CN103087404B - A kind of Graphene filled polymer based composites and preparation method thereof - Google Patents
A kind of Graphene filled polymer based composites and preparation method thereof Download PDFInfo
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- CN103087404B CN103087404B CN201110337141.9A CN201110337141A CN103087404B CN 103087404 B CN103087404 B CN 103087404B CN 201110337141 A CN201110337141 A CN 201110337141A CN 103087404 B CN103087404 B CN 103087404B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 101
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 229920000642 polymer Polymers 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000007822 coupling agent Substances 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 239000000314 lubricant Substances 0.000 claims abstract description 7
- 229920005992 thermoplastic resin Polymers 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 38
- 238000007731 hot pressing Methods 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 20
- QIQXTHQIDYTFRH-UHFFFAOYSA-N Stearic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 14
- 238000005453 pelletization Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000748 compression moulding Methods 0.000 claims description 8
- 238000010348 incorporation Methods 0.000 claims description 8
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 8
- 239000008188 pellet Substances 0.000 claims description 8
- 238000010008 shearing Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 235000021355 Stearic acid Nutrition 0.000 claims description 7
- 239000010410 layer Substances 0.000 claims description 7
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 7
- 239000002356 single layer Substances 0.000 claims description 7
- 239000008117 stearic acid Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000004793 Polystyrene Substances 0.000 claims description 6
- 229920001155 polypropylene Polymers 0.000 claims description 6
- 229920002223 polystyrene Polymers 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 5
- 235000019359 magnesium stearate Nutrition 0.000 claims description 4
- KREXGRSOTUKPLX-UHFFFAOYSA-N octadecanoic acid;zinc Chemical compound [Zn].CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O KREXGRSOTUKPLX-UHFFFAOYSA-N 0.000 claims description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- CJZGTCYPCWQAJB-UHFFFAOYSA-L Calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- RKISUIUJZGSLEV-UHFFFAOYSA-N N-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 2
- SMYKVLBUSSNXMV-UHFFFAOYSA-J aluminum;tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-J 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 230000001476 alcoholic Effects 0.000 claims 2
- 239000006185 dispersion Substances 0.000 claims 2
- -1 polypropylene Polymers 0.000 claims 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 239000005020 polyethylene terephthalate Substances 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000011031 large scale production Methods 0.000 abstract description 4
- 238000004220 aggregation Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 238000010528 free radical solution polymerization reaction Methods 0.000 abstract description 3
- 238000011068 load Methods 0.000 abstract description 3
- 239000000945 filler Substances 0.000 abstract description 2
- 238000005755 formation reaction Methods 0.000 abstract description 2
- 125000004432 carbon atoms Chemical group C* 0.000 description 6
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 4
- 239000011157 advanced composite material Substances 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 238000002036 drum drying Methods 0.000 description 2
- LNETULKMXZVUST-UHFFFAOYSA-M 1-naphthoate Chemical compound C1=CC=C2C(C(=O)[O-])=CC=CC2=C1 LNETULKMXZVUST-UHFFFAOYSA-M 0.000 description 1
- 206010068052 Mosaicism Diseases 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 210000003765 Sex Chromosomes Anatomy 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004429 atoms Chemical group 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009114 investigational therapy Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Abstract
The invention discloses a kind of Graphene filled polymer based composites, be made up of the component comprising following weight portion: thermoplastic resin 90 99 parts, graphene microchip 0.1 10 parts, coupling agent 0.01 1 parts, lubricant 1 10 parts.The invention also discloses the preparation method of this Graphene filled polymer based composites.Compared with other carbon system filled composite materials, the present invention have easily processing, easy-formation, filler loading is few, raw material sources are wide, the feature such as environmentally friendly.The conductivity of composite material energy of the present invention and excellent thermal conductivity; there is the features such as mechanical property good, good stability of the dimension, good weatherability; compare for using situ aggregation method or solution polymerization process to prepare the technique of Graphene/polymer composites at present, prepare Graphene filled polymer based composites with melt-blending process and there is the advantage producing continuously, being suitable for large-scale production.
Description
Technical field
The present invention relates to technical field of polymer composite materials, particularly relate to a kind of Graphene filled polymer base composite wood
Material and preparation method thereof.
Background technology
Graphene is to be currently known one the thinnest in material, very rigid.Graphene structure on an atomic scale
The most special, as simple substance, the speed that it at room temperature transmits electronics is faster than known conductor.Graphene-structured is highly stable,
Up to now, researcher does not finds the situation having carbon atom to lack in Graphene yet.Connection between each carbon atom in Graphene
The most pliable and the toughest.When applying external mechanical force, the meeting flexural deformation of carbon atom face, so that carbon atom need not be rearranged to adapt to
External force, has also been maintained for Stability Analysis of Structures.The most stable lattice structure makes carbon atom have outstanding electric conductivity.In Graphene
When electronics moves in track, will not scatter because of lattice defect or introducing foreign atom.And interatomic force ten
Dividing strong, at normal temperatures, even if around carbon atom telescopes, in Graphene, electronics experienced interference is the least.
The research of present stage graphene composite material is still at an early stage, and many important problems need further investigation,
The such as preparation of Graphene large-scale, low cost；The scattering problem of Graphene；Graphene and other matrix and system compatible
Sex chromosome mosaicism etc..The technological means of development innovation and route prepare composite based on Graphene, particularly Graphene/polymerization
Thing composite, and then the performance fully developing, utilizing its excellence is to need the problem of solution at present badly.Current both domestic and external a lot
Scholar uses solution polymerization process and situ aggregation method to prepare Graphene/polymer composites, and the operation of these methods is complicated,
Cost intensive, and use melt-blending process the fewest to the relevant report preparing Graphene/polymer composites, hence with this
Kind process is prepared Graphene/polymer composites and is had broad prospects undoubtedly.
Summary of the invention
The present invention be contemplated to solve preparation method that above-mentioned prior art exists complicated and be difficult to scale problem and
Thering is provided a kind of Graphene filled polymer based composites and preparation method thereof, this advanced composite material (ACM) has high conductivity, height
The features such as heat conductivity, strong mechanical performance, loading are few, preparation method is continuous, is suitable for large-scale production.
The purpose of the present invention is achieved through the following technical solutions:
A kind of Graphene filled polymer based composites, is made up of the component comprising following weight portion:
Thermoplastic resin 90-99 part,
Graphene microchip 0.1-10 part,
Coupling agent 0.01-1 part,
Lubricant 1-10 part.
Preferably, described thermoplastic resin is selected from polypropylene (PP), polrvinyl chloride (PVC), polystyrene (PS), gathers benzene
One or more in naphthalate (PET), polybutylene terephthalate (PBT) (PBT).
Preferably, the thickness of described graphene microchip is 5-15nm, is made up of average 10-30 layer single-layer graphene.
Preferably, described coupling agent one in silane coupler, titanate coupling agent or aluminate coupling agent or
Several.
Preferably, one or more in KH-550, NDZ-101, A-171 of described coupling agent.
Preferably, described lubricant is selected from N, N '-ethylene bis stearamide (EBS), stearic acid, zinc stearate, stearic acid
One or more in calcium, magnesium stearate, Tissuemat E, methyl-silicone oil.
The preparation method of a kind of Graphene filled polymer based composites, comprises the following steps:
(1) 0.1-10 part graphene microchip is dissolved in has added the ethanol solution of 0.01-1 part coupling agent, make dissolved with coupling agent
Ethanol solution be totally submerged graphene microchip, high-speed stirred is also concurrently placed in ultrasonic pond after ultrasonic disperse 20-50min, will
Finely dispersed graphene microchip is placed in drying in oven 8-24h of 90-120 DEG C, will be attached to the ethanol in graphene microchip
Solution completely removes；
(2) graphene microchip and the 1-10 part lubricant by 90-99 part thermoplastic resin, processed through step (1) adds
Mix homogeneously in high-speed mixer, mixing temperature is 60-90 DEG C, and incorporation time is 3-10min, is subsequently placed in vacuum drying oven
10-16h is dried at 100-110 DEG C；
(3) by pay-off by delicate metering of the material that mixes in step (2), send in double screw extruder,
Material screw rod shearing, mixing and conveying under sufficiently fuse, eventually pass die head extruding pelletization；
(4) pellet after extruding pelletization is added in hot pressing die, then mould is put into hot-forming in compression molding instrument,
Cooling, it is thus achieved that Graphene filled polymer based composites.
Preferably, in described step (3), the draw ratio of double screw extruder is 20-60:1, the temperature of each section of extruder
For 150-270 DEG C, extruder rotating speed is 20-30rpm.
Preferably, the hot pressing temperature of described step (4) middle plateform vulcameter is 170-270 DEG C, and preheating time is 5-
20min, hot pressing time is 5-20min, and hot pressing stress is 5-25MPa；Described cooling condition is water circulating cooling, and cool time is
3-20min。
Compared with prior art, the method have the advantages that
Compared with other carbon system filled composite materials, the Graphene filled polymer based composites of the present invention has and easily adds
Work, easy-formation, filler loading is few, raw material sources are wide, the feature such as environmentally friendly.And the electric conductivity of material and heat conductivity
Can be excellent, there is the features such as mechanical property good, good stability of the dimension, good weatherability, compare and use situ aggregation method or molten at present
For liquid polymerization prepares the technique of Graphene/polymer composites, prepare Graphene with melt-blending process and fill polymerization
Thing based composites has the advantage producing continuously, being especially suitable for large-scale production.
Detailed description of the invention
The present invention is described in detail below in conjunction with each embodiment.
Embodiment 1
Raw material is weighed according to following weight portion:
PP(oil of SPC, F800EPS) 99 parts,
Graphene microchip (Xiamen Kai Na, KNG150) 0.1 part,
KH-550 0.01 part,
Stearic acid 0.5 part,
Tissuemat E 9.5 parts,
Wherein the thickness of graphene microchip is 15nm, is made up of 10 layers of single-layer graphene；
(1) first graphene microchip is dissolved in and has added the ethanol solution of coupling agent, make the ethanol solution dissolved with coupling agent complete
Submergence graphene microchip, uses agitator high-speed stirred, is placed on ultrasonic disperse 30min in ultrasonic pond simultaneously, is subsequently placed in drum
16h is dried at 105 DEG C in wind baking oven；
(2) add after the graphene microchip handled well in step (1), PP resin, stearic acid and Tissuemat E precise
Enter high-speed mixer and mixing uniform, incorporation time 7min, mixing temperature 80 DEG C, it is subsequently placed in vacuum drying oven and dries at 105 DEG C
13h；
(3) by pay-off by delicate metering of the material handled well in step (2), send in double screw extruder,
Material screw rod shearing, mixing and conveying under sufficiently fuse, eventually pass die head extruding pelletization；Wherein double screw extruder
Draw ratio is 20:1, and each zone temperatures controls at 170 DEG C-220 DEG C, rotating speed 20rpm；
(4) will add in hot pressing die after Graphene/PP pellet precise, then mould is put into heat in compression molding instrument
Molded, preheating 5min, hot pressing temperature 180 DEG C, hot pressing time 5min, hot pressing stress 5MPa, then water circulating cooling 20min,
Depanning prepares Graphene/PP polymer composite board.
Embodiment 2
Raw material is weighed according to following weight portion:
PBT(orchid Tener rice, 130GRS) 95 parts,
Graphene microchip (Xiamen Kai Na, KNG150) 5 parts,
NDZ-101 0.5 part,
Stearic acid 1.5 parts,
Tissuemat E 1 part,
Wherein the thickness of graphene microchip is 12nm, is made up of 20 layers of single-layer graphene；
(1) first graphene microchip is dissolved in and has added the ethanol solution of coupling agent, make the ethanol solution dissolved with coupling agent complete
Submergence graphene microchip, uses agitator high-speed stirred, is placed on ultrasonic disperse 30min in ultrasonic pond, then in air blast simultaneously
Dry 8 hours at 120 DEG C in baking oven；
(2) by the graphene microchip handled well in step (1), PBT resin powder body, stearic acid and Tissuemat E precise
Rear addition high-speed mixer and mixing is uniform, incorporation time 3min, mixing temperature 90 DEG C, is subsequently placed in vacuum drying oven and dries at 110 DEG C
Dry 10h；
(3) by pay-off by delicate metering of the material handled well in step (2), send in double screw extruder,
Material screw rod shearing, mixing and conveying under sufficiently fuse, eventually pass die head extruding pelletization；Extruder draw ratio used
40:1, each zone temperatures controls at 200 DEG C-240 DEG C, rotating speed 25rpm；
(4) will add in hot pressing die after Graphene/PBT pellet precise, then mould is put in compression molding instrument
Hot-forming, preheating time 12min, hot pressing temperature 230 DEG C, hot pressing time 10min, hot pressing stress 15MPa, then water circulation cold
But 12min, depanning obtains Graphene/PBT polymer composite board.
Embodiment 3
Raw material is weighed according to following weight portion:
Anlong, PVC(Guizhou, SG-5) 90 parts,
Graphene microchip (Xiamen Kai Na, KNG150) 0.1 part,
A-171 1 part,
Zinc stearate 1.5 parts,
Methyl-silicone oil 5 parts,
Wherein the thickness of graphene microchip is 15nm, is made up of 10 layers of single-layer graphene；
(1) first graphene microchip is dissolved in and has added the ethanol solution of coupling agent, make the ethanol solution dissolved with coupling agent complete
Submergence graphene microchip, uses agitator high-speed stirred, is placed on ultrasonic disperse 30min in ultrasonic pond simultaneously, is subsequently placed in drum
24h is dried at 90 DEG C in wind baking oven；
(2) by after the graphene microchip handled well in step (1), polyvinyl chloride resin, zinc stearate and methyl-silicone oil precise
Add high-speed mixer and mixing uniform, incorporation time 10min, mixing temperature 60 DEG C, it is subsequently placed in vacuum drying oven and dries at 100 DEG C
16h；
(3) by pay-off by delicate metering of the material handled well in step (2), send in double screw extruder,
Material screw rod shearing, mixing and conveying under sufficiently fuse, eventually pass die head extruding pelletization；Wherein double screw extruder
Draw ratio 60:1, each zone temperatures controls at 150 DEG C-200 DEG C, rotating speed 30rpm；
(4) will add in hot pressing die after Graphene/PVC pellet precise, then mould is put in compression molding instrument
Hot-forming, preheat 20min, hot pressing temperature 170 DEG C, hot pressing time 20min, hot pressing stress 25MPa, then water circulating cooling
3min, depanning prepares Graphene/PVC polymer composite board.
Embodiment 4
Raw material is weighed according to following weight portion:
PS(Zhenjiang is the most beautiful, PG-33) 98 parts,
Graphene microchip (Xiamen Kai Na, KNG150) 10 parts,
KH-550 0.02 part,
Calcium stearate 0.5 part,
Tissuemat E 0.5 part,
Wherein the thickness of graphene microchip is 5nm, is made up of 30 layers of single-layer graphene；
(1) first graphene microchip is dissolved in and has added the ethanol solution of coupling agent, make the ethanol solution dissolved with coupling agent complete
Submergence graphene microchip, uses agitator high-speed stirred, is placed on ultrasonic disperse 50min in ultrasonic pond simultaneously, is subsequently placed in drum
Drying 12 hours at 105 DEG C in wind baking oven, the ethanol solution that will be attached in graphene microchip completely removes；
(2) by after the graphene microchip handled well in step (1), PS resin, calcium stearate and Tissuemat E precise
Add high-speed mixer and mixing uniform, incorporation time 10min, mixing temperature 80 DEG C, it is subsequently placed in vacuum drying oven and dries at 105 DEG C
12 hours；
(3) by pay-off by delicate metering of the material handled well in step (2), send in double screw extruder,
Material screw rod shearing, mixing and conveying under sufficiently fuse, eventually pass die head extruding pelletization；Wherein double screw extruder
Draw ratio 25:1, each zone temperatures controls at 170 DEG C-220 DEG C, rotating speed 20rpm；
(4) will add in hot pressing die after Graphene/PS pellet precise, then mould is put into heat in compression molding instrument
Molded, preheating time 5min, hot pressing temperature 200 DEG C, hot pressing time 10min, hot pressing stress 10MPa, then water circulating cooling
8min, depanning prepares Graphene/PS polymer composite board.
Embodiment 5
Raw material is weighed according to following weight portion:
PET(Du Pont, 415HP-NC) 95 parts,
Graphene microchip (Xiamen Kai Na, KNG150) 2 parts,
NDZ-101 0.5 part,
Magnesium stearate 4.5 parts,
Tissuemat E 0.5 part,
Wherein the thickness of graphene microchip is 12nm, is made up of 20 layers of single-layer graphene；
(1) first graphene microchip is dissolved in and has added the ethanol solution of coupling agent, make the ethanol solution dissolved with coupling agent complete
Submergence graphene microchip, uses agitator high-speed stirred, is placed on ultrasonic disperse 20min in ultrasonic pond simultaneously, is subsequently placed in drum
Drying 12 hours at 105 DEG C in wind baking oven, the ethanol solution that will be attached in graphene microchip completely removes；
(2) by after the graphene microchip handled well in step (1), PET resin, magnesium stearate and Tissuemat E precise
Add high-speed mixer and mixing uniform, incorporation time 10min, mixing temperature 80 DEG C, it is subsequently placed in vacuum drying oven and dries at 105 DEG C
12 hours；
(3) by pay-off by delicate metering of the material handled well in step (2), send in double screw extruder,
Material screw rod shearing, mixing and conveying under sufficiently fuse, eventually pass die head extruding pelletization；Wherein double screw extruder
Draw ratio 25:1, each zone temperatures controls at 170 DEG C-270 DEG C, rotating speed 20rpm；
(4) will add in hot pressing die after Graphene/PET pellet precise, then mould is put in compression molding instrument
Hot-forming, preheat 5min, hot pressing temperature 270 DEG C, hot pressing time 10min, hot pressing stress 10MPa, then water circulating cooling
8min, depanning prepares Graphene/pet polymer composite board.
Graphene filled polymer base composite board embodiment 1-5 prepared is with Chinese national standard conduction GB GB-
52261 and heat conduction GB GB-50051 as testing standard, the electric conductivity of test material and heat conductivility, test result is shown in Table
1。
Table 1
As it can be seen from table 1 the electric conductivity of the Graphene filled polymer based composites of the present invention and heat conductivility
Excellence, and there is the features such as excellent in mechanical performance, good stability of the dimension, good weatherability simultaneously.Meanwhile, compare and use at present in situ
For polymerization or solution polymerization process prepare the technique of Graphene/polymer composites, come with the melt-blending process of the present invention
Prepare Graphene filled polymer based composites and there is the advantage producing large-scale production continuous, applicable and reducing cost.
The several specific embodiments being only the application disclosed above, but the application is not limited to this, any this area
Technical staff can think change, all should fall in the protection domain of the application.
Claims (9)
1. a Graphene filled polymer based composites, it is characterised in that be made up of the component comprising following weight portion:
The preparation method of described Graphene filled polymer based composites, comprises the following steps:
(1) 0.1-10 part graphene microchip is dissolved in has added the ethanol solution of 0.01-1 part coupling agent, make the second dissolved with coupling agent
Alcoholic solution is totally submerged graphene microchip, and high-speed stirred is also concurrently placed in ultrasonic pond after ultrasonic disperse 20-50min, will dispersion
Uniform graphene microchip is placed in drying in oven 8-24h of 90-120 DEG C, will be attached to the ethanol solution in graphene microchip
Completely remove；
(2) graphene microchip and the 1-10 part lubricant by 90-99 part thermoplastic resin, processed through step (1) adds at a high speed
Mix homogeneously in mixer, mixing temperature is 60-90 DEG C, and incorporation time is 3-10min, is subsequently placed in 100-in vacuum drying oven
10-16h is dried at 110 DEG C；
(3) by pay-off by delicate metering of the material that mixes in step (2), send in double screw extruder, material
Screw rod shearing, mixing and conveying under sufficiently fuse, eventually pass die head extruding pelletization；
(4) pellet after extruding pelletization is added in hot pressing die, then mould is put into hot-forming in compression molding instrument, cold
But, it is thus achieved that Graphene filled polymer based composites.
2. Graphene filled polymer based composites as claimed in claim 1, it is characterised in that described thermoplastic resin selects
One in polypropylene, polrvinyl chloride, polystyrene, polyethylene terephthalate, polybutylene terephthalate (PBT)
Or it is several.
3. Graphene filled polymer based composites as claimed in claim 1, it is characterised in that described graphene microchip
Thickness is 5-15nm, is made up of average 10-30 layer single-layer graphene.
4. Graphene filled polymer based composites as claimed in claim 1, it is characterised in that described coupling agent is selected from silicon
One or more in alkane coupling agent, titanate coupling agent or aluminate coupling agent.
5. Graphene filled polymer based composites as claimed in claim 4, it is characterised in that described coupling agent is selected from
One or more in KH-550, NDZ-101, A-171.
6. Graphene filled polymer based composites as claimed in claim 1, it is characterised in that described lubricant is selected from N,
One in N '-ethylene bis stearamide, stearic acid, zinc stearate, calcium stearate, magnesium stearate, Tissuemat E, methyl-silicone oil
Or it is several.
7. the preparation method of a Graphene filled polymer based composites as claimed in claim 1, it is characterised in that bag
Include following steps:
(1) 0.1-10 part graphene microchip is dissolved in has added the ethanol solution of 0.01-1 part coupling agent, make the second dissolved with coupling agent
Alcoholic solution is totally submerged graphene microchip, and high-speed stirred is also concurrently placed in ultrasonic pond after ultrasonic disperse 20-50min, will dispersion
Uniform graphene microchip is placed in drying in oven 8-24h of 90-120 DEG C, will be attached to the ethanol solution in graphene microchip
Completely remove；
(2) graphene microchip and the 1-10 part lubricant by 90-99 part thermoplastic resin, processed through step (1) adds at a high speed
Mix homogeneously in mixer, mixing temperature is 60-90 DEG C, and incorporation time is 3-10min, is subsequently placed in 100-in vacuum drying oven
10-16h is dried at 110 DEG C；
(3) by pay-off by delicate metering of the material that mixes in step (2), send in double screw extruder, material
Screw rod shearing, mixing and conveying under sufficiently fuse, eventually pass die head extruding pelletization；
(4) pellet after extruding pelletization is added in hot pressing die, then mould is put into hot-forming in compression molding instrument, cold
But, it is thus achieved that Graphene filled polymer based composites.
8. the preparation method of Graphene filled polymer based composites as claimed in claim 7, it is characterised in that described step
Suddenly in (3), the draw ratio of double screw extruder is 20-60:1, and the temperature of each section of extruder is 150-270 DEG C, extruder rotating speed
For 20-30rpm.
9. the preparation method of Graphene filled polymer based composites as claimed in claim 7, it is characterised in that described step
Suddenly the hot pressing temperature of (4) middle plateform vulcameter is 170-270 DEG C, and preheating time is 5-20min, and hot pressing time is 5-20min, heat
Pressure stress is 5-25MPa；Described cooling condition is water circulating cooling, and cool time is 3-20min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110337141.9A CN103087404B (en) | 2011-10-31 | A kind of Graphene filled polymer based composites and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110337141.9A CN103087404B (en) | 2011-10-31 | A kind of Graphene filled polymer based composites and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN103087404A CN103087404A (en) | 2013-05-08 |
| CN103087404B true CN103087404B (en) | 2016-12-14 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812194A (en) * | 2010-03-17 | 2010-08-25 | 湖北大学 | Graphene-based barrier composite material and preparation method thereof |
| CN101987907A (en) * | 2010-10-18 | 2011-03-23 | 河南科技大学 | Polydicyclopentadiene composite material and preparation method thereof |
| CN102040761A (en) * | 2011-01-14 | 2011-05-04 | 华南理工大学 | High-heat-conductivity composite material and preparation method thereof |
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812194A (en) * | 2010-03-17 | 2010-08-25 | 湖北大学 | Graphene-based barrier composite material and preparation method thereof |
| CN101987907A (en) * | 2010-10-18 | 2011-03-23 | 河南科技大学 | Polydicyclopentadiene composite material and preparation method thereof |
| CN102040761A (en) * | 2011-01-14 | 2011-05-04 | 华南理工大学 | High-heat-conductivity composite material and preparation method thereof |
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Denomination of invention: Graphene filled polymer matrix composite material and its preparation method Effective date of registration: 20191202 Granted publication date: 20161214 Pledgee: Chuzhou economic and Technological Development Corporation Pledgor: Shanghai Jieshijie New Materials (Group) Co., Ltd. Registration number: Y2019980000815 |