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CN106183239B - 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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CN106183239B
CN106183239B CN201610570968.7A CN201610570968A CN106183239B CN 106183239 B CN106183239 B CN 106183239B CN 201610570968 A CN201610570968 A CN 201610570968A CN 106183239 B CN106183239 B CN 106183239B
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polyurethane resin
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heating film
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CN106183239A (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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  • Health & Medical Sciences (AREA)
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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 by thermosetting polyurethane resin conductive heating layer and polyurethane resin insulating layer through hot pressing.It is higher than the heat resistance and intensity of existing thermoplastic polyurethane Electric radiant Heating Film, will not all it soften in the range of 160 degree, intensity does not reduce, meet halogen-free flame-proof environmental protection requirement, reach 0 grade of UL 94V, application security can be high, improves heating efficiency up to 10%, the heat transfer efficiency 20 30% of Electric radiant Heating Film is improved, heating is rapid.

Description

A kind of macromolecule complex electrocaloric film and preparation method thereof
Technical field
The invention belongs to thermo electric material manufacturing technology fields, and in particular to a kind of macromolecule complex electrocaloric film and its preparation side Method.
Background technology
The heating principle of Heating System of Electric radiant Heating Film is to convert electrical energy into thermal energy, and the outside radiant heat in the form of infrared ray Amount, makes human body and object thermally equivalent.Compared with traditional air-conditioning, heating etc. are heated by forced convertion circulating air, electric heating Film heating system is with healthiness, saving space, energy-efficient, thermal stability is good, operating cost is low, service life is long and peace The advantages that good perfection, Heating System of Electric radiant Heating Film meet following energy-saving and environment-friendly demand for development as novel heating technology.
According to electrothermal film heater material type, four kinds of carbon-based ink, carbon fiber, metal and polymer electric heating membrane can be divided into Type.Compared with other heating materials, high molecular material type is more, performance is adjustable, processing forming is good, it is ageing-resistant, be easy to Other materials carries out the advantages that compound.It is conductive material and high molecular material progress is compound, thus it is possible to vary traditional thermo electric material knot The drawbacks such as structure and single, easy to aging, the heating power attenuation of function.Carbon nanotube has excellent electricity and mechanical characteristic, and Can be radiation infrared, in recent years Electric radiant Heating Film is used for as thermo electric material.Chinese patent notification number CN104918341A, bulletin Day be September in 2015 16, disclosed in entitled " carbon nanotube is applied to the method in floor heating Electric radiant Heating Film " with polyurethane with The conducting medium of carbon nanotube composition is equipped with heating material obtained from the polyester mesh shape matrix of tin plating copper foil wire for impregnating Material, but come with some shortcomings：The thermoplastic polyurethane resin material of use, heat resistance is not high, thus it is heated when easily soften, intensity It is low；Without effective flame-retardant composition in conducting medium, safety in utilization is low；The PE used outside exothermic material is with pet layer as protection Non-binding acts between insulating layer, with heater, and Electric radiant Heating Film cannot form integration, inconvenience installation, and safety is low during work；PE It is polymer material with pet layer protection insulating layer, without fire retardation, and heat transfer efficiency is low.
Invention content
In view of the above problems, it is an object of the invention to provide a kind of macromolecule complex electrocaloric film and preparation method thereof, There is this macromolecule complex electrocaloric film heat resistance height, thermal efficiency height, quick heating, exothermic material and insulation protection interlayer to have well Cementation, and macromolecule complex electrocaloric film meets UL 94V-0 grade non-halogen flame-retardant effects, so as to improve 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 layer and electrode, special Sign is：Carbon nano tube polyurethane resin heating film is by thermosetting polyurethane resin conductive heating layer and polyurethane resin insulating layer It is formed through hot pressing,
Material composition in the glass-fiber-fabric base material of the polyurethane resin conductive heating layer is：Aromatic polyester polyol 100 parts, 50 ~ 100 parts of carbon nanotube, 40 ~ 80 parts of fire retardant, 1 ~ 5 part of silane coupling agent, 5 ~ 20 parts of plasticizer, urge 200 ~ 300 parts of 0.5 ~ 2 part of agent and solvent, 65 ~ 85 parts of methyl diphenylene diisocyanate；
Material composition in the glass-fiber-fabric base material of the polyurethane resin insulating layer is：Aromatic polyester polyol 100 Part, 20 ~ 50 parts of ultra-fine heat conductive insulating powder, 40 ~ 80 parts of fire retardant, 1 ~ 5 part of silane coupling agent, 5 ~ 20 parts of plasticizer, 200 ~ 300 parts of 0.5 ~ 2 part of catalyst and solvent, 65 ~ 85 parts of methyl diphenylene diisocyanate.
The preparation method of above-mentioned macromolecule complex electrocaloric film, it is characterised in that include the following steps：
1）The preparation of polyurethane resin conducting resinl：100 parts of aromatic polyester polyol, carbon nanotube are weighed by weight 50 ~ 100 parts, 40 ~ 80 parts of fire retardant, 1 ~ 5 part of silane coupling agent, 5 ~ 20 parts of plasticizer, 0.5 ~ 2 part of catalyst and 200 ~ 300 parts of solvent is placed in grinding distribution machine after dispersion grinding, stands 1 hour, then by aromatic polyester polyol 100 Part meter, adds in 65 ~ 85 parts of methyl diphenylene diisocyanate, stirs evenly, obtain polyurethane resin conducting resinl；
2）The preparation of heating film：It is woven into a copper foil wire respectively in glass-fiber-fabric base material both sides, then with step 1）It obtains It after polyurethane resin conducting resinl is sufficiently impregnated glass fibre cloth base material, is placed in 60 ~ 70 DEG C of baking oven, cures 4 ~ 8h, obtain To thermosetting polyurethane resin heating film；
3）The preparation of polyurethane resin insulating cement：100 parts of aromatic polyester polyol, ultra-fine heat conduction are weighed by weight 20 ~ 50 parts of insulating powder, 40 ~ 80 parts of fire retardant, 1 ~ 5 part of silane coupling agent, 5 ~ 20 parts of plasticizer, catalyst 0.5 ~ 2 parts and 200 ~ 300 parts of solvent are placed in grinding distribution machine after dispersion grinding, stand 1 hour, then polynary by aromatic polyester 100 parts of meters of alcohol, add in 65 ~ 85 parts of methyl diphenylene diisocyanate, stir evenly, obtain polyurethane resin insulating cement；
4）The preparation of precuring insulating trip：With step 3）After the polyurethane resin insulating cement of preparation is sufficiently impregnated glass-fiber-fabric, It is placed in 50 ~ 60 DEG C of baking oven, 2 ~ 4h of precuring, obtains precuring insulating trip 2；
5）The preparation of macromolecule complex electrocaloric film：By step 2）Heating film obtained is clipped in step 4）In two layers obtained Among precuring insulating trip, temperature is 60 ~ 70 DEG C, pressure is 10 ~ 30kgf/cm2, hardening time be 2 ~ 4h conditions Under, electric heating film base material is obtained through hot pressing, macromolecule complex electrocaloric film is obtained after conducting wire connection and insulation processing.
Above-mentioned step 1）And step 3）In aromatic polyester polyol hydroxyl value for 200 ~ 450mgKOH/g, acid value ≤ 2.0mgKOH/g, viscosity at 25 DEG C are 200 ~ 4000mPas.
Above-mentioned step 1）In carbon nanotube for single-walled carbon nanotube or multi-walled carbon nanotube, wherein single-walled carbon nanotube A diameter of 0.6 ~ 2nm, a diameter of 2 ~ 100nm of multi-walled carbon nanotube.
Above-mentioned step 1）And step 3）In fire retardant be magnesium hydroxide, aluminium hydroxide, ammonium polyphosphate, in melamine One or two.
Above-mentioned step 1）And step 3）In silane coupling agent be KH-550, KH-560, KH-570, A-151, A-171 In one kind.
Above-mentioned step 1）And step 3）In plasticizer be dipropylene glycol dibenzoate or adipic acid two（Butoxy second Oxygroup second）One kind in ester.
Above-mentioned step 1）And step 3）In catalyst for stannous octoate, dibutyl tin laurate, stannous oxalate, two One kind in acetic acid dibutyl tin.
Above-mentioned step 3）In ultra-fine heat conductive insulating powder be aluminium nitride, boron nitride, one kind in aluminium oxide, grain size is less than 1.5μm。
Above-mentioned step 1）And step 3）In solvent be ethyl acetate, acetone, butanone, toluene, one kind in dimethylbenzene.
It is had the following advantages using the preparation-obtained macromolecule complex electrocaloric film of above technical scheme：
（1）It is anti-by being crosslinked using aromatic polyester polyol and heat-resist methyl diphenylene diisocyanate monomer Heat-curable urethane should be prepared, and is further enhanced with heat resistance and anti-flammability glass-fiber-fabric, thus the macromolecule being prepared Complex electrocaloric film is higher than the heat resistance and intensity of existing thermoplastic polyurethane Electric radiant Heating Film, all will not be soft in the range of 160 degree Change, intensity does not reduce.
（2）Halogen-free flame retardants is added in conductive polyurethane glue and insulating cement, the macromolecule compound electric being prepared Hotting mask meets halogen-free flame-proof environmental protection requirement, reaches 94V-0 grades of UL, and application security can be high.
（3）Coupling agent is employed in thermo electric material, improves dispersibility of the carbon nanotube in polyurethane, and enhance Interaction between carbon nanotube and polyurethane improves heating efficiency up to 10%, and it is more uniform to generate heat.
（4）Heat conductive insulating powder is introduced in insulating layer, improves the heat transfer efficiency 20-30% of Electric radiant Heating Film, heating is rapid, uses peace Quan Xinggao.
（5）In preparation process, Electric radiant Heating Film fully cures macromolecule complex electrocaloric film, using semi-solid preparation insulating film, through group Hot pressing, curing, had not only maintained the integrality of heating layer structure, but also improve the adhesion strength of insulating layer and electric membranous layer after conjunction, So that heating layer formed with insulating protective layer it is integrated.
Specific embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is further described.
Embodiment 1
1）The preparation of polyurethane resin conducting resinl：Aromatic polyester polyol 500g is weighed by weight（Hydroxyl value is 200mgKOH/g, acid value 1.0mgKOH/g, viscosity 4000mPas）, 2nm single-walled carbon nanotubes 500g, magnesium hydroxide 200g, Aluminium hydroxide 200g, KH-550 25g, dipropylene glycol dibenzoate 100g, stannous octoate 10g and ethyl acetate 1.5kg, put In grinding distribution machine after dispersion grinding, 1 hour is stood, methyl diphenylene diisocyanate 325g is added in, stirs evenly, obtain Polyurethane resin conducting resinl；
2）The preparation of heating film：It is woven into a copper foil wire respectively in glass-fiber-fabric base material both sides, then with step 1）It obtains It after polyurethane resin conducting resinl is sufficiently impregnated glass fibre cloth base material, is placed in 60 DEG C of baking oven, cures 8h, obtain thermosetting property and gather Urethane resin heating film；
3）The preparation of polyurethane resin insulating cement：Aromatic polyester polyol 1kg is weighed by weight（Hydroxyl value is 200mgKOH/g, acid value 1.0mgKOH/g, viscosity 4000mPas）, aluminium nitride 500g, magnesium hydroxide 400g, aluminium hydroxide 400g, KH-560 50g, dipropylene glycol dibenzoate 200g, stannous octoate 20g and ethyl acetate 3kg, are placed in grinding distribution In machine after dispersion grinding, 1 hour is stood, methyl diphenylene diisocyanate 650g is added in, stirs evenly, obtain polyurethane resin Insulating cement；
4）The preparation of precuring insulating trip：With step 3）After the polyurethane resin insulating cement of preparation is sufficiently impregnated glass-fiber-fabric, It is placed in 50 DEG C of baking oven, precuring 4h, obtains precuring insulating trip 2；
5）The preparation of macromolecule complex electrocaloric film：By step 2）Heating film obtained is clipped in step 4）In two obtained it is pre- Cure among insulating trip, temperature is 70 DEG C, pressure is 10 kgf/cm2, hardening time is under the conditions of 2h, electricity obtains through hot pressing Hotting mask base material obtains macromolecule complex electrocaloric film after conducting wire connection and insulation processing.
Embodiment 2
1）The preparation of polyurethane resin conducting resinl：Aromatic polyester polyol 500g is weighed by weight（Hydroxyl value is 300mgKOH/g, acid value 2.0mgKOH/g, viscosity 2000mPas）, a diameter of 2nm multi-walled carbon nanotube 400g, trimerization Cyanamide 300g, KH-560 15g, adipic acid two（Butoxyethoxy second）Ester 50g, dibutyl tin laurate 5g and acetone 1.25kg is placed in grinding distribution machine after dispersion grinding, stands 1 hour, adds in methyl diphenylene diisocyanate 360g, stirring Uniformly, polyurethane resin conducting resinl is obtained；
2）The preparation of heating film：It is woven into a copper foil wire respectively in glass-fiber-fabric base material both sides, then with step 1）It obtains It after polyurethane resin conducting resinl is sufficiently impregnated glass fibre cloth base material, is placed in 65 DEG C of baking oven, cures 6h, obtain thermosetting property and gather Urethane resin heating film；
3）The preparation of polyurethane resin insulating cement：Aromatic polyester polyol 1kg is weighed by weight（Hydroxyl value is 300mgKOH/g, acid value 2.0mgKOH/g, viscosity 2000mPas）, boron nitride 400g, melamine 600g, KH-560 30g, adipic acid two（Butoxyethoxy second）Ester 100g, dibutyl tin laurate 10g and acetone 2.5kg are placed in grinding point It dissipates in machine after dispersion grinding, standing 1 hour adds in methyl diphenylene diisocyanate 720g, stirs evenly, obtain polyurethane tree Fat insulating cement；
4）The preparation of precuring insulating trip：With step 3）After the polyurethane resin insulating cement of preparation is sufficiently impregnated glass-fiber-fabric, It is placed in 55 DEG C of baking oven, precuring 3h, obtains precuring insulating trip 2；
5）The preparation of macromolecule complex electrocaloric film：By step 2）Heating film obtained is clipped in step 4）In two obtained it is pre- Cure among insulating trip, temperature is 60 DEG C, pressure is 30 kgf/cm2, hardening time is under the conditions of 4h, electricity obtains through hot pressing Hotting mask base material obtains macromolecule complex electrocaloric film after conducting wire connection and insulation processing.
Embodiment 3
1）The preparation of polyurethane resin conducting resinl：Aromatic polyester polyol 500g is weighed by weight（Hydroxyl value is 450mgKOH/g, acid value 0.5mgKOH/g, viscosity 200mPas）, a diameter of 0.6nm single-walled carbon nanotube 350g, poly- phosphorus Sour ammonium 250g, KH-570 5g, dipropylene glycol dibenzoate 25g, stannous oxalate 2.5g and butanone 1.0kg, are placed in grinding distribution In machine after dispersion grinding, 1 hour is stood, methyl diphenylene diisocyanate 425g is added in, stirs evenly, obtain polyurethane resin Conducting resinl；
2）The preparation of heating film：It is woven into a copper foil wire respectively in glass-fiber-fabric base material both sides, then with step 1）It obtains It after polyurethane resin conducting resinl is sufficiently impregnated glass fibre cloth base material, is placed in 70 DEG C of baking oven, cures 4h, obtain thermosetting property and gather Urethane resin heating film；
3）The preparation of polyurethane resin insulating cement：Aromatic polyester polyol 1.0kg is weighed by weight（Hydroxyl value is 450mgKOH/g, acid value 0.5mgKOH/g, viscosity 200mPas）, aluminium oxide 300g, ammonium polyphosphate 500g, KH-570 10g, dipropylene glycol dibenzoate 50g, stannous oxalate 5g and butanone 2.0kg are placed in grinding distribution machine after dispersion grinding, quiet It puts 1 hour, adds in methyl diphenylene diisocyanate 850g, stir evenly, obtain polyurethane resin insulating cement；
4）The preparation of precuring insulating trip：With step 3）After the polyurethane resin insulating cement of preparation is sufficiently impregnated glass-fiber-fabric, It is placed in 60 DEG C of baking oven, precuring 2h, obtains precuring insulating trip；
5）The preparation of macromolecule complex electrocaloric film：By step 2）Heating film obtained and step 4）In two obtained it is pre- solid Change insulating trip combination, temperature is 65 DEG C, pressure is 20 kgf/cm2, hardening time is under the conditions of 3h, electric heating obtains through hot pressing Film base material obtains macromolecule complex electrocaloric film after conducting wire connection and insulation processing.
Embodiment 4
1）The preparation of polyurethane resin conducting resinl：Aromatic polyester polyol 500g is weighed by weight（Hydroxyl value is 400mgKOH/g, acid value 0.8mgKOH/g, viscosity 450mPas）, a diameter of 50nm multi-walled carbon nanotube 300g, hydrogen-oxygen Change aluminium 175g, ammonium polyphosphate 100g, A-151 20g, adipic acid two（Butoxyethoxy second）Ester 75g, dibutyltin diacetate 7.5g and toluene 1.4kg is placed in grinding distribution machine after dispersion grinding, stands 1 hour, add in methyl diphenylene diisocyanate 375g is stirred evenly, and obtains polyurethane resin conducting resinl；
2）The preparation of heating film：It is woven into a copper foil wire respectively in glass-fiber-fabric base material both sides, then with step 1）It obtains It after polyurethane resin conducting resinl is sufficiently impregnated glass fibre cloth base material, is placed in 60 DEG C of baking oven, cures 7h, obtain thermosetting property and gather Urethane resin heating film；
3）The preparation of polyurethane resin insulating cement：Aromatic polyester polyol 1.0kg is weighed by weight（Hydroxyl value is 400mgKOH/g, acid value 0.8mgKOH/g, viscosity 450mPas）, boron nitride 450g, aluminium hydroxide 350g, ammonium polyphosphate 200g, A-151 40g, adipic acid two（Butoxyethoxy second）Ester 150g, dibutyltin diacetate 15g and toluene 2.8kg, put In grinding distribution machine after dispersion grinding, 1 hour is stood, methyl diphenylene diisocyanate 750g is added in, stirs evenly, obtain Polyurethane resin insulating cement；
4）The preparation of precuring insulating trip：With step 3）After the polyurethane resin insulating cement of preparation is sufficiently impregnated glass-fiber-fabric, It is placed in 50 DEG C of baking oven, precuring 4h, obtains precuring insulating trip 2；
5）The preparation of macromolecule complex electrocaloric film：By step 2）Heating film obtained and step 4）In two obtained it is pre- solid Change insulating trip combination, temperature is 60 DEG C, pressure is 25 kgf/cm2, hardening time is under the conditions of 4h, electric heating obtains through hot pressing Film base material obtains macromolecule complex electrocaloric film after conducting wire connection and insulation processing.
Embodiment 5
1）The preparation of polyurethane resin conducting resinl：Aromatic polyester polyol 500g is weighed by weight（Hydroxyl value is 360mgKOH/g, acid value 1.0mgKOH/g, viscosity 1200mPas）, a diameter of 100nm multi-walled carbon nanotube 450g, hydrogen Magnesia 125, melamine 200g, A-171 10g, dipropylene glycol dibenzoate 60g, stannous oxalate 4g and dimethylbenzene 1.3kg is placed in grinding distribution machine after dispersion grinding, stands 1 hour, adds in methyl diphenylene diisocyanate 365g, stirring Uniformly, polyurethane resin conducting resinl is obtained；
2）The preparation of heating film：It is woven into a copper foil wire respectively in glass-fiber-fabric base material both sides, then with step 1）It obtains It after polyurethane resin conducting resinl is sufficiently impregnated glass fibre cloth base material, is placed in 70 DEG C of baking oven, cures 5h, obtain thermosetting property and gather Urethane resin heating film；
3）The preparation of polyurethane resin insulating cement：Aromatic polyester polyol 1.0kg is weighed by weight（Hydroxyl value is 360mgKOH/g, acid value 1.5mgKOH/g, viscosity 3000mPas）, aluminium oxide 250g, magnesium hydroxide 250, melamine 400g, A-171 20g, dipropylene glycol dibenzoate 120g, stannous oxalate 8g and dimethylbenzene 2.6kg, are placed in grinding distribution machine After middle dispersion grinding, 1 hour is stood, methyl diphenylene diisocyanate 730g is added in, stirs evenly, it is exhausted to obtain polyurethane resin Edge glue；
4）The preparation of precuring insulating trip：With step 3）After the polyurethane resin insulating cement of preparation is sufficiently impregnated glass-fiber-fabric, It is placed in 55 DEG C of baking oven, precuring 3h, obtains precuring insulating trip 2；
5）The preparation of macromolecule complex electrocaloric film：By step 2）Heating film obtained and step 4）In two obtained it is pre- solid Change insulating trip combination, temperature is 65 DEG C, pressure is 30 kgf/cm2, hardening time is under the conditions of 3h, electric heating obtains through hot pressing Film base material obtains macromolecule complex electrocaloric film after conducting wire connection and insulation processing.
Embodiment 6
1）The preparation of polyurethane resin conducting resinl：Aromatic polyester polyol 500g is weighed by weight（Hydroxyl value is 250mgKOH/g, acid value 1.5mgKOH/g, viscosity 3000mPas）, a diameter of 1nm single-walled carbon nanotube 425g, hydrogen-oxygen Change aluminium 350g, KH-570 22.5g, adipic acid two（Butoxyethoxy second）Ester 90g, stannous octoate 8g and ethyl acetate 1.1kg is placed in grinding distribution machine after dispersion grinding, stands 1 hour, adds in methyl diphenylene diisocyanate 340g, stirring Uniformly, polyurethane resin conducting resinl is obtained；
2）The preparation of heating film：It is woven into a copper foil wire respectively in glass-fiber-fabric base material both sides, then with step 1）It obtains It after polyurethane resin conducting resinl is sufficiently impregnated glass fibre cloth base material, is placed in 65 DEG C of baking oven, cures 5h, obtain thermosetting property and gather Urethane resin heating film；
3）The preparation of polyurethane resin insulating cement：Aromatic polyester polyol 1.0kg is weighed by weight（Hydroxyl value is 250mgKOH/g, acid value 1.5mgKOH/g, viscosity 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, are placed in grinding distribution machine After middle dispersion grinding, 1 hour is stood, methyl diphenylene diisocyanate 1.5kg is added in, stirs evenly, obtain polyurethane resin Insulating cement；
4）The preparation of precuring insulating trip：With step 3）After the polyurethane resin insulating cement of preparation is sufficiently impregnated glass-fiber-fabric, It is placed in 60 DEG C of baking oven, precuring 3h, obtains precuring insulating trip 2；
5）The preparation of macromolecule complex electrocaloric film：By step 2）Heating film obtained and step 4）In two obtained it is pre- solid Change insulating trip combination, temperature is 70 DEG C, pressure is 20 kgf/cm2, hardening time is under the conditions of 3h, electric heating obtains through hot pressing Film base material obtains macromolecule complex electrocaloric film after conducting wire connection and insulation processing.
Embodiment 7
1）The preparation of polyurethane resin conducting resinl：Aromatic polyester polyol 500g is weighed by weight（Hydroxyl value is 280mgKOH/g, acid value 1.0mgKOH/g, viscosity 2000mPas）, a diameter of 20nm multi-walled carbon nanotube 250g, poly- phosphorus Sour ammonium 225g, A-151 12.5g, dipropylene glycol dibenzoate 40g, dibutyl tin laurate 6g and acetone 1.2kg, are placed in In grinding distribution machine after dispersion grinding, 1 hour is stood, methyl diphenylene diisocyanate 350g is added in, stirs evenly, gathered Urethane resin conductive glue；
2）The preparation of heating film：It is woven into a copper foil wire respectively in glass-fiber-fabric base material both sides, then with step 1）It obtains It after polyurethane resin conducting resinl is sufficiently impregnated glass fibre cloth base material, is placed in 60 DEG C of baking oven, cures 7h, obtain thermosetting property and gather Urethane resin heating film；
3）The preparation of polyurethane resin insulating cement：Aromatic polyester polyol 1.0kg is weighed by weight（Hydroxyl value is 280mgKOH/g, acid value 1.0mgKOH/g, viscosity 2000mPas）, aluminium oxide 350g, ammonium polyphosphate 450g, A-151 25g, dipropylene glycol dibenzoate 80g, dibutyl tin laurate 12g and acetone 2.4kg, are placed in grinding distribution machine and disperse After grinding, 1 hour is stood, methyl diphenylene diisocyanate 730g is added in, stirs evenly, obtain polyurethane resin insulating cement；
4）The preparation of precuring insulating trip：With step 3）After the polyurethane resin insulating cement of preparation is sufficiently impregnated glass-fiber-fabric, It is placed in 50 DEG C of baking oven, precuring 3h, obtains precuring insulating trip 2；
5）The preparation of macromolecule complex electrocaloric film：By step 2）Heating film obtained and step 4）In two obtained it is pre- solid Change insulating trip combination, temperature is 60 DEG C, pressure is 15 kgf/cm2, hardening time is under the conditions of 4h, electric heating obtains through hot pressing Film base material obtains macromolecule complex electrocaloric film after conducting wire connection and insulation processing.
Embodiment 8
1）The preparation of polyurethane resin conducting resinl：Aromatic polyester polyol 500g is weighed by weight（Hydroxyl value is 420mgKOH/g, acid value 1.5mgKOH/g, viscosity 600mPas）, a diameter of 1.5nm single-walled carbon nanotube 275g, poly- phosphorus Sour ammonium 225g, melamine 150g, KH-550 17.5g, adipic acid two（Butoxyethoxy second）Ester 95g, two acetic acid dibutyl Tin 9g and toluene 1.45kg is placed in grinding distribution machine after dispersion grinding, stands 1 hour, add in diphenyl methyl diisocyanate Ester 400g, stirs evenly, and obtains polyurethane resin conducting resinl；
2）The preparation of heating film：It is woven into a copper foil wire respectively in glass-fiber-fabric base material both sides, then with step 1）It obtains It after polyurethane resin conducting resinl is sufficiently impregnated glass fibre cloth base material, is placed in 70 DEG C of baking oven, cures 6h, obtain thermosetting property and gather Urethane resin heating film；
3）The preparation of polyurethane resin insulating cement：Aromatic polyester polyol 1.0kg is weighed by weight（Hydroxyl value is 420mgKOH/g, acid value 1.5mgKOH/g, viscosity 600mPas）, aluminium nitride 480g, ammonium polyphosphate 450g, melamine 300g, KH-550 35g, adipic acid two（Butoxyethoxy second）Ester 190g, dibutyltin diacetate 18g and toluene 2.9kg, It is placed in grinding distribution machine after dispersion grinding, stands 1 hour, add in methyl diphenylene diisocyanate 800kg, stir evenly, Obtain polyurethane resin insulating cement；
4）The preparation of precuring insulating trip：With step 3）After the polyurethane resin insulating cement of preparation is sufficiently impregnated glass-fiber-fabric, It is placed in 55 DEG C of baking oven, precuring 3h, obtains precuring insulating trip 2；
5）The preparation of macromolecule complex electrocaloric film：By step 2）Heating film obtained and step 4）In two obtained it is pre- solid Change insulating trip combination, temperature is 65 DEG C, pressure is 25 kgf/cm2, hardening time is under the conditions of 2h, electric heating obtains through hot pressing Film base material obtains macromolecule complex electrocaloric film after conducting wire connection and insulation processing.
Comparative example 1
Compared with Example 1, in step 3）In be added without heat conductive insulating powder aluminium nitride, macromolecule is prepared by each step Complex electrocaloric film.
Comparative example 2
Compared with Example 7, in step 1）In the preparation of polyurethane resin conducting resinl, silane coupling A -151 are not added with, are obtained To polyurethane resin conducting resinl, then by step 2）Thermosetting polyurethane resin heating film is prepared.
Compared with comparative example 1, in the step 3 of embodiment 1）In add heat conductive insulating powder aluminium nitride, thus in insulating layer In be filled with the aluminium nitride with good heat conductive effect, the heat transfer efficiency of macromolecule complex electrocaloric film being prepared compared to comparison Example 1 improves 25%.Compared with comparative example 2, the step 1 in embodiment 7）In, silane coupling A -151 are added, are prepared poly- Urethane resin conductive glue, then by step 2）Thermosetting polyurethane resin heating film is prepared, since carbon nanotube is inorganic material Material, easily reunite, and with the poor compatibility of polyurethane high-molecular organic material.Carbon nanotube is after coupling agent A-151 processing, poly- Dispersibility in urethane is more preferable, forms more intact conductive path, improves the thermal efficiency, compared with comparative example 2,7 step of embodiment Rapid 2）In the thermal efficiency of heating film that is prepared improve 10%.

Claims (2)

1. a kind of macromolecule complex electrocaloric film, it includes carbon nano tube polyurethane resin heating film, insulating layer and electrode, feature It is：Carbon nano tube polyurethane resin heating film is passed through by thermosetting polyurethane resin conductive heating layer and polyurethane resin insulating layer Hot pressing forms,
Thermosetting polyurethane resin conductive exothermal in the glass-fiber-fabric base material of the thermosetting polyurethane resin conductive heating layer Layer material composition be：100 parts of aromatic polyester polyol, 50 ~ 100 parts of carbon nanotube, 40 ~ 80 parts of fire retardant, silane are even Join 200 ~ 300 parts of 1 ~ 5 part of agent, 5 ~ 20 parts of plasticizer, 0.5 ~ 2 part of catalyst and solvent, two isocyanide of diphenyl methyl 65 ~ 85 parts of acid esters；
Polyurethane resin insulating layer material composition in the glass-fiber-fabric base material of the polyurethane resin insulating layer is：Fragrant adoption 100 parts of ester polyol, 20 ~ 50 parts of ultra-fine heat conductive insulating powder, 40 ~ 80 parts of fire retardant, 1 ~ 5 part of silane coupling agent, plasticising 200 ~ 300 parts of 5 ~ 20 parts of agent, 0.5 ~ 2 part of catalyst and solvent, 65 ~ 85 parts of methyl diphenylene diisocyanate.
2. the preparation method of macromolecule complex electrocaloric film, it is characterised in that include the following steps：
1）The preparation of polyurethane resin conducting resinl：Weigh by weight 100 parts of aromatic polyester polyol, carbon nanotube 50 ~ 100 parts, 40 ~ 80 parts of fire retardant, 1 ~ 5 part of silane coupling agent, 5 ~ 20 parts of plasticizer, 0.5 ~ 2 part of catalyst and solvent It 200 ~ 300 parts, is placed in grinding distribution machine after dispersion grinding, stands 1 hour, then based on 100 parts of aromatic polyester polyol, 65 ~ 85 parts of methyl diphenylene diisocyanate is added in, stirs evenly, obtains polyurethane resin conducting resinl；
2）The preparation of heating film：It is woven into a copper foil wire respectively in glass-fiber-fabric base material both sides, then with step 1）Obtained poly- ammonia After ester resin conductive glue is sufficiently impregnated glass fibre cloth base material, it is placed in 60 ~ 70 DEG C of baking oven, cures 4 ~ 8h, obtain heat Curable polyurethane resin heating film；
3）The preparation of polyurethane resin insulating cement：100 parts of aromatic polyester polyol, ultra-fine heat conductive insulating powder are weighed by weight 20 ~ 50 parts, 40 ~ 80 parts of fire retardant, 1 ~ 5 part of silane coupling agent, 5 ~ 20 parts of plasticizer, 0.5 ~ 2 part of catalyst and 200 ~ 300 parts of solvent is placed in grinding distribution machine after dispersion grinding, stands 1 hour, then by aromatic polyester polyol 100 Part meter, adds in 65 ~ 85 parts of methyl diphenylene diisocyanate, stirs evenly, obtain polyurethane resin insulating cement；
4）The preparation of precuring insulating trip：With step 3）After the polyurethane resin insulating cement of preparation is sufficiently impregnated glass-fiber-fabric, it is placed in In 50 ~ 60 DEG C of baking oven, 2 ~ 4h of precuring, obtain precuring insulating trip；
5）The preparation of macromolecule complex electrocaloric film：By step 2）Heating film obtained and step 4）In two precuring obtained it is exhausted Embolium combines, temperature is 60 ~ 70 DEG C, pressure is 10 ~ 30kgf/cm2, hardening time under the conditions of 2 ~ 4h, through hot pressing Electric heating film base material is obtained, macromolecule complex electrocaloric film is obtained after conducting wire connection and insulation processing.
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