CN109629793A - Safety and environmental protection electric heating ceramic tile - Google Patents

Safety and environmental protection electric heating ceramic tile Download PDF

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Publication number
CN109629793A
CN109629793A CN201811600187.3A CN201811600187A CN109629793A CN 109629793 A CN109629793 A CN 109629793A CN 201811600187 A CN201811600187 A CN 201811600187A CN 109629793 A CN109629793 A CN 109629793A
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CN
China
Prior art keywords
ceramic tile
50min
mass ratio
safety
heating
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Pending
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CN201811600187.3A
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Chinese (zh)
Inventor
张玉强
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Liaoning Suchun Environmental Protection Technology Co Ltd
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Liaoning Suchun Environmental Protection Technology Co Ltd
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Priority to CN201811600187.3A priority Critical patent/CN109629793A/en
Publication of CN109629793A publication Critical patent/CN109629793A/en
Pending legal-status Critical Current

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Classifications

    • 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
    • E04F15/08—Flooring or floor layers composed of a number of similar elements only of stone or stone-like material, e.g. ceramics, concrete; of glass or with a top layer of stone or stone-like material, e.g. ceramics, concrete or glass
    • E04F15/082—Flooring or floor layers composed of a number of similar elements only of stone or stone-like material, e.g. ceramics, concrete; of glass or with a top layer of stone or stone-like material, e.g. ceramics, concrete or glass with a top layer of stone or stone-like material, e.g. ceramics, concrete or glass in combination with a lower layer of other material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/245—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it being a foam layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F15/00—Flooring
    • E04F15/18—Separately-laid insulating layers; Other additional insulating measures; Floating floors
    • E04F15/181—Insulating layers integrally formed with the flooring or the flooring elements
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24—HEATING; RANGES; VENTILATING
    • F24D—DOMESTIC- OR SPACE-HEATING SYSTEMS, e.g. CENTRAL HEATING SYSTEMS; DOMESTIC HOT-WATER SUPPLY SYSTEMS; ELEMENTS OR COMPONENTS THEREFOR
    • F24D13/00—Electric heating systems
    • F24D13/02—Electric heating systems solely using resistance heating, e.g. underfloor heating
    • F24D13/022—Electric heating systems solely using resistance heating, e.g. underfloor heating resistances incorporated in construction elements
    • F24D13/024—Electric heating systems solely using resistance heating, e.g. underfloor heating resistances incorporated in construction elements in walls, floors, ceilings
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/145—Carbon only, e.g. carbon black, graphite
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
    • H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
    • H05B3/26—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base
    • H05B3/265—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base the insulating base being an inorganic material, e.g. ceramic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/02—Coating on the layer surface on fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/20—Inorganic coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/26—Polymeric coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/101—Glass fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2266/00—Composition of foam
    • B32B2266/02—Organic
    • B32B2266/0214—Materials belonging to B32B27/00
    • B32B2266/0278—Polyurethane
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2419/00—Buildings or parts thereof
    • B32B2419/04—Tiles for floors or walls
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F2290/00—Specially adapted covering, lining or flooring elements not otherwise provided for
    • E04F2290/02—Specially adapted covering, lining or flooring elements not otherwise provided for for accommodating service installations or utility lines, e.g. heating conduits, electrical lines, lighting devices or service outlets
    • E04F2290/023—Specially adapted covering, lining or flooring elements not otherwise provided for for accommodating service installations or utility lines, e.g. heating conduits, electrical lines, lighting devices or service outlets for heating
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F2290/00—Specially adapted covering, lining or flooring elements not otherwise provided for
    • E04F2290/04—Specially adapted covering, lining or flooring elements not otherwise provided for for insulation or surface protection, e.g. against noise, impact or fire

Abstract

The invention discloses a kind of safety and environmental protection electric heating ceramic tiles.The safety and environmental protection electric heating ceramic tile includes ceramic tile, heating layer, insulating layer；The ceramic tile back side is successively arranged downwards heating layer and insulating layer；The heating layer is connect by adhesive with ceramic tile, insulating layer.Safety and environmental protection electric heating ceramic tile of the present invention has many advantages, such as safe and environment-friendly, energy-efficient, beautiful health, durable, and installs simple and fast, and as common floor tile, longer life expectancy is easy to maintenance, and replacement is convenient.

Description

Safety and environmental protection electric heating ceramic tile
Technical field
The present invention relates to fitment material for family fields, and in particular to safety and environmental protection electric heating ceramic tile.
Background technique
With the improvement of living standards, the heating mode in winter is more and more, the overwhelming majority is by heat medium, so It is transmitted in air by medium afterwards.The current heating system in China mainly has: central heating, radiator heating, heating floor are adopted Warm, central air-conditioning heating divides family wall-hanging gas-fired heating, electric heat membrane heating etc..Various heating systems have the advantages that it is respective and Disadvantage, wherein central heating, radiator heating, heating floor heating are the heating system that city uses in flakes on a large scale, advantage It is that technology is more mature, it is safe and convenient to use, it round-the-clock can heat, expense is relatively cheap.It also has apparent defect: heating Temperature and time not by oneself control, three-dimensional cooling fin unsightly, take up space, influence indoor finishing effect, supplying Front and back is without heat source etc. between warm period.Central air-conditioning heating, point family wall-hanging gas-fired heating, electric heat membrane heating are more personalized adopt Warm mode, it is easier to realize that the temperature and time of heating freely controls.Most of central air-conditioning heating system is in high-grade building It uses, its advantage is that class is high, good appearance, comfort level are high, temperature and time is adjustable, and compared with being suitable for, area is biggish low close Spend house and villa.But this heating system equally exists apparent defect: the investment of early period is big and operating cost is higher, consumption Electricity is big, can not enjoy the preferential policy of national valley power consumption.Point family wall-hanging gas-fired heating is burnt natural gas by wall-hung boiler Achieve the purpose that heating, advantage is can be set by oneself the time of heating, is opened at any time, room temperature can be in a certain range Arbitrarily adjust.The disadvantage is that service life only has l5 or so, it is high to update maintenance cost, heat pump starting and flame combustion, noise compared with Greatly, and there are certain air pollution problems inherents.Electric heating thin-film mode is using electric power as heat source, using Electric radiant Heating Film as heater, greatly Most Electric radiant Heating Films are ceiling-type or wall-mounted, and snugness sense is good, and controllability is strong；And by then passing through electromagnetic infrared wave Infrared ray direct heat transfer, so not will cause dusty without air circulation；Investment cost is lower.Its shortcomings that, is: consumption Electricity is big, and operating cost is higher.Now with a kind of emerging heating mode, that is, electric heating ceramic tile passes through electrothermal tube and fever Cable carrys out heating floor.Electric heating ceramic tile has many advantages, such as that heat dissipation is uniform, saves space, heating is fast, safe and reliable.But electric heating ceramic tile Integral structure is mostly used, is repaired very difficult.
Existing electric heating ceramic tile technology, be heating film is sticked in back using adhesive at traditional ceramic tile back side, then With layer of polyurethane on gluing behind heating film, it is outer to have the disadvantages that adhesive is easy for the ceramic tile made by above-mentioned technique Leakage, causes back appearance coarse；It because layer of polyurethane is soft material, can be deformed under weight, so that ceramic tile be made to have weight to sink Risk；Since heat insulation effect can be reduced after the layer of polyurethane stress deformation of bottom, to increase the heat damage of electric heating ceramic tile It loses；；Because of the problems such as largely using adhesive when fixed electric hot plate and layer of polyurethane, increase indoor environmental pollution, especially state The calandria that interior charcoal crystalline substance floor uses is to be produced using different slurries, and many enterprises have used slurry not up to standard, from And make product electric hot plate power becomes larger in use, to increase fire risk.
Therefore a kind of new electric heating ceramic tile is needed at present, it is of the existing technology to solve the problems, such as.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the present invention provides a kind of safety and environmental protection electric heating ceramic tiles.
A kind of safety and environmental protection electric heating ceramic tile, including ceramic tile, heating layer, insulating layer；The ceramic tile back side is followed successively by downwards institute State heating layer and the insulating layer；The heating layer is connect by adhesive with the ceramic tile, the insulating layer；The heating layer For heating film or heating blanket.
The heating film the preparation method comprises the following steps:
I, mixes graphene, carbon black, stabilizer, Thermal conductive additives, dimethylformamide, after ball milling 30-60min, then plus Enter polyamide rouge, continue ball milling, obtains heating film slurry；
Heating film slurry is evenly coated on glass fabric by II, by coating machine, dry, obtains naked mould, routinely work Skill is arranged after conductive bar, insulating layer on naked film to obtain the final product.
The graphene, carbon black, stabilizer, Thermal conductive additives, dimethylformamide, polyamide rouge mass ratio be (10-20): (5-8): (5-15): (5-15): (15-30): (15-30).
The stabilizer includes one of aluminium oxide, titanium dioxide, silver powder or a variety of.
The Thermal conductive additives include one of organically-modified aluminium nitride, boron nitride, modified boron nitride or a variety of.
Preferably, the Thermal conductive additives press (1-3) by organically-modified aluminium nitride, boron nitride: the mass ratio of (1-3) mixes It forms.
It is highly preferred that the Thermal conductive additives press (1-3) by organically-modified aluminium nitride, modified boron nitride: the quality of (1-3) Than mixing.
The graphene the preparation method comprises the following steps:
Graphite, the concentrated sulfuric acid, concentrated nitric acid are pressed into 1:(60-80): the mass ratio of (15-30) mixes, and is placed at 0-4 DEG C and stirs 20-50min is subsequently added into 5-8 times of graphite quality of potassium permanganate, is placed at 30-35 DEG C after stirring 1-3h, obtains mixture； It is subsequently added into 0.5-1.5 times of mixture quality of water, 20-50min is stirred at 85-100 DEG C, is eventually adding mixture quality 0.1-0.4 times of hydrogenperoxide steam generator stirs 10-30min at 80-90 DEG C, filters, after washed, dry, ball-milling treatment, To obtain the final product.
Preferably, the graphene the preparation method comprises the following steps: press (0.05-0.15): 20 mass ratio, by modifying agent, solvent Mixing is ultrasonically treated 20-50min, obtains mixed liquor；The graphite of mixed liquor quality 0.5-2.5% is added to above-mentioned mixed liquor In, it is homogenized 20-50min under the revolving speed of 16000-28000r/min, then ultrasonication 20-50min, obtains suspension, Standing, centrifugation filter processing gained supernatant, after washed, drying to obtain the final product.
It is highly preferred that the graphene the preparation method comprises the following steps: pressing (0.05-0.15): 20 mass ratio, by modifying agent, molten Agent mixing, is ultrasonically treated 20-50min, obtains mixed liquor；Graphite is placed in microwave bulking 5- under the microwave power of 200-400W 15min is cooled to microwave bulking 5-15min under the microwave power that 20-35 DEG C is followed by placed in 200-400W, cooling, obtains swollen Change the graphite of processing；The graphite of the expanding treatment of mixed liquor quality 0.5-2.5% is added in above-mentioned mixed liquor, in 16000- It is homogenized 20-50min under the revolving speed of 28000r/min, then ultrasonication 20-50min, obtains suspension, stand, be centrifuged, takes out Filter processing gained supernatant, after washed, drying to obtain the final product.
It is further preferred that the graphene the preparation method comprises the following steps: press (0.05-0.15): 20 mass ratio will be modified Agent, solvent mixing, are ultrasonically treated 20-50min, obtain mixed liquor；It is swollen that graphite is placed in microwave under the microwave power of 200-400W Change 5-15min, is cooled to microwave bulking 5-15min under the microwave power that 20-35 DEG C is followed by placed in 200-400W, it is cooling, it obtains To the graphite of expanding treatment；The graphite of the expanding treatment of mixed liquor quality 0.5-2.5% is added in above-mentioned mixed liquor, It is homogenized 20-50min under the revolving speed of 16000-28000r/min, then ultrasonication 20-50min, obtains suspension；Then plus Enter dispersing aid, the dispersing aid, suspension mass ratio be (0.3-0.6): 100, be ultrasonically treated 20-50min, stand, Centrifugation filters processing gained supernatant, after washed, drying to obtain the final product.
The modifying agent includes 4,4'- benzidine, 4'- hydroxyazobenzene -2- carboxylic acid, 3,3', 5,5'- biphenyl tetracarboxylic One of acid is a variety of.
The solvent includes one of N-Methyl pyrrolidone, ethyl alcohol, gamma-butyrolacton, acetone, cyclohexanone, toluene.
The dispersing aid presses (1-2) by polyvinylpyrrolidone, polyvinyl alcohol, oleic acid: (1-2): the mass ratio of (2-4) It mixes.
The preparation method of the organically-modified aluminium nitride: by the mass ratio of 100:(2-4), by aluminium nitride, 3- (methyl-prop Alkene acyl-oxygen) propyl trimethoxy silicane mixing, mixture is obtained, the dehydrated alcohol of mixture quality 20-40%, ball are subsequently added into Mill obtains organically-modified aluminium nitride after washed, drying process.
The preparation method of the modified boron nitride: press 100:(6-8): (1.5-2): the mass ratio of (2-5), by boron nitride, Fluorographite, yttrium fluoride, titanium carbide mixing, ball milling obtain mixture A；Then aluminium nitride, polyethylene are added into mixture A Butyral, hexagonal boron nitride, tributyl phosphate, dehydrated alcohol, acrylic resin, the mixture A, aluminium nitride, polyethylene Butyral, hexagonal boron nitride, tributyl phosphate, dehydrated alcohol, acrylic resin mass ratio be 100:(4-8): (4-8): (0.5-1.5): (2-6): (70-140): (1.5-3), ball milling obtain mixture B；Mixture B is placed at 40 DEG C dry 10- 20h is warming up to 1800-1900 DEG C then under gas nitrogen protection, after keeping the temperature 8-16h at 1800-1900 DEG C, is cooled to 1300-1400 DEG C, 8-16h is kept the temperature at 1300-1400 DEG C, is then cooled to 400-500 DEG C, is cooled to 25-35 DEG C, is changed Property boron nitride.
By adopting the above-described technical solution, compared with prior art, the present invention has the following advantages: using this hair The electric heating ceramic tile that bright safety and environmental protection electric heating ceramic tile preparation method is prepared, have it is safe and environment-friendly, energy-efficient, beautiful health, The advantages that durable, and installation is simple and fast, as common floor tile, longer life expectancy is easy to maintenance, and replacement is convenient.
Specific embodiment
Foregoing invention content of the invention is described in further detail With reference to embodiment, but should not be incited somebody to action This range for being interpreted as the above-mentioned theme of the present invention is only limitted to following embodiments.
Each raw material and equipment introduction in embodiment:
Polyurethane foam material, material are polyurethane, and specification is 1.2m × 60cm × 20mm, article No. 003, flame retardant rating B1 is purchased from the auspicious thermal insulation material agency of the Dezhou City Decheng District rising sun.
Epoxide-resin glue, model 8100 are purchased from Shandong Yu Bang Energy Saving Technology Co.
Ceramic tile, type throw glaze floor tile entirely, and specification is 800mm × 800mm, are purchased from Foshan City De Laibao building materials Co., Ltd.
Graphite, crystal particle diameter 0.01mm are purchased from Qingdao Sheng Ping graphite factory.
4,4'- benzidines, No. CAS: 92-87-5, product number: B802554 is purchased from Shanghai Mike woods biochemical technology Co., Ltd.
N-Methyl pyrrolidone, No. CAS: 872-50-4, top grade product are purchased from BASF Aktiengesellschaft.
Polyvinylpyrrolidone, No. CAS: 9003-39-8, density: 1.69g/cm3, model PVPK30, purchased from Guangdong Guangdong U.S. Chemical Co., Ltd..
Polyvinyl alcohol, No. CAS: 9002-89-5, average degree of polymerization 1750 is limited purchased from the sub- safe joint chemical industry of Wuxi City Company.
Oleic acid, No. CAS: 112-80-1, density 0.891g/cm3, it is purchased from Guangzhou Xu Xiang Chemical Co., Ltd..
Carbon black, partial size 25nm, specific surface area 180m2/ g, technical grade are limited purchased from the bright Pu development of information science and technology in Shanghai Company.
Aluminium oxide, partial size 100nm, article No. NO-O-005-1 are purchased from Shanghai Nai Ou nanosecond science and technology Co., Ltd.
Titanium dioxide, No. CAS: 13463-67-7, partial size 21nm, model P25, purchased from the international trade of Guangzhou person of virtue remittance Easy Co., Ltd.
Aluminium nitride, No. CAS: 24304-00-5,300 mesh are purchased from Jinzhou Hai Xin metal material Co., Ltd.
3- (methacryloxypropyl) propyl trimethoxy silicane, No. CAS: 2530-85-0, model KH570 are purchased from Dongguan Lv Wei plasthetics Co., Ltd, city.
Boron nitride, No. CAS: 10043-11-5, average grain diameter 1um, article No. NO-N-003-3 are Europe nanometer purchased from Shanghai Science and Technology Ltd..
Fluorographite, No. CAS: 51311-17-2,300 mesh, model 325116 is purchased from the limited public affairs of Shanghai shriek chemical industry Department.
Yttrium fluoride, No. CAS: 13709-49-4,100 mesh are purchased from 100,000 Chemical Co., Ltd. of Shandong.
Titanium carbide, No. CAS: 12070-08-5,1000 mesh, purchased from Qinghe County be full of alloy belong to Materials Co., Ltd.
Polyvinyl butyral, No. CAS: 63148-65-2, it is new to melt (Liaoning) chemical institute purchased from Tianyuan army for top grade product Material incubator limited liability company.
Hexagonal boron nitride, No. CAS: 10043-11-5, density 2.25g/cm3, limited purchased from the good prompt chemical products in Zhengzhou Company.
Tributyl phosphate, No. CAS: 126-73-8, model X-8054 are purchased from Guangzhou De Tian new material Co., Ltd.
Acrylic resin, No. CAS: 9003-01-4, model RL100 are purchased from germany rohm company.
N, N- dimethylmethacryl amide, No. CAS: 6976-91-6, product number: TCI-DO745 is stepped purchased from Shanghai Riel chemical technology Co., Ltd.
Polyamide rouge, No. CAS: 68410-23-1, density 0.9578kg/m3, trade mark DN-23 is high purchased from Shandong power New material Science and Technology Ltd..
Glass fabric is purchased from Sichuan Glass Fiber Co., Ltd. with a thickness of 0.2mm, model EW200-127.
Ball-grinding machine is MITR-YXQM-12L type nanometer formula planetary ball mill, is purchased from the limited public affairs of Changsha meter Qi instrument and equipment Department.
Coating machine is AT-TB-1100 type knife type coater, is purchased from Shandong An Nimaite Instrument Ltd..
Ultrasonic device is JY96-IIN ultrasonic cell disruptor instrument, is purchased from Zhengzhou north and south experimental instruments and equipment limited.
Centrifugation apparatus is TGL-16L type supercentrifuge, purchased from Beijing day even harmonious instrument and meter Co., Ltd.
Embodiment 1
A kind of safety and environmental protection electric heating ceramic tile, including ceramic tile, heating film, polyurethane foam material；The ceramic tile back side is downward It is successively arranged heating film and polyurethane foam material；The heating film is connect by epoxide-resin glue with ceramic tile, insulating layer.
The insulating layer is polyurethane foam material.
The heating film the preparation method comprises the following steps:
I, is by graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, boron nitride, N, N- dimethyl methyl The mixing of base acrylamide is placed in 30 DEG C, carries out ball milling 30min under conditions of 800r/min, using the zirconia ball of diameter 10mm As ball-milling medium, the ratio of grinding media to material is 2:1, is subsequently added into polyamide rouge, maintains ball milling condition constant, continues ball milling 1.5h, Obtain heating film slurry；
Heating film slurry is evenly coated on glass fabric by II, by coating machine, and the coating thickness is 20 μm, then It is placed at 45 DEG C after drying for 24 hours, obtains naked mould, routinely technique is arranged after conductive bar, insulating layer on naked film to obtain the final product.
The graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, boron nitride, N, N- dimethyl methyl Base acrylamide, polyamide rouge mass ratio be 15:7:5:5:5:5:25:25.
The graphene the preparation method comprises the following steps: by graphite, the 98wt% concentrated sulfuric acid, 65wt% concentrated nitric acid press 1:75:25 matter Amount after being placed at 0 DEG C, stirring 30min under conditions of 350r/min, is subsequently added into 6 times of graphite quality of potassium permanganate than mixing, After being placed in 35 DEG C, stirring 1h under conditions of 350r/min, mixture is obtained；It is subsequently added into 0.8 times of mixture quality of deionization Water is eventually adding 0.1 times of mixture quality of 30wt% hydrogen peroxide after stirring 30min under conditions of 90 DEG C, 350r/min Solution stirs 10min under the conditions of 85 DEG C, 350r/min, filters, and products therefrom successively uses 2wt% dilute hydrochloric acid and deionization again Water is washed, the product, dilute hydrochloric acid, deionized water mass ratio be 1:1:1.5, washing is placed at 100 DEG C dry 50min, then be placed in 30 DEG C, carry out ball milling 30min under conditions of 800r/min, using the zirconia ball of diameter 10mm as ball milling Medium, the ratio of grinding media to material be 2:1 to get.
The preparation method of the organically-modified aluminium nitride: by the mass ratio of 100:3, by aluminium nitride, 3- (methacryl Oxygen) propyl trimethoxy silicane mixing, obtain mixture, be subsequently added into the dehydrated alcohol of mixture quality 30%, be placed in 30 DEG C, Ball milling is carried out under conditions of 800r/min, using the zirconia ball of diameter 10mm as ball-milling medium, the ratio of grinding media to material is 2:1, Ball milling 2h is washed with 2 times of stock quality of dehydrated alcohol of ball-milling treatment, at last 50 DEG C after dry 4h, is obtained organically-modified Aluminium nitride.
Embodiment 2
Substantially the same manner as Example 1, difference is only in that: the heating film the preparation method comprises the following steps:
I, is by graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, N, N- dimethyl methacryl Amine mixing is placed in 30 DEG C, carries out ball milling 30min under conditions of 800r/min, using the zirconia ball of diameter 10mm as ball milling Medium, the ratio of grinding media to material are 2:1, are subsequently added into polyamide rouge, maintain ball milling condition constant, continue ball milling 1.5h, generated heat Film slurry；
Heating film slurry is evenly coated on glass fabric by II, by coating machine, and the coating thickness is 20 μm, then It is placed at 45 DEG C after drying for 24 hours, obtains naked mould, routinely technique is arranged after conductive bar, insulating layer on naked film to obtain the final product.
The graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride N, N- dimethyl methacryl Amine, polyamide rouge mass ratio be 15:7:5:5:10:25:25.
Embodiment 3
Substantially the same manner as Example 1, difference is only in that: the heating film the preparation method comprises the following steps:
I, sets graphene, carbon black, aluminium oxide, titanium dioxide, boron nitride, N, the mixing of N- dimethylmethacryl amide Ball milling 30min is carried out under conditions of 30 DEG C, 800r/min, it is described using the zirconia ball of diameter 10mm as ball-milling medium Ratio of grinding media to material is 2:1, is subsequently added into polyamide rouge, maintains ball milling condition constant, continues ball milling 1.5h, obtains heating film slurry；
Heating film slurry is evenly coated on glass fabric by II, by coating machine, and the coating thickness is 20 μm, then It is placed at 45 DEG C after drying for 24 hours, obtains naked mould, routinely technique is arranged after conductive bar, insulating layer on naked film to obtain the final product.
The graphene, carbon black, aluminium oxide, titanium dioxide, boron nitride, N, N- dimethylmethacryl amide, polyamide The mass ratio of rouge is 15:7:5:5:10:25:25.
Embodiment 4
Substantially the same manner as Example 1, difference is only in that: the heating film the preparation method comprises the following steps:
I, is by graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, modified boron nitride, N, N- diformazan Butylmethacrylamide mixing is placed in 30 DEG C, carries out ball milling 30min under conditions of 800r/min, using the oxidation of diameter 10mm For zirconium ball as ball-milling medium, the ratio of grinding media to material is 2:1, is subsequently added into polyamide rouge, maintains ball milling condition constant, continues ball milling 1.5h obtains heating film slurry；
Heating film slurry is evenly coated on glass fabric by II, by coating machine, and the coating thickness is 20 μm, then It is placed at 45 DEG C after drying for 24 hours, obtains naked mould, routinely technique is arranged after conductive bar, insulating layer on naked film to obtain the final product.
The graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, modified boron nitride, N, N- diformazan Butylmethacrylamide, polyamide rouge mass ratio be 15:7:5:5:5:5:25:25.
The preparation method of the modified boron nitride: by the mass ratio of 100:6:1.5:3, by boron nitride, fluorographite, fluorination Yttrium, titanium carbide mixing, are placed in 30 DEG C, carry out ball milling under conditions of 800r/min, using the zirconia ball of diameter 10mm as ball Grinding media, the ratio of grinding media to material is 2:1, after ball milling 6h, obtains mixture A；Then aluminium nitride, polyethylene are added into mixture A Butyral, hexagonal boron nitride, tributyl phosphate, dehydrated alcohol, acrylic resin, the mixture A, aluminium nitride, polyethylene Butyral, hexagonal boron nitride, tributyl phosphate, dehydrated alcohol, acrylic resin mass ratio be 100:4:4:1:2:100: 2, it maintains ball milling condition constant, after continuing ball milling 4h, obtains mixture B；Mixture B is placed at 40 DEG C dry 12h, is then existed Gas flow is 0.001m3Under the nitrogen protection of/h, 1850 DEG C are warming up to, after keeping the temperature 12h at 1850 DEG C, is cooled to 1400 DEG C, 10h is kept the temperature at 1400 DEG C, is then cooled to 400 DEG C, and wherein heating rate and rate of temperature fall are all 10 DEG C/min, finally 30 DEG C are cooled to, modified boron nitride is obtained.
Embodiment 5
Substantially the same manner as Example 1, difference is only in that: the heating film the preparation method comprises the following steps:
I, is by graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, modified boron nitride, N, N- diformazan Butylmethacrylamide mixing is placed in 30 DEG C, carries out ball milling 30min under conditions of 800r/min, using the oxidation of diameter 10mm For zirconium ball as ball-milling medium, the ratio of grinding media to material is 2:1, is subsequently added into polyamide rouge, maintains ball milling condition constant, continues ball milling 1.5h obtains heating film slurry；
Heating film slurry is evenly coated on glass fabric by II, by coating machine, and the coating thickness is 20 μm, then It is placed at 45 DEG C after drying for 24 hours, obtains naked mould, routinely technique is arranged after conductive bar, insulating layer on naked film to obtain the final product.
The graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, modified boron nitride, N, N- diformazan Butylmethacrylamide, polyamide rouge mass ratio be 15:7:5:5:5:5:25:25.
The graphene the preparation method comprises the following steps: press 0.1:20 mass ratio, by 4,4'- benzidine, acetone mix, It is ultrasonically treated 10min at 35 DEG C, the ultrasonic power of the ultrasonic treatment is 400W, supersonic frequency 28kHz, obtains mixed liquor； The graphite of mixed liquor quality 1% is added in above-mentioned mixed liquor, is first homogenized 50min under conditions of 30 DEG C, 16000r/min, Then the ultrasonication 30min at 35 DEG C, the ultrasonic power of the ultrasonic treatment is 400W, supersonic frequency 28kHz, is obtained Suspension stands 12h at 35 DEG C, and 10min is finally centrifuged under the conditions of 20 DEG C, 12000r/min, filters processing gained supernatant Liquid obtains product, with 1.5 times of ethanol washing of products therefrom quality, be placed at 100 DEG C after dry 50min to get.
The preparation method of the modified boron nitride: by the mass ratio of 100:6:1.5:3, by boron nitride, fluorographite, fluorination Yttrium, titanium carbide mixing, are placed in 30 DEG C, carry out ball milling under conditions of 800r/min, using the zirconia ball of diameter 10mm as ball Grinding media, the ratio of grinding media to material is 2:1, after ball milling 6h, obtains mixture A；Then aluminium nitride, polyethylene are added into mixture A Butyral, hexagonal boron nitride, tributyl phosphate, dehydrated alcohol, acrylic resin, the mixture A, aluminium nitride, polyethylene Butyral, hexagonal boron nitride, tributyl phosphate, dehydrated alcohol, acrylic resin mass ratio be 100:4:4:1:2:100: 2, it maintains ball milling condition constant, after continuing ball milling 4h, obtains mixture B；Mixture B is placed at 40 DEG C dry 12h, is then existed Gas flow is 0.001m3Under the nitrogen protection of/h, 1850 DEG C are warming up to, after keeping the temperature 12h at 1850 DEG C, is cooled to 1400 DEG C, 10h is kept the temperature at 1400 DEG C, is then cooled to 400 DEG C, and wherein heating rate and rate of temperature fall are all 10 DEG C/min, finally 30 DEG C are cooled to, modified boron nitride is obtained.
Embodiment 6
Substantially the same manner as Example 1, difference is only in that: the heating film the preparation method comprises the following steps:
I, is by graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, modified boron nitride, N, N- diformazan Butylmethacrylamide mixing is placed in 30 DEG C, carries out ball milling 30min under conditions of 800r/min, using the oxidation of diameter 10mm For zirconium ball as ball-milling medium, the ratio of grinding media to material is 2:1, is subsequently added into polyamide rouge, maintains ball milling condition constant, continues ball milling 1.5h obtains heating film slurry；
Heating film slurry is evenly coated on glass fabric by II, by coating machine, and the coating thickness is 20 μm, then It is placed at 45 DEG C after drying for 24 hours, obtains naked mould, routinely technique is arranged after conductive bar, insulating layer on naked film to obtain the final product.
The graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, modified boron nitride, N, N- diformazan Butylmethacrylamide, polyamide rouge mass ratio be 15:7:5:5:5:5:25:25.
The graphene the preparation method comprises the following steps: press 0.1:20 mass ratio, by 4,4'- benzidine, acetone mix, It is ultrasonically treated 10min at 35 DEG C, the ultrasonic power of the ultrasonic treatment is 400W, supersonic frequency 28kHz, obtains mixed liquor； Graphite is first placed in microwave bulking 10min under the microwave power of 400W, after being cooled to 20 DEG C, is then placed in the microwave power of 400W Lower extruding 10min, obtains the graphite of expanding treatment after being cooled to 20 DEG C；The graphite of the expanding treatment of mixed liquor quality 1% is added Enter into above-mentioned mixed liquor, is first homogenized 50min under conditions of 30 DEG C, 16000r/min, then the ultrasonication at 35 DEG C 30min, the ultrasonic power of the ultrasonic treatment is 400W, supersonic frequency 28kHz, obtains suspension, stands at 35 DEG C 12h is finally centrifuged 10min under the conditions of 20 DEG C, 12000r/min, filters processing gained supernatant, obtains product, produced with gained The ethanol washing that 1.5 times of amount of substance, be placed at 100 DEG C after dry 50min to get.
The preparation method of the modified boron nitride: by the mass ratio of 100:6:1.5:3, by boron nitride, fluorographite, fluorination Yttrium, titanium carbide mixing, are placed in 30 DEG C, carry out ball milling under conditions of 800r/min, using the zirconia ball of diameter 10mm as ball Grinding media, the ratio of grinding media to material is 2:1, after ball milling 6h, obtains mixture A；Then aluminium nitride, polyethylene are added into mixture A Butyral, hexagonal boron nitride, tributyl phosphate, dehydrated alcohol, acrylic resin, the mixture A, aluminium nitride, polyethylene Butyral, hexagonal boron nitride, tributyl phosphate, dehydrated alcohol, acrylic resin mass ratio be 100:4:4:1:2:100: 2, it maintains ball milling condition constant, after continuing ball milling 4h, obtains mixture B；Mixture B is placed at 40 DEG C dry 12h, is then existed Gas flow is 0.001m3Under the nitrogen protection of/h, 1850 DEG C are warming up to, after keeping the temperature 12h at 1850 DEG C, is cooled to 1400 DEG C, 10h is kept the temperature at 1400 DEG C, is then cooled to 400 DEG C, and wherein heating rate and rate of temperature fall are all 10 DEG C/min, finally 30 DEG C are cooled to, modified boron nitride is obtained.
Embodiment 7
Substantially the same manner as Example 1, difference is only in that: the heating film the preparation method comprises the following steps:
I, is by graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, modified boron nitride, N, N- diformazan Butylmethacrylamide mixing is placed in 30 DEG C, carries out ball milling 30min under conditions of 800r/min, using the oxidation of diameter 10mm For zirconium ball as ball-milling medium, the ratio of grinding media to material is 2:1, is subsequently added into polyamide rouge, maintains ball milling condition constant, continues ball milling 1.5h obtains heating film slurry；
Heating film slurry is evenly coated on glass fabric by II, by coating machine, and the coating thickness is 20 μm, then It is placed at 45 DEG C after drying for 24 hours, obtains naked mould, routinely technique is arranged after conductive bar, insulating layer on naked film to obtain the final product.
The graphene, carbon black, aluminium oxide, titanium dioxide, organically-modified aluminium nitride, modified boron nitride, N, N- diformazan Butylmethacrylamide, polyamide rouge mass ratio be 15:7:5:5:5:5:25:25.
The graphene the preparation method comprises the following steps: press 0.1:20 mass ratio, by 4,4'- benzidine, acetone mix, It is ultrasonically treated 10min at 35 DEG C, the ultrasonic power of the ultrasonic treatment is 400W, supersonic frequency 28kHz, obtains mixed liquor； Graphite is first placed in microwave bulking 10min under the microwave power of 400W, after being cooled to 20 DEG C, is then placed in the microwave power of 400W Lower extruding 10min, obtains the graphite of expanding treatment after being cooled to 20 DEG C；The graphite of the expanding treatment of mixed liquor quality 1% is added Enter into above-mentioned mixed liquor, is first homogenized 50min under conditions of 30 DEG C, 16000r/min, then the ultrasonication at 35 DEG C 30min, the ultrasonic power of the ultrasonic treatment is 400W, supersonic frequency 28kHz, obtains suspension；Dispersion is subsequently added into help Agent, the dispersing aid, suspension mass ratio be 0.3:100,35min is ultrasonically treated at 75 DEG C, the ultrasonic treatment Ultrasonic power is 400W, supersonic frequency 28kHz, and 12h is stood at 35 DEG C, finally under the conditions of 20 DEG C, 12000r/min from Heart 10min filters processing gained supernatant, obtains product, with 1.5 times of ethanol washing of products therefrom quality, be placed at 100 DEG C After dry 50min to get.
The dispersing aid is mixed by polyvinylpyrrolidone, polyvinyl alcohol, oleic acid by the mass ratio of 1:1:2.
The preparation method of the modified boron nitride: by the mass ratio of 100:6:1.5:3, by boron nitride, fluorographite, fluorination Yttrium, titanium carbide mixing, are placed in 30 DEG C, carry out ball milling under conditions of 800r/min, using the zirconia ball of diameter 10mm as ball Grinding media, the ratio of grinding media to material is 2:1, after ball milling 6h, obtains mixture A；Then aluminium nitride, polyethylene are added into mixture A Butyral, hexagonal boron nitride, tributyl phosphate, dehydrated alcohol, acrylic resin, the mixture A, aluminium nitride, polyethylene Butyral, hexagonal boron nitride, tributyl phosphate, dehydrated alcohol, acrylic resin mass ratio be 100:4:4:1:2:100: 2, it maintains ball milling condition constant, after continuing ball milling 4h, obtains mixture B；Mixture B is placed at 40 DEG C dry 12h, is then existed Gas flow is 0.001m3Under the nitrogen protection of/h, 1850 DEG C are warming up to, after keeping the temperature 12h at 1850 DEG C, is cooled to 1400 DEG C, 10h is kept the temperature at 1400 DEG C, is then cooled to 400 DEG C, and wherein heating rate and rate of temperature fall are all 10 DEG C/min, finally 30 DEG C are cooled to, modified boron nitride is obtained.
Comparative example 1
Substantially the same manner as Example 1, difference is only in that: the heating film the preparation method comprises the following steps:
I, is by graphene, carbon black, aluminium oxide, titanium dioxide, N, the mixing of N- dimethylmethacryl amide, be placed in 30 DEG C, Ball milling 30min is carried out under conditions of 800r/min, using the zirconia ball of diameter 10mm as ball-milling medium, the ratio of grinding media to material is 2:1 is subsequently added into polyamide rouge, maintains ball milling condition constant, continues ball milling 1.5h, obtains heating film slurry；
Heating film slurry is evenly coated on glass fabric by II, by coating machine, and the coating thickness is 20 μm, then It is placed at 45 DEG C after drying for 24 hours, obtains naked mould, routinely technique is arranged after conductive bar, insulating layer on naked film to obtain the final product.
The graphene, carbon black, aluminium oxide, titanium dioxide, N, the quality of N- dimethylmethacryl amide, polyamide rouge Than for 15:7:5:5:25:25.
Test case 1
Heating conduction test: material is saved referring to periodical literature " preparation and research of the high thermal conductivity graphene film " 1.3.2 of Xu Bin The test method of the heating conduction of material is measured the heating conduction of heating film in safety and environmental protection electric heating ceramic tile of the present invention, tool Body test result is shown in Table 1.
Table 1: heating conduction test result table
Group Thermal conductivity/(Wm-1·K-1)
Embodiment 1 573.8
Embodiment 2 496.1
Embodiment 3 486.8
Embodiment 4 662.8
Embodiment 5 687.7
Embodiment 6 730.1
Embodiment 7 788.5
Comparative example 1 421.4
By test result it is found that in 1 heating film of embodiment Thermal conductive additives by organically-modified aluminium nitride, boron nitride mixing and At heating conduction is better than embodiment 2-3 (Thermal conductive additives are mixed by organically-modified aluminium nitride, any two kinds of boron nitride) The comparative example 1 of Thermal conductive additives is not used；And embodiment 4 is modified boron nitride, heating conduction is better than embodiment 1.
Test case 2
Tensile strength test: referring to the periodical literature of Zheng Kai, " the compound film preparation of carbon fiber/graphite alkene and its tensile property are ground Study carefully " in 1.4 sections test method, using universal testing machine (model QT-1136, purchased from the high safe detecting instrument of Dongguan City Co., Ltd) tensile strength of heating film in safety and environmental protection electric heating ceramic tile of the present invention is measured, the rate of extension is 500mm/min, each sample are tested 3 times, are averaged, compare each group test result, obtain P < by statistical analysis method 0.05, show that sample average difference has statistical significance.In addition basement membrane glass fibers have been subtracted when this measuring and calculation tensile strength The tensile strength of cloth is tieed up, specific test result is shown in Table 2.
Table 2: heating conduction test result table
Group Tensile strength/MPa
Embodiment 1 32.5
Embodiment 2 30.1
Embodiment 3 31.4
Embodiment 4 34.5
Embodiment 5 39.7
Embodiment 6 44.5
Embodiment 7 48.9
By test result it is found that graphene uses modifying agent, dispersing aid in embodiment 7, at microwave treatment, ultrasound The processing methods such as reason are prepared, and better than embodiment 1-4, (graphene is prepared into tensile strength using strong acid, strong oxidizer To).
The above described is only a preferred embodiment of the present invention, limitation in any form not is done to the present invention, therefore The equivalent or simple change that all principles described according to the invention patent design are done, is included in the scope of protection of the patent of the present invention It is interior；Those skilled in the art can make various modifications or additions to the described embodiments Or be substituted in a similar manner, without departing from structure of the invention or beyond the scope defined by this claim, It is within the scope of protection of the invention.

Claims (9)

1. a kind of safety and environmental protection electric heating ceramic tile, which is characterized in that including ceramic tile, heating layer, insulating layer；The ceramic tile back side is downward It is followed successively by the heating layer and the insulating layer；The heating layer is connect by adhesive with the ceramic tile, the insulating layer；Institute Stating heating layer is heating film or heating blanket；
The heating film the preparation method comprises the following steps:
I, mixes graphene, carbon black, stabilizer, Thermal conductive additives, dimethylformamide, after ball milling 30-60min, is subsequently added into poly- Amide rouge, continues ball milling, obtains heating film slurry；
Heating film slurry is evenly coated on glass fabric by II, by coating machine, dry, obtains naked mould, routinely technique exists It is arranged after conductive bar, insulating layer on naked film to obtain the final product；
The graphene, carbon black, stabilizer, Thermal conductive additives, dimethylformamide, polyamide rouge mass ratio be (10-20): (5- 8): (5-15): (5-15): (15-30): (15-30)；
The stabilizer includes one of aluminium oxide, titanium dioxide, silver powder or a variety of.
2. safety and environmental protection electric heating ceramic tile as described in claim 1, which is characterized in that the Thermal conductive additives include organically-modified nitrogen Change one of aluminium, boron nitride, modified boron nitride or a variety of.
3. safety and environmental protection electric heating ceramic tile as claimed in claim 2, which is characterized in that the preparation side of the organically-modified aluminium nitride Method: by the mass ratio of 100:(2-4), aluminium nitride, 3- (methacryloxypropyl) propyl trimethoxy silicane is mixed, mixed Material, is subsequently added into the dehydrated alcohol of mixture quality 20-40%, and ball milling obtains organically-modified after washed, drying process Aluminium nitride.
4. safety and environmental protection electric heating ceramic tile as claimed in claim 2, which is characterized in that the preparation method of the modified boron nitride: press 100:(6-8): (1.5-2): the mass ratio of (2-5) mixes boron nitride, fluorographite, yttrium fluoride, titanium carbide, and ball milling obtains Mixture A；Then aluminium nitride, polyvinyl butyral, hexagonal boron nitride, tributyl phosphate, anhydrous second are added into mixture A Alcohol, acrylic resin, the mixture A, aluminium nitride, polyvinyl butyral, hexagonal boron nitride, tributyl phosphate, anhydrous second Alcohol, acrylic resin mass ratio be 100:(4-8): (4-8): (0.5-1.5): (2-6): (70-140): (1.5-3), ball milling, Obtain mixture B；Mixture B is placed at 40 DEG C dry 10-20h and is warming up to 1800-1900 then under gas nitrogen protection DEG C, after keeping the temperature 8-16h at 1800-1900 DEG C, it is cooled to 1300-1400 DEG C, 8-16h is kept the temperature at 1300-1400 DEG C, then It is cooled to 400-500 DEG C, is cooled to 25-35 DEG C, obtains modified boron nitride.
5. safety and environmental protection electric heating ceramic tile as described in claim 1, which is characterized in that the graphene the preparation method comprises the following steps: by stone Ink, the concentrated sulfuric acid, concentrated nitric acid press 1:(60-80): the mass ratio mixing of (15-30) is placed at 0-4 DEG C and stirs 20-50min, then 5-8 times of graphite quality of potassium permanganate is added, is placed at 30-35 DEG C after stirring 1-3h, obtains mixture；It is subsequently added into mixture 0.5-1.5 times of quality of water stirs 20-50min at 85-100 DEG C, is eventually adding 0.1-0.4 times of mixture quality of peroxide Change hydrogen solution, 10-30min stirred at 80-90 DEG C, filter, after washed, dry, ball-milling treatment to get.
6. safety and environmental protection electric heating ceramic tile as described in claim 1, which is characterized in that the graphene the preparation method comprises the following steps: pressing (0.05-0.15): modifying agent, solvent are mixed, are ultrasonically treated 20-50min, obtain mixed liquor by 20 mass ratio；By mixed liquor The graphite of quality 0.5-2.5% is added in above-mentioned mixed liquor, is homogenized 20-50min under the revolving speed of 16000-28000r/min, Then ultrasonication 20-50min obtains suspension, stands, centrifugation, processing gained supernatant is filtered, after washed, dry To obtain the final product.
7. safety and environmental protection electric heating ceramic tile as described in claim 1, which is characterized in that the graphene the preparation method comprises the following steps: pressing (0.05-0.15): modifying agent, solvent are mixed, are ultrasonically treated 20-50min, obtain mixed liquor by 20 mass ratio；Graphite is set The microwave bulking 5-15min under the microwave power of 200-400W is cooled to the 20-35 DEG C of microwave function for being followed by placed in 200-400W Microwave bulking 5-15min under rate, it is cooling, obtain the graphite of expanding treatment；By the expanding treatment of mixed liquor quality 0.5-2.5% Graphite is added in above-mentioned mixed liquor, 20-50min is homogenized under the revolving speed of 16000-28000r/min, then ultrasonication 20-50min obtains suspension, standing, centrifugation, filters processing gained supernatant, after washed, drying to obtain the final product.
8. safety and environmental protection electric heating ceramic tile as described in claim 1, which is characterized in that the graphene the preparation method comprises the following steps: pressing (0.05-0.15): modifying agent, solvent are mixed, are ultrasonically treated 20-50min, obtain mixed liquor by 20 mass ratio；Graphite is set The microwave bulking 5-15min under the microwave power of 200-400W is cooled to the 20-35 DEG C of microwave function for being followed by placed in 200-400W Microwave bulking 5-15min under rate, it is cooling, obtain the graphite of expanding treatment；By the expanding treatment of mixed liquor quality 0.5-2.5% Graphite is added in above-mentioned mixed liquor, 20-50min is homogenized under the revolving speed of 16000-28000r/min, then ultrasonication 20-50min obtains suspension；Be subsequently added into dispersing aid, the dispersing aid, suspension mass ratio be (0.3-0.6): 100, it is ultrasonically treated 20-50min, standing, centrifugation filters processing gained supernatant, after washed, drying to obtain the final product；
The dispersing aid presses (1-2) by polyvinylpyrrolidone, polyvinyl alcohol, oleic acid: (1-2): the mass ratio of (2-4) mixes It forms.
9. the safety and environmental protection electric heating ceramic tile as described in any one of claim 6-8, which is characterized in that the modifying agent includes 4, 4'- benzidine, 4'- hydroxyazobenzene -2- carboxylic acid, 3,3', one of 5,5'- bibenzene tetracarboxylic or a variety of.
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CN111844394A (en) * 2019-10-31 2020-10-30 佛山裕德天智科技合伙企业(有限合伙) Heating ceramic tile and preparation method thereof
CN111851921A (en) * 2019-10-31 2020-10-30 广东源稀新材料科技有限公司 Heating ceramic tile and preparation method thereof
CN111004038A (en) * 2020-01-02 2020-04-14 杭州诺贝尔陶瓷有限公司 Ultra-large specification thin porcelain plate with electric heating function and production method thereof
CN111004039A (en) * 2020-01-02 2020-04-14 杭州诺贝尔陶瓷有限公司 Ultra-large thin porcelain plate with electric heating function and manufacturing method thereof
CN111004039B (en) * 2020-01-02 2022-04-15 杭州诺贝尔陶瓷有限公司 Ultra-large thin porcelain plate with electric heating function and manufacturing method thereof
CN111004038B (en) * 2020-01-02 2022-05-03 杭州诺贝尔陶瓷有限公司 Super-large-specification thin porcelain plate with electrothermal function and production method thereof
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CN115838275B (en) * 2022-11-14 2023-12-19 佛山市东鹏陶瓷有限公司 Production system of heating rock plate
CN117229686A (en) * 2023-11-13 2023-12-15 福建宏华集团有限公司 Anti-slip wear-resistant glazed paint for ceramic tiles and preparation method and application thereof
CN117229686B (en) * 2023-11-13 2024-02-23 福建宏华集团有限公司 Anti-slip wear-resistant glazed paint for ceramic tiles and preparation method and application thereof

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