CN106750279A - The preparation method of the hollow ferroso-ferric oxide polyaniline nano-composite material of Graphene - Google Patents
The preparation method of the hollow ferroso-ferric oxide polyaniline nano-composite material of Graphene Download PDFInfo
- Publication number
- CN106750279A CN106750279A CN201611120619.1A CN201611120619A CN106750279A CN 106750279 A CN106750279 A CN 106750279A CN 201611120619 A CN201611120619 A CN 201611120619A CN 106750279 A CN106750279 A CN 106750279A
- Authority
- CN
- China
- Prior art keywords
- preparation
- graphene
- ferric oxide
- composite material
- polyaniline nano
- 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.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 title claims abstract description 16
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 16
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 15
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title abstract description 15
- 229940056319 ferrosoferric oxide Drugs 0.000 title abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 13
- 239000010439 graphite Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 12
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 9
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 239000003999 initiator Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical class [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000002131 composite material Substances 0.000 abstract description 5
- 229920003023 plastic Polymers 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 229920003002 synthetic resin Polymers 0.000 abstract description 2
- 239000000057 synthetic resin Substances 0.000 abstract description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
-
- 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
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to synthetic resin and plastics arts, and in particular to a kind of preparation method of the hollow ferroso-ferric oxide polyaniline nano-composite material of Graphene.The preparation method of the hollow ferroso-ferric oxide polyaniline nano-composite material of Graphene, comprises the following steps：（1）Pre-oxidize the preparation of graphite；（2）The preparation of GO；（3）The preparation of the hollow ferroso-ferric oxide polyaniline nano-composite material of Graphene.There is not GO in the diffraction maximum that the angle of diffraction is 10.24 in being successfully supported on graphenic surface, and composite in the hollow ferroso-ferric oxide of the present invention, shows GO in solvent thermal reaction, and Graphene is successfully reduced into the presence of ethylene glycol.
Description
Technical field
The present invention relates to synthetic resin and plastics arts, and in particular to a kind of Graphene-hollow ferroso-ferric oxide-poly-
The preparation method of aniline nano composite.
Background technology
With science and technology and the development of electronics industry, various electronic equipments are in business, industry, health care etc.
Using increasing, electromagnetic interference has become the fourth-largest environomental pollution source after Industrial " three Waste ", electromagnetic pollution into
It is " the stealthy killer " of human society.
The unique single layer structure of Graphene makes it have that density is small, specific surface area is big, electric conductivity is excellent and dielectric constant
High the features such as, as a kind of novel wave-absorbing material.In addition, in the presence of electromagnetic field, graphene oxide (GO) surface is largely sudden and violent
The chemical bond of dew is more prone to the dielectric relaxor of outer-shell electron and electromagnetic wave of decaying, and is that Graphene is opened up in the application for inhaling ripple field
Prospect wide；But used as absorbing material, the maximum shortcoming of Graphene is that do not have magnetic and magnetic loss, and Graphene Jie high
Electrical loss will cause the difficult problem of impedance matching, so as to influence absorbing property.Therefore, it is hollow in graphenic surface carried magnetic
Fe3O4Nano-particle, can not only improve the magnetic property of composite, strengthen magnetic loss, be conducive to the impedance of composite
Match somebody with somebody, and H- Fe3O4Particle can reduce Graphene as spacer medium, and stacking is in three-dimensional graphite structure again in drying process,
To stablize graphene film Rotating fields serve it is considerable.Simultaneously, it is considered to conducting polymer conduct is added in compound system
Clad, not only strengthens magnetic H- Fe3O4The interface cohesion of particle and Graphene, and due to the height of conducting polymer itself
Dielectric loss, enhances absorbing property of the composite in high band.
The content of the invention
The present invention is directed to propose a kind of preparation method of Graphene-hollow ferroso-ferric oxide-polyaniline nano-composite material.
Technical program of the present invention lies in：
The preparation method of Graphene-hollow ferroso-ferric oxide-polyaniline nano-composite material, comprises the following steps：
（1）Pre-oxidize the preparation of graphite：
Add people in 10~16 mL concentrated sulfuric acids successively 2.0~4.0 g graphite powders and 2.0 ~ 3.5 g sodium peroxydisulfates, stirred in 80 DEG C
Mix after 9.0 h with 150~250 mL distilled water dilutings, scrubbed, filtering is dried to constant weight；Pre-oxidation graphite is added to 100
Stirred in~150 mL concentrated sulfuric acids, and the KMnO of 20.0~40.0 g is slowly added under the conditions of ice-water bath4, stirring 0.5~1.0
H, and ultrasonically treated 0.5 h, it is standby；
（2）The preparation of GO：
Pre-oxidation graphite system is warmed up to 35 DEG C, 2.0 h are reacted；Then, the mL distilled water of people 200 is slowly added in system, then instead
2.0 h are answered, control temperature is no more than 50 DEG C, it is 30% that 150~250 mL distilled water and 10~40 mL mass fractions are added again
H2O2Terminating reaction, it is scrubbed and dialyse 5~7 days；
（3）The preparation of Graphene-hollow ferroso-ferric oxide-polyaniline nano-composite material：
By the GO of 0.010 ~ 0.015 g, ultrasonic disperse forms uniform dispersion liquid in 60 mL ethylene glycol, it is subsequently adding 0.42~
The FeCl of 1.68 g3And FeCl3Mixture；0.62 ~ 2.49 g polyvinylpyrrolidones are dissolved in 70 mL ethylene glycol, are stirred into
Settled solution；By in resulting solution 100 mL reactors of immigration, 200~230 DEG C are heated to, and be incubated 10.0 ~ 15.0h；By institute
Black powder centrifugation is obtained, with respectively washing 3 times of absolute ethyl alcohol and deionized water, 24.0 h is vacuum dried in 50~70 DEG C, obtained
To product A；By product A and 0.8 ~ 1.2 g aniline monomers, the pre-dispersed solution for there are a 10.65 g DBSAs is added to
In, the min of ultrasonic disperse 30~60 forms homogeneous system B；1.96~2.94 g ammonium persulfate initiators are dissolved in 50~100
In mL distilled water, it is slowly dropped in system B, the h of stirring reaction 12.0；Through suction filtration, wash colourless to filtrate, in 50~70 DEG C
24.0 ~ 36.0 h of vacuum drying, obtain Graphene-hollow ferroso-ferric oxide-polyaniline nano-composite material.
Described FeCl3And FeCl3The mass ratio of mixture is 1：1.
The technical effects of the invention are that：
The hollow ferroso-ferric oxide of the present invention is successfully supported in graphenic surface, and composite to be there is not GO and is in the angle of diffraction
10.24 diffraction maximum, shows GO in solvent thermal reaction, and Graphene is successfully reduced into the presence of ethylene glycol.
Specific embodiment
The preparation method of Graphene-hollow ferroso-ferric oxide-polyaniline nano-composite material, comprises the following steps：
Embodiment 1
（1）Pre-oxidize the preparation of graphite：
Add people in 10~16 mL concentrated sulfuric acids successively 2.0~4.0 g graphite powders and 2.0 ~ 3.5 g sodium peroxydisulfates, stirred in 80 DEG C
Mix after 9.0 h with 150~250 mL distilled water dilutings, scrubbed, filtering is dried to constant weight；Pre-oxidation graphite is added to 100
Stirred in~150 mL concentrated sulfuric acids, and the KMnO of 20.0~40.0 g is slowly added under the conditions of ice-water bath4, stirring 0.5~1.0
H, and ultrasonically treated 0.5 h, it is standby；
（2）The preparation of GO：
Pre-oxidation graphite system is warmed up to 35 DEG C, 2.0 h are reacted；Then, the mL distilled water of people 200 is slowly added in system, then instead
2.0 h are answered, control temperature is no more than 50 DEG C, it is 30% that 150~250 mL distilled water and 10~40 mL mass fractions are added again
H2O2Terminating reaction, it is scrubbed and dialyse 5~7 days；
（3）The preparation of Graphene-hollow ferroso-ferric oxide-polyaniline nano-composite material：
By the GO of 0.010 ~ 0.015 g, ultrasonic disperse forms uniform dispersion liquid in 60 mL ethylene glycol, it is subsequently adding 0.42~
The FeCl of 1.68 g3And FeCl3Mixture；0.62 ~ 2.49 g polyvinylpyrrolidones are dissolved in 70 mL ethylene glycol, are stirred into
Settled solution；By in resulting solution 100 mL reactors of immigration, 200~230 DEG C are heated to, and be incubated 10.0 ~ 15.0h；By institute
Black powder centrifugation is obtained, with respectively washing 3 times of absolute ethyl alcohol and deionized water, 24.0 h is vacuum dried in 50~70 DEG C, obtained
To product A；By product A and 0.8 ~ 1.2 g aniline monomers, the pre-dispersed solution for there are a 10.65 g DBSAs is added to
In, the min of ultrasonic disperse 30~60 forms homogeneous system B；1.96~2.94 g ammonium persulfate initiators are dissolved in 50~100
In mL distilled water, it is slowly dropped in system B, the h of stirring reaction 12.0；Through suction filtration, wash colourless to filtrate, in 50~70 DEG C
24.0 ~ 36.0 h of vacuum drying, obtain Graphene-hollow ferroso-ferric oxide-polyaniline nano-composite material.
Embodiment 2
On the basis of embodiment 1, described FeCl3And FeCl3The mass ratio of mixture is 1：1.
Claims (2)
1. the preparation method of Graphene-hollow ferroso-ferric oxide-polyaniline nano-composite material, it is characterised in that：Including as follows
Step：
（1）Pre-oxidize the preparation of graphite：
Add people in 10~16 mL concentrated sulfuric acids successively 2.0~4.0 g graphite powders and 2.0 ~ 3.5 g sodium peroxydisulfates, stirred in 80 DEG C
Mix after 9.0 h with 150~250 mL distilled water dilutings, scrubbed, filtering is dried to constant weight；Pre-oxidation graphite is added to 100
Stirred in~150 mL concentrated sulfuric acids, and the KMnO of 20.0~40.0 g is slowly added under the conditions of ice-water bath4, stirring 0.5~1.0
H, and ultrasonically treated 0.5 h, it is standby；
（2）The preparation of GO：
Pre-oxidation graphite system is warmed up to 35 DEG C, 2.0 h are reacted；Then, the mL distilled water of people 200 is slowly added in system, then instead
2.0 h are answered, control temperature is no more than 50 DEG C, it is 30% that 150~250 mL distilled water and 10~40 mL mass fractions are added again
H2O2Terminating reaction, it is scrubbed and dialyse 5~7 days；
（3）The preparation of Graphene-hollow ferroso-ferric oxide-polyaniline nano-composite material：
By the GO of 0.010 ~ 0.015 g, ultrasonic disperse forms uniform dispersion liquid in 60 mL ethylene glycol, it is subsequently adding 0.42~
The FeCl of 1.68 g3And FeCl3Mixture；0.62 ~ 2.49 g polyvinylpyrrolidones are dissolved in 70 mL ethylene glycol, are stirred into
Settled solution；By in resulting solution 100 mL reactors of immigration, 200~230 DEG C are heated to, and be incubated 10.0 ~ 15.0h；By institute
Black powder centrifugation is obtained, with respectively washing 3 times of absolute ethyl alcohol and deionized water, 24.0 h is vacuum dried in 50~70 DEG C, obtained
To product A；By product A and 0.8 ~ 1.2 g aniline monomers, the pre-dispersed solution for there are a 10.65 g DBSAs is added to
In, the min of ultrasonic disperse 30~60 forms homogeneous system B；1.96~2.94 g ammonium persulfate initiators are dissolved in 50~100
In mL distilled water, it is slowly dropped in system B, the h of stirring reaction 12.0；Through suction filtration, wash colourless to filtrate, in 50~70 DEG C
24.0 ~ 36.0 h of vacuum drying, obtain Graphene-hollow ferroso-ferric oxide-polyaniline nano-composite material.
2. the preparation method of Graphene according to claim 1-hollow ferroso-ferric oxide-polyaniline nano-composite material,
It is characterized in that：Described FeCl3And FeCl3The mass ratio of mixture is 1：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611120619.1A CN106750279A (en) | 2016-12-08 | 2016-12-08 | The preparation method of the hollow ferroso-ferric oxide polyaniline nano-composite material of Graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611120619.1A CN106750279A (en) | 2016-12-08 | 2016-12-08 | The preparation method of the hollow ferroso-ferric oxide polyaniline nano-composite material of Graphene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106750279A true CN106750279A (en) | 2017-05-31 |
Family
ID=58882513
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611120619.1A Pending CN106750279A (en) | 2016-12-08 | 2016-12-08 | The preparation method of the hollow ferroso-ferric oxide polyaniline nano-composite material of Graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106750279A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108410350A (en) * | 2018-01-29 | 2018-08-17 | 清华大学 | A kind of preparation method for the intelligent self-lubricating composite including electromagnetism triggering microcapsules |
| CN114284748A (en) * | 2021-12-22 | 2022-04-05 | 四川轻化工大学 | Composite material and preparation method and application thereof |
-
2016
- 2016-12-08 CN CN201611120619.1A patent/CN106750279A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108410350A (en) * | 2018-01-29 | 2018-08-17 | 清华大学 | A kind of preparation method for the intelligent self-lubricating composite including electromagnetism triggering microcapsules |
| CN114284748A (en) * | 2021-12-22 | 2022-04-05 | 四川轻化工大学 | Composite material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liang et al. | Structural design strategies of polymer matrix composites for electromagnetic interference shielding: a review | |
| CN104448305B (en) | A kind of nano combined absorbing material and preparation method thereof | |
| Wang et al. | The green synthesis rGO/Fe3O4/PANI nanocomposites for enhanced electromagnetic waves absorption | |
| CN106496554B (en) | A kind of preparation method of graphene/Fe3O4/ polyaniline ternary Wave suction composite materials | |
| CN103613760B (en) | The preparation method of polyaniline/ferroferoxide oxide electromagnetic composite material | |
| CN104650498B (en) | A kind of Graphene/polymer composite conductive thin film material and preparation method thereof | |
| CN101798462B (en) | Graphene/conductive polymer composite film and preparation method thereof | |
| CN103342904A (en) | Method for preparing water-soluble graphene by titanate coupling agent modification process | |
| CN108034408A (en) | A kind of preparation method of graphite alkenyl composite wave-absorbing material | |
| CN104356381A (en) | Graphene/hollow ferroferric oxide/polyaniline nanocomposite and preparation method thereof | |
| CN101286375B (en) | Conductive compound material and method for making same | |
| CN105062070B (en) | A kind of graphene/thermoset ting resin composite of poly ion liquid modification and preparation method thereof | |
| CN110724493B (en) | Multi-walled carbon nanotube/ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof | |
| CN107283949A (en) | A kind of preparation of high electromagnet shield effect graphene/high polymer multilayer material | |
| CN107556510A (en) | A kind of preparation method of flexible sensor electrode | |
| CN105197899A (en) | Method for preparing boron nitride nano-plate/ferroferric oxide magnetic nano-composite materials | |
| CN104479424A (en) | Graphene-polyaniline modified carbon nanotube composite and preparation method thereof | |
| CN106634134B (en) | The preparation of magnetic ferroferric oxide/graphene composite material and its application in the magnetic paint of preparation | |
| CN106750279A (en) | The preparation method of the hollow ferroso-ferric oxide polyaniline nano-composite material of Graphene | |
| CN105085907A (en) | Method for preparing polyaniline grafted carbon material | |
| CN107938432A (en) | A kind of preparation method of carbon nanometer paper composites | |
| CN111732743A (en) | Preparation method of carbon nanotube/graphene flexible film | |
| CN105085915B (en) | A kind of high dielectric polyimides/carbon nano tube compound material and preparation method thereof | |
| CN107840324A (en) | A kind of lightweight, Flexible graphene Quito member composite wave-absorbing film and preparation method thereof | |
| CN1247690C (en) | Prepn process of composite material of polypyrrole-magnetic ferric oxide particle |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170531 |
|
| WD01 | Invention patent application deemed withdrawn after publication |