CN112661970A - Graphene crosslinked polystyrene material with high thermal stability and preparation method thereof - Google Patents
Graphene crosslinked polystyrene material with high thermal stability and preparation method thereof Download PDFInfo
- Publication number
- CN112661970A CN112661970A CN202011451503.2A CN202011451503A CN112661970A CN 112661970 A CN112661970 A CN 112661970A CN 202011451503 A CN202011451503 A CN 202011451503A CN 112661970 A CN112661970 A CN 112661970A
- Authority
- CN
- China
- Prior art keywords
- graphene
- polystyrene
- thermal stability
- high thermal
- oil bath
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Images
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to the technical field of polystyrene and discloses a graphene crosslinked polystyrene material with high thermal stability, the alkynyl functionalized graphene is used as neutral crosslinking, the alkynyl is used as a crosslinking active site, so that the alkynyl of the functionalized graphene, click cycloaddition reaction is carried out on the graphene and azide groups of the polystyrene to lead the polystyrene to be chemically crosslinked on the surface of the graphene, by the combination of chemical covalent bonds, the compatibility and the interface affinity of the graphene and the polystyrene are improved, the agglomeration and sedimentation of the graphene nano particles are avoided, the high-dispersion graphene nano particles obviously enhance the tensile strength, the Young modulus and other toughness and mechanical strength of the polystyrene, the graphene with excellent thermodynamic property also obviously enhances the glass transition temperature and the initial decomposition temperature of the polystyrene, and the thermal stability of the polystyrene is enhanced.
Description
Technical Field
The invention relates to the technical field of polystyrene, in particular to a graphene crosslinked polystyrene material with high thermal stability and a preparation method thereof.
Background
Polymer materials such as plastics, rubber and fiber are widely used in human life, and play an indispensable important role, with the development of science and technology, the performance requirements of people on polymer materials are continuously improved, and the single performance of traditional polymer materials such as epoxy resin and polystyrene can not meet the requirements of industrial development and life production, so that the development of high-performance functional polymer materials is needed.
Polystyrene has the advantages of good insulating property, good processing fluidity, strong chemical corrosion resistance and the like, and has important application in the fields of light industry markets, daily decoration, electrical insulation, heat insulation and heat preservation materials, parts of optical chemical instruments and the like, but the traditional polystyrene has large brittleness, lower toughness and impact resistance, poorer mechanical properties such as tensile strength and the like, limits the development and application of the polystyrene, has low thermal stability and is easy to decompose and burn at high temperature, so the mechanical strength and the thermal stability of the polystyrene material need to be improved, graphene is a two-dimensional nano material, has unique mechanical property, thermodynamic property, electrical property and the like, can be used as a nano filler, has wide application in high polymer, but has poor compatibility and interface affinity with the polystyrene, and has larger van der Waals force among graphene particles, is easy to be dispersed unevenly in polystyrene to form agglomeration and sedimentation, thereby influencing the service performance of polystyrene.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a graphene cross-linked polystyrene material with high thermal stability and a preparation method thereof, which solve the problem that graphene is easy to agglomerate in polystyrene and solve the problems of low mechanical properties such as toughness, tensile strength and the like and poor thermal stability of the polystyrene material.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a high-thermal-stability graphene cross-linked polystyrene material is prepared by the following steps:
(1) adding a mixed solvent of deionized water and ethanol into a reaction bottle, adding graphene oxide, uniformly dispersing, adding 4-aminophenylacetylene, placing in an oil bath reaction pot, heating to 90-120 ℃, carrying out reflux reaction for 24-48h, carrying out centrifugal separation, washing with ethanol, and drying to obtain the alkynyl functionalized graphene.
(2) Adding deionized water, styrene, 4-bromostyrene and dispersant sodium dodecyl sulfate into a reaction bottle, heating to 70-80 ℃, dropwise adding initiator azobisisobutyronitrile, reacting for 5-10h, carrying out reduced pressure distillation, washing with deionized water and ethanol, and drying to obtain the brominated polystyrene copolymer.
(3) Adding an N, N-dimethylformamide solvent and a brominated polystyrene copolymer into a reaction bottle, stirring and swelling for 6-12h, adding a catalyst cuprous iodide and a ligand L-proline in a nitrogen atmosphere, placing the mixture into an oil bath reaction kettle, heating to 90-110 ℃, uniformly stirring, adding accelerators potassium carbonate and sodium azide, reacting for 20-40h, centrifugally separating to remove the solvent, and washing with ethanol and diethyl ether to obtain the azide polystyrene.
(4) Adding azide polystyrene into an N, N-dimethylformamide solvent, stirring and swelling for 6-12h, adding alkynyl functionalized graphene in a nitrogen atmosphere, adding a cocatalyst sodium ascorbate and a catalyst copper sulfate after uniform dispersion, heating to 80-120 ℃, reacting for 24-48h, centrifugally separating to remove the solvent, and washing with distilled water and ethanol to obtain the graphene crosslinked polystyrene material with high thermal stability.
Preferably, the mass ratio of the graphene oxide to the 4-aminophenylacetylene in the step (1) is 100: 5-15.
Preferably, the oil bath reaction pot in the step (1) comprises a constant temperature heater, the oil bath pot is arranged above the constant temperature heater, a supporting block is fixedly connected inside the oil bath pot, a telescopic rod is fixedly connected with the supporting block, the telescopic rod is fixedly connected with a supporting rod, a clamping plate is fixedly connected with the supporting rod, and a reaction bottle is movably connected with the clamping plate.
Preferably, the mass ratio of the styrene to the 4-bromostyrene to the sodium dodecyl sulfate to the azobisisobutyronitrile in the step (2) is 100:1.5-6:0.2-0.5: 4-8.
Preferably, the mass ratio of the brominated polystyrene copolymer, the cuprous iodide, the L-proline, the potassium carbonate and the sodium azide in the step (3) is 100:1.5-6:1-4:1.2-5: 0.5-3.
Preferably, the mass ratio of the azide polystyrene, the alkynyl functionalized graphene, the sodium ascorbate and the copper sulfate in the step (4) is 100:0.5-2:1.5-2.5:0.02-0.08: 0.03-0.1.
Drawings
FIG. 1 is a schematic view of the structure of an oil bath reactor;
FIG. 2 is a schematic view of the telescopic rod structure;
figure 3 is a schematic diagram of card adjustment.
1-constant temperature heater; 2-oil bath pan; 3-a support block; 4, a telescopic rod; 5-a support rod; 6-clamping plate; 7-reaction flask.
(III) advantageous technical effects
Compared with the prior art, the invention has the following chemical mechanism and beneficial technical effects:
according to the graphene cross-linked polystyrene material with high thermal stability, rich epoxy groups and carboxyl groups of graphene oxide react with amino groups of 4-aminophenylacetylene to obtain alkynyl functionalized graphene, alkynyl functional modification of the graphene is realized, styrene and 4-bromostyrene are copolymerized to obtain a brominated polystyrene copolymer, L-proline is used as a ligand, cuprous iodide is used as a catalyst, potassium carbonate is used as an accelerator, sodium azide and bromine atoms of the brominated polystyrene copolymer are subjected to substitution reaction to obtain azido polystyrene, and thus the azido groups are introduced to para-carbon atoms of aromatic rings of the polystyrene.
According to the graphene crosslinked polystyrene material with high thermal stability, in a copper sulfate and sodium ascorbate concerted catalysis system, alkynyl functionalized graphene is used as crosslinking neutrality, and alkynyl is used as a crosslinking active site, so that alkynyl of the functionalized graphene and azide groups of azide polystyrene are subjected to rapid and efficient click cycloaddition reaction, polystyrene is subjected to chemical crosslinking on the surface of the graphene, the compatibility and interface affinity of the graphene and the polystyrene are greatly improved through the combination of chemical covalent bonds, under the modification effect of the chemical covalent bonds, agglomeration and sedimentation among graphene nanoparticles are avoided, the high-dispersion graphene nanoparticles remarkably enhance the tensile strength, the toughness such as Young modulus and the like and the mechanical strength of the polystyrene, and meanwhile, the graphene with excellent thermodynamic properties obviously improves the glass transition temperature and the initial decomposition temperature of the polystyrene, the thermal stability of polystyrene is enhanced.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: a graphene cross-linked polystyrene material with high thermal stability is prepared by the following steps:
(1) adding a mixed solvent of deionized water and ethanol into a reaction bottle, adding graphene oxide, uniformly dispersing, adding 4-aminophenylacetylene, wherein the mass ratio of the deionized water to the ethanol is 100:5-15, placing the reaction bottle in an oil bath reaction pot, wherein the oil bath reaction pot comprises a constant temperature heater, the oil bath pot is arranged above the constant temperature heater, a supporting block is fixedly connected inside the oil bath pot, a telescopic rod is fixedly connected with the supporting block, the telescopic rod is fixedly connected with a supporting rod, the supporting rod is fixedly connected with a clamping plate, the clamping plate is movably connected with the reaction bottle, heating is carried out to 90-120 ℃, carrying out reflux reaction for 24-48h, carrying out centrifugal separation, washing with ethanol and drying.
(2) Adding deionized water as a solvent, styrene, 4-bromostyrene and a dispersant sodium dodecyl sulfate into a reaction bottle, heating to 70-80 ℃, dropwise adding an initiator azobisisobutyronitrile with the mass ratio of 100:1.5-6:0.2-0.5:4-8, reacting for 5-10h, distilling under reduced pressure, washing with deionized water and ethanol, and drying to obtain the brominated polystyrene copolymer.
(3) Adding an N, N-dimethylformamide solvent and a brominated polystyrene copolymer into a reaction bottle, stirring and swelling for 6-12h, adding a catalyst cuprous iodide and a ligand L-proline in a nitrogen atmosphere, placing the mixture into an oil bath reaction kettle, heating to 90-110 ℃, uniformly stirring, adding accelerators potassium carbonate and sodium azide, reacting for 20-40h, centrifugally separating to remove the solvent, and washing with ethanol and diethyl ether to obtain the azido polystyrene, wherein the mass ratio of the brominated polystyrene copolymer, the cuprous iodide, the L-proline, the potassium carbonate and the sodium azide is 100:1.5-6:1-4:1.2-5: 0.5-3.
(4) Adding azido polystyrene into an N, N-dimethylformamide solvent, stirring and swelling for 6-12h, adding alkynyl functionalized graphene in a nitrogen atmosphere, uniformly dispersing, adding a cocatalyst sodium ascorbate and a catalyst copper sulfate, wherein the mass ratio of the azido polystyrene to the alkynyl functionalized graphene to the sodium ascorbate to the copper sulfate is 100:0.5-2:1.5-2.5:0.02-0.08:0.03-0.1, heating to 80-120 ℃, reacting for 24-48h, centrifugally separating to remove the solvent, and washing with distilled water and ethanol to obtain the graphene crosslinked polystyrene material with high thermal stability.
Example 1
(1) Adding a mixed solvent of deionized water and ethanol into a reaction bottle, adding graphene oxide, uniformly dispersing, adding 4-aminophenylacetylene, wherein the mass ratio of the deionized water to the ethanol is 100:5, placing the reaction bottle in an oil bath reaction pot, wherein the oil bath reaction pot comprises a constant temperature heater, the oil bath pot is arranged above the constant temperature heater, a supporting block is fixedly connected inside the oil bath pot, a telescopic rod is fixedly connected with the supporting block, the telescopic rod is fixedly connected with a supporting rod, a clamping plate is fixedly connected with the supporting rod, the clamping plate is movably connected with the reaction bottle, heating is carried out to 90 ℃, carrying out reflux reaction for 24 hours, carrying out centrifugal separation, washing with ethanol and drying.
(2) Adding deionized water serving as a solvent, styrene, 4-bromostyrene and a dispersant sodium dodecyl sulfate into a reaction bottle, heating to 70 ℃, dropwise adding an initiator azobisisobutyronitrile with the mass ratio of 100:1.5:0.2:4, reacting for 5 hours, distilling under reduced pressure, washing with deionized water and ethanol, and drying to obtain the brominated polystyrene copolymer.
(3) Adding an N, N-dimethylformamide solvent and a brominated polystyrene copolymer into a reaction bottle, stirring and swelling for 6h, adding cuprous iodide and a ligand L-proline as catalysts in a nitrogen atmosphere, placing the mixture into an oil bath reaction kettle, heating to 90 ℃, uniformly stirring, adding potassium carbonate and sodium azide as accelerators, wherein the mass ratio of the cuprous iodide to the L-proline to the potassium carbonate to the sodium azide is 100:1.5:1:1.2:0.5, reacting for 20h, centrifugally separating to remove the solvent, and washing with ethanol and ether to obtain the azido polystyrene.
(4) Adding azide polystyrene into an N, N-dimethylformamide solvent, stirring and swelling for 6h, adding alkynyl functionalized graphene in a nitrogen atmosphere, uniformly dispersing, adding a cocatalyst sodium ascorbate and a catalyst copper sulfate, heating to 80 ℃, reacting for 24h, centrifugally separating to remove the solvent, and washing with distilled water and ethanol to obtain the graphene crosslinked polystyrene material with high thermal stability.
Example 2
(1) Adding a mixed solvent of deionized water and ethanol into a reaction bottle, adding graphene oxide, uniformly dispersing, adding 4-aminophenylacetylene, wherein the mass ratio of the deionized water to the ethanol is 100:8, placing the reaction bottle in an oil bath reaction pot, wherein the oil bath reaction pot comprises a constant temperature heater, the oil bath pot is arranged above the constant temperature heater, a supporting block is fixedly connected inside the oil bath pot, a telescopic rod is fixedly connected with the supporting block, the telescopic rod is fixedly connected with a supporting rod, a clamping plate is fixedly connected with the supporting rod, the clamping plate is movably connected with the reaction bottle, heating is carried out to 100 ℃, carrying out reflux reaction for 36 hours, carrying out centrifugal separation, washing with ethanol and drying.
(2) Adding deionized water serving as a solvent, styrene, 4-bromostyrene and a dispersant sodium dodecyl sulfate into a reaction bottle, heating to 80 ℃, dropwise adding an initiator azobisisobutyronitrile with the mass ratio of 100:3:0.3:5, reacting for 5 hours, distilling under reduced pressure, washing with deionized water and ethanol, and drying to obtain the brominated polystyrene copolymer.
(3) Adding an N, N-dimethylformamide solvent and a brominated polystyrene copolymer into a reaction bottle, stirring and swelling for 12h, adding cuprous iodide and a ligand L-proline as catalysts in a nitrogen atmosphere, placing the mixture into an oil bath reaction kettle, heating to 110 ℃, uniformly stirring, adding potassium carbonate and sodium azide as accelerators, wherein the mass ratio of the cuprous iodide to the L-proline to the potassium carbonate to the sodium azide is 100:3:2:2:1, reacting for 40h, centrifugally separating to remove the solvent, and washing with ethanol and diethyl ether to obtain the azido polystyrene.
(4) Adding azide polystyrene into an N, N-dimethylformamide solvent, stirring and swelling for 12h, adding alkynyl functionalized graphene in a nitrogen atmosphere, uniformly dispersing, adding a cocatalyst sodium ascorbate and a catalyst copper sulfate, heating to 120 ℃, reacting for 36h, centrifugally separating to remove the solvent, and washing with distilled water and ethanol to obtain the graphene crosslinked polystyrene material with high thermal stability.
Example 3
(1) Adding a mixed solvent of deionized water and ethanol into a reaction bottle, adding graphene oxide, uniformly dispersing, adding 4-aminophenylacetylene, wherein the mass ratio of the deionized water to the ethanol is 100:15, placing the reaction bottle in an oil bath reaction pot, wherein the oil bath reaction pot comprises a constant temperature heater, the oil bath pot is arranged above the constant temperature heater, a supporting block is fixedly connected inside the oil bath pot, a telescopic rod is fixedly connected with the supporting block, the telescopic rod is fixedly connected with a supporting rod, a clamping plate is fixedly connected with the supporting rod, the clamping plate is movably connected with the reaction bottle, heating is carried out to 120 ℃, carrying out reflux reaction for 48 hours, carrying out centrifugal separation, washing with ethanol and drying.
(2) Adding deionized water serving as a solvent, styrene, 4-bromostyrene and a dispersant sodium dodecyl sulfate into a reaction bottle, heating to 80 ℃, dropwise adding an initiator azobisisobutyronitrile with the mass ratio of 100:6:0.5:8, reacting for 10 hours, distilling under reduced pressure, washing with deionized water and ethanol, and drying to obtain the brominated polystyrene copolymer.
(3) Adding an N, N-dimethylformamide solvent and a brominated polystyrene copolymer into a reaction bottle, stirring and swelling for 12h, adding cuprous iodide and a ligand L-proline as catalysts in a nitrogen atmosphere, placing the mixture into an oil bath reaction kettle, heating to 110 ℃, uniformly stirring, adding potassium carbonate and sodium azide as accelerators, wherein the mass ratio of the cuprous iodide to the L-proline to the potassium carbonate to the sodium azide is 100:6:4:5:3, reacting for 40h, centrifugally separating to remove the solvent, and washing with ethanol and diethyl ether to obtain the azido polystyrene.
(4) Adding azide polystyrene into an N, N-dimethylformamide solvent, stirring and swelling for 12h, adding alkynyl functionalized graphene in a nitrogen atmosphere, uniformly dispersing, adding a cocatalyst sodium ascorbate and a catalyst copper sulfate, heating to 120 ℃, reacting for 48h, centrifugally separating to remove the solvent, and washing with distilled water and ethanol to obtain the graphene crosslinked polystyrene material with high thermal stability.
Comparative example 1
(1) Adding a mixed solvent of deionized water and ethanol into a reaction bottle, adding graphene oxide, uniformly dispersing, adding 4-aminophenylacetylene, wherein the mass ratio of the deionized water to the ethanol is 100:2, placing the reaction bottle in an oil bath reaction pot, wherein the oil bath reaction pot comprises a constant-temperature heater, the oil bath pot is arranged above the constant-temperature heater, a supporting block is fixedly connected inside the oil bath pot, a telescopic rod is fixedly connected with the supporting block, the telescopic rod is fixedly connected with a supporting rod, the supporting rod is fixedly connected with a clamping plate, the clamping plate is movably connected with the reaction bottle, heating is carried out to 110 ℃, carrying out reflux reaction for 48 hours, carrying out centrifugal separation, washing with ethanol and.
(2) Adding deionized water serving as a solvent, styrene, 4-bromostyrene and a dispersant sodium dodecyl sulfate into a reaction bottle, heating to 80 ℃, dropwise adding an initiator azobisisobutyronitrile with the mass ratio of 100:0.5:0.08:2, reacting for 5 hours, distilling under reduced pressure, washing with deionized water and ethanol, and drying to obtain the brominated polystyrene copolymer.
(3) Adding an N, N-dimethylformamide solvent and a brominated polystyrene copolymer into a reaction bottle, stirring and swelling for 6h, adding cuprous iodide and a ligand L-proline as catalysts in a nitrogen atmosphere, placing the mixture into an oil bath reaction kettle, heating to 110 ℃, uniformly stirring, adding potassium carbonate and sodium azide as accelerators, wherein the mass ratio of the cuprous iodide to the L-proline to the potassium carbonate to the sodium azide is 100:0.5:0.4:0.5:0.1, reacting for 40h, centrifugally separating to remove the solvent, and washing with ethanol and ether to obtain the azido polystyrene.
(4) Adding azide polystyrene into an N, N-dimethylformamide solvent, stirring and swelling for 10h, adding alkynyl functionalized graphene in a nitrogen atmosphere, uniformly dispersing, adding a cocatalyst sodium ascorbate and a catalyst copper sulfate, heating to 120 ℃, reacting for 48h, centrifugally separating to remove the solvent, and washing with distilled water and ethanol to obtain the graphene crosslinked polystyrene material with high thermal stability.
Comparative example 2
(1) Adding a mixed solvent of deionized water and ethanol into a reaction bottle, adding graphene oxide, uniformly dispersing, adding 4-aminophenylacetylene, wherein the mass ratio of the deionized water to the ethanol is 100:20, placing the reaction bottle in an oil bath reaction pot, wherein the oil bath reaction pot comprises a constant temperature heater, the oil bath pot is arranged above the constant temperature heater, a supporting block is fixedly connected inside the oil bath pot, a telescopic rod is fixedly connected with the supporting block, the telescopic rod is fixedly connected with a supporting rod, a clamping plate is fixedly connected with the supporting rod, the clamping plate is movably connected with the reaction bottle, heating is carried out to 90 ℃, carrying out reflux reaction for 48 hours, carrying out centrifugal separation, washing with ethanol and drying.
(2) Adding deionized water serving as a solvent, styrene, 4-bromostyrene and a dispersant sodium dodecyl sulfate into a reaction bottle, heating to 75 ℃, dropwise adding an initiator azobisisobutyronitrile with the mass ratio of 100:7:0.65:10, reacting for 8 hours, distilling under reduced pressure, washing with deionized water and ethanol, and drying to obtain the brominated polystyrene copolymer.
(3) Adding an N, N-dimethylformamide solvent and a brominated polystyrene copolymer into a reaction bottle, stirring and swelling for 12h, adding cuprous iodide and a ligand L-proline as catalysts in a nitrogen atmosphere, placing the mixture into an oil bath reaction kettle, heating to 90 ℃, uniformly stirring, adding potassium carbonate and sodium azide as accelerators, wherein the mass ratio of the cuprous iodide to the L-proline to the potassium carbonate to the sodium azide is 100:8:5:6:4.5, reacting for 40h, centrifugally separating to remove the solvent, and washing with ethanol and diethyl ether to obtain the azido polystyrene.
(4) Adding azido polystyrene into an N, N-dimethylformamide solvent, stirring and swelling for 6-12h, adding alkynyl functionalized graphene in a nitrogen atmosphere, uniformly dispersing, adding a cocatalyst sodium ascorbate and a catalyst copper sulfate, wherein the mass ratio of the azido polystyrene to the alkynyl functionalized graphene to the sodium ascorbate to the copper sulfate is 100:2.5:3:2:0.12, heating to 80-120 ℃, reacting for 24-48h, centrifugally separating to remove the solvent, and washing with distilled water and ethanol to obtain the high-thermal-stability graphene crosslinked polystyrene material.
The glass transition temperature and the decomposition temperature of the graphene cross-linked polystyrene material with high thermal stability are tested by using a STA449F5 synchronous thermal analyzer, and the test standard is GB/T31850-2015.
And testing the tensile strength and Young modulus of the graphene cross-linked polystyrene material with high thermal stability by using a CMT-200 microcomputer control electronic universal testing machine, wherein the test standard is GB/T1040.3-2006.
Claims (6)
1. A high thermal stability graphene cross-linked polystyrene material is characterized in that: the preparation method of the graphene crosslinked polystyrene material with high thermal stability comprises the following steps:
(1) adding a mixed solvent of deionized water and ethanol into a reaction bottle, adding graphene oxide, uniformly dispersing, adding 4-aminophenylacetylene, placing the mixture into an oil bath reaction pot, heating to 90-120 ℃, carrying out reflux reaction for 24-48h, carrying out centrifugal separation and washing to obtain alkynyl functionalized graphene;
(2) adding deionized water, styrene, 4-bromostyrene and dispersant sodium dodecyl sulfate into a reaction bottle, heating to 70-80 ℃, dropwise adding initiator azobisisobutyronitrile, reacting for 5-10h, distilling under reduced pressure and washing to obtain brominated polystyrene copolymer;
(3) adding an N, N-dimethylformamide solvent and a brominated polystyrene copolymer into a reaction bottle, stirring and swelling for 6-12h, adding a catalyst cuprous iodide and a ligand L-proline in a nitrogen atmosphere, placing the mixture into an oil bath reaction kettle, heating to 90-110 ℃, uniformly stirring, adding accelerators potassium carbonate and sodium azide, reacting for 20-40h, centrifugally separating and washing to obtain azide polystyrene;
(4) adding azide polystyrene into an N, N-dimethylformamide solvent, stirring and swelling for 6-12h, adding alkynyl functionalized graphene in a nitrogen atmosphere, adding a cocatalyst sodium ascorbate and a catalyst copper sulfate after uniform dispersion, heating to 80-120 ℃, reacting for 24-48h, and performing centrifugal separation and washing to obtain the graphene crosslinked polystyrene material with high thermal stability.
2. The graphene cross-linked polystyrene material with high thermal stability as claimed in claim 1, wherein: the mass ratio of the graphene oxide to the 4-aminophenylacetylene in the step (1) is 100: 5-15.
3. The graphene cross-linked polystyrene material with high thermal stability as claimed in claim 1, wherein: the oil bath reaction pot in the step (1) comprises a constant temperature heater, the oil bath pot is arranged above the constant temperature heater, a supporting block is fixedly connected inside the oil bath pot, a telescopic rod is fixedly connected with the supporting block, the telescopic rod is fixedly connected with a supporting rod, a clamping plate is fixedly connected with the supporting rod, and a reaction bottle is movably connected with the clamping plate.
4. The graphene cross-linked polystyrene material with high thermal stability as claimed in claim 1, wherein: the mass ratio of the styrene to the 4-bromostyrene to the sodium dodecyl sulfate to the azobisisobutyronitrile in the step (2) is 100:1.5-6:0.2-0.5: 4-8.
5. The graphene cross-linked polystyrene material with high thermal stability as claimed in claim 1, wherein: the mass ratio of the brominated polystyrene copolymer, the cuprous iodide, the L-proline, the potassium carbonate and the sodium azide in the step (3) is 100:1.5-6:1-4:1.2-5: 0.5-3.
6. The graphene cross-linked polystyrene material with high thermal stability as claimed in claim 1, wherein: the mass ratio of the azide polystyrene, the alkynyl functionalized graphene, the sodium ascorbate and the copper sulfate in the step (4) is 100:0.5-2:1.5-2.5:0.02-0.08: 0.03-0.1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011451503.2A CN112661970A (en) | 2020-12-10 | 2020-12-10 | Graphene crosslinked polystyrene material with high thermal stability and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011451503.2A CN112661970A (en) | 2020-12-10 | 2020-12-10 | Graphene crosslinked polystyrene material with high thermal stability and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112661970A true CN112661970A (en) | 2021-04-16 |
Family
ID=75402436
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011451503.2A Withdrawn CN112661970A (en) | 2020-12-10 | 2020-12-10 | Graphene crosslinked polystyrene material with high thermal stability and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112661970A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112812754A (en) * | 2021-02-07 | 2021-05-18 | 广西师范大学 | Phenylacetylene functionalized graphene/copper composite heat conduction material and preparation method thereof |
-
2020
- 2020-12-10 CN CN202011451503.2A patent/CN112661970A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112812754A (en) * | 2021-02-07 | 2021-05-18 | 广西师范大学 | Phenylacetylene functionalized graphene/copper composite heat conduction material and preparation method thereof |
| CN112812754B (en) * | 2021-02-07 | 2021-07-16 | 广西师范大学 | Phenylacetylene functionalized graphene/copper composite heat conduction material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108264735B (en) | Preparation method of toughened, heat-conducting and insulating epoxy resin-based composite material | |
| CN115806685B (en) | Polyimide film and preparation method thereof | |
| CN109762436B (en) | Low-temperature-resistant heat-conducting insulating resin paint suitable for superconducting insulating material and preparation method and application thereof | |
| CN112661970A (en) | Graphene crosslinked polystyrene material with high thermal stability and preparation method thereof | |
| CN109929273B (en) | Preparation and application of modified graphene oxide | |
| CN112321852A (en) | High-strength graphene-polyacrylic acid composite conductive hydrogel and preparation method thereof | |
| CN111849105A (en) | Polyphosphazene-boron nitride modified acrylic resin flame retardant material and preparation method thereof | |
| CN111363311A (en) | Graphene-anhydride curing agent modified waterborne epoxy resin material and preparation method thereof | |
| CN111234897B (en) | Silicone oil modified carbon material heat-conducting lubricating additive and preparation method thereof | |
| CN111334001A (en) | High-thermal-conductivity boron nitride modified epoxy resin insulating material and preparation method thereof | |
| CN110105718B (en) | New energy automobile battery encapsulating material and preparation method thereof | |
| CN111484626A (en) | Modified boron nitride grafted waterborne acrylic resin insulating material and preparation method thereof | |
| CN106751839A (en) | Fuel cell polymer microsphere/sulfonated poly aryl ether ketone sulfone proton exchange membrane material, preparation method and applications containing amino | |
| CN108587068A (en) | A kind of hydrophobic fire retarding epoxide resin and preparation method thereof | |
| CN114806090B (en) | High-heat-conductivity insulating epoxy resin composite material and preparation method thereof | |
| CN111500018A (en) | SiO2 modified fluorinated epoxy resin super-hydrophobic material and preparation method thereof | |
| CN113871634B (en) | Carbon fiber composite material for fuel cell bipolar plate | |
| CN111495321B (en) | Magnetic hyperbranched polymer-based porous carbon adsorption material and preparation method thereof | |
| CN110294915B (en) | Graphene in-situ modified epoxy SBS resin and preparation method thereof | |
| CN109553929B (en) | Nano flame-retardant epoxy resin composite material and preparation method thereof | |
| CN111393993A (en) | Super-hydrophobic polyaniline-acrylate copolymer anticorrosive coating and preparation method thereof | |
| CN110591081A (en) | Carboxyl-functionalized fluorine-containing polyarylether resin and preparation method thereof | |
| CN111471175A (en) | Wear-resistant nano SiO2-polyurea in-situ modified polyimide material and preparation method thereof | |
| CN111471275A (en) | Carbon nanotube-acrylic resin synergistic modified epoxy resin and preparation method thereof | |
| CN116454307B (en) | Manufacturing method of composite graphite bipolar plate for fuel cell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20210416 |
|
| WW01 | Invention patent application withdrawn after publication |