parts of tetrabutyl titanate; 2 parts of triammonium phosphate; 1 part of boric acid; 3 parts of simple substance boron powder; 3 parts of titanium boride; 5 parts of a dispersing agent; 6 parts of amino resin; 2 parts of dipropylene glycol butyl ether DPNB; 2 parts of a leveling agent; 0.5 part of anti-settling agent; 0.5 part of defoaming agent; 0.1 part of thickening agent and 50 parts of water.
Correspondingly, the preparation method of the heating slurry comprises the following steps:
uniformly mixing the aluminum-based sol, aluminum dihydrogen phosphate, triammonium phosphate, boric acid and water at the temperature of 80 ℃ to prepare a first mixed solution;
adding glass powder, few-layer graphene powder, simple substance boron powder, titanium boride powder, ruthenium oxide powder, synthetic mica powder and modified cordierite powder into the first mixed solution, and dispersing at high speed for 1h to prepare a second mixed solution;
adding tetrabutyl titanate into the second mixed solution, and stirring for 3 hours at the temperature of 80 ℃ and at the rotating speed of 2000 r/min;
cooling to room temperature, adding the auxiliary agent, and stirring at the rotating speed of 1000r/min for 1h to prepare a third mixed solution;
and rolling the third mixed solution to 10 mu m by using a three-roller rolling mill to prepare the water-soluble high-temperature graphene heating slurry.
The prepared slurry is prepared into an electric heating element through screen printing, the thickness of the obtained electric heating element is 15 mu m, the sheet resistance is 100 omega cm, the TCR value is 120 ppm/DEG C, and the electric heating element can realize the heating function of 500 ℃ when electrified at 220V.
Example 3:
in the embodiment, the components of the heated slurry are mixed according to the following weight ratio:
10 parts of aluminum-based sol; 20 parts of aluminum chromium phosphate; 12 parts of low-melting-point glass powder; 15 parts of carbon fiber; 4 parts of synthetic mica powder; 4 parts of bismuth oxide powder; 3 parts of tetrabutyl titanate; 2 parts of triammonium phosphate; 3 parts of boric acid; 5 parts of elemental boron powder; 5 parts of a dispersing agent; 6 parts of amino resin; 2 parts of DPNB; 2 parts of a leveling agent; 0.5 part of anti-settling agent; 0.5 part of defoaming agent; 0.1 part of thickening agent and 50 parts of water.
Correspondingly, the preparation method of the heating slurry comprises the following steps:
uniformly mixing the aluminum-based sol, aluminum chromium phosphate, triammonium phosphate, boric acid and water at the temperature of 80 ℃ to prepare a first mixed solution;
adding glass powder, carbon fiber powder, elemental boron powder, synthetic mica powder, bismuth oxide powder and modified cordierite powder into the first mixed solution, and dispersing at high speed for 1h to prepare a second mixed solution;
adding tetrabutyl titanate into the second mixed solution, stirring for 2 hours at the temperature of 80 ℃ at the rotating speed of 1000r/min, cooling to room temperature, adding an auxiliary agent, and stirring for 1 hour at the rotating speed of 800r/min to prepare a third mixed solution;
and rolling the third mixed solution to 20 mu m by using a three-roller rolling mill to prepare the water-soluble high-temperature graphene heating slurry.
The prepared slurry is prepared into an electric heating element through screen printing, the thickness of the obtained electric heating element is 30 mu m, the square resistance is 300 omega cm, the TCR value is-300 ppm/DEG C, and the heating function at 400 ℃ can be realized by electrifying 220V.
Example 4:
in the embodiment, the components of the heated slurry are mixed according to the following weight ratio:
12 parts of aluminum-based sol; 20 parts of aluminum dihydrogen phosphate; 8 parts of low-melting-point glass powder; 0.5 part of few-layer graphene; 5 parts of nano graphite sheet; synthesizing 3 parts of mica powder; 3 parts of tetrabutyl titanate; 4 parts of boric acid; 4 parts of elemental boron powder; 5 parts of a dispersing agent; 6 parts of amino resin; 2 parts of DPNB; 2 parts of a leveling agent; 0.5 part of anti-settling agent; 0.5 part of defoaming agent; 0.1 part of thickening agent and 50 parts of water.
Correspondingly, the preparation method of the heating slurry comprises the following steps:
uniformly mixing the aluminum-based sol, aluminum dihydrogen phosphate, triammonium phosphate, boric acid and water at the temperature of 80 ℃ to prepare a first mixed solution;
adding glass powder, few-layer graphene powder, nano graphite flakes, elemental boron powder and synthetic mica powder into the first mixed solution, and dispersing at a high speed for 1h to prepare a second mixed solution;
adding tetrabutyl titanate into the second mixed solution, and stirring for 3 hours at the temperature of 80 ℃ and the rotating speed of 2000 r/min; cooling to room temperature, adding the auxiliary agent, and stirring at the rotating speed of 1000r/min for 1h to prepare a third mixed solution;
and rolling the third mixed solution to 10 mu m by using a three-roller rolling mill to prepare the water-soluble high-temperature graphene heating slurry.
The prepared heating slurry is prepared into an electric heating element through screen printing, the thickness of the obtained electric heating element is 20 mu m, the sheet resistance is 20 omega cm, the TCR value is-200 ppm/DEG C, and the heating function at 500 ℃ can be realized by electrifying 220V.
The water-soluble high-temperature graphene heating slurry has excellent high-temperature oxidation resistance and aging resistance after film formation, and can reliably and stably work at high temperature for a long time. Meanwhile, the heated slurry has extremely high infrared emissivity at high temperature, so that a relatively obvious energy-saving effect can be realized, and the cost of the heated slurry is relatively low, so that the heated slurry is expected to be widely applied to high-temperature scenes such as household appliances, industrial baking, boiler heating and the like.
It should be noted that, although the foregoing embodiments describe each step in a specific sequence, those skilled in the art may understand that, in order to achieve the effect of the present invention, different steps do not have to be executed in such a sequence, and may be executed simultaneously or in other sequences, and some steps may be added, replaced or omitted.
It should be noted that, although the preparation method of the water-soluble high temperature resistant infrared carbon-based heating slurry constituted in the above-described specific manner is described as an example, those skilled in the art can understand that the present invention should not be limited thereto. In fact, the user can flexibly adjust the relevant steps and the parameters and other elements in the steps according to the situations such as practical application scenes, and the like, for example, the parameters such as the stirring time, the rolling thickness and the like can be adjusted according to the practical requirements.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is apparent to those skilled in the art that the scope of the present invention is not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.

Claims (10)

1. The water-soluble high-temperature-resistant infrared carbon-based heating slurry is characterized by comprising water and a slurry matrix, wherein the slurry matrix is prepared by mixing the following components in parts by weight:
15-20 parts of 40-50wt% phosphate solution or the amount of phosphate equivalent to the phosphate solution; 2-14 parts of glass powder; 1-40 parts of carbon-based conductive powder; 5-10 parts of inorganic filler powder; 1-3 parts of tetrabutyl titanate; 1-5 parts of high-temperature resistant oxidant; 0.1-5 parts of a dispersant; 1-20 parts of a film forming agent; 0.1-3 parts of a leveling agent; 0.1-3 parts of anti-settling agent; 0.01-3 parts of a defoaming agent; 0.01-3 parts of thickening agent.
2. The water-soluble high-temperature-resistant infrared carbon-based heating slurry as claimed in claim 1, wherein the slurry matrix further comprises the following components mixed according to the following weight ratio:
8-12 parts of inorganic sol; and/or
0.1-10 parts of oxygen absorbent.
3. The water-soluble high temperature resistant infrared carbon-based heating slurry according to claim 2, wherein the inorganic sol comprises an aluminum-based sol; and/or
The oxygen absorbent is simple substance boron powder and/or metal boride.
4. The water-soluble high temperature resistant infrared carbon-based heating slurry according to claim 3, wherein the aluminum-based sol has the following properties:
the pH is 5-7; the colloidal particle diameter of the sol is 20-80nm.
5. The water soluble high temperature resistant infrared carbon based heating paste of claim 1, wherein the solutes of the phosphate solution comprise aluminum dihydrogen phosphate, aluminum chromium phosphate; and/or
The glass powder is one or more of silicate glass, borate glass, borosilicate glass and phosphate glass; and/or
The carbon-based conductive powder is one or more of graphene, nano graphite sheets, conductive carbon black, carbon fibers and carbon nano tubes; and/or
The inorganic filler comprises heat-conducting powder, insulating powder and a TCR regulator; and/or
The high-temperature resistant oxidant is one or more of phosphoric acid, zinc phosphate, triammonium phosphate and boric acid.
6. The water-soluble high temperature resistant infrared carbon-based heating slurry according to claim 5, wherein the phosphate solution comprises a curing agent.
7. The water soluble high temperature resistant infrared carbon based heating paste according to claim 6, wherein the curing agent comprises oxides and/or hydroxides of magnesium, copper, zinc, zirconium and/or aluminum; and/or
The content of the curing agent is 2-10wt% of the solute of the phosphate solution.
8. The water-soluble high-temperature-resistant infrared carbon-based heating slurry as claimed in claim 5, wherein the heat-conducting powder is one or more of inert ceramic powder, cordierite-based infrared radiation powder, transition metal oxide infrared radiation powder and boron nitride; and/or
The insulating powder is mica and/or kaolin; and/or
The TCR regulator is one or more of ruthenium oxide, modified barium titanate, eucryptite and zirconium phosphate.
9. A method for preparing the water-soluble high temperature resistant infrared carbon-based heating paste according to any one of claims 1 to 8, wherein the preparation method comprises;
s101, at least uniformly mixing a phosphate solution, a high-temperature-resistant oxidant and water at the temperature of 40-80 ℃ to prepare a first mixed solution;
s103, at least adding glass powder, carbon-based conductive powder and inorganic filler powder into the first mixed solution, dispersing for 0.5-1h, and cooling to obtain a second mixed solution;
s105, adding tetrabutyl titanate into the second mixed solution, and stirring at the rotating speed of 500-2000r/min for 1-4h to prepare a third mixed solution;
s107, rolling the third mixed solution to a set thickness to obtain the water-soluble high-temperature-resistant infrared carbon-based heating slurry.
10. The method for preparing water-soluble high temperature resistant infrared carbon-based heating slurry according to claim 9,
the S101 comprises: mixing phosphate solution, high-temperature-resistant oxidant, aluminum-based sol and water to prepare first mixed solution; and/or
The step S103 comprises: adding glass powder, carbon-based conductive powder, an oxygen absorbent and inorganic filler powder into the first mixed solution, dispersing for 0.5-1h, and cooling to prepare a second mixed solution;
the S105 includes:
adding tetrabutyl titanate into the second mixed solution, and stirring for the first time at the rotating speed of 500-2000r/min under the temperature condition of 40-80 ℃;
after cooling, adding a dispersing agent, a film forming agent, a flatting agent, an anti-settling agent, a defoaming agent and a thickening agent, and stirring for the second time at the rotating speed of 500-2000r/min to prepare a third mixed solution.
CN202210899979.5A 2022-07-28 2022-07-28 Water-soluble high-temperature-resistant infrared carbon-based heating slurry and preparation method thereof Pending CN115175385A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115029022A (en) * 2022-06-08 2022-09-09 郑州新世纪材料基因组工程研究院有限公司 High-temperature electric heating slurry, electric infrared heating film and preparation method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115029022A (en) * 2022-06-08 2022-09-09 郑州新世纪材料基因组工程研究院有限公司 High-temperature electric heating slurry, electric infrared heating film and preparation method

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