CN110386776A - A kind of novel heat-conducting plastics and preparation method thereof - Google Patents
A kind of novel heat-conducting plastics and preparation method thereof Download PDFInfo
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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Abstract
A kind of novel heat-conducting plastics and preparation method thereof, belong to field of material technology.The heat-conducting plastic is made of resin, graphene and thermally conductive toughening filler, the mass percentage content of the resin, graphene and thermally conductive toughening filler are as follows: resin 2~70%, graphene 0.0001~10%, thermally conductive toughening filler 20~95%.The novel heat-conducting plastics-production that the present invention obtains is at low cost and can take into account thermally conductive and insulation performance height.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of novel heat-conducting plastics and preparation method thereof.
Background technique
LED has energy conservation and environmental protection, small in size, light emission color temperature is friendly, the service life is long etc. as a kind of novel energy-conserving light source product
Advantage is widely applied in the every field for producing and living.The work temperature in the light extraction efficiency of LED and service life and chip
Degree has direct relationship, if cannot effectively radiate, LED internal temperature can be made to increase, the luminous efficiency of LED is caused to reduce,
The service life of LED chip is directly affected, therefore heat dissipation is great power LED key application place.Due to plastics design freedom it is high,
Easily molded processing, light weight and it is at low cost etc. the advantages of, people are by the lamps and lanterns manufacture of plastic applications to LED industry, so
And the thermal coefficient very little of most of plastics, influence their application.Improve the approach of plastics thermal conductivity: first is that synthetic material sheet
Body is exactly the resin matrix with high thermal conductivity, such as polyaniline, polypyrrole with Thermal conductivity, but such material
There is a problem of expensive；Second is that being realized using having high thermal conductivity filler filled plastics, the filler generallyd use has metal
Powder filler such as aluminium powder, copper powder etc., metal oxide filler such as aluminium oxide, bismuth oxide, beryllium oxide, magnesia and zinc oxide etc.,
Inorganic non-metallic filler such as graphite, silicon carbide, glass fibre etc., such as using metal oxide, silicon carbide insulating packing as filling out
The thermal coefficient of product is made between 2~4 W/mK (ZL200510101700.0) in material.But currently, most of thermally conductive modeling
Expect the problems such as heating conduction is not high enough, and mechanical performance is unstable or heating conduction is fine but stability is bad, on the high side still
So annoying LED illumination manufacturing enterprise.In recent years, it has been found that graphene is that one kind is arranged simultaneously by carbon atom according to hexagon
Special two-dimensional material made of interconnection, have high conductivity, superelevation mechanical strength, extra specific surface area, high thermal conductivity,
The extremely excellent comprehensive physical performance such as high transparency can be used to prepare high sensor, touch display screen, super
The various news device such as battery and high performance solar batteries has important answer in various fields such as electronics, space flight military project, new energy
With value.Thus, improve heat-conducting plastic performance with excellent properties such as the high thermal conductivity of graphene and superior mechanical intensity
As recent hot spot concerned by people, but the high cost of graphene itself and the usage in heat-conducting plastic product still lack research
Graphene is limited in the extensive use in heat-conducting plastic field.
Grown rapidly as LED illuminates application, and move towards consuming public, the automation size production of lamps and lanterns product, at
The requirements such as this control, safety, lightweight also increasingly improve, and the market demand of heat-conducting plastic also increases year by year.Therefore, seek
It is a kind of graphene to be used and the novel heat-conducting plastics-production skill that production cost is low, thermally conductive and high insulation performance can be taken into account
Art has very big commercial value.
Summary of the invention
In view of the problems of the existing technology, it is an object of the invention to design to provide a kind of to obtain life with graphene
It produces at low cost and the thermally conductive technical solution with the high novel heat-conducting plastics of insulation performance and preparation method thereof can be taken into account.
A kind of novel heat-conducting plastics, it is characterised in that the heat-conducting plastic is filled out by resin, graphene and thermally conductive toughening
Material composition, the mass percentage content of the resin, graphene and thermally conductive toughening filler are as follows:
Resin 2~70%
Graphene 0.0001~10%
Thermally conductive toughening filler 20~95%；
The resin is polyamide, polycarbonate, polybutylene terephthalate (PBT), polyethylene terephthalate, gathers
Formaldehyde, polyphenylene oxide, acrylonitrile-butadiene-styrene (ABS), polypropylene, polyphenylene sulfide, polysulfones, polyethylene, poly-methyl methacrylate
One of ester, polytetrafluoroethylene (PTFE), polystyrene, polyvinyl chloride or any several mixture；
The thermally conductive toughening filler is quartz, mica, diopside, wollastonite, amphibole, calcite, bauxite, feldspar, weight crystalline substance
Stone, serpentine, lime stone, gypsum, nepheline, talcum, fluorite, leucite, dolomite, marble, mullite, one in kaolinite
Kind or any several mixture.
A kind of novel heat-conducting plastics, it is characterised in that the matter of the resin, graphene and thermally conductive toughening filler
Measure degree are as follows:
Resin 5~65%
Graphene 0.001~8%
Thermally conductive toughening filler 30~91%.
A kind of novel heat-conducting plastics, it is characterised in that the thermal conductivity of the novel heat-conducting plastics is 2.5~4.5 W/
m·K。
The preparation method of a kind of novel heat-conducting plastics, it is characterised in that comprise the following steps that:
(1) graphene of the formula ratio is added in water or/and organic solvent and forms graphene solution；
(2) the thermally conductive toughening filler of the formula ratio is added in this graphene solution after mixing fills out graphene with thermally conductive toughening
Material occurs interaction combination and obtains graphene/thermally conductive toughening filler complex mixed liquor；
(3) after this graphene/thermally conductive toughening filler complex mixed liquor stratification, by resulting graphene/thermally conductive toughening
Filler complex mixed liquor removes solvent to get graphene/thermally conductive toughening filler composite materials are arrived；
(4) heat-conducting plastic product is made using plastics molding process after mixing this composite material with the resin of the formula ratio.
A kind of preparation method of novel heat-conducting plastics, it is characterised in that graphene solution in the step (1)
Are as follows: the graphene solution formed in water or/and organic solvent is added in graphene or is directly obtained by graphene preparation method
Graphene solution, the graphene preparation method is oxidation-reduction method, mechanical stripping method, liquid phase stripping method, graft process, micro-
Wave method, solvent-thermal method.
The preparation method of a kind of novel heat-conducting plastics, it is characterised in that add graphene in the step (1)
The surface tension viscosity parameter value for entering the graphene solution formed in water or/and organic solvent is 8~60000, the table
Surface tension and viscosity common definition of the face tension viscosity parameter by solution, the numerical value of the surface tension viscosity parameter
=solution surface tension numerical value × solution viscosity values, surface tension numerical value is as unit of mN/m, and viscosity is as unit of mPas, table
Face tension value range is 21~70, and viscosity value range is 0.2~1200.
A kind of preparation method of novel heat-conducting plastics, it is characterised in that graphene in the step (3)/thermally conductive
Surface tension viscosity parameter value after toughening filler mixed liquor stratification is 22~70000, and the surface tension is viscous
Spend surface tension and viscosity common definition of the parameter by mixed liquor, numerical value=mixed liquor of the surface tension viscosity parameter
Surface tension numerical value × viscosity of mixed liquid value, surface tension numerical value is as unit of mN/m, and viscosity is as unit of mPas, surface
Power value range is 30~73, and viscosity value range is 0.5~1500.
A kind of preparation method of novel heat-conducting plastics, it is characterised in that graphene in the step (3)/thermally conductive
Toughening filler mixed liquor removal solvent method is that centrifugation, suction filtration, heating, drying, freeze-drying, spray drying or other commonly use are removed
One of solvent means are a variety of.
A kind of preparation method of novel heat-conducting plastics, it is characterised in that plastic shaping work in the step (4)
Skill injection moulding, extrusion molding, compression moulding, blow molding or cast molding.
A kind of novel heat-conducting plastics are as thermally conductive and/or mechanics toughening reinforcing material application.
It is compared with existing technology, the invention has the following advantages:
1) Good All-around Property of graphene can promote the overall performance of conductive plastic material, but face cost and be substantially increased
The problem of, various mineral materials have the advantage of low cost, but performance boost is limited, and the present invention promotes the two combined use
The heating conduction of conductive plastic material, cost performance are high.
2) compared to being simply directly stirred graphene powder with mineral material, various mines are utilized in the method for the present invention
Object can enable graphene to pass through in a solvent with mineral material in water or/and other organic solvents in the characteristic of surface electrification
Charge interaction is efficiently combined in molecule rank and avoids the reunion of graphene powder together and mixing is uneven etc. asks
Topic, so as to play optimal modified gain effect, and is greatly decreased the additive amount of graphene simultaneously, makes the graphite obtained
Alkene/mineral composite has splendid cost performance, and then can reduce the application cost of the modified heat-conducting plastic of graphene.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1
Content calculates by mass percentage, takes 5% graphene to be added to the water and is made into graphene aqueous solution, and is added into container,
(surface tension viscosity) parameter value for measuring the solution is 50, then 60% thermally conductive toughening filler (wollastonite and amphibole powder) is taken to add
Enter to make after mixing graphene and thermally conductive toughening filler to occur to interact and combined to obtain graphene/thermally conductive in this graphene aqueous solution
Toughening filler complex mixed liquor measures after this graphene/thermally conductive toughening filler complex mixed liquor stands layering in 5 minutes
Mixed liquor (surface tension viscosity) parameter value is 73, and resulting graphene/thermally conductive toughening filler complex mixed liquor is centrifuged
Water removal is gone to be placed on 80 DEG C of baking oven heating, dryings to get graphene/thermally conductive toughening filler composite materials are arrived.
Content calculates by mass percentage, takes 35% resin (polycarbonate 10%, polyphenylene oxide 5% and polyamide 20%) and above-mentioned
Graphene/thermally conductive toughening filler composite materials are placed in mixing and blending machine after mixing, by double screw extruder extruding pelletization,
Obtain a kind of heat-conducting plastic product of the invention.After gained heat-conducting plastic is melted and molded, measured with heat conduction coefficient tester
The thermal coefficient of sample is 3.5 W/mK
Thermally conductive toughening filler uses quartz, mica, diopside, wollastonite, amphibole, calcite, bauxite, length in the embodiment 1
Stone, barite, serpentine, lime stone, gypsum, nepheline, talcum, fluorite, leucite, dolomite, marble, mullite, kaolinite
One of stone or any several mixture, resin use polyamide, polycarbonate, polybutylene terephthalate (PBT), gather
Ethylene glycol terephthalate, polyphenylene oxide, acrylonitrile-butadiene-styrene (ABS), polypropylene, polyphenylene sulfide, polysulfones, gathers polyformaldehyde
One of ethylene, polymethyl methacrylate, polytetrafluoroethylene (PTFE), polystyrene, polyvinyl chloride or any several mixture,
It finally can also reach same as Example 1 or similar technical effect.
For solvent without water is confined to, the organic solvent used meets the following conditions in the embodiment 1: mixed with graphene
Solution surface tension value range after conjunction is 21~70mN/m, and solution viscosity value range is 0.2~1200mPas, and
Stone graphene/thermally conductive toughening filler mixed liquor surface tension value range is 30~73mN/m, and solution viscosity value range is 0.5
~1500mPas.
Embodiment 2
Content calculates by mass percentage, takes 2% graphene to be added in ethyl alcohol and is made into graphene ethanol solution, and is added into appearance
In device, (surface tension viscosity) parameter value for measuring the solution is 13, then take 65% thermally conductive toughening filler (barite, gypsum and
Calcite) be added in this graphene ethanol solution mix after so that graphene and thermally conductive toughening filler is occurred to interact and is combined to obtain
Graphene/thermally conductive toughening filler complex mixed liquor stands 10 minutes to this graphene/thermally conductive toughening filler complex mixed liquor
After layering, measuring mixed liquor (surface tension viscosity) parameter value is 25, by resulting graphene/thermally conductive toughening filler complex
Mixed liquor filtering removal upper layer ethyl alcohol is placed on 70 DEG C of baking oven heating, dryings to get graphene/thermally conductive toughening filler composite wood is arrived
Material.
By mass percentage content calculate, take 33% resin (polypropylene 13% and polybutylene terephthalate (PBT) 20%) and
Above-mentioned graphene/thermally conductive toughening filler composite materials are placed in high-speed mixer after mixing, are squeezed out by double screw extruder
It is granulated to get a kind of heat-conducting plastic product of the invention is arrived.After gained heat-conducting plastic is melted and molded, heat conduction coefficient tester is used
The thermal coefficient for measuring sample is 2.5W/mK.
Embodiment 3
Content calculates by mass percentage, takes 8% graphene to be added in glycerol and is made into graphene glycerite, and is added into appearance
In device, (surface tension viscosity) parameter value for measuring the solution is 51000, then takes 50% thermally conductive toughening filler (mica, saturating brightness
Stone, feldspar, serpentine, lime stone, talcum and mullite) be added in this graphene glycerite mix after make graphene with it is thermally conductive
Toughening filler occurs interaction combination and obtains graphene/thermally conductive toughening filler complex mixed liquor, to this graphene/thermally conductive increasing
After tough filler complex mixed liquor stands layering in 15 minutes, measuring mixed liquor (surface tension viscosity) parameter value is 62000, will
Resulting graphene/thermally conductive toughening filler complex mixed liquor is centrifuged and filters after removal solvent to arrive graphene/thermally conductive increasing
Tough filler composite materials.
Content calculates by mass percentage, takes 41% resin (acrylonitrile-butadiene-styrene (ABS) 15%, polyformaldehyde 21% and poly-
Ethylene 5%) and above-mentioned graphene/thermally conductive toughening filler composite materials be placed in high-speed mixer after mixing, squeezed by twin-screw
Out machine extruding pelletization to get arrive a kind of heat-conducting plastic product of the invention.After gained heat-conducting plastic is melted and molded, with thermally conductive system
The thermal coefficient of number tester measurement sample is 4.2 W/mK.
Embodiment 4
Content calculates by mass percentage, takes 3% graphene to be added to the water and is made into graphene aqueous solution, and is added into container,
(surface tension viscosity) parameter value for measuring the solution is 40, then take 70% thermally conductive toughening filler (quartz, lime stone, gypsum,
Nepheline and leucite) be added in this graphene aqueous solution mix after so that graphene and thermally conductive toughening filler is occurred to interact and is combined
Graphene/thermally conductive toughening filler complex mixed liquor is obtained, stands 3 to this graphene/thermally conductive toughening filler complex mixed liquor
After minute layering, measuring mixed liquor (surface tension viscosity) parameter value is 70, and resulting graphene/thermally conductive toughening filler is answered
Fit mixed liquor centrifugation goes water removal to be placed on 80 DEG C of baking oven heating, dryings to get graphene/thermally conductive toughening filler composite materials are arrived.
Content calculates by mass percentage, takes 27% resin (polyethylene terephthalate 2%, poly-methyl methacrylate
Ester 15% and polypropylene 10%) and above-mentioned graphene/thermally conductive toughening filler composite materials be placed in high-speed mixer after mixing,
By double screw extruder extruding pelletization to get to a kind of heat-conducting plastic product of the invention.Gained heat-conducting plastic is melted and molded
It afterwards, is 4.5 W/mK with the thermal coefficient of heat conduction coefficient tester measurement sample.
Embodiment 5
Content calculates by mass percentage, and 8% graphene (graphene aqueous solution that liquid phase method is directly prepared) is taken to be added to the container,
(surface tension viscosity) parameter value for measuring the solution is 43, then takes 45% thermally conductive toughening filler (barite, serpentine, stone
Cream, talcum, fluorite, dolomite, marble, kaolinite) be added in this graphene aqueous solution mix after make graphene and thermally conductive increasing
Tough filler occurs interaction combination and obtains graphene/thermally conductive toughening filler complex mixed liquor, to this graphene/thermally conductive toughening
After filler complex mixed liquor stands layering in 6 minutes, measuring mixed liquor (surface tension viscosity) parameter value is 75, will be resulting
Graphene/thermally conductive toughening filler complex mixed liquor filter off water removal be placed on 80 DEG C of baking oven heating, dryings to get to graphene/
Thermally conductive toughening filler composite materials.
Content calculates by mass percentage, takes 47% resin (polyformaldehyde 20%, acrylonitrile-butadiene-styrene (ABS) 7%, poly- second
Alkene 10% and polyvinyl chloride 10%) and above-mentioned graphene/thermally conductive toughening filler composite materials be placed in high-speed mixer be uniformly mixed
Afterwards, by double screw extruder extruding pelletization to get to a kind of heat-conducting plastic product of the invention.Gained heat-conducting plastic is fused into
After type, the thermal coefficient with heat conduction coefficient tester measurement sample is 3.4 W/mK.
Embodiment 6
Content calculates by mass percentage, takes 1% graphene to be added to the water and is made into graphene aqueous solution, and is added into container,
(surface tension viscosity) parameter value for measuring the solution is 55, then takes 75% thermally conductive toughening filler (mica, wollastonite, Fang Xie
Stone, serpentine, gypsum, talcum, fluorite, marble and kaolinite) be added in this graphene aqueous solution mix after make graphene with
Interaction occur for thermally conductive toughening filler combine to obtain graphene/thermally conductive toughening filler complex mixed liquor, to this graphene/lead
After hot toughening filler complex mixed liquor stands layering in 5 minutes, measuring mixed liquor (surface tension viscosity) parameter value is 63, will
Resulting graphene/thermally conductive toughening filler complex mixed liquor centrifugation goes water removal to be placed on 80 DEG C of baking oven heating, dryings to get arriving
Graphene/thermally conductive toughening filler composite materials.
Content calculates by mass percentage, takes 24% resin (polyethylene terephthalate 4% and polypropylene 20%) and upper
It states graphene/thermally conductive toughening filler composite materials to be placed in high-speed mixer after mixing, be made by double screw extruder extrusion
Grain to get arrive a kind of heat-conducting plastic product of the invention.After gained heat-conducting plastic is melted and molded, surveyed with heat conduction coefficient tester
The thermal coefficient of random sample product is 2.8 W/mK.
Embodiment 7
Content calculates by mass percentage, takes 0.001% graphene to be added to the water and is made into graphene aqueous solution, and is added into appearance
In device, (surface tension viscosity) parameter value for measuring the solution is 55, then takes 74.999% thermally conductive toughening filler (mica, silicon ash
Stone, calcite, serpentine, gypsum, talcum, fluorite, marble and kaolinite) be added in this graphene aqueous solution mix after make stone
Black alkene occurs interaction with thermally conductive toughening filler and is combined to obtain graphene/thermally conductive toughening filler complex mixed liquor, to this stone
After black alkene/thermally conductive toughening filler complex mixed liquor stands layering in 5 minutes, mixed liquor (surface tension viscosity) parameter value is measured
It is 63, goes water removal to be placed on 80 DEG C of baking oven heating, dryings resulting graphene/thermally conductive toughening filler complex mixed liquor centrifugation,
Obtain graphene/thermally conductive toughening filler composite materials.
Content calculates by mass percentage, takes 25% resin (polyethylene terephthalate 5% and polypropylene 20%) and upper
It states graphene/thermally conductive toughening filler composite materials to be placed in high-speed mixer after mixing, be made by double screw extruder extrusion
Grain to get arrive a kind of heat-conducting plastic product of the invention.After gained heat-conducting plastic is melted and molded, surveyed with heat conduction coefficient tester
The thermal coefficient of random sample product is 2.5 W/mK.
Claims (10)
1. a kind of novel heat-conducting plastics, it is characterised in that the heat-conducting plastic is made of resin, graphene and thermally conductive toughening filler, institute
The mass percentage content of the resin, graphene and thermally conductive toughening filler stated are as follows:
Resin 2~70%
Graphene 0.0001~10%
Thermally conductive toughening filler 20~95%；
The resin is polyamide, polycarbonate, polybutylene terephthalate (PBT), polyethylene terephthalate, gathers
Formaldehyde, polyphenylene oxide, acrylonitrile-butadiene-styrene (ABS), polypropylene, polyphenylene sulfide, polysulfones, polyethylene, poly-methyl methacrylate
One of ester, polytetrafluoroethylene (PTFE), polystyrene, polyvinyl chloride or any several mixture；
The thermally conductive toughening filler is quartz, mica, diopside, wollastonite, amphibole, calcite, bauxite, feldspar, weight crystalline substance
Stone, serpentine, lime stone, gypsum, nepheline, talcum, fluorite, leucite, dolomite, marble, mullite, one in kaolinite
Kind or any several mixture.
2. a kind of novel heat-conducting plastics as described in claim 1, it is characterised in that resin, graphene and the thermally conductive toughening
The mass percentage content of filler are as follows:
Resin 5~65%
Graphene 0.001~8%
Thermally conductive toughening filler 30~91%.
3. a kind of novel heat-conducting plastics as described in claim 1, it is characterised in that the thermal conductivity of the novel heat-conducting plastics is 2.5
~4.5 W/mK.
4. a kind of preparation method of novel heat-conducting plastics as described in claims 1 or 2 or 3, it is characterised in that including following work
Skill step:
(1) graphene of the formula ratio is added in water or/and organic solvent and forms graphene solution；
(2) the thermally conductive toughening filler of the formula ratio is added in this graphene solution after mixing fills out graphene with thermally conductive toughening
Material occurs interaction combination and obtains graphene/thermally conductive toughening filler complex mixed liquor；
(3) after this graphene/thermally conductive toughening filler complex mixed liquor stratification, by resulting graphene/thermally conductive toughening
Filler complex mixed liquor removes solvent to get graphene/thermally conductive toughening filler composite materials are arrived；
(4) heat-conducting plastic product is made using plastics molding process after mixing this composite material with the resin of the formula ratio.
5. a kind of preparation method of novel heat-conducting plastics as claimed in claim 4, it is characterised in that stone in the step (1)
Black alkene solution are as follows: the graphene solution formed in water or/and organic solvent is added in graphene or passes through graphene preparation method
The graphene solution directly obtained, the graphene preparation method be oxidation-reduction method, mechanical stripping method, liquid phase stripping method,
Graft process, microwave method, solvent-thermal method.
6. a kind of preparation method of novel heat-conducting plastics as claimed in claim 4, it is characterised in that will in the step (1)
The surface tension viscosity parameter value that the graphene solution formed in water or/and organic solvent is added in graphene is 8~60000,
Surface tension and viscosity common definition of the surface tension viscosity parameter by solution, the surface tension viscosity ginseng
Several numerical value=solution surface tension numerical value × solution viscosity values, as unit of mN/m, viscosity is surface tension numerical value with mPas
Unit, surface tension value range are 21~70, and viscosity value range is 0.2~1200.
7. a kind of preparation method of novel heat-conducting plastics as claimed in claim 4, it is characterised in that stone in the step (3)
Surface tension viscosity parameter value after black alkene/thermally conductive toughening filler mixed liquor stratification is 22~70000, the surface
Surface tension and viscosity common definition of the tension viscosity parameter by mixed liquor, the numerical value of the surface tension viscosity parameter
=mixed liquor surface tension numerical value × viscosity of mixed liquid value, for surface tension numerical value as unit of mN/m, viscosity is single with mPas
Position, surface tension value range are 30~73, and viscosity value range is 0.5~1500.
8. a kind of preparation method of novel heat-conducting plastics as claimed in claim 4, it is characterised in that stone in the step (3)
Black alkene/thermally conductive toughening filler mixed liquor removal solvent method be centrifugation, suction filtration, heating, drying, freeze-drying, spray drying or its
It is common except one of solvent means or a variety of.
9. a kind of preparation method of novel heat-conducting plastics as claimed in claim 4, it is characterised in that modeling in the step (4)
Expect moulding process injection moulding, extrusion molding, compression moulding, blow molding or cast molding.
10. a kind of novel heat-conducting plastics as claimed in claim 1,2 or 3 are as thermally conductive and/or mechanics toughening reinforcing material
Using.
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