CN106183239A - A kind of macromolecule complex electrocaloric film and preparation method thereof - Google Patents

A kind of macromolecule complex electrocaloric film and preparation method thereof Download PDF

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CN106183239A
CN106183239A CN201610570968.7A CN201610570968A CN106183239A CN 106183239 A CN106183239 A CN 106183239A CN 201610570968 A CN201610570968 A CN 201610570968A CN 106183239 A CN106183239 A CN 106183239A
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polyurethane resin
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film
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CN106183239B (en
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刘子寒
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Jiangsu Connie Textile Co Ltd
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    • 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
    • B32B5/22—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
    • B32B5/26—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 also being fibrous or filamentary
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4205—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups
    • C08G18/4208—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/06—Polyurethanes from polyesters
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
    • 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
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/02—Composition of the impregnated, bonded or embedded layer
    • B32B2260/021—Fibrous or filamentary layer
    • B32B2260/023—Two or more layers
    • 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
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/04—Impregnation, embedding, or binder material
    • B32B2260/046—Synthetic resin
    • 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
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

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Abstract

A kind of macromolecule complex electrocaloric film, it includes carbon nano tube polyurethane resin heating film and electrode, it is characterised in that: carbon nano tube polyurethane resin heating film is formed through hot pressing by thermosetting polyurethane resin conductive heating layer and polyurethane resin insulating barrier.Higher than the thermostability of existing thermoplastic polyurethane Electric radiant Heating Film and intensity, all without softening in the range of 160 degree, intensity does not reduces, meet halogen-free flame-proof environmental protection requirement, reaching UL 94V 0 grade, application safety performance is high, improves heating efficiency and reaches 10%, improve the heat transfer efficiency 20 30% of Electric radiant Heating Film, heat up rapidly.

Description

A kind of macromolecule complex electrocaloric film and preparation method thereof
Technical field
The invention belongs to thermo electric material manufacturing technology field, be specifically related to a kind of macromolecule complex electrocaloric film and preparation side thereof Method.
Background technology
The heating principle of Heating System of Electric radiant Heating Film is to convert electrical energy into heat energy, and with the outside radiant heat of infrared ray form Amount, makes human body and object thermally equivalent.With traditional air-conditioning, heating installation etc. by forced convertion circulating air heat compared with, electric heating Film heating system have healthiness, save space, energy-efficient, Heat stability is good, operating cost are low, length in service life and peace The advantages such as good perfection, Heating System of Electric radiant Heating Film meets the demand for development of following energy-conserving and environment-protective as Novel heating technology.
According to electrothermal film heater material type, carbon back ink, carbon fiber, metal and polymer electric heating membrane four kinds can be divided into Type.Compared with other heating materials, macromolecular material kind is many, performance is adjustable, processing forming is good, ageing-resistant, be prone to Other materials carries out the advantage such as being combined.Conductive material is combined with macromolecular material, thus it is possible to vary tradition thermo electric material knot Structure and the drawback such as function singleness, the most aging, heating power decay.CNT has electricity and the mechanical characteristic of excellence, and Can be radiation infrared, in recent years as thermo electric material for Electric radiant Heating Film.Chinese patent notification number CN104918341A, bulletin Day be JIUYUE in 2015 16, entitled " CNT is applied to the method in floor heating Electric radiant Heating Film " discloses with polyurethane with The heating material that the conducting medium of CNT composition is provided with the polyester mesh shape matrix of tin plating copper foil wire for dipping and obtains Material, but come with some shortcomings: the TPU material of employing, thermostability is the highest, thus easily softens when being heated, intensity Low；Without effective flame-retardant composition in conducting medium, safety in utilization is low；The PE used outside exothermic material and pet layer are as protection Non-binding effect between insulating barrier, and heater, Electric radiant Heating Film can not form integration, and inconvenience is installed, and during work, safety is low；PE It is polymeric material with pet layer protection insulating barrier, not there is fire retardation, and heat transfer efficiency is low.
Summary of the invention
For the problem of above-mentioned existence, it is an object of the invention to provide a kind of macromolecule complex electrocaloric film and preparation method thereof, This macromolecule complex electrocaloric film has thermostability height, thermal efficiency height, quick heating, exothermic material have well with insulation protection interlayer Cementation, and macromolecule complex electrocaloric film meets UL 94V-0 grade non-halogen flame-retardant effect, thus improves security reliability.
The present invention is to be achieved through the following technical solutions:
A kind of macromolecule complex electrocaloric film, it includes carbon nano tube polyurethane resin heating film, insulating barrier and electrode, and its feature exists In: carbon nano tube polyurethane resin heating film by thermosetting polyurethane resin conductive heating layer and polyurethane resin insulating barrier through heat Pressure forms,
Material composition in the glass-fiber-fabric base material of described polyurethane resin conductive heating layer is: aromatic polyester polyol 100 Part, CNT 50 ~ 100 parts, fire retardant 40 ~ 80 parts, silane coupler 1 ~ 5 part, plasticizer 5 ~ 20 parts, catalyst 0.5 ~ 2 part and solvent 200 ~ 300 parts, methyl diphenylene diisocyanate 65 ~ 85 parts；
Material composition in the glass-fiber-fabric base material of described polyurethane resin insulating barrier is: aromatic polyester polyol 100 parts, super Thin 20 ~ 50 parts of heat conductive insulating powder, fire retardant 40 ~ 80 parts, silane coupler 1 ~ 5 part, plasticizer 5 ~ 20 parts, catalyst 0.5 ~ 2 part and solvent 200 ~ 300 parts, methyl diphenylene diisocyanate 65 ~ 85 parts.
The preparation method of above-mentioned macromolecule complex electrocaloric film, it is characterised in that comprise the following steps:
1) preparation of polyurethane resin conducting resinl: weigh by weight aromatic polyester polyol 100 parts, CNT 50 ~ 100 parts, fire retardant 40 ~ 80 parts, silane coupler 1 ~ 5 part, plasticizer 5 ~ 20 parts, catalyst 0.5 ~ 2 part and solvent 200 ~ 300 parts, after being placed in grinding distribution machine dispersion grinding, stand 1 hour, then based on aromatic polyester polyol 100 parts, Add methyl diphenylene diisocyanate 65 ~ 85 parts, stir, obtain polyurethane resin conducting resinl；
2) preparation of heating film: inweave a copper foil wire, the poly-ammonia then obtained by step 1) in glass-fiber-fabric base material both sides respectively After ester resin conductive glue is sufficiently impregnated with glass fibre cloth base material, it is placed in the baking oven of 60 ~ 70 DEG C, solidifies 4 ~ 8h, obtain heat Curable polyurethane resin heating film；
3) preparation of polyurethane resin insulating cement: weigh aromatic polyester polyol 100 parts, ultra-fine heat conductive insulating by weight 20 ~ 50 parts of powder, fire retardant 40 ~ 80 parts, silane coupler 1 ~ 5 part, plasticizer 5 ~ 20 parts, catalyst 0.5 ~ 2 part And solvent 200 ~ 300 parts, after being placed in grinding distribution machine dispersion grinding, stand 1 hour, then press aromatic polyester polyol 100 parts of meters, add methyl diphenylene diisocyanate 65 ~ 85 parts, stir, obtain polyurethane resin insulating cement；
4) preparation of precuring insulating trip: after being sufficiently impregnated with glass-fiber-fabric with the polyurethane resin insulating cement of step 3) preparation, be placed in In the baking oven of 50 ~ 60 DEG C, precuring 2 ~ 4h, obtain precuring insulating trip 2；
5) preparation of macromolecule complex electrocaloric film: by step 2) prepare heating film be clipped in step 4) prepare two-layer pre-solid Change in the middle of insulating trip, temperature be 60 ~ 70 DEG C, pressure be 10 ~ 30kgf/cm2, under the conditions of hardening time is 2 ~ 4h, warp Hot pressing obtains Electric radiant Heating Film base material, connects through wire and i.e. obtains macromolecule complex electrocaloric film after insulation processing.
The hydroxyl value of the aromatic polyester polyol in above-mentioned step 1) and step 3) is 200 ~ 450mgKOH/g, acid number ≤ 2.0mgKOH/g, viscosity when 25 DEG C is 200 ~ 4000mPas.
The above-mentioned CNT in step 1) is SWCN or multi-walled carbon nano-tubes, wherein SWCN A diameter of 0.6 ~ 2nm, a diameter of 2 ~ 100nm of multi-walled carbon nano-tubes.
Fire retardant in above-mentioned step 1) and step 3) is in magnesium hydroxide, aluminium hydroxide, APP, tripolycyanamide One or both.
Silane coupler in above-mentioned step 1) and step 3) is KH-550, KH-560, KH-570, A-151, A-171 In one.
Plasticizer in above-mentioned step 1) and step 3) is dipropylene glycol dibenzoate or adipic acid two (butoxy second Epoxide second) one in ester.
Catalyst in above-mentioned step 1) and step 3) be stannous octoate, dibutyl tin laurate, stannous oxalate, two One in acetic acid dibutyl tin.
Ultra-fine heat conductive insulating powder in above-mentioned step 3) is the one in aluminium nitride, boron nitride, aluminium oxide, and particle diameter is less than 1.5μm。
Solvent in above-mentioned step 1) and step 3) is the one in ethyl acetate, acetone, butanone, toluene, dimethylbenzene.
Above technical scheme preparation-obtained macromolecule complex electrocaloric film is used to have the advantage that
(1) use aromatic polyester polyol and heat-resist methyl diphenylene diisocyanate monomer by cross-linking reaction system Standby heat-curable urethane, and further enhance with thermostability and anti-flammability glass-fiber-fabric, thus the macromolecule prepared is combined Electric radiant Heating Film is higher than the thermostability of existing thermoplastic polyurethane Electric radiant Heating Film and intensity, all without softening in the range of 160 degree, by force Degree does not reduces.
(2) in conductive polyurethane glue and insulating cement, all with the addition of halogen-free flame retardants, the macromolecule compound electric prepared Hotting mask meets halogen-free flame-proof environmental protection requirement, reaches UL 94V-0 level, and application safety performance is high.
(3) in thermo electric material, have employed coupling agent, improve CNT dispersibility in polyurethane, and enhance Interaction between CNT and polyurethane, improves heating efficiency and reaches 10%, and it is more uniform to generate heat.
(4) insulating barrier introduces heat conductive insulating powder, improve the heat transfer efficiency 20-30% of Electric radiant Heating Film, heat up rapidly, use peace Quan Xinggao.
(5) macromolecule complex electrocaloric film is in preparation process, and Electric radiant Heating Film fully solidifies, and uses semi-solid preparation dielectric film, through group Hot pressing after conjunction, solidification, both maintained the integrity of heating layer structure, improve again the adhesion strength of insulating barrier and electric membranous layer, Heating layer is formed integrated with insulating protective layer.
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is further described.
Embodiment 1
1) preparation of polyurethane resin conducting resinl: weighing aromatic polyester polyol 500g(hydroxyl value by weight is 200mgKOH/ G, acid number is 1.0mgKOH/g, and viscosity is 4000mPas), 2nm SWCN 500g, magnesium hydroxide 200g, aluminium hydroxide 200g, KH-550 25g, dipropylene glycol dibenzoate 100g, stannous octoate 10g and ethyl acetate 1.5kg, be placed in grinding point Dissipate after machine disperseing grind, stand 1 hour, add methyl diphenylene diisocyanate 325g, stir, obtain polyurethane tree Fat conducting resinl；
2) preparation of heating film: inweave a copper foil wire, the poly-ammonia then obtained by step 1) in glass-fiber-fabric base material both sides respectively After ester resin conductive glue is sufficiently impregnated with glass fibre cloth base material, it is placed in the baking oven of 60 DEG C, solidifies 8h, obtain heat-curable urethane Resin heating film；
3) preparation of polyurethane resin insulating cement: weighing aromatic polyester polyol 1kg(hydroxyl value by weight is 200mgKOH/ G, acid number is 1.0mgKOH/g, and viscosity is 4000mPas), aluminium nitride 500g, magnesium hydroxide 400g, aluminium hydroxide 400g, KH- 560 50g, dipropylene glycol dibenzoate 200g, stannous octoate 20g and ethyl acetate 3kg, be placed in grinding distribution machine dispersion After grinding, stand 1 hour, add methyl diphenylene diisocyanate 650g, stir, obtain polyurethane resin insulating cement；
4) preparation of precuring insulating trip: after being sufficiently impregnated with glass-fiber-fabric with the polyurethane resin insulating cement of step 3) preparation, be placed in In the baking oven of 50 DEG C, precuring 4h, obtain precuring insulating trip 2；
5) preparation of macromolecule complex electrocaloric film: by step 2) prepare heating film be clipped in step 4) prepare two precuring In the middle of insulating trip, temperature be 70 DEG C, pressure be 10 kgf/cm2, under the conditions of hardening time is 2h, obtain Electric radiant Heating Film through hot pressing Base material, connects through wire and i.e. obtains macromolecule complex electrocaloric film after insulation processing.
Embodiment 2
1) preparation of polyurethane resin conducting resinl: weighing aromatic polyester polyol 500g(hydroxyl value by weight is 300mgKOH/ G, acid number is 2.0mgKOH/g, and viscosity is 2000mPas), the multi-walled carbon nano-tubes 400g of a diameter of 2nm, tripolycyanamide 300g, KH-560 15g, adipic acid two (Butoxyethoxy second) ester 50g, dibutyl tin laurate 5g and acetone 1.25kg, be placed in After dispersion is ground in grinding distribution machine, stand 1 hour, add methyl diphenylene diisocyanate 360g, stir, gathered Urethane resin conductive glue；
2) preparation of heating film: inweave a copper foil wire, the poly-ammonia then obtained by step 1) in glass-fiber-fabric base material both sides respectively After ester resin conductive glue is sufficiently impregnated with glass fibre cloth base material, it is placed in the baking oven of 65 DEG C, solidifies 6h, obtain heat-curable urethane Resin heating film；
3) preparation of polyurethane resin insulating cement: weighing aromatic polyester polyol 1kg(hydroxyl value by weight is 300mgKOH/ G, acid number is 2.0mgKOH/g, and viscosity is 2000mPas), boron nitride 400g, tripolycyanamide 600g, KH-560 30g, adipic acid Two (Butoxyethoxy second) ester 100g, dibutyl tin laurate 10g and acetone 2.5kg, be placed in grinding distribution machine dispersion After grinding, stand 1 hour, add methyl diphenylene diisocyanate 720g, stir, obtain polyurethane resin insulating cement；
4) preparation of precuring insulating trip: after being sufficiently impregnated with glass-fiber-fabric with the polyurethane resin insulating cement of step 3) preparation, be placed in In the baking oven of 55 DEG C, precuring 3h, obtain precuring insulating trip 2；
5) preparation of macromolecule complex electrocaloric film: by step 2) prepare heating film be clipped in step 4) prepare two precuring In the middle of insulating trip, temperature be 60 DEG C, pressure be 30 kgf/cm2, under the conditions of hardening time is 4h, obtain Electric radiant Heating Film through hot pressing Base material, connects through wire and i.e. obtains macromolecule complex electrocaloric film after insulation processing.
Embodiment 3
1) preparation of polyurethane resin conducting resinl: weighing aromatic polyester polyol 500g(hydroxyl value by weight is 450mgKOH/ G, acid number is 0.5mgKOH/g, and viscosity is 200mPas), the SWCN 350g of a diameter of 0.6nm, APP 250g, KH-570 5g, dipropylene glycol dibenzoate 25g, stannous oxalate 2.5g and butanone 1.0kg, be placed in grinding distribution machine dispersion After grinding, stand 1 hour, add methyl diphenylene diisocyanate 425g, stir, obtain polyurethane resin conducting resinl；
2) preparation of heating film: inweave a copper foil wire, the poly-ammonia then obtained by step 1) in glass-fiber-fabric base material both sides respectively After ester resin conductive glue is sufficiently impregnated with glass fibre cloth base material, it is placed in the baking oven of 70 DEG C, solidifies 4h, obtain heat-curable urethane Resin heating film；
3) preparation of polyurethane resin insulating cement: weighing aromatic polyester polyol 1.0kg(hydroxyl value by weight is 450mgKOH/g, acid number is 0.5mgKOH/g, and viscosity is 200mPas), aluminium oxide 300g, APP 500g, KH-570 10g, dipropylene glycol dibenzoate 50g, stannous oxalate 5g and butanone 2.0kg, after being placed in grinding distribution machine dispersion grinding, quiet Put 1 hour, add methyl diphenylene diisocyanate 850g, stir, obtain polyurethane resin insulating cement；
4) preparation of precuring insulating trip: after being sufficiently impregnated with glass-fiber-fabric with the polyurethane resin insulating cement of step 3) preparation, be placed in In the baking oven of 60 DEG C, precuring 2h, obtain precuring insulating trip；
5) preparation of macromolecule complex electrocaloric film: by step 2) prepare heating film and step 4) in prepare two precuring exhausted Embolium combines, temperature be 65 DEG C, pressure be 20 kgf/cm2, under the conditions of hardening time is 3h, obtain Electric radiant Heating Film base through hot pressing Material, connects through wire and i.e. obtains macromolecule complex electrocaloric film after insulation processing.
Embodiment 4
1) preparation of polyurethane resin conducting resinl: weighing aromatic polyester polyol 500g(hydroxyl value by weight is 400mgKOH/ G, acid number is 0.8mgKOH/g, and viscosity is 450mPas), the multi-walled carbon nano-tubes 300g of a diameter of 50nm, aluminium hydroxide 175g, APP 100g, A-151 20g, adipic acid two (Butoxyethoxy second) ester 75g, dibutyltin diacetate 7.5g and toluene 1.4kg, after being placed in grinding distribution machine dispersion grinding, stands 1 hour, adds methyl diphenylene diisocyanate 375g, stirring Uniformly, polyurethane resin conducting resinl is obtained；
2) preparation of heating film: inweave a copper foil wire, the poly-ammonia then obtained by step 1) in glass-fiber-fabric base material both sides respectively After ester resin conductive glue is sufficiently impregnated with glass fibre cloth base material, it is placed in the baking oven of 60 DEG C, solidifies 7h, obtain heat-curable urethane Resin heating film；
3) preparation of polyurethane resin insulating cement: weighing aromatic polyester polyol 1.0kg(hydroxyl value by weight is 400mgKOH/g, acid number is 0.8mgKOH/g, and viscosity is 450mPas), boron nitride 450g, aluminium hydroxide 350g, APP 200g, A-151 40g, adipic acid two (Butoxyethoxy second) ester 150g, dibutyltin diacetate 15g and toluene 2.8kg, put After dispersion is ground in grinding distribution machine, stand 1 hour, add methyl diphenylene diisocyanate 750g, stir, obtain Polyurethane resin insulating cement；
4) preparation of precuring insulating trip: after being sufficiently impregnated with glass-fiber-fabric with the polyurethane resin insulating cement of step 3) preparation, be placed in In the baking oven of 50 DEG C, precuring 4h, obtain precuring insulating trip 2；
5) preparation of macromolecule complex electrocaloric film: by step 2) prepare heating film and step 4) in prepare two precuring exhausted Embolium combines, temperature be 60 DEG C, pressure be 25 kgf/cm2, under the conditions of hardening time is 4h, obtain Electric radiant Heating Film base through hot pressing Material, connects through wire and i.e. obtains macromolecule complex electrocaloric film after insulation processing.
Embodiment 5
1) preparation of polyurethane resin conducting resinl: weighing aromatic polyester polyol 500g(hydroxyl value by weight is 360mgKOH/ G, acid number is 1.0mgKOH/g, and viscosity is 1200mPas), the multi-walled carbon nano-tubes 450g of a diameter of 100nm, magnesium hydroxide 125, Tripolycyanamide 200g, A-171 10g, dipropylene glycol dibenzoate 60g, stannous oxalate 4g and dimethylbenzene 1.3kg, be placed in grinding After dispersion is ground in dispersion machine, stand 1 hour, add methyl diphenylene diisocyanate 365g, stir, obtain polyurethane Resin conductive glue；
2) preparation of heating film: inweave a copper foil wire, the poly-ammonia then obtained by step 1) in glass-fiber-fabric base material both sides respectively After ester resin conductive glue is sufficiently impregnated with glass fibre cloth base material, it is placed in the baking oven of 70 DEG C, solidifies 5h, obtain heat-curable urethane Resin heating film；
3) preparation of polyurethane resin insulating cement: weighing aromatic polyester polyol 1.0kg(hydroxyl value by weight is 360mgKOH/g, acid number is 1.5mgKOH/g, and viscosity is 3000mPas), aluminium oxide 250g, magnesium hydroxide 250, tripolycyanamide 400g, A-171 20g, dipropylene glycol dibenzoate 120g, stannous oxalate 8g and dimethylbenzene 2.6kg, be placed in grinding distribution machine After middle dispersion is ground, stand 1 hour, add methyl diphenylene diisocyanate 730g, stir, obtain polyurethane resin exhausted Edge glue；
4) preparation of precuring insulating trip: after being sufficiently impregnated with glass-fiber-fabric with the polyurethane resin insulating cement of step 3) preparation, be placed in In the baking oven of 55 DEG C, precuring 3h, obtain precuring insulating trip 2；
5) preparation of macromolecule complex electrocaloric film: by step 2) prepare heating film and step 4) in prepare two precuring exhausted Embolium combines, temperature be 65 DEG C, pressure be 30 kgf/cm2, under the conditions of hardening time is 3h, obtain Electric radiant Heating Film base through hot pressing Material, connects through wire and i.e. obtains macromolecule complex electrocaloric film after insulation processing.
Embodiment 6
1) preparation of polyurethane resin conducting resinl: weighing aromatic polyester polyol 500g(hydroxyl value by weight is 250mgKOH/ G, acid number is 1.5mgKOH/g, and viscosity is 3000mPas), the SWCN 425g of a diameter of 1nm, aluminium hydroxide 350g, KH-570 22.5g, adipic acid two (Butoxyethoxy second) ester 90g, stannous octoate 8g and ethyl acetate 1.1kg, be placed in grinding After dispersion is ground in dispersion machine, stand 1 hour, add methyl diphenylene diisocyanate 340g, stir, obtain polyurethane Resin conductive glue；
2) preparation of heating film: inweave a copper foil wire, the poly-ammonia then obtained by step 1) in glass-fiber-fabric base material both sides respectively After ester resin conductive glue is sufficiently impregnated with glass fibre cloth base material, it is placed in the baking oven of 65 DEG C, solidifies 5h, obtain heat-curable urethane Resin heating film；
3) preparation of polyurethane resin insulating cement: weighing aromatic polyester polyol 1.0kg(hydroxyl value by weight is 250mgKOH/g, acid number is 1.5mgKOH/g, and viscosity is 3000mPas), aluminium nitride 200g, aluminium hydroxide 700g, KH-570 45g, adipic acid two (Butoxyethoxy second) ester 180g, stannous octoate 16g and ethyl acetate 2.2kg, be placed in grinding distribution machine After middle dispersion is ground, stand 1 hour, add methyl diphenylene diisocyanate 1.5kg, stir, obtain polyurethane resin Insulating cement；
4) preparation of precuring insulating trip: after being sufficiently impregnated with glass-fiber-fabric with the polyurethane resin insulating cement of step 3) preparation, be placed in In the baking oven of 60 DEG C, precuring 3h, obtain precuring insulating trip 2；
5) preparation of macromolecule complex electrocaloric film: by step 2) prepare heating film and step 4) in prepare two precuring exhausted Embolium combines, temperature be 70 DEG C, pressure be 20 kgf/cm2, under the conditions of hardening time is 3h, obtain Electric radiant Heating Film base through hot pressing Material, connects through wire and i.e. obtains macromolecule complex electrocaloric film after insulation processing.
Embodiment 7
1) preparation of polyurethane resin conducting resinl: weighing aromatic polyester polyol 500g(hydroxyl value by weight is 280mgKOH/ G, acid number is 1.0mgKOH/g, and viscosity is 2000mPas), the multi-walled carbon nano-tubes 250g of a diameter of 20nm, APP 225g, A-151 12.5g, dipropylene glycol dibenzoate 40g, dibutyl tin laurate 6g and acetone 1.2kg, be placed in grinding distribution After dispersion is ground in machine, stand 1 hour, add methyl diphenylene diisocyanate 350g, stir, obtain polyurethane resin Conducting resinl；
2) preparation of heating film: inweave a copper foil wire, the poly-ammonia then obtained by step 1) in glass-fiber-fabric base material both sides respectively After ester resin conductive glue is sufficiently impregnated with glass fibre cloth base material, it is placed in the baking oven of 60 DEG C, solidifies 7h, obtain heat-curable urethane Resin heating film；
3) preparation of polyurethane resin insulating cement: weighing aromatic polyester polyol 1.0kg(hydroxyl value by weight is 280mgKOH/g, acid number is 1.0mgKOH/g, and viscosity is 2000mPas), aluminium oxide 350g, APP 450g, A-151 25g, dipropylene glycol dibenzoate 80g, dibutyl tin laurate 12g and acetone 2.4kg, be placed in grinding distribution machine dispersion After grinding, stand 1 hour, add methyl diphenylene diisocyanate 730g, stir, obtain polyurethane resin insulating cement；
4) preparation of precuring insulating trip: after being sufficiently impregnated with glass-fiber-fabric with the polyurethane resin insulating cement of step 3) preparation, be placed in In the baking oven of 50 DEG C, precuring 3h, obtain precuring insulating trip 2；
5) preparation of macromolecule complex electrocaloric film: by step 2) prepare heating film and step 4) in prepare two precuring exhausted Embolium combines, temperature be 60 DEG C, pressure be 15 kgf/cm2, under the conditions of hardening time is 4h, obtain Electric radiant Heating Film base through hot pressing Material, connects through wire and i.e. obtains macromolecule complex electrocaloric film after insulation processing.
Embodiment 8
1) preparation of polyurethane resin conducting resinl: weighing aromatic polyester polyol 500g(hydroxyl value by weight is 420mgKOH/ G, acid number is 1.5mgKOH/g, and viscosity is 600mPas), the SWCN 275g of a diameter of 1.5nm, APP 225g, Tripolycyanamide 150g, KH-550 17.5g, adipic acid two (Butoxyethoxy second) ester 95g, dibutyltin diacetate 9g and first Benzene 1.45kg, after being placed in grinding distribution machine dispersion grinding, stands 1 hour, adds methyl diphenylene diisocyanate 400g, stir Mix uniformly, obtain polyurethane resin conducting resinl；
2) preparation of heating film: inweave a copper foil wire, the poly-ammonia then obtained by step 1) in glass-fiber-fabric base material both sides respectively After ester resin conductive glue is sufficiently impregnated with glass fibre cloth base material, it is placed in the baking oven of 70 DEG C, solidifies 6h, obtain heat-curable urethane Resin heating film；
3) preparation of polyurethane resin insulating cement: weighing aromatic polyester polyol 1.0kg(hydroxyl value by weight is 420mgKOH/g, acid number is 1.5mgKOH/g, and viscosity is 600mPas), aluminium nitride 480g, APP 450g, tripolycyanamide 300g, KH-550 35g, adipic acid two (Butoxyethoxy second) ester 190g, dibutyltin diacetate 18g and toluene 2.9kg, After being placed in grinding distribution machine dispersion grinding, stand 1 hour, add methyl diphenylene diisocyanate 800kg, stir, Obtain polyurethane resin insulating cement；
4) preparation of precuring insulating trip: after being sufficiently impregnated with glass-fiber-fabric with the polyurethane resin insulating cement of step 3) preparation, be placed in In the baking oven of 55 DEG C, precuring 3h, obtain precuring insulating trip 2；
5) preparation of macromolecule complex electrocaloric film: by step 2) prepare heating film and step 4) in prepare two precuring exhausted Embolium combines, temperature be 65 DEG C, pressure be 25 kgf/cm2, under the conditions of hardening time is 2h, obtain Electric radiant Heating Film base through hot pressing Material, connects through wire and i.e. obtains macromolecule complex electrocaloric film after insulation processing.
Comparative example 1
Compared with Example 1, step 3) is added without heat conductive insulating powder aluminium nitride, prepares macromolecule by each step and be combined Electric radiant Heating Film.
Comparative example 2
Compared with Example 7, in the preparation of step 1) polyurethane resin conducting resinl, it is not added with silane coupling A-151, is gathered Urethane resin conductive glue, then by step 2) prepare thermosetting polyurethane resin heating film.
Compared with comparative example 1, the step 3) of embodiment 1 adds heat conductive insulating powder aluminium nitride, thus at insulating barrier In be filled with the aluminium nitride with good heat conductive effect, the heat transfer efficiency of the macromolecule complex electrocaloric film prepared compares contrast Example 1 improves 25%.Compared with comparative example 2, in the step 1) in embodiment 7, adding silane coupling A-151, preparation is poly- Urethane resin conductive glue, then by step 2) prepare thermosetting polyurethane resin heating film, owing to CNT is inorganic material Material, easily reunites, and with the poor compatibility of polyurethane high-molecular organic material.CNT is after coupling agent A-151 processes, poly- Dispersibility in urethane is more preferable, forms more intact conductive path, improves the thermal efficiency, compared with comparative example 2, and embodiment 7 step Rapid 2) thermal efficiency of the heating film prepared in improves 10%.

Claims (2)

1. a macromolecule complex electrocaloric film, it includes carbon nano tube polyurethane resin heating film, insulating barrier and electrode, its feature It is: carbon nano tube polyurethane resin heating film is by thermosetting polyurethane resin conductive heating layer and polyurethane resin insulating barrier warp Hot pressing forms,
Material composition in the glass-fiber-fabric base material of described thermosetting polyurethane resin conductive heating layer is: aromatic polyester is polynary Alcohol 100 parts, CNT 50 ~ 100 parts, fire retardant 40 ~ 80 parts, silane coupler 1 ~ 5 part, plasticizer 5 ~ 20 parts, Catalyst 0.5 ~ 2 part and solvent 200 ~ 300 parts, methyl diphenylene diisocyanate 65 ~ 85 parts；
Material composition in the glass-fiber-fabric base material of described polyurethane resin insulating barrier is: aromatic polyester polyol 100 parts, super Thin 20 ~ 50 parts of heat conductive insulating powder, fire retardant 40 ~ 80 parts, silane coupler 1 ~ 5 part, plasticizer 5 ~ 20 parts, catalyst 0.5 ~ 2 part and solvent 200 ~ 300 parts, methyl diphenylene diisocyanate 65 ~ 85 parts.
2. the preparation method of macromolecule complex electrocaloric film, it is characterised in that comprise the following steps:
1) preparation of polyurethane resin conducting resinl: weigh by weight aromatic polyester polyol 100 parts, CNT 50 ~ 100 parts, fire retardant 40 ~ 80 parts, silane coupler 1 ~ 5 part, plasticizer 5 ~ 20 parts, catalyst 0.5 ~ 2 part and solvent 200 ~ 300 parts, after being placed in grinding distribution machine dispersion grinding, stand 1 hour, then based on aromatic polyester polyol 100 parts, Add methyl diphenylene diisocyanate 65 ~ 85 parts, stir, obtain polyurethane resin conducting resinl；
2) preparation of heating film: inweave a copper foil wire, the poly-ammonia then obtained by step 1) in glass-fiber-fabric base material both sides respectively After ester resin conductive glue is sufficiently impregnated with glass fibre cloth base material, it is placed in the baking oven of 60 ~ 70 DEG C, solidifies 4 ~ 8h, obtain heat Curable polyurethane resin heating film；
3) preparation of polyurethane resin insulating cement: weigh aromatic polyester polyol 100 parts, ultra-fine heat conductive insulating by weight 20 ~ 50 parts of powder, fire retardant 40 ~ 80 parts, silane coupler 1 ~ 5 part, plasticizer 5 ~ 20 parts, catalyst 0.5 ~ 2 part And solvent 200 ~ 300 parts, after being placed in grinding distribution machine dispersion grinding, stand 1 hour, then press aromatic polyester polyol 100 parts of meters, add methyl diphenylene diisocyanate 65 ~ 85 parts, stir, obtain polyurethane resin insulating cement；
4) preparation of precuring insulating trip: after being sufficiently impregnated with glass-fiber-fabric with the polyurethane resin insulating cement of step 3) preparation, be placed in In the baking oven of 50 ~ 60 DEG C, precuring 2 ~ 4h, obtain precuring insulating trip；
5) preparation of macromolecule complex electrocaloric film: by step 2) prepare heating film and step 4) in prepare two precuring Insulating trip combines, temperature be 60 ~ 70 DEG C, pressure be 10 ~ 30kgf/cm2, under the conditions of hardening time is 2 ~ 4h, through heat Pressure obtains Electric radiant Heating Film base material, connects through wire and i.e. obtains macromolecule complex electrocaloric film after insulation processing.
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CN109575463A (en) * 2018-12-10 2019-04-05 李佳峻 A kind of preparation method of mobile phone screen protector
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CN107241819A (en) * 2017-06-20 2017-10-10 武汉纺织大学 A kind of preparation method of halogen-free flameproof flexible macromolecule complex electrocaloric film
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CN108966380A (en) * 2018-08-20 2018-12-07 深圳市同益高新电子科技有限公司 A kind of novel heating film
CN109575463A (en) * 2018-12-10 2019-04-05 李佳峻 A kind of preparation method of mobile phone screen protector
CN109679061B (en) * 2018-12-24 2021-08-06 山东一诺威聚氨酯股份有限公司 Thermoplastic polyurethane elastomer for flexible electrothermal film and preparation method thereof
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CN111109811A (en) * 2020-01-03 2020-05-08 侯美英 Novel electric hair drier and temperature control method
CN113999515A (en) * 2021-12-10 2022-02-01 南京经略复合材料有限公司 Glass fiber reinforced polyurethane material, supporting beam and preparation process of supporting beam
CN114889253A (en) * 2022-07-14 2022-08-12 广东简一(集团)陶瓷有限公司 Conductive thermosetting film, anti-leakage current heating plate and manufacturing process thereof
CN114889253B (en) * 2022-07-14 2022-12-06 广东简一(集团)陶瓷有限公司 Conductive thermosetting film, anti-leakage current heating plate and manufacturing process thereof

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