CN106432861A - High-thermal-conductive composite plastics filled with three-dimensional graphene and preparation method and application thereof - Google Patents
High-thermal-conductive composite plastics filled with three-dimensional graphene and preparation method and application thereof Download PDFInfo
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- CN106432861A CN106432861A CN201610707278.1A CN201610707278A CN106432861A CN 106432861 A CN106432861 A CN 106432861A CN 201610707278 A CN201610707278 A CN 201610707278A CN 106432861 A CN106432861 A CN 106432861A
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- C09K5/14—Solid materials, e.g. powdery or granular
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses high-thermal-conductive composite plastics filled with three-dimensional graphene and a preparation method thereof. The thermal-conductive composite plastics include surface modified three-dimensional graphene and a plastic matrix; the three-dimensional graphene and a surfactant are mechanically stirred for 30-120 min, and the mixture is dried to obtain the thermal-conductive composite plastics of the surface modified three-dimensional graphene and the plastic matrix. When the addition amount is 300 wt.% of the plastic matrix, the thermal conductivity of the matrix can be significantly increased and is increased by 8 times that of plastics without addition of three-dimensional graphene.
Description
Technical field
The invention belongs to heat-conducting plastic technical field of composite materials, more particularly, to a kind of three-dimensional grapheme of filling
High heat conduction composite plastic and its preparation method and application.
Background technology
Metal material is the conduction on traditional concept, Heat Conduction Material, but with the progress of polymer science, macromolecular material
Also becoming conduction, the new role in heat conduction field, it has overturned the heat insulation concept of conventional polymer insulated with material.Conducting polymer material
Material is to study one focus in ground in recent years, heat-conducting polymer material constantly expanding gradually by people's weight also with application
Depending on such as heat exchange engineering, electromagnetic shielding, electronic apparatus, friction material etc..Information industry flourish in the last few years, to high score
The performance of sub-material proposes new requirement, and the especially development for heat-conducting plastic provides development space.In plastics industry, lead
Maximum and the most important application of thermoplastic materials is alternative metals and the heat exchanger of alloy manufacture.It can be applied to need with alternative metals
Want the environment of thermal conductive resin and excellent corrosion resistance, such as heat exchanger, solar water heater, the cooler etc. of battery.Electricity
Sub-electrical equipment industry is also a more field of application heat-conducting plastic, is mainly used to the higher heat-conduction circuit board of manufacture requirements.
It in order to manufacture the heat-conducting plastic with excellent heat conductivity performance, is typically all the metal by high-termal conductivity or inorganic filler
Macromolecular material is filled with.The Heat Conduction Material so obtaining shaping cheap, machined, through suitable PROCESS FOR TREATMENT
Or formula adjustment can apply to some special dimension.But, traditional metal heat-conducting filler easily corrodes, and then impact is compound
The performance of material, and the heat conductivility of metal oxide filler is poor, it is impossible to meet the demand to heat radiation for the modern industry.In recent years
Coming, compared with traditional material, New Two Dimensional graphene carbon material is owing to having excellent heat conductivility and good anticorrosive
Ability, has been considered as the filler with application potential quality.But, actually used in, add the heat-conducting plastic of two-dimensional graphene
Heat conduction increase rate can not show a candle to expected.Research discovery, during use, two-dimensional graphene makes composite due to phenomenons such as reunions
Heat conductivility by strong influence.This is owing to having very strong Van der Waals force or dangling bond effect between two-dimensional graphene
Power.Therefore, in order to solve this problem, two-dimensional graphene is built into the three-dimensional grapheme of self supporting structure by us.Compared to
Two-dimensional graphene and conventional filler, three-dimensional grapheme has the three-dimensional net structure of self-supporting, can prevent material originally well
The reunion of body；Compared to grapheme material, this filler can disperse very well in plastic substrate, improves the thermal conductivity of plastic substrate
Energy.
Content of the invention
The technical problem to be solved is to overcome heat-conducting plastic in prior art to there is being not enough to of heat conductivility
And the feature such as the perishable hydraulic performance decline causing of conventional filler, a kind of heat conduction composite plastics material filling three-dimensional grapheme is provided
Preparation method.
Another object of the present invention is to provide the heat-conducting plastic composite of filling three-dimensional grapheme prepared by said method.Should
Material has excellent heat conductivility, also has good corrosion resistance simultaneously.
Still a further object of the present invention is to provide the high heat conduction composite plastics material of above-mentioned filling three-dimensional grapheme at heat exchanger
Application in field.
Above-mentioned purpose of the present invention is to be achieved by the following technical programs：
The preparation method of a kind of high heat conduction composite plastic filling three-dimensional grapheme, comprises the following specific steps that：
S1. three-dimensional grapheme and surfactant are mixed by mechanical agitation in proportion, after being dried, obtain surface
Modified three-dimensional grapheme；
S2. plastic substrate is heated to 160～200 DEG C, prepares the plastic substrate of molten condition；
The molten plastic matrix that the three-dimensional grapheme of the surface modification S3. preparing S1 and S2 prepare uniformly mixes, and prepares
Uniform plastic substrate/three-dimensional grapheme mixture；
S4. plastic substrate/three-dimensional grapheme the mixture preparing S3 carries out pressing mold, uses pressure to be 10～20MPa,
To the three-dimensional grapheme height heat conduction composite plastic filling surface modification.
Preferably, three-dimensional grapheme described in step S1 is spherical, and the particle diameter of described three-dimensional grapheme is 200～500nm.
Preferably, surfactant described in step S1 is neopelex, stearic acid or fatty glyceride
In one or more.
Preferably, the surfactant that step S1 is added is (1～10) with the mass ratio of three-dimensional grapheme:100.
Preferably, plastic substrate described in step S2 be polypropylene, polystyrene, Merlon, acrylonitrile-butadiene-
Any one in styrol copolymer, polyethylene or Research of Grafting Malaic Anhydride Onto Polyethylene.
Preferably, the plastic substrate described in step S3 and the mass ratio of the three-dimensional grapheme of surface modification are 100:(1～
300).
Preferably, incorporation time described in step S3 is 10～30min.
Said method prepare filling three-dimensional grapheme high heat conduction composite plastic and in heat exchanger field should
With also in protection scope of the present invention.
The present invention, using the three-dimensional grapheme of three-dimensional porous network structure as filler, constructs high heat-conducting plastic composite.
Utilize the heat transfer pathway of the self-supporting porous network structure that three-dimensional graphite has and various dimensions, join energy in plastic substrate
Being prevented effectively from Graphene to reunite, the intrinsic high thermal conductivity making Graphene have efficiently plays, and recycling three-dimensional grapheme has
The advantage of various dimensions heat transfer pathway, thus be effectively improved the heat conductivility of thermal interfacial material.
Owing to surfactant one end is the hydrophobic grouping of long-chain carbochain, the other end is hydrophilic radical.With three-dimensional grapheme
After mixing, three-dimensional grapheme surface is wrapped up by its hydrophobic grouping.When three-dimensional grapheme is dispersed in water, hydrophilic radical with
Aqueous phase contacts, so that three-dimensional grapheme can be dispersed in water, plays the effect of surface modification.
Compared with prior art, the invention have the advantages that：
1. heat filling used in the present invention is innovated on traditional heat filling, employs a kind of novel
Three-dimensional grapheme material prepares thermal interfacial material as heat filling.The three-dimensional grapheme of surface modification is excellent at reservation Graphene
Thermal conductivity and under conditions of superhigh specific surface area, because of its three-dimensional crosslinked network structure, and the feature of self-supporting enables it to
Enough well prevent the reunion of self.As filler can well in plastic substrate disperse, again due to its macroscopic view micron and
The feature of microcosmic nanometer so that this filler can form thermal conducting path at loading 300wt.%, and reaching exceeding of heat conduction oozes threshold values,
Improving the heat conductivility of plastic substrate, ratio improves 8 times when being not added with.Loading phase with conventional filler 800～1000wt.%
Ratio, three-dimensional grapheme heat filling can be issued to good enhanced thermal conduction effect at low loading.This is due to three-dimensional graphite
Alkene has superhigh specific surface area and extremely-low density, thus only needs less amount of conductive additive just can form good three-dimensional and lead
Ther mal network.
2. three-dimensional grapheme prepared by the present invention has excellent heat conductivility and corrosion resistance, with conventional metals and
Metal oxide filler is compared, and can guarantee that during the heat conductivility Long-Time Service of composite unaffected.
Brief description
Fig. 1 is the SEM figure of the three-dimensional grapheme used by embodiment 1～12.
Fig. 2 is the polystyrene used by polystyrene and embodiment 8～12/three-dimensional grapheme height heat conduction composite plastic
Heat conductivility.
Detailed description of the invention
Further illustrate present disclosure below in conjunction with Figure of description and specific embodiment, but should not be construed as to this
The restriction of invention.If not specializing, conventional hand that technological means used in embodiment is well known to those skilled in the art
Section.Unless stated otherwise, the present invention uses reagent, method and apparatus are the art conventional reagent, method and apparatus.
The preparation of embodiment 1 three-dimensional grapheme
Three-dimensional grapheme used in the present invention, mostly in reference to the preparation method of patent 201210455913.3, specifically walks
Rapid as follows：
1. the KOH solution that macropore acidulous acrylic acid's cationic ion-exchange resin concentration is 1mol/L is pre-processed 12h；
2. being dissolved in 0.005mol nickel acetate in 100ml deionized water, the macropore adding pretreatment in 10g step 1 is weak
Acidic acrylate's cationic ion-exchange resin, magnetic agitation 6h, filters post-drying；
3. macropore acidulous acrylic acid's cationic ion-exchange resin of the pretreatment in step 2 is joined the second containing 40gKOH
In alcoholic solution, stirring and drying；
4. it is placed in tube furnace is warming up to 850 DEG C by step 3 obtains product, be incubated 2h；
5. by the HCl process of the product of step 4, after be washed with deionized water to neutrality, be dried, i.e. obtain three-dimensional grapheme powder
End.
The preparation of embodiment 2 surface modification three-dimensional grapheme
The neopelex of 0.1g and the three-dimensional grapheme of 1g are mixed, mechanical agitation 20min, obtain after being dried
The three-dimensional grapheme of surface modification.
The preparation of embodiment 3 polyethylene/three-dimensional grapheme height heat conduction composite plastic
S1. the polyethylene of 1g is heated to 200 DEG C, prepares the polyethylene of molten state；
S2. surface modification three-dimensional grapheme powder filler as prepared by embodiment 2 step for the 3g is joined step S1 institute
In the molten polyethylene being formed, by three-dimensional grapheme and base polyethylene mechanical agitation 30min of surface modification so that poly-second
Thiazolinyl body mixes with three-dimensional grapheme uniform filling, and the gross mass of filler should be the 300wt.% of matrix plastic；
S3. carrying out injection moulding to uniform mixture, using pressure to be 20MPa, hot pressing temperature is 200 DEG C, during hot pressing
Between be 5min, obtain polyethylene/three-dimensional grapheme height heat conduction composite plastic.
Embodiment 4
The preparation of surface modification three-dimensional grapheme is different from embodiment 2 to be, the surfactant being used is stearic acid.
The preparation of polyethylene/three-dimensional grapheme height heat conduction composite plastic is different from embodiment 3 to be, described in step S1, heating-up temperature is
190℃；Surface modification three-dimensional grapheme powder described in step S2 is 2.5g, the three-dimensional grapheme of described surface modification and
Vinyon incorporation time is 25min, and the gross mass of the three-dimensional grapheme powder filler of surface modification is that base polyethylene is moulded
The 250wt.% of material；Hot pressing temperature described in step S3 is 180 DEG C, and the time of colding pressing is 6min.
Embodiment 5
The preparation of surface modification three-dimensional grapheme is different from embodiment 2 to be, the surfactant being used is aliphatic acid
Glyceride.The preparation of polyethylene/three-dimensional grapheme height heat conduction composite plastic is different from embodiment 3 to be, adds described in step S1
Hot temperature is 180 DEG C；Surface modification three-dimensional grapheme powder described in step S2 is 2g, and the gross mass of filler is matrix plastic
200wt.%；Hot pressing temperature described in step S3 is 180 DEG C.
Embodiment 6
Different from embodiment 3 being, heating-up temperature described in step S1 is 180 DEG C；Surface modification described in step S2
Three-dimensional grapheme powder is 0.5g, and the gross mass of filler is the 50wt.% of matrix plastic；Hot pressing temperature described in step S3 is 180
℃.
Embodiment 7
Different from embodiment 3 being, heating-up temperature described in step S1 is 180 DEG C；Surface modification described in step S2
Three-dimensional grapheme powder is 0.1g, and the gross mass of filler is the 10wt.% of matrix plastic；Hot pressing temperature described in step S3 is 180
℃.
Embodiment 8
Different from embodiment 3 being, plastic substrate described in step S1 is polystyrene；Surface modification described in step S2
Three-dimensional grapheme is 0.5g, and the gross mass of filler is the 50wt.% of matrix plastic；Hot pressing temperature described in step S3 is 180 DEG C.
Embodiment 9
Different from embodiment 8 being, the surface modification three-dimensional grapheme powder described in step S2 is 1g, the gross mass of filler
100wt.% for matrix plastic.
Embodiment 10
Different from embodiment 8 being, the surface modification three-dimensional grapheme powder described in step S2 is 1.5g, total matter of filler
The 150wt.% that amount is matrix plastic.
Embodiment 11
Different from embodiment 8 being, the surface modification three-dimensional grapheme powder described in step S2 is 2g, the gross mass of filler
200wt.% for matrix plastic.
Embodiment 12
Different from embodiment 8 being, the surface modification three-dimensional grapheme powder described in step S2 is 3g, the gross mass of filler
300wt.% for matrix plastic.
Using Hot Disk thermal constant tester to carry out the measurement of thermal conductivity to the heat-conducting plastic sample of preparation, table 1 is poly-
The thermal conductivity of the polyethylene prepared by ethene and embodiment 3～7/three-dimensional grapheme height heat conduction composite plastic.Its results detailed in
Shown in table 1.It can be seen that, the thermal conductivity of composite plastic significantly improves, result table with the increase of three-dimensional grapheme loading
Bright three-dimensional grapheme can effectively improve the thermal conductivity of plastic substrate.Fig. 2 is prepared by polystyrene and embodiment 8～12
The heat conductivility of polystyrene/three-dimensional grapheme height heat conduction composite plastic.From figure 2 it can be seen that with polyethylene composite plastic
Equally, with the raising of loading, the thermal conductivity of composite plastic also improves therewith, shows that this material is applicable to multiple different moulding
Material matrix, has the feature of applied range.Meanwhile, compared with the loading of conventional metals filler 800～1000wt.%, three
Dimension Graphene heat filling can be issued to good enhanced thermal conduction effect at low loading.
Table 1. polyethylene and the thermal conductivity of embodiment 3～7 polyethylene/three-dimensional grapheme height heat conduction composite plastic
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, change, modification, replacement, combination and the simplification made under other any Spirit Essence without departing from the present invention and principle,
All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. the preparation method of the high heat conduction composite plastic filling three-dimensional grapheme, it is characterised in that include following concrete step
Suddenly：
S1. three-dimensional grapheme and surfactant are mixed by mechanical agitation in proportion, after being dried, obtain surface modification
Three-dimensional grapheme；
S2. plastic substrate is heated to 160～200 DEG C, prepares the plastic substrate of molten condition；
The molten plastic matrix that the three-dimensional grapheme of the surface modification S3. preparing S1 and S2 prepare uniformly mixes, and prepares uniformly
Plastic substrate/three-dimensional grapheme mixture；
S4. plastic substrate/three-dimensional grapheme the mixture preparing S3 carries out pressing mold, and pressure is 10～20MPa, obtains filling three
The high heat conduction composite plastic of dimension Graphene.
2. preparation method according to claim 1, it is characterised in that three-dimensional grapheme described in step S1 is spherical, institute
The particle diameter stating three-dimensional grapheme is 200～500nm.
3. preparation method according to claim 1, it is characterised in that surfactant described in step S1 is dodecyl
One or more in benzene sulfonic acid sodium salt, stearic acid or fatty glyceride.
4. preparation method according to claim 1, it is characterised in that the surfactant that step S1 is added and three-dimensional stone
The mass ratio of ink alkene is (1～10):100.
5. preparation method according to claim 1, it is characterised in that plastic substrate described in step S2 is polypropylene, gathers
Any in styrene, Merlon, acrylonitrile-butadiene-styrene copolymer, polyethylene or Research of Grafting Malaic Anhydride Onto Polyethylene
A kind of.
6. preparation method according to claim 1, it is characterised in that the plastic substrate described in step S3 and surface modification
The mass ratio of three-dimensional grapheme be 100:(1～300).
7. preparation method according to claim 1, it is characterised in that the time of mixing described in step S3 is 10～
30min.
8. the high heat conduction composite plastic of the filling three-dimensional grapheme that a kind is prepared by method described in any one of claim 1-7.
9. application in heat exchanger field for the high heat conduction composite plastic of the filling three-dimensional grapheme described in claim 8.
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| CN201610707278.1A CN106432861A (en) | 2016-08-23 | 2016-08-23 | High-thermal-conductive composite plastics filled with three-dimensional graphene and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201021A (en) * | 2018-11-26 | 2019-01-15 | 西安科技大学 | A kind of gas adsorption agent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992306A (en) * | 2012-11-14 | 2013-03-27 | 中山大学 | Graphitized carbon with high specific surface area and hierarchical pores and preparation method thereof |
| CN103213980A (en) * | 2013-05-13 | 2013-07-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of three-dimensional graphene or composite system thereof |
-
2016
- 2016-08-23 CN CN201610707278.1A patent/CN106432861A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992306A (en) * | 2012-11-14 | 2013-03-27 | 中山大学 | Graphitized carbon with high specific surface area and hierarchical pores and preparation method thereof |
| CN103213980A (en) * | 2013-05-13 | 2013-07-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of three-dimensional graphene or composite system thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201021A (en) * | 2018-11-26 | 2019-01-15 | 西安科技大学 | A kind of gas adsorption agent and preparation method thereof |
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