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CN106046362A - Graphene foam-nylon 6 high-thermal-conductivity nanocomposite and preparation method thereof - Google Patents

Graphene foam-nylon 6 high-thermal-conductivity nanocomposite and preparation method thereof Download PDF

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Publication number
CN106046362A
CN106046362A CN201610249237.2A CN201610249237A CN106046362A CN 106046362 A CN106046362 A CN 106046362A CN 201610249237 A CN201610249237 A CN 201610249237A CN 106046362 A CN106046362 A CN 106046362A
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nylon
grapheme foam
preparation
foam
high heat
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丁鹏
邵临博
崔谢亮
施利毅
李顼珩
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/08Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
    • C08G69/14Lactams
    • C08G69/16Preparatory processes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

The invention discloses a graphene foam-nylon 6 high-thermal-conductivity nanocomposite and a preparation method thereof. The preparation method comprises the following steps: subjecting graphene oxide to hydrothermal reduction and self-assembling and then carrying out freeze drying so as to obtain graphene foam; mixing the graphene foam with nylon 6 monomer and a catalyst or initiator so as to form a graphene foam-nylon 6 precursor mixture; and subjecting the nylon 6 precursor in the mixture to polymerization so as to form the high-thermal-conductivity nylon 6 nanocomposite. According to the invention, a three-dimensional fully-communicated graphene foam network is used as a heat-conduction additive for the nanocomposite, so a three-dimensional fully-communicated rapid heat-conducting network is constructed in the nanocomposite and the heat conductivity of the nanocomposite is improved by 2 to 5 times compared with the heat conductivity of traditional nylon; and the nanocomposite has the characteristics of low addition of graphene and high heat conductivity, is good in mechanical properties and processing performance and low in cost and can be widely applied to the field of heat radiation of automobiles, computers, LEDs and the like.

Description

Grapheme foam-nylon 6 high heat conducting nano composite material and preparation method thereof
Technical field
The present invention relates to a kind of composite and preparation method thereof, particularly relate to a kind of graphene-based composite or Nylon 6 is composite of matrix and preparation method thereof, belongs to heat-conductivity polymer composite technical field.
Background technology
Along with the development of modern electronics industry, information industry and new and high technology, small-sized in particular with microelectronic component Being constantly increasing of change, densification, and power, the heat dissipation problem of device becomes to become more and more important, and therefore Heat Conduction Material is carried by people Go out the highest requirement, it is desirable to obtain the material with good heat conductive performance with satisfied actual heat radiation needs.With traditional The radiator of metallic aluminium is compared, and heat-conducting polymer material has many advantages:
The most lightweight, macromolecular material density is about the half of metallic aluminium, macromolecular material density 1.49g/cm, and metallic aluminium Density be 2.79 g/cm;The most easy to process, can process with injection moulding;3. can make baroque assembly, improve Design freedom;4. environmental protection, renewable etc..Therefore, the thermoplastic composite of high heat conduction of new generation is expected to substituted metal material Do radiator material.
Graphene is a kind of emerging Two-dimensional Carbon nano material, and it not only has the theoretical heat conductivity of 5300 w/m/k, also Having the highest specific surface area and Young's modulus, the character of these uniquenesses makes Graphene be considered a kind of efficient hot interface, heat Control material, but with Graphene as additive, graphene uniform is added in a lot of matrix material and all there is difficulty, and to fill The heat conductivility of Graphene is waved in distribution, needs to add more multi-component Graphene in matrix material, and this too increases system undoubtedly The cost of standby composite.
Nylon 6 is the thermoplastic engineering plastic of a kind of excellent performance, has excellent mechanical property!Preferably electrical property, And wear-resisting, oil resistant, solvent resistant, self-lubricating, corrosion-resistant and good processing characteristics etc..Be widely used in automobile, electronic apparatus, In the industrial circles such as machinery, Aero-Space and daily life.But, as other macromolecular materials, the structure of nylon 6 itself It is heat insulation body that feature determines it, thus limits its application in Heat Conduction Material field.Low for nylon guide heating rate Situation, Chinese scholars done substantial amounts of research, and existing frequently-used method is to add BN, AIN, Si3The heat conduction such as N, SiC are filled out Material, to reach to improve the purpose of nylon guide heating rate, because the thermal conductivity of itself is relatively low, and only just can make multiple under high addition Condensation material obtains higher thermal conductivity.But higher addition frequently can lead to filler reunites, thus reduce nylon 6 and other height Other performance of molecular material itself.
Summary of the invention
In order to solve prior art problem, it is an object of the invention to the deficiency overcoming prior art to exist, it is provided that a kind of Grapheme foam-nylon 6 high heat conducting nano composite material and preparation method thereof, uses the grapheme foam of a kind of three-dimensional full-mesh Network, as the heat conduction additive of composite, has Graphene addition low, the feature that thermal conductivity is high, and possesses good Mechanical property and processing characteristics.
Purpose is created, employing following technical proposals for reaching foregoing invention:
A kind of grapheme foam-nylon 6 high heat conducting nano composite material, with nylon 6 as matrix material, with grapheme foam for leading Hot filler, forms composite, makes grapheme foam constitute the network structure of three-dimensional full-mesh in nylon-6 matrix body material, from And making the network of the grapheme foam in nylon 6 form the heat bridge of composite, the parts by weight of each component of composite are: stone Ink alkene foam proportion is 1-10 wt%, and nylon 6 proportion is 90-99 wt%.
The density of above-mentioned grapheme foam is preferably 0.01-0.1g/cm.
Above-mentioned nylon 6 is preferably pure polyamide 6.
The preparation method of a kind of grapheme foam-nylon 6 high heat conducting nano composite material, comprises the steps:
A. prepared by grapheme foam: use graphene oxide hydrothermal reduction self-assembling method as grapheme foam preparation technology, The graphene oxide water solution that concentration is 1-10mg/ml is poured into hydrothermal reaction kettle seal in interior cup, be heated to 120-180 DEG C, and it is incubated 6-12 hour, make the graphene oxide generation chemical reduction reaction in graphene oxide water solution, and reunion becomes Graphene wet gel block, then by Graphene wet gel block lyophilization 48 hours under the conditions of-60 DEG C, obtains having three The grapheme foam of the network structure of dimension full-mesh;The graphene oxide concentration of the graphene oxide water solution used is preferably 2- 9mg/ml;Employing graphene oxide hydrothermal reduction self-assembling method is as grapheme foam preparation technology, preferred during heat temperature raising And it is incubated 6-10 hour, make the graphene oxide generation chemical reduction reaction in graphene oxide water solution;
B. according to grapheme foam and the mixed proportion of nylon 6 monomer, by grapheme foam and the Buddhist nun of preparation in described step a Dragon 6 monomers mixing, and also mixes with catalyst or initiator, and at 90-120 DEG C, make nylon 6 monomer and catalyst or Melt with initiator and penetrate in gap and the duct of grapheme foam network;Nylon 6 monomer is preferably epsilon-caprolactams;Adopt Described catalyst or initiator, be respectively preferably 6-aminocaprolc acid or phosphoric acid;
C. through described step b by nylon 6 monomer and grapheme foam and with catalyst or after mixing with initiator, the most right Mixed material carries out application of vacuum, until the bubble removed in mixed material, and make nylon 6 monomer and catalyst or and initiator Till penetrating in the space of grapheme foam, then at 160-200 DEG C and under nitrogen atmosphere protective condition, to mixed material Carry out prepolymerization at least 1 hour, form composite prepolymer;
D., at 240-260 DEG C and under nitrogen atmosphere protective condition, the composite prepolymer of preparation in described step c is entered Row polyreaction 4-10 hour, prepares grapheme foam-nylon 6 high heat conducting nano composite material, and composite is with nylon 6 For matrix material, with grapheme foam as heat filling, grapheme foam is made to constitute three-dimensional full-mesh in nylon-6 matrix body material Network structure so that the grapheme foam in nylon 6 network formed composite heat bridge, grapheme foam-nylon 6 The parts by weight of each component of high heat conducting nano composite material are: grapheme foam proportion is 1-10 wt%, shared by nylon 6 Ratio is 90-99 wt%;
E. under nitrogen atmosphere is protected, to grapheme foam-nylon 6 high heat conducting nano composite wood of preparation in described step d Material carries out natural cooling, then after composite is washed and cut, finally gives the high heat conduction of grapheme foam-nylon 6 and receive Nano composite material.
The present invention compared with prior art, has and the most obviously highlights substantive distinguishing features and remarkable advantage:
1. the present invention has abandoned the technology path of conventional composite materials dispersion-stirring-solidification, the heat conduction additive-graphite of employing Alkene three-dimensional porous foams is the overall network of a connection, remains the intrinsic property of Graphene;
2. the present invention is made without the routine operations such as mechanical agitation when admixed graphite alkene is with high molecular polymer, it is only necessary to letter Single dipping filling processes, and without the problem occurring reuniting in local, can reach higher uniformity;
3. the present invention uses the grapheme foam network of three-dimensional full-mesh as the heat conduction additive of composite, constructs out compound The quick conductive network of material internal three-dimensional full-mesh, the capacity of heat transmission improves 2-5 times than conventional nylon;
Grapheme foam/nylon 6 heat-conductive composite material the most provided by the present invention not only has the heat conductivility of excellence, Er Qieqi Preparation technology is simple, with low cost, can be widely applied to the field of radiatings such as automobile, computer, LED.
Detailed description of the invention
Details are as follows for the preferred embodiments of the present invention:
Embodiment one:
In the present embodiment, the preparation method of a kind of grapheme foam-nylon 6 high heat conducting nano composite material, including walking as follows Rapid:
A. prepared by grapheme foam: use graphene oxide hydrothermal reduction self-assembling method as grapheme foam preparation technology, The graphene oxide water solution that concentration is 2mg/ml that volume is 40 ml being poured in hydrothermal reaction kettle seals in cup, heating rises Temperature is to 120 DEG C, and is incubated 6 hours, makes the graphene oxide generation chemical reduction reaction in graphene oxide water solution, and reunites Become Graphene wet gel block, then Graphene wet gel block is put into refrigerator ,-10 DEG C of freezings so that it is be fully crystallized into For gel crystals solid, under the conditions of-60 DEG C, then carry out vacuum sublimation lyophilization 48 hours, obtain that there is three-dimensional and entirely connect The grapheme foam of logical network structure, gained grapheme foam density is 0.02 g/cm;
B. according to grapheme foam and the mixed proportion of nylon 6 monomer, use epsilon-caprolactams as nylon 6 monomer, use 6- Aminocaproic acid as the polymerization initiator of nylon 6 composite material, by the grapheme foam of preparation in described step a, 36 grams of ε- Caprolactam and 4 grams of 6-aminocaprolc acids mix, and add there-necked flask, and at 100 DEG C, make epsilon-caprolactams and 6-amino Caproic acid melts and penetrates in gap and the duct of grapheme foam network;
C., after epsilon-caprolactams, grapheme foam and 6-aminocaprolc acid are mixed by described step b, further mixed material is entered Row application of vacuum, extracts the air of remaining in grapheme foam out, until the bubble removed in mixed material, and make nylon 6 monomer With catalyst or penetrate into grapheme foam with initiator space in till, make polymer precursor penetrate into stone more fully In the space of ink alkene foam, then at 180 DEG C and under nitrogen atmosphere protective condition, mixed material is carried out prepolymerization 1 Hour, form composite prepolymer;
D., at 260 DEG C and under nitrogen atmosphere protective condition, the composite prepolymer of preparation in described step c is gathered Closing reaction 4 hours, prepare grapheme foam-nylon 6 high heat conducting nano composite material, composite is with nylon 6 as matrix Material, with grapheme foam as heat filling, makes grapheme foam constitute the network of three-dimensional full-mesh in nylon-6 matrix body material Structure, so that the network of the grapheme foam in nylon 6 forms the heat bridge of composite, the high heat conduction of grapheme foam-nylon 6 The parts by weight of each component of nano composite material are: grapheme foam proportion is 2wt%, and nylon 6 proportion is 98 wt%;
E. under nitrogen atmosphere is protected, to grapheme foam-nylon 6 high heat conducting nano composite wood of preparation in described step d Material carries out natural cooling, then after composite is washed and cut, finally gives the high heat conduction of grapheme foam-nylon 6 and receive Nano composite material.
The mensuration of heat conductivity:
Laser heat conductivity instrument (NETZSCHLFA447) using Nai Chi instrument manufacturing company limited of Germany measures the present embodiment stone The thermal conductivity of ink alkene foam-nylon 6 high heat conducting nano composite material sample.Before test, at Graphene bubble prepared by the present embodiment Foam-nylon 6 high heat conducting nano composite material sample surfaces sprays one layer of graphite to reduce sample to sharp scattering of light, each temperature Point repeated measure three times, takes its meansigma methods as final result, records grapheme foam-nylon 6 height prepared by the present embodiment and leads Hot nano composite material thermal conductivity is 0.4 wm-1 k-1
In the present embodiment, prepared grapheme foam-nylon 6 high heat conducting nano composite material is with nylon 6 as matrix Material, with grapheme foam as heat filling, forms composite, makes grapheme foam constitute three in nylon-6 matrix body material The network structure of dimension full-mesh, so that the network of the grapheme foam in nylon 6 forms the heat bridge of composite.The present embodiment Graphene oxide is obtained grapheme foam through hydrothermal reduction self assembly, lyophilization;By grapheme foam and nylon 6 monomer And catalyst or initiator mix, form Graphene/nylon 6 presoma mixture;Nylon 6 presoma in polymerization mixture, Thus form the nylon 6 composite material of high heat conduction.Nylon 6 composite material be by grapheme foam and nylon 6 monomer, catalyst or Initiator, through melting, immerses, pre-polymerization, and polymerization, cutting obtains.Grapheme foam by graphene oxide through hydrothermal reduction from group Dress, lyophilization obtains, and grapheme foam is the network structure that graphene oxide is constituted three-dimensional full-mesh in the way of self assembly. Embodiment uses the grapheme foam network of three-dimensional full-mesh as the heat conduction additive of composite, constructs out in composite The quick conductive network of portion's three-dimensional full-mesh, the capacity of heat transmission significantly improves than conventional nylon.The present embodiment uses Graphene from group Dress method is suitable for preparing in a large number high-quality graphene foam, uses the grapheme foam network of three-dimensional full-mesh as composite Additive, develop effective preparation method of a kind of high thermal conductivity graphene based composites.
Embodiment two:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, the preparation method of a kind of grapheme foam-nylon 6 high heat conducting nano composite material, including walking as follows Rapid:
A. prepared by grapheme foam: use graphene oxide hydrothermal reduction self-assembling method as grapheme foam preparation technology, The graphene oxide water solution that concentration is 4mg/ml that volume is 40 ml being poured in hydrothermal reaction kettle seals in cup, heating rises Temperature is to 140 DEG C, and is incubated 6 hours, makes the graphene oxide generation chemical reduction reaction in graphene oxide water solution, and reunites Become Graphene wet gel block, then Graphene wet gel block is put into refrigerator ,-10 DEG C of freezings so that it is be fully crystallized into For gel crystals solid, under the conditions of-60 DEG C, then carry out vacuum sublimation lyophilization 48 hours, obtain that there is three-dimensional and entirely connect The grapheme foam of logical network structure, gained grapheme foam density is 0.04 g/cm;
B. according to grapheme foam and the mixed proportion of nylon 6 monomer, use epsilon-caprolactams as nylon 6 monomer, use 6- Aminocaproic acid as the polymerization initiator of nylon 6 composite material, by the grapheme foam of preparation in described step a, 36 grams of ε- Caprolactam and 4 grams of 6-aminocaprolc acids mix, and add there-necked flask, and at 100 DEG C, make epsilon-caprolactams and 6-amino Caproic acid melts and penetrates in gap and the duct of grapheme foam network;
C. this step is identical with embodiment one;
D., at 260 DEG C and under nitrogen atmosphere protective condition, the composite prepolymer of preparation in described step c is gathered Closing reaction 6 hours, prepare grapheme foam-nylon 6 high heat conducting nano composite material, composite is with nylon 6 as matrix Material, with grapheme foam as heat filling, makes grapheme foam constitute the network of three-dimensional full-mesh in nylon-6 matrix body material Structure, so that the network of the grapheme foam in nylon 6 forms the heat bridge of composite, the high heat conduction of grapheme foam-nylon 6 The parts by weight of each component of nano composite material are: grapheme foam proportion is 4wt%, and nylon 6 proportion is 96 wt%;
E. this step is identical with embodiment one.
The mensuration of heat conductivity:
This example uses the Measured Results of Thermal Conductivity method identical with embodiment one, record grapheme foam prepared by the present embodiment- Nylon 6 high heat conducting nano composite material thermal conductivity is 0.6 wm-1 k-1
Embodiment three:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, the preparation method of a kind of grapheme foam-nylon 6 high heat conducting nano composite material, including walking as follows Rapid:
A. prepared by grapheme foam: use graphene oxide hydrothermal reduction self-assembling method as grapheme foam preparation technology, By volume be 40 ml concentration be that the graphene oxide water solution of 6mg/ml is poured in hydrothermal reaction kettle seals in cup, heat temperature raising To 160 DEG C, and it is incubated 6 hours, makes the graphene oxide generation chemical reduction reaction in graphene oxide water solution, and be agglomerated into For Graphene wet gel block, then Graphene wet gel block is put into refrigerator ,-10 DEG C of freezings so that it is be fully crystallized and become Gel crystals solid, then carries out vacuum sublimation lyophilization 48 hours under the conditions of-60 DEG C, obtains having three-dimensional full-mesh The grapheme foam of network structure, gained grapheme foam density is 0.06 g/cm;
B. according to grapheme foam and the mixed proportion of nylon 6 monomer, use epsilon-caprolactams as nylon 6 monomer, use 6- Aminocaproic acid as the polymerization initiator of nylon 6 composite material, by the grapheme foam of preparation in described step a, 36 grams of ε- Caprolactam and 4 grams of 6-aminocaprolc acids mix, and add there-necked flask, and at 100 DEG C, make epsilon-caprolactams and 6-amino Caproic acid melts and penetrates in gap and the duct of grapheme foam network;
C. this step is identical with embodiment one;
D., at 260 DEG C and under nitrogen atmosphere protective condition, the composite prepolymer of preparation in described step c is gathered Closing reaction 8 hours, prepare grapheme foam-nylon 6 high heat conducting nano composite material, composite is with nylon 6 as matrix Material, with grapheme foam as heat filling, makes grapheme foam constitute the network of three-dimensional full-mesh in nylon-6 matrix body material Structure, so that the network of the grapheme foam in nylon 6 forms the heat bridge of composite, the high heat conduction of grapheme foam-nylon 6 The parts by weight of each component of nano composite material are: grapheme foam proportion is 6wt%, and nylon 6 proportion is 94 wt%;
E. this step is identical with embodiment one.
The mensuration of heat conductivity:
This example uses the Measured Results of Thermal Conductivity method identical with embodiment one, record grapheme foam prepared by the present embodiment- Nylon 6 high heat conducting nano composite material thermal conductivity is 0.7 wm-1 k-1
Embodiment four:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, the preparation method of a kind of grapheme foam-nylon 6 high heat conducting nano composite material, including walking as follows Rapid:
A. prepared by grapheme foam: use graphene oxide hydrothermal reduction self-assembling method as grapheme foam preparation technology, The graphene oxide water solution that concentration is 9mg/ml that volume is 40 ml being poured in hydrothermal reaction kettle seals in cup, heating rises Temperature is to 180 DEG C, and is incubated 6 hours, makes the graphene oxide generation chemical reduction reaction in graphene oxide water solution, and reunites Become Graphene wet gel block, then Graphene wet gel block is put into refrigerator ,-10 DEG C of freezings so that it is be fully crystallized into For gel crystals solid, under the conditions of-60 DEG C, then carry out vacuum sublimation lyophilization 48 hours, obtain that there is three-dimensional and entirely connect The grapheme foam of logical network structure, gained grapheme foam density is 0.09 g/cm;
B. according to grapheme foam and the mixed proportion of nylon 6 monomer, use epsilon-caprolactams as nylon 6 monomer, use 6- Aminocaproic acid as the polymerization initiator of nylon 6 composite material, by the grapheme foam of preparation in described step a, 36 grams of ε- Caprolactam and 4 grams of 6-aminocaprolc acids mix, and add there-necked flask, and at 100 DEG C, make epsilon-caprolactams and 6-amino Caproic acid melts and penetrates in gap and the duct of grapheme foam network;
C. this step is identical with embodiment one;
D., at 260 DEG C and under nitrogen atmosphere protective condition, the composite prepolymer of preparation in described step c is gathered Closing reaction 8 hours, prepare grapheme foam-nylon 6 high heat conducting nano composite material, composite is with nylon 6 as matrix Material, with grapheme foam as heat filling, makes grapheme foam constitute the network of three-dimensional full-mesh in nylon-6 matrix body material Structure, so that the network of the grapheme foam in nylon 6 forms the heat bridge of composite, the high heat conduction of grapheme foam-nylon 6 The parts by weight of each component of nano composite material are: grapheme foam proportion is 9wt%, and nylon 6 proportion is 91 wt%;
E. this step is identical with embodiment one.
The mensuration of heat conductivity:
This example uses the Measured Results of Thermal Conductivity method identical with embodiment one, record grapheme foam prepared by the present embodiment- Nylon 6 high heat conducting nano composite material thermal conductivity is 0.9 wm-1 k-1
Above the embodiment of the present invention is illustrated, but the invention is not restricted to above-described embodiment, it is also possible to according to this The purpose of bright innovation and creation makes multiple change, and that does under all spirit according to technical solution of the present invention and principle changes Becoming, modify, substitute, combine or simplify, all should be the substitute mode of equivalence, as long as meeting the goal of the invention of the present invention, as long as not Deviate from know-why and the inventive concept of grapheme foam-nylon 6 high heat conducting nano composite material of the present invention and preparation method thereof, Broadly fall into protection scope of the present invention.

Claims (8)

1. grapheme foam-nylon 6 high heat conducting nano composite material, it is characterised in that: with nylon 6 as matrix material, with Grapheme foam is heat filling, forms composite, makes grapheme foam constitute three-dimensional full-mesh in nylon-6 matrix body material Network structure so that the grapheme foam in nylon 6 network formed composite heat bridge, each component of composite Parts by weight are: grapheme foam proportion is 1-10 wt%, and nylon 6 proportion is 90-99 wt%.
Grapheme foam-nylon 6 high heat conducting nano composite material the most according to claim 1, it is characterised in that: described graphite The density of alkene foam is 0.01-0.1g/cm.
Grapheme foam-nylon 6 high heat conducting nano composite material the most according to claim 1 or claim 2, it is characterised in that: described Nylon 6 is pure polyamide 6.
4. the preparation method of grapheme foam-nylon 6 high heat conducting nano composite material, it is characterised in that include walking as follows Rapid:
A. prepared by grapheme foam: use graphene oxide hydrothermal reduction self-assembling method as grapheme foam preparation technology, The graphene oxide water solution that concentration is 1-10mg/ml is poured into hydrothermal reaction kettle seal in interior cup, be heated to 120-180 DEG C, and it is incubated 6-12 hour, make the graphene oxide generation chemical reduction reaction in graphene oxide water solution, and reunion becomes Graphene wet gel block, then by Graphene wet gel block lyophilization 48 hours under the conditions of-60 DEG C, obtains having three The grapheme foam of the network structure of dimension full-mesh;
B. according to grapheme foam and the mixed proportion of nylon 6 monomer, by grapheme foam and the Buddhist nun of preparation in described step a Dragon 6 monomers mixing, and also mixes with catalyst or initiator, and at 90-120 DEG C, make nylon 6 monomer and catalyst or Melt with initiator and penetrate in gap and the duct of grapheme foam network;
C. through described step b by nylon 6 monomer and grapheme foam and with catalyst or after mixing with initiator, the most right Mixed material carries out application of vacuum, until the bubble removed in mixed material, and make nylon 6 monomer and catalyst or and initiator Till penetrating in the space of grapheme foam, then at 160-200 DEG C and under nitrogen atmosphere protective condition, to mixed material Carry out prepolymerization at least 1 hour, form composite prepolymer;
D., at 240-260 DEG C and under nitrogen atmosphere protective condition, the composite prepolymer of preparation in described step c is entered Row polyreaction 4-10 hour, prepares grapheme foam-nylon 6 high heat conducting nano composite material, and composite is with nylon 6 For matrix material, with grapheme foam as heat filling, grapheme foam is made to constitute three-dimensional full-mesh in nylon-6 matrix body material Network structure so that the grapheme foam in nylon 6 network formed composite heat bridge, grapheme foam-nylon 6 The parts by weight of each component of high heat conducting nano composite material are: grapheme foam proportion is 1-10 wt%, shared by nylon 6 Ratio is 90-99 wt%;
E. under nitrogen atmosphere is protected, to grapheme foam-nylon 6 high heat conducting nano composite wood of preparation in described step d Material carries out natural cooling, then after composite is washed and cut, finally gives the high heat conduction of grapheme foam-nylon 6 and receive Nano composite material.
The most according to claim 4, the preparation method of grapheme foam-nylon 6 high heat conducting nano composite material, its feature exists In: in described step b, described nylon 6 monomer is epsilon-caprolactams.
6. according to the preparation method of grapheme foam-nylon 6 high heat conducting nano composite material, its feature described in claim 4 or 5 It is: in described step b, the described catalyst of employing or initiator, respectively 6-aminocaprolc acid or phosphoric acid.
7. according to the preparation method of grapheme foam-nylon 6 high heat conducting nano composite material, its feature described in claim 4 or 5 Being: in described step a, the graphene oxide concentration of the graphene oxide water solution of employing is 2-9mg/ml.
8. according to the preparation method of grapheme foam-nylon 6 high heat conducting nano composite material, its feature described in claim 4 or 5 It is: in described step a, uses graphene oxide hydrothermal reduction self-assembling method as grapheme foam preparation technology, add Heat heats up and is incubated 6-10 hour, makes the graphene oxide generation chemical reduction reaction in graphene oxide water solution.
CN201610249237.2A 2016-04-21 2016-04-21 Graphene foam-nylon 6 high-thermal-conductivity nanocomposite and preparation method thereof Pending CN106046362A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106633037A (en) * 2016-12-15 2017-05-10 西南交通大学 Preparation method of graphene/nylon-6 composite
CN106977768A (en) * 2017-05-03 2017-07-25 杭州高烯科技有限公司 A kind of method that spitball shape graphene improves the impact strength of nylon 6
WO2018036423A1 (en) * 2016-08-22 2018-03-01 广东纳路纳米科技有限公司 Plastic composite material based on three-dimensional graphene modification
CN110951114A (en) * 2019-11-24 2020-04-03 上海大学 Three-dimensional carbon fiber graphene aerogel high-molecular composite material and preparation method thereof

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