CN107383764A - A kind of compound low Heat Conduction Material and preparation method thereof - Google Patents
A kind of compound low Heat Conduction Material and preparation method thereof Download PDFInfo
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- C08L2312/00—Crosslinking
Abstract
The invention provides a kind of compound low Heat Conduction Material and preparation method thereof, cladding material, middle layer material and inner layer material are combined successively to obtain the compound low Heat Conduction Material presoma system, hot pressing obtains compound low Heat Conduction Material;Pass through resin matrix and the selection compatibility of small-molecule substance, with reference to rational preparation technology, the heat-insulation composite material for being molded preparation after preforming again possesses excellent heat resistance, fire resistance, there is good processing characteristics simultaneously, cladding material is provided with graphene, with N, N dimethyl lauryl amine and strontium titanates can improve the corrosion resistance of material together.
Description
Technical field
The invention belongs to compound low Heat Conduction Material technical field, and in particular to a kind of compound low Heat Conduction Material and its preparation side
Method.
Background technology
Compound low Heat Conduction Material has in fields such as metallurgy, non-ferrous metal, machinery, petrochemical industry, electric power to be extremely widely applied.
Compound low Heat Conduction Material has the characteristics such as density is small, pliability is high, waterproof, collectable waste heat, random good, no cavity,
Negative blast tear can be avoided and come off.Compound low Heat Conduction Material is generally divided into two kinds of inorganic and organic.Organic material advantage
It is raw material abundance, low, the easy for construction, technical maturity of product thermal conductivity factor etc., its major defect is that the resistance to heat problem of material is difficult to solve
Certainly;And inorganic non-ignitable compound low Heat Conduction Material, because thermal conductivity factor is higher, or low intensity, it can not meet that design uses mostly
It is required that.And existing compound low Heat Conduction Material decay resistance deficiency, its application in special is limited, limitation is special in turn
The development of kind industry.
The content of the invention
The invention provides a kind of compound low Heat Conduction Material and preparation method thereof, with epoxy combination cyanate, pass through resin
The selection compatibility of matrix and small-molecule substance, with reference to rational preparation technology, the heat-insulated composite wood of preparation is molded after preforming again
Material possesses excellent heat resistance, fire resistance, while has good processing characteristics.
To achieve the above object of the invention, the present invention adopts the following technical scheme that:
A kind of preparation method of compound low Heat Conduction Material, comprises the following steps:
(1) add graphene oxide into N, in N- dimethyl lauryl amines, 100 DEG C of stirrings added after 1 hour diphenyl phosphine oxide with
Strontium titanates, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal
System;Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, nanoporous nickel oxide are done
Mill is uniformly rear to be added in extruder, and particle is obtained in 195 DEG C of extrusions;Then cladding material is prepared using film-making machine;
(2) by fullerene derivate add cyanate in, 110 DEG C reaction 20 minutes after add diethylbenzene phosphate and four
Ethoxysilane, reaction add triglycidyl group cyamelide ester monomer after 30 minutes, add after being stirred 2 hours in 120 DEG C
Enter isotridecyl acrylate, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain middle layer material;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic aldehyde tree
Fat and polyvinyl alcohol are added in extruder, and particle is obtained in 185 DEG C of extrusions;Then internal layer material is prepared using film-making machine
Material;
(4) cladding material, middle layer material, inner layer material are sequentially placed into mould, hot pressing obtains compound low Heat Conduction Material.
In above-mentioned technical proposal, graphene oxide, N, N- dimethyl lauryl amine, diphenyl phosphine oxide, strontium titanates, six chloro-iridic acids
Ammonium, polyester resin, naphthol novolac resin, maleic anhydride, the mass ratio of nanoporous nickel oxide are 5: 18: 20: 5: 3: 60:
100∶20∶4;Fullerene derivate, cyanate, diethylbenzene phosphate, tetraethoxysilane, triglycidyl group trimerization isocyanide
Acid ester monomer, isotridecyl acrylate, the mass ratio of uramit are 0.8: 100: 8: 10: 60: 15: 25;Polystyrene,
Polyphenylene sulfide, hollow alumina, bicyclopentadiene, organosilicon phenolic resin, the mass ratio of polyvinyl alcohol are 70: 100: 10: 3:
30∶45。
In above-mentioned technical proposal, the cladding material, middle layer material, the thickness ratio of inner layer material are 30: 100: 15;Step
(2) in, the mould by 115 DEG C of preheatings is poured at 105 DEG C;The condition of the hot pressing be 0MPa/140 DEG C/10 minutes+
+ 1.5MPa/180 DEG C/15 minutes 0.5MPa/160 DEG C/20 minutes;Pressurize Temperature fall after the completion of hot pressing.
The invention also discloses a kind of preparation method of compound low Heat Conduction Material cladding material, comprise the following steps, will
Graphene oxide adds N, and in N- dimethyl lauryl amines, 100 DEG C of stirrings add diphenyl phosphine oxide and strontium titanates, stirring 0.5 after 1 hour
Hour, six ammonium chloroiridates are then added, stirs 10 minutes, natural cooling, obtains graphene composition metal system;By terylene tree
Added after fat, graphene composition metal system, naphthol novolac resin, maleic anhydride, the dry grinding uniformly of nanoporous nickel oxide
In extruder, particle is obtained in 195 DEG C of extrusions;Then compound low Heat Conduction Material cladding material is prepared using film-making machine.
The preparation method of layer material, comprises the following steps in being used the invention also discloses a kind of compound low Heat Conduction Material, will
Fullerene derivate is added in cyanate, and 110 DEG C of reactions add diethylbenzene phosphate and tetraethoxysilane after 20 minutes, instead
Triglycidyl group cyamelide ester monomer is added after answering 30 minutes, isotridecyl third is added after being stirred 2 hours in 120 DEG C
Olefin(e) acid ester, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain layer material during compound low Heat Conduction Material is used.
The invention also discloses a kind of preparation method of compound low Heat Conduction Material inner layer material, comprise the following steps, will
Polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic resin and polyvinyl alcohol
Add in extruder, particle is obtained in 185 DEG C of extrusions;Then compound low Heat Conduction Material internal layer material is prepared using film-making machine
Material.
The invention also discloses a kind of preparation method of compound low Heat Conduction Material presoma system, by cladding material, middle level
Material and inner layer material combine to obtain the compound low Heat Conduction Material presoma system successively;The cladding material, middle level material
The preparation method of material or inner layer material comprises the following steps:
(1) add graphene oxide into N, in N- dimethyl lauryl amines, 100 DEG C of stirrings added after 1 hour diphenyl phosphine oxide with
Strontium titanates, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal
System;Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, nanoporous nickel oxide are done
Mill is uniformly rear to be added in extruder, and particle is obtained in 195 DEG C of extrusions;Then cladding material is prepared using film-making machine;
(2) by fullerene derivate add cyanate in, 110 DEG C reaction 20 minutes after add diethylbenzene phosphate and four
Ethoxysilane, reaction add triglycidyl group cyamelide ester monomer after 30 minutes, add after being stirred 2 hours in 120 DEG C
Enter isotridecyl acrylate, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain middle layer material;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic aldehyde tree
Fat and polyvinyl alcohol are added in extruder, and particle is obtained in 185 DEG C of extrusions;Then internal layer material is prepared using film-making machine
Material.
The invention also discloses a kind of compound low Heat Conduction Material, and the preparation method of the compound low Heat Conduction Material is including following
Step:
(1) add graphene oxide into N, in N- dimethyl lauryl amines, 100 DEG C of stirrings added after 1 hour diphenyl phosphine oxide with
Strontium titanates, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal
System;Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, nanoporous nickel oxide are done
Mill is uniformly rear to be added in extruder, and particle is obtained in 195 DEG C of extrusions;Then cladding material is prepared using film-making machine;
(2) by fullerene derivate add cyanate in, 110 DEG C reaction 20 minutes after add diethylbenzene phosphate and four
Ethoxysilane, reaction add triglycidyl group cyamelide ester monomer after 30 minutes, add after being stirred 2 hours in 120 DEG C
Enter isotridecyl acrylate, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain middle layer material;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic aldehyde tree
Fat and polyvinyl alcohol are added in extruder, and particle is obtained in 185 DEG C of extrusions;Then internal layer material is prepared using film-making machine
Material;
(4) cladding material, middle layer material, inner layer material are sequentially placed into mould, hot pressing obtains compound low Heat Conduction Material.
In being used the invention also discloses a kind of compound low Heat Conduction Material cladding material, compound low Heat Conduction Material layer material or
The compound low Heat Conduction Material inner layer material of person, the compound low Heat Conduction Material is with cladding material, compound low Heat Conduction Material middle level
The preparation method of material or compound low Heat Conduction Material inner layer material comprises the following steps:
(1) add graphene oxide into N, in N- dimethyl lauryl amines, 100 DEG C of stirrings added after 1 hour diphenyl phosphine oxide with
Strontium titanates, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal
System;Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, nanoporous nickel oxide are done
Mill is uniformly rear to be added in extruder, and particle is obtained in 195 DEG C of extrusions;Then compound low Heat Conduction Material is prepared using film-making machine
Use cladding material;
(2) by fullerene derivate add cyanate in, 110 DEG C reaction 20 minutes after add diethylbenzene phosphate and four
Ethoxysilane, reaction add triglycidyl group cyamelide ester monomer after 30 minutes, add after being stirred 2 hours in 120 DEG C
Enter isotridecyl acrylate, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain compound low heat conduction material
Layer material during material is used;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic aldehyde tree
Fat and polyvinyl alcohol are added in extruder, and particle is obtained in 185 DEG C of extrusions;Then compound low lead is prepared using film-making machine
Hot material inner layer material.
The invention also discloses cladding material, middle layer material or inner layer material answering in compound low Heat Conduction Material is prepared
With the preparation method of the cladding material, middle layer material or inner layer material comprises the following steps:
(1) add graphene oxide into N, in N- dimethyl lauryl amines, 100 DEG C of stirrings added after 1 hour diphenyl phosphine oxide with
Strontium titanates, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal
System;Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, nanoporous nickel oxide are done
Mill is uniformly rear to be added in extruder, and particle is obtained in 195 DEG C of extrusions;Then cladding material is prepared using film-making machine;
(2) by fullerene derivate add cyanate in, 110 DEG C reaction 20 minutes after add diethylbenzene phosphate and four
Ethoxysilane, reaction add triglycidyl group cyamelide ester monomer after 30 minutes, add after being stirred 2 hours in 120 DEG C
Enter isotridecyl acrylate, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain middle layer material;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic aldehyde tree
Fat and polyvinyl alcohol are added in extruder, and particle is obtained in 185 DEG C of extrusions;Then internal layer material is prepared using film-making machine
Material.
Cladding material disclosed by the invention, middle layer material, inner layer material are prepared in the application of compound low Heat Conduction Material;According to
Actual installation position restriction outer layer, middle level, internal layer, it is bonded being corrosive the one side of material for inner layer material or contact for wall
For cladding material, middle layer material is between cladding material and inner layer material.
In the present invention, cladding material need to have excellent corrosion resistance and it is good process, be heat-resisting, fire resistance,
Also need to form stable reactive interfaces transition region with middle layer material simultaneously;The present invention is with polyester resin and naphthol novolac tree
Fat is matrix, and rigid structure can ensure heat resistance, and simultaneously added with machine small molecule, one side increases the compatibility of each component,
On the other hand the processing characteristics of material is improved, avoids local defect, especially nanometer porous nickel oxide can slightly improve acidproof
Alkali ability, and can provide low heat-conducting effect.
Middle layer material needs to have excellent heat resistance, thermal insulation, and good processing, fire resistance, passes through cyanic acid
Ester polymerize with epoxy, it is ensured that the hot property of material settling out, especially fullerene derivate PCBM possess reactive ester group
Functional group, good reactivity can be both formed with cyanate under limited amount, cause that fullerene is dispersed again, to fire-retardant
Favorably;The processing characteristics of cyanic acid ester epoxy resin mixed system is improved by the addition of small molecule, and small molecule can join
With cross-linked network, while can also react mutually, for example, diethylbenzene phosphate and tetraethoxysilane can with it is compound enter height
Molecular backbone, reach excellent flame retardant effect so as to coordinate beneficial to phosphorus silicon, isotridecyl acrylate can improve polyureas first
The dispersion level of aldehyde is uniform beneficial to micro-nano hole is resolved into;Small molecule both can avoid macromolecule local reaction not as diluent
, high molecular reaction can be participated in again, such as connection cyanate and epoxy resin, while so as to realize excellent machinability
Do not reduce heat resistance.
Inner layer material needs to have excellent elastic and good heat resistance, anti-flammability, while needs and middle layer material
Form stable interfacial reaction area;By the addition of organosilicon phenolic resin, the polystyrene of tenacity excellent can be improved with gathering
The heat resistance of diphenyl sulfide copolymer, and organosilicon is additionally favorable for the holding of elasticity, and polyvinyl alcohol can improve the phase of several components
Hold reactivity, hollow alumina can increase overall heat-insulating capability and raising prepares the effect of through hole, prevent localized crackses, lead to
Cross the peptizaiton of bicyclopentadiene and polyvinyl alcohol so that alumina dispersion is uniform.
In the present invention, the cladding material, middle layer material, the thickness ratio and preparation technology of inner layer material, especially in
Layer material technique, beneficial to shaping, avoid producing flow field problem.Trilaminate material interacts, and forms stable compound entirety, can
To apply in high fever corrosion field.The present invention, which limits hot pressing condition, can cause three kinds of materials progressively to melt, and start in mould certainly
Under band pressure, formed and melt interpenetrating for interface, avoid gummosis or trilaminate material excessively to merge again;Subsequently progressively it is crosslinked again
Solidification, the solidification level of system was both improved, turn avoid the gummosis of thermoplastic, under small molecule series connection, and catalysis
Under agent regulation and control, high polymer step-reaction, the 3-layer composite material of entirety, excellent effect have been finally given.
The present invention is by process choice, and during the course of the reaction, the probability to be contacted with each other between raw material is higher, in mixed process
Overreact is avoided to cause hot pressure reaction uneven, faster, cross-linked network production rate is higher for reaction speed during hot pressing;Stirred by regulation
Mix, hot pressure reaction temperature and time, extent of reaction when control mixes, method is ingenious in design and reasonable;By adding additive bag
Inorganic material, metallic compound etc. are included, adds the compression strength of the compound low Heat Conduction Material of resin matrix, corrosion-resistant intensity, is dropped
Low thermal conductivity factor, effect of heat insulation is more preferably.
The low Heat Conduction Material of existing organic composite does not possess antiseptic property or antiseptic property is poor, and this is compound low by preparing
What the raw material of Heat Conduction Material determined, cause to be restricted when applying as corrosive substance, service life is short, maintenance cost
It is high;The present invention heat-insulation composite material molecule cross-link is compact-sized, compactness is good, while cladding material is provided with graphene, and N,
N- dimethyl lauryl amine and strontium titanates can improve the corrosion resistance of material together;Especially the present invention adds a small amount of iridium
Compound, one side organo-iridium compounds can form interfacial reaction effect with organic component, improve the compatibility of integral material, separately
On the one hand the cross-linked structure of organic matter can be improved, the activity that the third aspect can increase graphene is good corrosion-resistant so as to realize
Performance, more important is, the present invention limits the ratio of several additives, avoid to heat-proof quality slacken and hot pressing is anti-
The interference answered.
General compound low Heat Conduction Material is all disposed within surface of wall, existing compound low Heat Conduction Material mostly by bonded adhesives with
Effect of heat insulation is realized in wall combination, if necessary to corrosion-resistant, then in outer layer brushing corrosion-resistant finishes;Prior art is clearly present more
Kind defect, for example construct cumbersome, it is necessary to which multistep process, the impact of performance is poor, although being combined by being bonded, between several layer materials
Or Presence of an interface inhomogeneity, especially anti-corrosion layer fall off on compound low Heat Conduction Material surface, aging, gluing or
When brushing, solvent contamination can be produced at the scene;In addition, modular architectural is shown up prominently in terms of building, it is by assembling
The manufacture of monolithic architecture can be achieved, but this has a problem that, i.e., if still by gluing mode combination wall and again
Low Heat Conduction Material is closed, then is unfavorable for modular assembling, because gluing intensity and technique mismatch with modularization, if adopted
The mechanical bond matched with modularization, then compound low Heat Conduction Material and wall there may be microgap, small area is perhaps had nothing to do, but
It is for whole building building, effect of heat insulation can be influenceed.The method comprises the steps of firstly, preparing the compound low Heat Conduction Material of one, it is divided into three
Individual functional layer, adjacent functional bed boundary are interpenetrated, and form stable overall transition zone, and trilaminate material is integrally standardized, and has
There is excellent processability, mounting hole and filler plug can be set, it is possible to achieve the technique effect of mechanical erection, and in internal layer bullet
Property heat proof material effect under, during mechanical package, can make it that compound low Heat Conduction Material and wall are seamless applying, realize height first
Heat-resisting, the compound low Heat Conduction Material of the integrated anti-corrosion of flame retardant type mechanical seamless integration.
Embodiment
A kind of preparation method of compound low Heat Conduction Material of embodiment one, comprises the following steps:
(1) add graphene oxide into N, in N- dimethyl lauryl amines, 100 DEG C of stirrings added after 1 hour diphenyl phosphine oxide with
Strontium titanates, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal
System;Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, nanoporous nickel oxide are done
Mill is uniformly rear to be added in extruder, and particle is obtained in 195 DEG C of extrusions;Then cladding material is prepared using film-making machine;
(2) by fullerene derivate PCBM add cyanate in, 110 DEG C reaction 20 minutes after add diethylbenzene phosphate
With tetraethoxysilane, reaction adds triglycidyl group cyamelide ester monomer after 30 minutes, stirred 2 hours in 120 DEG C
Isotridecyl acrylate, uramit are added afterwards, continues stirring 20 minutes, pour into what is preheated by 115 DEG C at 105 DEG C
Mould, natural cooling obtain middle layer material;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic aldehyde tree
Fat and polyvinyl alcohol are added in extruder, and particle is obtained in 185 DEG C of extrusions;Then internal layer material is prepared using film-making machine
Material;
(4) layer material, 1.5mm inner layer materials in 3mm cladding materials, 10mm are sequentially placed into mould, hot pressing is answered
Close low Heat Conduction Material, the condition of hot pressing for+0.5MPa/160 DEG C/20 minutes 0MPa/140 DEG C/10 minutes+1.5MPa/180 DEG C/
15 minutes;Pressurize Temperature fall after the completion of hot pressing.
In the present embodiment, graphene oxide, N, N- dimethyl lauryl amine, diphenyl phosphine oxide, strontium titanates, six ammonium chloroiridates, wash
Synthetic fibre resin, naphthol novolac resin, maleic anhydride, the mass ratio of nanoporous nickel oxide are 5: 18: 20: 5: 3: 60: 100:
20∶4;Fullerene derivate, cyanate, diethylbenzene phosphate, tetraethoxysilane, triglycidyl group isocyanuric acid ester
Monomer, isotridecyl acrylate, the mass ratio of uramit are 0.8: 100: 8: 10: 60: 15: 25;Polystyrene, polyphenyl
Thioether, hollow alumina, bicyclopentadiene, organosilicon phenolic resin, the mass ratio of polyvinyl alcohol are 70: 100: 10: 3: 30:
45。
Comparative example one
Consistent with embodiment one, wherein difference is, strontium titanates and six ammonium chloroiridates are free of in step (1).
Comparative example two
Consistent with embodiment one, wherein difference is, step is added without uramit in (2).
Comparative example three
Consistent with embodiment one, wherein difference is, step is added without fullerene derivate in (2).
Comparative example four
Consistent with embodiment one, wherein difference is, step is added without bicyclopentadiene, polyvinyl alcohol in (3).
The composite property of table 1 characterizes
Tg | Td | Bending strength | Thermal conductivity factor | Oxygen index (OI) | Hole number | |
Embodiment one | 233℃ | 428℃ | 173MPa | 0.019w/(mK) | 38 | > 3500 |
Comparative example one | 218℃ | 419℃ | 162MPa | 0.028w/(mK) | 37 | > 3500 |
Comparative example two | 228℃ | 426℃ | 168MPa | 0.082w/(mK) | 35 | 3450 |
Comparative example three | 208℃ | 405℃ | 153MPa | 0.025w/(mK) | 34 | 3350 |
Comparative example four | 226℃ | 421℃ | 163MPa | 0.060w/(mK) | 34 | 3450 |
Table 1 is the correlated performance of composite prepared by embodiment and comparative example, it can be clearly seen that, production of the invention
Product possess excellent combination property, especially anti-flammability;Simultaneously with 3mol/L sodium hydroxide solutions, 3mol/L sodium chloride solutions and
3mol/L acetum carries out corrosion-resistant test respectively, and the time is 10 days, and embodiment product surface does not change, is kept
Original state, has good anticorrosion effect, corrosion phenomenon occurs in the product surface of comparative example one, and color is slightly turned to be yellow, right
The product surface of ratio two is unchanged, and the product surface of comparative example three is unchanged, and the product surface of comparative example four is unchanged.Therefore, this hair
Bright product can be used for corrosion-resistant heat-insulated special occasions, and can be mass, and scene only assembles, laborsaving, be adapted to industrialization
Prepare.
Claims (10)
1. a kind of preparation method of compound low Heat Conduction Material, it is characterised in that comprise the following steps:
(1) N is added graphene oxide into, in N- dimethyl lauryl amines, 100 DEG C of stirrings add diphenyl phosphine oxide and metatitanic acid after 1 hour
Strontium, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal system;
Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, the dry grinding of nanoporous nickel oxide is equal
Added after even in extruder, particle is obtained in 195 DEG C of extrusions:Then cladding material is prepared using film-making machine;
(2) fullerene derivate is added in cyanate, 110 DEG C of reactions add diethylbenzene phosphate and four ethoxies after 20 minutes
Base silane, reaction add triglycidyl group cyamelide ester monomer after 30 minutes, are added after being stirred 2 hours in 120 DEG C different
Tridecyl acrylate, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain middle layer material;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic resin with
And polyvinyl alcohol is added in extruder, and particle is obtained in 185 DEG C of extrusions;Then inner layer material is prepared using film-making machine;
(4) cladding material, middle layer material, inner layer material are sequentially placed into mould, hot pressing obtains compound low Heat Conduction Material.
2. preparation method according to claim 1, it is characterised in that graphene oxide, N, N- dimethyl lauryl amine, hexichol
Phosphine oxide, strontium titanates, six ammonium chloroiridates, polyester resin, naphthol novolac resin, maleic anhydride, the matter of nanoporous nickel oxide
Amount is than being 5: 18: 20: 5: 3: 60: 100: 20: 4;Fullerene derivate, cyanate, diethylbenzene phosphate, tetraethoxy-silicane
Alkane, triglycidyl group cyamelide ester monomer, isotridecyl acrylate, the mass ratio of uramit are 0.8: 100:
8∶10∶60∶15∶25;Polystyrene, polyphenylene sulfide, hollow alumina, bicyclopentadiene, organosilicon phenolic resin, polyvinyl alcohol
Mass ratio be 70: 100: 10: 3: 30: 45.
3. preparation method according to claim 1, it is characterised in that the cladding material, middle layer material, inner layer material
Thickness ratio is 30: 100: 15;In step (2), the mould by 115 DEG C of preheatings is poured at 105 DEG C;The condition of the hot pressing is
+ 1.5MPa/180 DEG C/15 minutes+0.5MPa/160 DEG C/20 minutes 0MPa/140 DEG C/10 minutes;Pressurize is natural after the completion of hot pressing
Cooling.
4. a kind of preparation method of compound low Heat Conduction Material cladding material, it is characterised in that comprise the following steps, stone will be aoxidized
Black alkene adds N, and in N- dimethyl lauryl amines, 100 DEG C of stirrings add diphenyl phosphine oxide and strontium titanates after 1 hour, stir 0.5 hour,
Then six ammonium chloroiridates are added, stirs 10 minutes, natural cooling, obtains graphene composition metal system;By polyester resin, graphite
Extruder is added after alkene composition metal system, naphthol novolac resin, maleic anhydride, the dry grinding uniformly of nanoporous nickel oxide
In, obtain particle in 195 DEG C of extrusions;Then compound low Heat Conduction Material cladding material is prepared using film-making machine.
The preparation method of layer material during 5. a kind of compound low Heat Conduction Material is used, it is characterised in that comprise the following steps, by fullerene
Derivative is added in cyanate, and 110 DEG C of reactions add diethylbenzene phosphate and tetraethoxysilane after 20 minutes, react 30 points
Triglycidyl group cyamelide ester monomer is added after clock, isotridecyl acrylic acid is added after being stirred 2 hours in 120 DEG C
Ester, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain layer material during compound low Heat Conduction Material is used.
6. a kind of preparation method of compound low Heat Conduction Material inner layer material, it is characterised in that comprise the following steps, by polyphenyl second
Add and squeeze with bicyclopentadiene, organosilicon phenolic resin and polyvinyl alcohol after alkene, polyphenylene sulfide, hollow alumina dry grinding mixing
Go out in machine, particle is obtained in 185 DEG C of extrusions;Then compound low Heat Conduction Material inner layer material is prepared using film-making machine.
A kind of 7. preparation method of compound low Heat Conduction Material presoma system, it is characterised in that by cladding material, middle layer material with
And inner layer material combines to obtain the compound low Heat Conduction Material presoma system successively;The cladding material, middle layer material or
The preparation method of inner layer material comprises the following steps:
(1) N is added graphene oxide into, in N- dimethyl lauryl amines, 100 DEG C of stirrings add diphenyl phosphine oxide and metatitanic acid after 1 hour
Strontium, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal system;
Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, the dry grinding of nanoporous nickel oxide is equal
Added after even in extruder, particle is obtained in 195 DEG C of extrusions;Then cladding material is prepared using film-making machine;
(2) fullerene derivate is added in cyanate, 110 DEG C of reactions add diethylbenzene phosphate and four ethoxies after 20 minutes
Base silane, reaction add triglycidyl group cyamelide ester monomer after 30 minutes, are added after being stirred 2 hours in 120 DEG C different
Tridecyl acrylate, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain middle layer material;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic resin with
And polyvinyl alcohol is added in extruder, and particle is obtained in 185 DEG C of extrusions;Then inner layer material is prepared using film-making machine.
8. a kind of compound low Heat Conduction Material, it is characterised in that the preparation method of the compound low Heat Conduction Material comprises the following steps:
(1) N is added graphene oxide into, in N- dimethyl lauryl amines, 100 DEG C of stirrings add diphenyl phosphine oxide and metatitanic acid after 1 hour
Strontium, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal system;
Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, the dry grinding of nanoporous nickel oxide is equal
Added after even in extruder, particle is obtained in 195 DEG C of extrusions;Then cladding material is prepared using film-making machine;
(2) fullerene derivate is added in cyanate, 110 DEG C of reactions add diethylbenzene phosphate and four ethoxies after 20 minutes
Base silane, reaction add triglycidyl group cyamelide ester monomer after 30 minutes, are added after being stirred 2 hours in 120 DEG C different
Tridecyl acrylate, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain middle layer material;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic resin with
And polyvinyl alcohol is added in extruder, and particle is obtained in 185 DEG C of extrusions;Then inner layer material is prepared using film-making machine;
(4) cladding material, middle layer material, inner layer material are sequentially placed into mould, hot pressing obtains compound low Heat Conduction Material.
Layer material or compound low Heat Conduction Material during 9. a kind of compound low Heat Conduction Material cladding material, compound low Heat Conduction Material are used
With inner layer material, it is characterised in that during the compound low Heat Conduction Material cladding material, compound low Heat Conduction Material are used layer material or
The preparation method of the compound low Heat Conduction Material inner layer material of person comprises the following steps:
(1) N is added graphene oxide into, in N- dimethyl lauryl amines, 100 DEG C of stirrings add diphenyl phosphine oxide and metatitanic acid after 1 hour
Strontium, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal system;
Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, the dry grinding of nanoporous nickel oxide is equal
Added after even in extruder, particle is obtained in 195 DEG C of extrusions;Then it is outer compound low Heat Conduction Material use to be prepared using film-making machine
Layer material;
(2) fullerene derivate is added in cyanate, 110 DEG C of reactions add diethylbenzene phosphate and four ethoxies after 20 minutes
Base silane, reaction add triglycidyl group cyamelide ester monomer after 30 minutes, are added after being stirred 2 hours in 120 DEG C different
Tridecyl acrylate, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain compound low Heat Conduction Material use
Middle layer material;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic resin with
And polyvinyl alcohol is added in extruder, and particle is obtained in 185 DEG C of extrusions;Then compound low heat conduction material is prepared using film-making machine
Material inner layer material.
10. the application of cladding material, middle layer material or inner layer material in compound low Heat Conduction Material is prepared, it is characterised in that
The preparation method of the cladding material, middle layer material or inner layer material comprises the following steps:
(1) N is added graphene oxide into, in N- dimethyl lauryl amines, 100 DEG C of stirrings add diphenyl phosphine oxide and metatitanic acid after 1 hour
Strontium, stir 0.5 hour, then add six ammonium chloroiridates, stir 10 minutes, natural cooling, obtain graphene composition metal system;
Polyester resin, graphene composition metal system, naphthol novolac resin, maleic anhydride, the dry grinding of nanoporous nickel oxide is equal
Added after even in extruder, particle is obtained in 195 DEG C of extrusions;Then cladding material is prepared using film-making machine;
(2) fullerene derivate is added in cyanate, 110 DEG C of reactions add diethylbenzene phosphate and four ethoxies after 20 minutes
Base silane, reaction add triglycidyl group cyamelide ester monomer after 30 minutes, are added after being stirred 2 hours in 120 DEG C different
Tridecyl acrylate, uramit, continue stirring 20 minutes, pour into mould natural cooling and obtain middle layer material;
(3) by polystyrene, polyphenylene sulfide, hollow alumina dry grinding mixing after with bicyclopentadiene, organosilicon phenolic resin with
And polyvinyl alcohol is added in extruder, and particle is obtained in 185 DEG C of extrusions;Then inner layer material is prepared using film-making machine.
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