CN107325421A - A kind of preparation method of polymer/graphene/carbon nano tube compound material - Google Patents
A kind of preparation method of polymer/graphene/carbon nano tube compound material Download PDFInfo
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- CN107325421A CN107325421A CN201710485841.XA CN201710485841A CN107325421A CN 107325421 A CN107325421 A CN 107325421A CN 201710485841 A CN201710485841 A CN 201710485841A CN 107325421 A CN107325421 A CN 107325421A
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Abstract
The present invention discloses a kind of preparation method of polymer/graphene/carbon nano tube compound material, and methods described includes：Under ul-trasonic irradiation, in acidic aqueous solution, finely dispersed polystyrene microsphere, graphene and carbon nano tube suspension are prepared respectively.Then preparation-obtained three's uniform suspension is mixed, and by regulating and controlling mixed solution pH value, assigns three's oppositely charged.Due to electrostatic interaction, graphene and CNT will be uniformly wrapped on Surfaces of Polystyrene Microparticles, obtain polystyrene/graphene/carbon nanometer pipe ternary hybrid.Finally, the poly styrene composite material with three-dimensional grapheme carbon nano-tube hybridization network is prepared by hot press forming technology.The polystyrene/graphene that the present invention is obtained/carbon nanometer pipe ternary hybrid can mutually suppress respective reunion behavior, promote graphene and CNT to build three-dimensional hybridization network in polymeric matrix, form substantial amounts of conductive path.Under low sizing consumption, it can significantly assign composite excellent electric conductivity.
Description
Technical field
The present invention relates to a kind of preparation method of polymer/graphene/carbon nano tube compound material, and in particular to Yi Zhongji
In the preparation method of the conducting polymer composite material of graphene-carbon nano tube network.
Background technology
Graphene and CNT are led due to performances such as its excellent electricity, heat, mechanics in high strength composite, conduction
The occasions such as hot composite, electrode and electronic device have a wide range of applications.As new conductive filler, graphene and carbon are received
The chemiluminescence of both mitrons, can be advantageously in preparing highly conductive polymer composites.But, graphene due to
Its stronger van der Waals interaction and easily occur irreversible reunion and stacking, it is difficult to play its excellent in the polymer
Different in nature energy.Meanwhile, CNT makes it equally easily go out in polymeric matrix due to its great draw ratio and specific surface area
Now serious reunion and tangling phenomenon, cause can not embodying for CNT excellent properties, and destroy the comprehensive of composite
Energy.Therefore, improve scattered, the effective electron propagation ducts of structure of graphene and CNT in the polymer, be that lifting is poly-
The key of compound composite material electric conductivity.
The problem disperseed in the polymer for graphene and CNT, by by graphene and CNT with hydridization
The form of structure is constructed, and forms the network of interspersed interconnection, on the one hand can effectively suppress graphene and CNT
Reunion behavior, on the other hand, the graphene/carbon nano-tube hybridization network of formation can provide significantly more efficient conductive path, subtract
It is few both amount of filler (reduction percolation threshold), reduction prepare the cost of composite.Such as, Chinese patent
The report such as CN105000542A and CN102923686B uses chemical vapour deposition technique, and CNT is grown in graphenic surface,
The graphene-carbon nano tube hybrid material with three-dimensional structure is prepared, but this method preparation technology is complicated, condition is harsh, into
This costliness, it is impossible to mass produced, also, prepared graphene-carbon nano tube hybrid material can not shift effectively,
And be difficult to apply to prepare polymer composites.In addition, Chinese patent CN104672357A, using chemical vapor deposition skill
Art, grows CNT, and prepare with graphene-carbon nano tube by in-situ dispersion polymerization method in the graphenic surface of synthesis
Hybrid/polymer composites.But, because the graphene-carbon nano tube hybrid with three-dimensional structure is difficult uniform point
Dissipate in solution, cause hybrid in the polymer that in-situ dispersion polymerization method prepares to disperse poor, further influence is conductive
The structure of path, so that hybrid addition is larger, influences the combination property of composite.Chinese patent CN105732036A,
Report and polystyrene resin/Graphene/carbon nanotube composite material is prepared for using solution blended process, due to can not be effective
Regulate and control the conductive path of graphene-carbon nano tube, it is therefore desirable to add substantial amounts of graphene and CNT, percolation threshold compared with
Greatly, higher cost is caused.
Therefore, the present invention is prepared for polystyrene microsphere/Graphene/carbon nanotube composite material by electrostatic self-assembled.
Acted on, while very big both consumptions of reduction, effectively constructed by one-dimensional CNT and the bridge joint of two-dimensional graphene
Three-dimensional grapheme-carbon nano-tube hybridization network, it is to avoid both serious agglomeration behaviors, forms flourishing in polystyrene matrix
Conductive path, significantly improve the electric conductivity of composite.By the structure of various dimensions conductive network, graphite is adequately achieved
Collaboration enhancing in both alkene and CNT structure and performance, this has weight to preparing high-performance conductive polymer composites
The directive function wanted.
The content of the invention
The present invention prepares graphene suspension by chemical reduction method first.Then, it is prepared for gathering using electrostatic self-assembled
Phenylethylene micro ball/graphene/carbon nano-tube ternary hybrid thing.Prepared finally by heat pressing process with three-dimensional hybridization network
Polystyrene/graphene/carbon nano tube compound material.
The present invention carries out electronation to graphene oxide, is prepared into first using ammoniacal liquor and hydrazine hydrate as complex reducing agent
To the electronegative graphene suspension in finely dispersed surface.Under ul-trasonic irradiation, in acidic aqueous solution, it is prepared into respectively
, will be preparation-obtained to finely dispersed polystyrene microsphere, graphene and carbon nano tube suspension, and with certain mass ratio
Three's uniform suspension is mixed, mutually exclusive because three surface is positively charged, dispersed.Then, it is molten by the way that alkalescence is added dropwise
Liquid regulates and controls mixed solution pH=6, and polystyrene microsphere is positively charged, and graphene and CNT are negatively charged, due to electrostatic phase
Interaction, graphene and CNT will be uniformly wrapped on Surfaces of Polystyrene Microparticles, prepare polystyrene microsphere/graphite
Alkene/carbon nanometer pipe ternary hybrid.Finally, at high temperature, hot-forming prepare has three-dimensional grapheme-carbon nano-tube hybridization net
The poly styrene composite material of network.
This programme purpose is realized by following scheme:
1. a kind of preparation method of polymer/graphene/carbon nano tube compound material, it is characterised in that including following step
Suddenly：
(1) graphene suspension is prepared：Graphite oxide ultrasonic disperse is taken in water, centrifugation obtains the graphite oxide of brown color
Alkene suspension；Add ammoniacal liquor and hydrazine hydrate carries out electronation and prepares graphene suspension.
(2) polystyrene microsphere/graphene/carbon nano-tube ternary hybrid thing is prepared：By graphene, CNT and polyphenyl
Ethene microballoon ultrasonic disperse respectively obtains finely dispersed suspension in acidic aqueous solution.By three's suspension according to certain
Ratio uniform is mixed, 0.5~2h of ultrasonic disperse；Mixed solution is adjusted to pH=6 by the way that alkaline solution is added dropwise, due to Electrostatic Absorption
Effect, graphene and CNT will be uniformly wrapped on Surfaces of Polystyrene Microparticles, and prepare polystyrene/graphene/carbon
Nanotube ternary hybrid thing.
(3) polystyrene/graphene/carbon nano tube compound material is prepared：The ternary hybrid thing that will be obtained in step (2),
Polystyrene/graphene/carbon nano tube compound material is directly obtained using heat pressing process.
The particle diameter of described polystyrene microsphere is 500nm~2 μm.
Described acidic aqueous solution is a kind of aqueous solution in hydrochloric acid, nitric acid, sulfuric acid, and pH is 1.5~3.0.
Described alkaline aqueous solution is a kind of aqueous solution in sodium hydroxide, potassium hydroxide.
Described graphene and the quality of polystyrene microsphere are 1 than scope:80~1:120.
Described CNT and the quality of polystyrene microsphere are 1 than scope:60~1:100.
The heat pressing process is that hot pressing temperature control is carried out into processing and forming at a certain temperature in the range of 100~120 DEG C,
Briquetting pressure is 10MPa.
Compared with prior art, advantage of the invention is that：
(1) it can effectively suppress the reunion of graphene and CNT by electrostatic assembly method, improve both in polymerization
Dispersive property in thing.Solve graphene and CNT in current preparation method (solution blending etc.) and be difficult scattered difficulty
Topic.
(2) graphene, CNT are coated on polymer microballoon surface jointly because electrostatic assembly is acted on, and then passed through
Mould pressing process prepares the composite with three-dimensional grapheme-carbon nano-tube hybridization network, in low percolation threshold (low sizing
Consumption) under, due to the effect of various dimensions bridge joint, substantial amounts of conducting connection point is formed, flourishing conductive path is built, composite wood is assigned
The performances such as the excellent conductive and heat-conductive of material.This effectively overcomes stone in the general preparation such as solution blended process and situ aggregation method at present
Black alkene and CNT are difficult to form the problem of continuous conduction network, and significantly reduce the percolation threshold of composite, reduction
Cost.
(3) processing technology is simple and easy to do, and reaction condition is gentle, operability and reproducible, can carry out large-scale industry
Metaplasia is produced.Gained graphene-carbon nano tube hybridization network structure-controllable, can be widely applied for preparing highly conductive polymer composite
Material.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of pure nano-carbon tube；
Fig. 2 is the transmission electron microscope picture of pure graphene；
Fig. 3 is the scanning electron microscope (SEM) photograph of pure polystyrene；
Fig. 4 is the ESEM of graphene/carbon nano-tube/polystyrene microsphere ternary hybrid thing prepared by embodiment 1
Figure；
Fig. 5 is the ESEM of graphene/carbon nano-tube/polystyrene microsphere ternary hybrid thing prepared by embodiment 2
Figure.
Embodiment
Embodiment 1：
(1) graphene suspension is prepared：0.5g graphite oxide ultrasonic disperses are taken in water, centrifugation obtains the oxidation of brown color
Graphene suspension；Add 140 μ L ammoniacal liquor and 20 μ L hydrazine hydrates carry out electronation and prepare graphene suspension.
(2) polystyrene microsphere/graphene/carbon nano-tube ternary hybrid thing is prepared：By 0.075g graphenes, 0.1g carbon
Nanotube and 6.0g polystyrene microspheres ultrasonic disperse are respectively obtained finely dispersed outstanding in pH=1.5 aqueous hydrochloric acid solution
Supernatant liquid.Three's uniform suspension is mixed, ultrasonic disperse 1h；Regulate and control mixed solution extremely by the way that 1mol/L sodium hydroxide solutions are added dropwise
PH=6, due to electrostatic adsorption, graphene and CNT will be uniformly wrapped on Surfaces of Polystyrene Microparticles, prepare
Polystyrene/graphene/carbon nanometer pipe ternary hybrid.
(3) polystyrene/graphene/carbon nano tube compound material is prepared：The ternary hybrid thing obtained in step (2) is put
Polystyrene/graphene/carbon nano tube compound material is made in being molded under 120 DEG C, 10MPa heat pressing process.
It is miscellaneous that prepared polystyrene/graphene/carbon nanometer pipe ternary hybrid in (3), wherein graphene account for ternary
The mass percent of compound is 1.21%, and the mass percent that CNT accounts for ternary hybrid thing is 1.62%.Such as Fig. 1,2,3 institutes
Show, pure nano-carbon tube 30~60nm of diameter, mutual entanglement behavior is presented；Graphene sheet layer size is 200~500nm, and polyphenyl
Ethene microspherulite diameter is 1~3 μm.The ternary hybrid thing prepared by electrostatic assembly technique, as shown in figure 4, graphene and carbon are received
Mitron is successfully uniformly wrapped on Surfaces of Polystyrene Microparticles, it is suppressed that the serious entanglement of CNT and the serious group of graphene
Poly-, good bridge joint behavior is presented in both.Now, the electrical conductivity of pure polystyrene is 4.2 × 10-16S/m, and it is prepared poly-
The electrical conductivity of styrene/Graphene/carbon nanotube composite material is 8.9 × 10-2S/m, improves 14 orders of magnitude.
Embodiment 2：
(1) graphene suspension is prepared：0.5g graphite oxide ultrasonic disperses are taken in water, centrifugation obtains brown color oxidation stone
Black alkene suspension；Add 140 μ L ammoniacal liquor and 20 μ L hydrazine hydrates carry out electronation and prepare graphene suspension.
(2) polystyrene microsphere/graphene/carbon nano-tube ternary hybrid thing is prepared：By 0.1g graphenes, 0.128g carbon
Nanotube and 9.0g polystyrene microspheres ultrasonic disperse are respectively obtained finely dispersed outstanding in pH=2.0 aqueous hydrochloric acid solution
Supernatant liquid.Three's uniform suspension is mixed, ultrasonic disperse 1.5h；Regulate and control mixed solution by the way that 1mol/L sodium hydroxide solutions are added dropwise
To pH=6, due to electrostatic adsorption, graphene and CNT will be uniformly wrapped on Surfaces of Polystyrene Microparticles, be prepared into
To polystyrene/graphene/carbon nanometer pipe ternary hybrid.
(3) polystyrene/graphene/carbon nano tube compound material is prepared：The ternary hybrid thing obtained in step (2) is put
Polystyrene/graphene/carbon nano tube compound material is made in being molded under 115 DEG C, 10MPa heat pressing process.
It is miscellaneous that prepared polystyrene/graphene/carbon nanometer pipe ternary hybrid in (3), wherein graphene account for ternary
The mass percent of compound is 1.08%, and the mass percent that CNT accounts for ternary hybrid thing is 1.39%.As shown in figure 5,
For prepared ternary hybrid thing, graphene and CNT can effectively be coated on Surfaces of Polystyrene Microparticles, it is suppressed that
Both serious agglomerations, the various dimensions bridge coil of formation.Compared to pure polystyrene, prepared polystyrene/graphene/
The electrical conductivity of carbon nano tube compound material is 1.8 × 10-2S/m, improves 14 orders of magnitude.
Embodiment 3：
(1) graphene suspension is prepared：0.5g graphite oxide ultrasonic disperses are taken in water, centrifugation obtains brown color oxidation stone
Black alkene suspension；Add 140 μ L ammoniacal liquor and 20 μ L hydrazine hydrates carry out electronation and prepare graphene suspension.
(2) polystyrene microsphere/graphene/carbon nano-tube ternary hybrid thing is prepared：By 0.1g graphenes, 0.125g carbon
Nanotube and 10.0g polystyrene microspheres ultrasonic disperse are respectively obtained finely dispersed outstanding in pH=2.5 aqueous hydrochloric acid solution
Supernatant liquid.Three's uniform suspension is mixed, ultrasonic disperse 2.0h；Regulate and control mixed solution by the way that 1mol/L sodium hydroxide solutions are added dropwise
To pH=6, due to electrostatic adsorption, graphene and CNT will be uniformly wrapped on Surfaces of Polystyrene Microparticles, be prepared into
To polystyrene/graphene/carbon nanometer pipe ternary hybrid.
(3) polystyrene/graphene/carbon nano tube compound material is prepared：The ternary hybrid thing obtained in step (2) is put
Polystyrene/graphene/carbon nano tube compound material is made in being molded under 110 DEG C, 10MPa heat pressing process.
It is miscellaneous that prepared polystyrene/graphene/carbon nanometer pipe ternary hybrid in (3), wherein graphene account for ternary
The mass percent of compound is 0.98%, and the mass percent that CNT accounts for ternary hybrid thing is 1.22%.It is poly- compared to pure
Styrene, the electrical conductivity of prepared polystyrene/graphene/carbon nano tube compound material is 9.5 × 10-3S/m, is improved
13 orders of magnitude.
Embodiment 4：
(1) graphene suspension is prepared：0.5g graphite oxide ultrasonic disperses are taken in water, centrifugation obtains the oxidation of brown color
Graphene suspension；Add 140 μ L ammoniacal liquor and 20 μ L hydrazine hydrates carry out electronation and prepare graphene suspension.
(2) polystyrene microsphere/graphene/carbon nano-tube ternary hybrid thing is prepared：By 0.1g graphenes, 0.122g carbon
Nanotube and 11.0g polystyrene microspheres ultrasonic disperse are respectively obtained finely dispersed outstanding in pH=3.0 aqueous sulfuric acid
Supernatant liquid.Three's uniform suspension is mixed, ultrasonic disperse 2.0h；Regulate and control mixed solution by the way that 1mol/L sodium hydroxide solutions are added dropwise
To pH=6, due to electrostatic adsorption, graphene and CNT will be uniformly wrapped on Surfaces of Polystyrene Microparticles, be prepared into
To polystyrene/graphene/carbon nanometer pipe ternary hybrid.
(3) polystyrene/graphene/carbon nano tube compound material is prepared：The ternary hybrid thing obtained in step (2) is put
Polystyrene/graphene/carbon nano tube compound material is made in being molded under 105 DEG C, 10MPa heat pressing process.
It is miscellaneous that prepared polystyrene/graphene/carbon nanometer pipe ternary hybrid in (3), wherein graphene account for ternary
The mass percent of compound is 0.89%, and the mass percent that CNT accounts for ternary hybrid thing is 1.09%.It is poly- compared to pure
Styrene, the electrical conductivity of prepared polystyrene/graphene/carbon nano tube compound material is 4.2 × 10-3S/m, is improved
13 orders of magnitude.
Embodiment 5：
(1) graphene suspension is prepared：0.5g graphite oxide ultrasonic disperses are taken in water, centrifugation obtains the oxidation of brown color
Graphene suspension；Add 140 μ L ammoniacal liquor and 20 μ L hydrazine hydrates carry out electronation and prepare graphene suspension.
(2) polystyrene microsphere/graphene/carbon nano-tube ternary hybrid thing is prepared：By 0.1g graphenes, 0.133g carbon
Nanotube and 12.0g polystyrene microspheres ultrasonic disperse are respectively obtained finely dispersed outstanding in pH=3.0 aqueous sulfuric acid
Supernatant liquid.Three's uniform suspension is mixed, ultrasonic disperse 2.0h；Regulate and control mixed solution by the way that 1mol/L sodium hydroxide solutions are added dropwise
To pH=6, due to electrostatic adsorption, graphene and CNT will be uniformly wrapped on Surfaces of Polystyrene Microparticles, be prepared into
To polystyrene/graphene/carbon nanometer pipe ternary hybrid.
(3) polystyrene/graphene/carbon nano tube compound material is prepared：The ternary hybrid thing obtained in step (2) is put
Polystyrene/graphene/carbon nano tube compound material is made in being molded under 100 DEG C, 10MPa heat pressing process.
It is miscellaneous that prepared polystyrene/graphene/carbon nanometer pipe ternary hybrid in (3), wherein graphene account for ternary
The mass percent of compound is 0.81%, and the mass percent that CNT accounts for ternary hybrid thing is 1.09%.It is poly- compared to pure
Styrene, the electrical conductivity of prepared polystyrene/graphene/carbon nano tube compound material is 1.1 × 10-3S/m, is improved
13 orders of magnitude.
Claims (6)
1. a kind of preparation method of polymer/graphene/carbon nano tube compound material, it is characterised in that comprise the following steps:
(1) graphene suspension is prepared：Graphite oxide ultrasonic disperse is taken in water, centrifugation obtains the suspension of brown color graphene oxide
Liquid；Add ammoniacal liquor and hydrazine hydrate carries out electronation and prepares graphene suspension.
(2) polystyrene microsphere/graphene/carbon nano-tube ternary hybrid thing is prepared：By certain mass than graphene, carbon nanometer
Pipe and polystyrene microsphere ultrasonic disperse obtain finely dispersed suspension in the acidic aqueous solution that pH is 1.5~3.0.Will
Three's uniform suspension is mixed, 0.5~2h of ultrasonic disperse；Mixed solution is adjusted to pH=6 by the way that alkaline solution is added dropwise, due to quiet
Electro Sorb is acted on, and graphene and CNT will be uniformly wrapped on Surfaces of Polystyrene Microparticles, and prepare polystyrene/graphite
Alkene/carbon nanometer pipe ternary hybrid.
(3) polystyrene/graphene/carbon nano tube compound material is prepared：The ternary hybrid thing that will be obtained in step (2), directly
Polystyrene/graphene/carbon nano tube compound material is made using being molded under heat pressing process.
2. a kind of polymer/graphene/carbon nano tube compound material as claimed in claim 1 and preparation method thereof, its feature
It is：The particle diameter of described polystyrene microsphere is 500nm~2 μm.
3. a kind of preparation method of polymer/graphene/carbon nano tube compound material as claimed in claim 1, its feature exists
In：Acidic aqueous solution is a kind of aqueous solution in hydrochloric acid, nitric acid, sulfuric acid.
4. a kind of preparation method of polymer/graphene/carbon nano tube compound material as claimed in claim 1, its feature exists
In：Described graphene and the quality of polystyrene microsphere are 1 than scope:80~1:120.CNT and polystyrene microsphere
Quality than scope be 1:60~1:100.
5. a kind of preparation method of polymer/graphene/carbon nano tube compound material as claimed in claim 1, its feature exists
In：Described alkaline aqueous solution position is a kind of aqueous solution in sodium hydroxide, potassium hydroxide.
6. a kind of preparation method of polymer/graphene/carbon nano tube compound material as claimed in claim 1, its feature exists
In：The heat pressing process is that hot pressing temperature control is carried out into processing and forming at a certain temperature in the range of 100~120 DEG C, is molded
Pressure is 10MPa.
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| CN108084627A (en) * | 2017-12-27 | 2018-05-29 | 上海统慧科技发展有限公司 | HIPS base conductive agglomerates based on carbon nanotubes and graphene compound system and preparation method thereof |
| CN108250603A (en) * | 2018-01-19 | 2018-07-06 | 广州润锋科技有限公司 | Polystyrene carrier material that a kind of carbon nanotube conducting is modified and preparation method thereof |
| CN108630459A (en) * | 2018-05-10 | 2018-10-09 | 河北工业大学 | A kind of preparation method of all solid state multilevel hierarchy transparent flexible ultracapacitor of low cost |
| CN109265712A (en) * | 2018-09-06 | 2019-01-25 | 中国科学院金属研究所 | The preparation method of the polyacrylic acid composite conducting particles of graphene Gradient Coated |
| CN109796682A (en) * | 2018-12-18 | 2019-05-24 | 武汉金牛经济发展有限公司 | Heat-resisting PPR pipe of toughening and preparation method thereof |
| CN109796682B (en) * | 2018-12-18 | 2021-08-17 | 武汉金牛经济发展有限公司 | Toughened heat-resistant PPR pipe and preparation method thereof |
| CN110562963A (en) * | 2019-09-19 | 2019-12-13 | 深圳烯创先进材料研究院有限公司 | preparation method of graphene-carbon nanotube hybrid sponge |
| CN113527819A (en) * | 2021-08-13 | 2021-10-22 | 河北科技大学 | Reduced graphene oxide polystyrene composite material and preparation method thereof |
| CN113527819B (en) * | 2021-08-13 | 2022-07-29 | 河北科技大学 | Reduced graphene oxide polystyrene composite material and preparation method thereof |
| CN115521553A (en) * | 2022-10-11 | 2022-12-27 | 昆明理工大学 | Preparation method and application of graphene/MXene/polystyrene composite material |
| WO2024093718A1 (en) * | 2022-11-01 | 2024-05-10 | 黄晓 | Hollow microsphere composite thermally-conductive filler coated with low-dimensional nanometer high-thermal-conductivity material, preparation method therefor, and use thereof |
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