CN108342026A - A method of graphene-poly styrene composite material is prepared by graphite and styrene - Google Patents
A method of graphene-poly styrene composite material is prepared by graphite and styrene Download PDFInfo
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- CN108342026A CN108342026A CN201810242465.6A CN201810242465A CN108342026A CN 108342026 A CN108342026 A CN 108342026A CN 201810242465 A CN201810242465 A CN 201810242465A CN 108342026 A CN108342026 A CN 108342026A
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 title claims abstract description 146
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 46
- 239000010439 graphite Substances 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000004793 Polystyrene Substances 0.000 title claims abstract description 34
- 229920002223 polystyrene Polymers 0.000 title claims abstract description 34
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 68
- 239000006185 dispersion Substances 0.000 claims abstract description 53
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 229920000642 polymer Polymers 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000008236 heating water Substances 0.000 claims description 7
- 210000003739 neck Anatomy 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 6
- SYWDWCWQXBUCOP-UHFFFAOYSA-N benzene;ethene Chemical group C=C.C1=CC=CC=C1 SYWDWCWQXBUCOP-UHFFFAOYSA-N 0.000 claims 2
- 239000002994 raw material Substances 0.000 abstract description 10
- 238000007720 emulsion polymerization reaction Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 239000002114 nanocomposite Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000002604 ultrasonography Methods 0.000 abstract description 3
- 238000001291 vacuum drying Methods 0.000 abstract description 3
- 238000007306 functionalization reaction Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 150000001336 alkenes Chemical class 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000945 filler Substances 0.000 description 4
- 229920006389 polyphenyl polymer Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000001721 carbon Chemical group 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- -1 azo Nitrile Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 101710141544 Allatotropin-related peptide Proteins 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 238000010560 atom transfer radical polymerization reaction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
A kind of method preparing graphene poly styrene composite material by graphite and styrene of the present invention, is combined using mechanical force and chemical ultrasound and emulsion polymerization, is raw material rather than graphene for raw material using graphite, to prepare graphene and high molecular composite material.Mechanical stripping is first carried out to graphite by ball-milling method in styrene, the styrene dispersion liquid containing graphene is obtained, then further disperseed to dispersion liquid by ultrasonic method, finally carries out emulsion polymerization；Filtering, vacuum drying obtain object.Due to using graphite as raw material, solve key technical problems present in current technology of preparing, it is a kind of environmental-friendly, it is environmentally protective, mild condition and can largely prepare functionalization polystyrene/graphene nanocomposite new method, the thermal coefficient of graphene/poly styrene composite material of preparation can 0.2508W/ (m DEG C), heat decomposition temperature be 360 DEG C, can be used as heat-conductive composite material.
Description
Technical field
The invention belongs to the preparation of high molecular nanometer filler composite materials and application fields, are related to one kind by graphite and styrene
The method for preparing graphene-poly styrene composite material.
Background technology
Conventional thermal conductive plastics mainly carry out macromolecule matrix material with the metal of high heat conduction or inorganic filler particle equal
Even filling.When amount of filler reaches a certain level, filler forms similar chain and netted form in system, that is, is formed and led
Heat supply network chain.When the differently- oriented directivity of these heat conduction network chains is parallel with direction of heat flow, leading for system will be largely improved
It is hot.
Graphene is a kind of Novel Carbon Nanomaterials for the individual layer laminated structure being made of carbon atom, and thickness is only
0.35nm.Due to it with prodigious specific surface area, good thermal stability and chemical stability, stronger hydrophobicity, be easy to
The advantages that being chemically modified is expected in high performance electronics, composite material, field emmision material, gas sensor and energy
The fields such as storage obtain extensive use.And it is formed by sp2 hydbridized carbon atoms close-packed arrays, has unique two-dimension periodic
Honeycomb lattice structure, the Stable Carbon hexatomic ring in the presence of structural unit assign its excellent hot property, it is considered to be excellent
Elegant heat control material.
Heat management, electronics industry middle-high density, high integration group are disclosure satisfy that by the high heat conduction plastics of filler of graphene
The requirement of development is filled, development prospect is boundless.Currently, preparing the preparation method of graphene/polymer composites is all
Using graphene as raw material, prepared using solution mixing method, melt-blending process, situ aggregation method and emulsion polymerization.But solution
Mixing method needs that organic solvent, post-processing is used to cause harmful effect to environment.Melt-blending process graphene collects in the polymer
Gather and be not easy to disperse, and is poor with the interface interaction of polymer.The reaction condition of situ aggregation method is difficult to control.Emulsion polymerization
Composite material prepared by method has better dispersion effect and spatial stability, and this method does not use organic solvent, does not break
Bad environment, but have certain requirement to well dispersed dispersion liquid is made.
Stankovich etc. utilizes the hydroxyl and carboxyl of isocyanate group and surface of graphene oxide to chemically react for the first time,
It is prepared for the isocyanate-modified graphene nanocomposite material using polystyrene as matrix by solution intercalation method.Zhang Wenling
Polystyrene microsphere is obtained by polymerisation Deng first with anionic initiator (AIBN), microballoon liquid is added to oxidation
In graphene solution, graphene oxide is made to be adsorbed on the surface of microballoon, hydrazine hydrate reduction is recycled to obtain polystyrene/oxidation stone
Black alkene microballoon.Picketing emulsion polymerisation process is to first pass through Hummers methods to prepare graphene oxide water solution, adds benzene
Vinyl monomer, AIBN obtain the styrene emulsion that the graphene oxide of white is stablized.Polyphenyl is prepared by surfactant- free emulsion polymerization
Ethylene colloidal solid.Lee etc. causes ATRP using controlled surface for the first time and obtains the polyphenyl second of surface of graphene oxide covalence graft
Alkene obtains the composite material of polystyrene/graphene（The composite material can be well dispersed in dimethylformamide, toluene,
In chloroform and dichloromethane, and make the polyphenyl that graphene surface is grafted using the covalent object of saponification removal graphene surface
Ethylene falls off, and it is excellent to obtain graphene oxide）.Difficult, valence height is prepared due to graphene and is disperseed in polymeric system
Difficulty, graphene composite material prepared by above method all have that manufacturing cost is high, graphene dispersion is uneven and procedure quality
Unstable problem.
Invention content
For technical barrier existing for current this field, the purpose of the present invention is use mechanical force and chemical-ultrasound and lotion
Polymerization is combined, and is raw material rather than graphene for raw material using graphite, to prepare graphene and high molecular composite material.First
Mechanical stripping is carried out to graphite by ball-milling method in styrene, obtains the styrene dispersion liquid containing graphene；Again by super
Sound method further disperses dispersion liquid, obtains the graphene with good dispersion/styrene dispersion liquid；Finally carry out
Emulsion polymerization；Filtering obtains graphene/poly styrene composite material after vacuum drying.Since graphite is raw material, mesh is solved
Key technical problems present in preceding technology of preparing.
A kind of the step of method of graphene-poly styrene composite material is prepared by graphite and styrene of the present invention and item
Part is as follows：
The first step, by the volume of styrene（mL）With graphite（g）Ratio be 1000: 1-1000：7, by styrene and graphite
Mixing is placed on ball milling in type planetary ball mill and removes 6h-36h, obtains the styrene dispersion liquid containing graphene；
Second step, then the dispersion liquid of above-mentioned graphene and styrene is placed in ultrasonic disperse 2h-8h in digital control type ultrasonic device, it carries out
Further dispersion, obtains the graphene with good dispersion/styrene dispersion liquid；
Third walks, and is 1 by polyvinyl alcohol and deionized water quality ratio：3 are added to three necks equipped with blender and reflux condensing tube
In reactor, when heating water bath is warming up to 70 DEG C, by the volume of graphene and styrene dispersion liquid（mL）With azodiisobutyronitrile
（g）Ratio be 80：1 adds in reactor, with mixing speed be 420 r/min be stirred, increase bath temperature to 87 DEG C,
2 h of constant temperature then raises temperature to 90 DEG C, and constant temperature half an hour, polymerisation terminates, and obtains solid polymer；
4th step, the solid polymer being obtained by filtration, dry 4-6h, obtains object under 60-80 DEG C of vacuum.
Advantageous effect：A kind of method that graphene-poly styrene composite material is prepared by graphite and styrene of the present invention,
It is combined using mechanical force and chemical-ultrasound and emulsion polymerization, is raw material rather than graphene for raw material using graphite, to prepare stone
Black alkene and high molecular composite material.Mechanical stripping is first carried out to graphite by ball-milling method in styrene, is obtained containing graphite
The styrene dispersion liquid of alkene, then dispersion liquid is further disperseed by ultrasonic method, obtain the stone with good dispersion
Black alkene/styrene dispersion liquid, finally carries out emulsion polymerization；It is compound to obtain graphene/polystyrene for filtering after vacuum drying
Material.Since graphite is raw material, key technical problems present in current technology of preparing are solved.The method of the present invention is a kind of ring
Border is friendly, mild condition and can largely prepare functionalization polystyrene/graphene nanocomposite new method, have
Simple process and low cost, environmentally protective advantage.The thermal coefficient of graphene/poly styrene composite material prepared by the present invention
Up to 0.2508W/ (m DEG C), heat decomposition temperature is 360 DEG C, can be used as heat-conductive composite material.
Description of the drawings
Fig. 1 is a kind of FT-IR light preparing graphene-poly styrene composite material by graphite and styrene of the present invention
Spectrogram.
Fig. 2 is a kind of XRD spectra preparing graphene-poly styrene composite material by graphite and styrene of the present invention.
Fig. 3 is a kind of Raman spectrum preparing graphene-poly styrene composite material by graphite and styrene of the present invention
Figure.
Fig. 4 is a kind of TEM image preparing graphene-poly styrene composite material by graphite and styrene of the present invention.
Fig. 5 is a kind of TG curves preparing graphene-poly styrene composite material by graphite and styrene of the present invention.
Specific implementation mode
In conjunction with specific embodiments, the content of present invention is described in detail.
A kind of method that graphene-poly styrene composite material is prepared by graphite and styrene of embodiment 1.The first step,
By the volume of styrene（mL）With the quality of graphite（g）Ratio be 1000:1, styrene and graphite are mixed and are placed on type star
Ball milling removes 6h in formula ball mill, obtains the styrene dispersion liquid containing graphene；
Second step, then the dispersion liquid of above-mentioned graphene and styrene is placed in ultrasonic disperse 2h in digital control type ultrasonic device, into traveling
The dispersion of one step obtains the graphene with good dispersion/styrene dispersion liquid；
Third walks, and is 1 in mass ratio by polyvinyl alcohol and deionized water：3 are added to three equipped with blender and reflux condensing tube
In neck reactor, when heating water bath is warming up to 70 DEG C, the volume for closing liquid is dissipated by graphene and styrene（mL）With two isobutyl of azo
Nitrile（g）Ratio be 80：1 adds in reactor, is that 420 r/min are stirred with mixing speed, increases bath temperature to 87
DEG C, 2 h of constant temperature then raises temperature to 90 DEG C, and constant temperature half an hour, polymerisation terminates, and obtains solid polymer；
4th step, the solid polymer being obtained by filtration, dry 6h, obtains object under 80 DEG C of vacuum.
The structure of graphene-poly styrene composite material is prepared by IR, XRD, RAMAN and TEM by graphite and styrene
Phenetic analysis；Thermal coefficient measures the thermal coefficient of composite material with DZDR-S type conductometers.Electrical conductivity is high using ZC36 types
It hinders instrument and UT70A new digital multimeters measures the resistance of composite material.
The thermal coefficient of graphene/poly styrene composite material prepared by embodiment 1- embodiments 4, is shown in Table 1.
Fig. 1 is the FT-IR spectrograms of 1 composite material of embodiment.Wherein, 755 cm-1It is nearby the carbon atom on phenyl ring
Deformation vibration peak between its connected hydrogen, 1450-1600 cm-1It is the peak that phenyl ring skeletal vibration generates, 2843-3000
cm-1It is CH stretching vibration appearances, 3000-3100cm-1It is the stretching vibration peak of unsaturated carbon hydrogen group on phenyl ring.
Fig. 2 is 4 composite material XRD spectra of embodiment 1- embodiments.Wherein, the figure of 4 embodiments is at 2 θ=11.2 °
The peak that d=0.79nm is presented, illustrates there are graphite-like structure, 2 θ=20 ° or so appearance, it is known that there are polystyrene.
Fig. 3 is the Raman spectrograms of 1 composite material of embodiment.Wherein, 1350cm-1Neighbouring D band appearances are due to graphite
The SP that the defect of alkene lattice is generated with disordering induction2Caused by hydridization defect symmetrical stretching vibration, the crystalline substance of graphene is indicated
Lattice defect, 1580cm-1Neighbouring G band appearances are orderly SP in graphene2Stretching vibration characteristic peak in carbon atom face, 2700 cm-1
For neighbouring 2D with the increase that appearance is with the number of plies, peak value is transferred to higher wave number, 3100 cm-1What is nearby represented is polyphenyl
The characteristic peak of ethylene.
Fig. 4 is the TEM image of 1 composite material of embodiment.It can be seen that orderly build stack, and it is observed that it is left
The graphene of inferior horn, shows and contains graphene in polystyrene.
Fig. 5 is the TG curves of 1 composite material of embodiment.As can be seen from the figure the temperature of initial decomposition of material is 360 DEG C.
A kind of method that graphene-poly styrene composite material is prepared by graphite and styrene of embodiment 2.The first step,
By the volume of styrene（mL）With the quality of graphite（g）Ratio be 1000:3, styrene and graphite are mixed and are placed on planet
Ball milling removes 12h in formula ball mill, obtains the styrene dispersion liquid containing graphene；
Second step, then the dispersion liquid of above-mentioned graphene and styrene is placed in ultrasonic disperse 4h in digital control type ultrasonic device, into traveling
The dispersion of one step obtains the graphene with good dispersion/styrene dispersion liquid；
Third walks, and is 1 in mass ratio by polyvinyl alcohol and deionized water：3 are added to three equipped with blender and reflux condensing tube
In neck reactor, when heating water bath is warming up to 70 DEG C, the volume for closing liquid is dissipated by graphene and styrene（mL）With two isobutyl of azo
Nitrile（g）Ratio be 80：1 adds in reactor, is that 420 r/min are stirred with mixing speed, increases bath temperature to 87
DEG C, 2 h of constant temperature then raises temperature to 90 DEG C, and constant temperature half an hour, polymerisation terminates, and obtains solid polymer；
4th step, the solid polymer being obtained by filtration, dry 6h, obtains object under 80 DEG C of vacuum.
A kind of method that graphene-poly styrene composite material is prepared by graphite and styrene of embodiment 3.The first step is pressed
The volume of styrene（mL）With the quality of graphite（g）Ratio be 1000:5, styrene and graphite are mixed and are placed on type planetary
Ball milling stripping for 24 hours, obtains the styrene dispersion liquid containing graphene in ball mill；
Second step, then the dispersion liquid of above-mentioned graphene and styrene is placed in ultrasonic disperse 6h in digital control type ultrasonic device, into traveling
The dispersion of one step obtains the graphene with good dispersion/styrene dispersion liquid；
Third walks, and is 1 in mass ratio by polyvinyl alcohol and deionized water：3 are added to three equipped with blender and reflux condensing tube
When heating water bath is warming up to 70 DEG C, the volume for closing liquid is dissipated by graphene and styrene for neck reactor（mL）With azodiisobutyronitrile
（g）Ratio be 80：1 adds in reactor, with mixing speed be 420 r/min be stirred, increase bath temperature to 87 DEG C,
2 h of constant temperature then raises temperature to 90 DEG C, and constant temperature half an hour, polymerisation terminates, and obtains solid polymer；
4th step, the solid polymer being obtained by filtration, dry 6h, obtains object under 80 DEG C of vacuum.
A kind of method that graphene-poly styrene composite material is prepared by graphite and styrene of embodiment 4.The first step is pressed
The volume of styrene（mL）With the quality of graphite（g）Ratio be 1000:7, styrene and graphite are mixed and are placed on type planetary
Ball milling removes 36h in ball mill, obtains the styrene dispersion liquid containing graphene；
Second step, then the dispersion liquid of above-mentioned graphene and styrene is placed in ultrasonic disperse 8h in digital control type ultrasonic device, into traveling
The dispersion of one step obtains the graphene with good dispersion/styrene dispersion liquid；
Third walks, and is 1 in mass ratio by polyvinyl alcohol and deionized water：3 are added to three equipped with blender and reflux condensing tube
When heating water bath is warming up to 70 DEG C, the volume for closing liquid is dissipated by graphene and styrene for neck reactor（mL）With azodiisobutyronitrile
（g）Ratio be 80：1 adds in reactor, with mixing speed be 420 r/min be stirred, increase bath temperature to 87 DEG C,
2 h of constant temperature then raises temperature to 90 DEG C, and constant temperature half an hour, polymerisation terminates, and obtains solid polymer；
4th step, the solid polymer being obtained by filtration, dry 6h, obtains object under 80 DEG C of vacuum.
Comparative example
It is 1 in mass ratio by polyvinyl alcohol and deionized water：3 are added to equipped with the reaction of three necks of blender and reflux condensing tube
Device when heating water bath is warming up to 70 DEG C, is added the styrene solvent dissolved with 0.125g azodiisobutyronitriles, is with mixing speed
420 r/min are stirred, and increase bath temperature to 87 DEG C, 2 h of constant temperature, then raise temperature to 90 DEG C, and constant temperature half an hour polymerize
Reaction terminates；The solid polymer being obtained by filtration, dry 6h obtains polystyrene product under 80 DEG C of vacuum.
The thermal coefficient of graphene/poly styrene composite material prepared by the present invention, is shown in Table 1.
。
Claims (3)
1. a kind of method preparing graphene-poly styrene composite material by graphite and styrene, it is characterised in that step and item
Part is as follows：
The first step, by the volume of styrene（mL）With graphite（g）Ratio be 1000: 1-1000：7, by styrene and graphite
Mixing is placed on ball milling in type planetary ball mill and removes 6h-36h, obtains the styrene dispersion liquid containing graphene；
Second step, then the dispersion liquid of above-mentioned graphene and styrene is placed in ultrasonic disperse 2h-8h in digital control type ultrasonic device, it carries out
Further dispersion, obtains the graphene with good dispersion/styrene dispersion liquid；
Third walks, and is 1 by polyvinyl alcohol and deionized water quality ratio：3 are added to three necks equipped with blender and reflux condensing tube
In reactor, when heating water bath is warming up to 70 DEG C, by the volume of graphene and styrene dispersion liquid（mL）With azodiisobutyronitrile
（g）Ratio be 80：1 adds in reactor, with mixing speed be 420 r/min be stirred, increase bath temperature to 87 DEG C,
2 h of constant temperature then raises temperature to 90 DEG C, and constant temperature half an hour, polymerisation terminates, and obtains solid polymer；
4th step, the solid polymer being obtained by filtration, dry 4-6h, obtains object under 60-80 DEG C of vacuum.
2. a kind of method that graphene-poly styrene composite material is prepared by graphite and styrene according to claim 1,
It is characterized in that, the first step, by the volume of styrene（mL）With the quality of graphite（g）Ratio be 1000:1, by benzene
Ethylene and graphite mixing are placed on ball milling in type planetary ball mill and remove 6h, obtain the styrene dispersion liquid containing graphene；
The second step, then the dispersion liquid of above-mentioned graphene and styrene is placed in ultrasonic disperse 2h in digital control type ultrasonic device,
Further disperseed, obtains the graphene with good dispersion/styrene dispersion liquid；
4th step, the solid polymer being obtained by filtration, dry 6h, obtains object under 80 DEG C of vacuum.
3. a kind of method that graphene-poly styrene composite material is prepared by graphite and styrene according to claim 1,
It is characterized in that, the first step, by the volume of styrene（mL）With the quality of graphite（g）Ratio be 1000:7, by benzene
Ethylene and graphite mixing are placed on ball milling in type planetary ball mill and remove 36h, obtain the styrene dispersion liquid containing graphene；
The second step, then the dispersion liquid of above-mentioned graphene and styrene is placed in ultrasonic disperse 8h in digital control type ultrasonic device,
Further disperseed, obtains the graphene with good dispersion/styrene dispersion liquid；
4th step, the solid polymer being obtained by filtration, dry 6h, obtains object under 80 DEG C of vacuum.
Priority Applications (1)
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| CN113387700A (en) * | 2021-07-06 | 2021-09-14 | 山东利特纳米技术有限公司 | Preparation method of compact and flexible graphene/PS composite heat-conducting film |
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| CN102827315A (en) * | 2012-08-30 | 2012-12-19 | 合肥工业大学 | Graphene oxide/polystyrene nano composite and preparation method thereof |
| CN103724869A (en) * | 2013-12-03 | 2014-04-16 | 华侨大学 | Preparation method for mixture of polymer and graphene |
| WO2016101208A1 (en) * | 2014-12-25 | 2016-06-30 | 北京航空航天大学 | Single-layer graphene dispersion liquid and preparation method therefor |
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| CN101864005A (en) * | 2010-06-03 | 2010-10-20 | 华侨大学 | Method for preparing polymer/graphene composite material |
| CN102827315A (en) * | 2012-08-30 | 2012-12-19 | 合肥工业大学 | Graphene oxide/polystyrene nano composite and preparation method thereof |
| CN103724869A (en) * | 2013-12-03 | 2014-04-16 | 华侨大学 | Preparation method for mixture of polymer and graphene |
| WO2016101208A1 (en) * | 2014-12-25 | 2016-06-30 | 北京航空航天大学 | Single-layer graphene dispersion liquid and preparation method therefor |
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| CN113387700A (en) * | 2021-07-06 | 2021-09-14 | 山东利特纳米技术有限公司 | Preparation method of compact and flexible graphene/PS composite heat-conducting film |
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