CN106477571A - To the modified method of graphene oxide microplate under multiple external force fields - Google Patents
To the modified method of graphene oxide microplate under multiple external force fields Download PDFInfo
- Publication number
- CN106477571A CN106477571A CN201610862441.1A CN201610862441A CN106477571A CN 106477571 A CN106477571 A CN 106477571A CN 201610862441 A CN201610862441 A CN 201610862441A CN 106477571 A CN106477571 A CN 106477571A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- modified
- microplate
- revs
- stirring
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention discloses to the modified method of graphene oxide microplate under multiple external force fields, by choosing carbon content 90%～99%, it is raw material 1g that granularity is the graphite of 10～300 mesh, graphite is added in the concentrated sulfuric acid of 98% concentration, 60～240min of stirring, 3000 revs/min of rotating speed, after stirring is transferred to solution bottle in ultrasonic generator, and the step such as ultrasonically treated ... obtains modified graphene oxide microplate.The modified graphene oxide microplate of preparation is added in SBS modified pitch, obtains the SBS modified pitch of modified graphene oxide microplate.This modified graphene oxide microplate has more preferable surface roughness and oxygen-containing functional group, and the combination between making pitch and gathering materials is more firm, and the long durability of road improvement, the present invention can be used in traffic engineering and road engineering by this.
Description
Technical field
The invention belongs to macromolecule modified field.To the modified method of graphene oxide microplate under specifically multiple external force fields.
Background technology
Verified nanometer technology is that the property for improving asphalt mixture material provides one kind very for research work before
Interesting way.For by this advanced Application of micron in bituminous industry, maximum obstacle is exactly becoming for its great number
This.Therefore, the maximum power of the present invention be to develop some suitable bituminous pavings and after inspection pitch and compound machine
Tool performance is all good with compacting technique, and the good nano material of cost benefit.
Graphene microchip is to be only one nanometer, Graphene of the shape just as nanometer pad by one micron of diameter, thickness
Piece stacking is formed.One Graphene is formed by hexagonal array by individual layer carbon atom.Grapheme material shows superior
Both mechanically and electrically transmission characteristic：The rigidity of Graphene is 1TPa, and the intensity of Graphene is 100 times of steel or so, and graphite
The electrical conductance of alkene is higher than copper.Additionally, research has shown that its special heat endurance of Graphene is minimum in 2600K.Grapheme material
Cost is depending on its type and carbon purity.For large-scale application, material cost can as little as every pound 3-4 dollar, its cost
Be significantly lower than multilayer carbon nanotube.It can be seen that the material cost of Graphene is can be with styrene-butadiene-benzene second
Alkene etc. some still using asphalt modifier compare.
A series of researchs with regard to graphene microchip are all concentrated in the application in cement mortar in the recent period, and research finds graphite
The addition of alkene microplate can effectively improve the electric conductivity of cement mortar.This causes cement this lost material carrying with electric conductivity
High this it appears that level to damage of materials.Meanwhile, this also demonstrates that graphene microchip can reduce the critical of cement mortar
Aperture, and the water resistant permeability of cement mortar, corrosion resistance of chloride ion effect and resisting chloride ion penetration migration property is therefore improved, this is to material
The durability of material produces significant impact.Experiment also indicate that additions of graphene microchip can improve the coefficient of elasticity of cement mortar with
Tensile strength.
These study potential value of the verified graphene microchip in civil engineering material application.Use cost is relative
Relatively low graphene microchip can meet the application of large-scale basis facility.In order to improve the overall performance of bituminous paving, graphite
These application potentials that alkene microplate is shown in asphalt modifier are all promoting the research to which.Developing graphene microchip makes drip
Blue or green and between gathering materials combination is more firm, this by the long durability of road improvement, this engineering construction to improving bituminous paving
Quality all has important scientific research and instructs the meaning of practical application.
Content of the invention
It is an object of the invention to provide to the modified method of graphene oxide microplate under multiple external force fields.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
1., to the modified method of graphene oxide microplate under many kinds of external force fields, comprise the steps：
1) with carbon content 90%～99%, it is raw material 1g that granularity is the graphite of 10～300 mesh, and graphite is added to quality
Concentration is in 98% concentrated sulfuric acid, stirs 60～240min with rotating speed as 3000 revs/min.
2) by step 1) in the solution that obtains stir after be transferred in ultrasonic generator, ultrasonic power is 100～
400w, obtains ultrasonically treated rear solution.
3) by step 2) the ultrasonically treated rear solution that obtains adds 0.5～5g of potassium permanganate, in 30 DEG C～50 DEG C temperature strip
Continue 60～240min of stirring under part, obtain reactant liquor.
4) deionized water dilution step 3) reactant liquor, the liquor capacity after dilution be 500mL, add mass concentration be
1%～10% hydrogen peroxide is to solution no longer effervescent.
5) survey step 4 with pH test paper) pH value of solution, the amount of acid needed for estimation, calculate good after add watery hydrochloric acid or dilute sulfuric acid,
And a large amount of deionized water rinsings are used, until neutral, finally filter and graphene oxide is obtained.
6) by step 5) graphene oxide that obtains adds deionized water and graphene oxide suspension, graphite oxide is obtained
Alkene suspension stirs 10～60min with a high speed dispersion homogenizer under ultrasound field, and rotating speed is 6000 revs/min～10000 turns/
Point, add modification liquid 50～200mL of ethylene glycol to obtain disperseing mother liquor, after dispersion mother liquor is centrifuged, modified oxygen is obtained
Graphite alkene microplate.
2. application of the modified graphene oxide microplate in SBS modified pitch, modified graphene oxide microplate is put into work(
For etching 1～20min under the argon-arc plasma field of 100w～800w, etching is added it in SBS modified pitch after terminating rate, with
1500 revs/min～3000 revs/min of speed stirring, temperature is 170 DEG C～190 DEG C；Stirring was had after 30～60 minutes
The SBS modified pitch of modified graphene oxide microplate.
This modified graphene oxide microplate has more preferable surface roughness and oxygen-containing functional group, make SBS modified pitch with
Combination between gathering materials is more firm, and this is by the long durability of road improvement.
Specific embodiment
For a better understanding of the present invention, the present invention is further described with reference to embodiment.
Embodiment 1
1., to the modified method of graphene oxide microplate under many kinds of external force fields, comprise the steps：
(1) with carbon content 90%, it is raw material 1g that granularity is the graphite of 10 mesh, and graphite is added to the dense sulphur of 98% concentration
In acid, 60min, 3000 revs/min of rotating speed is stirred；
(2) transfer in ultrasonic generator after the solution obtained in step (1) stirring, ultrasonic power 100w,
Obtain ultrasonically treated rear solution.
(3) by step (2) obtain ultrasonically treated after solution add potassium permanganate 0.5g, at 30 DEG C continue stirring 60min,
Obtain reactant liquor.
(4) reactant liquor of deionized water dilution step (3), the liquor capacity after dilution are 500mL, and addition concentration is
1% hydrogen peroxide is to solution no longer effervescent；
(5) with the pH value of pH test paper survey step (4) solution, the amount of required acid is estimated, good rear addition watery hydrochloric acid is calculated, and with greatly
Amount deionized water rinsing, until neutral, finally filter and graphene oxide is obtained.
(6) graphene oxide for obtaining step (5) adds deionized water and graphene oxide suspension is obtained, and aoxidizes stone
Black alkene suspension continues to stir 10min with dispersion homogenizer at a high speed under ultrasound field, and rotating speed is 6000 revs/min, adds modified
Liquid (ethylene glycol) 50mL obtains disperseing mother liquor, modified graphene oxide microplate is obtained after dispersion mother liquor is centrifuged.
2. application of the modified graphene oxide microplate in SBS modified pitch, modified graphene oxide microplate is put into work(
For etching 1min under the argon-arc plasma field of 100w, etching is added it in SBS modified pitch after terminating rate, with 1500 revs/min
Speed stirring, temperature be 170 DEG C；Stirring obtains the SBS modified pitch of modified graphene oxide microplate after 30 minutes.
This modified graphene oxide microplate has more preferable surface roughness and oxygen-containing functional group, make SBS modified pitch with
Combination between gathering materials is more firm, and this is by the long durability of road improvement.
The specific surface of the Graphene (microplate) of the different preparation methods of table 1
The oxygen-containing functional group content of the Graphene (microplate) of the different preparation methods of table 2
Embodiment 2
1., to the modified method of graphene oxide microplate under many kinds of external force fields, comprise the steps：
(1) by carbon content 95%, it is raw material 1g that granularity is the graphite of 150 mesh, and graphite is added to the dense of 98% concentration
In sulfuric acid, 120min, 3000 revs/min of rotating speed is stirred.
(2) transfer in ultrasonic generator after the solution obtained in step (1) stirring, ultrasonic power 200w,
Obtain ultrasonically treated rear solution.
(3) by step (2) obtain ultrasonically treated after solution add potassium permanganate 3g, at 40 DEG C continue stirring 120min,
Obtain reactant liquor.
(4) reactant liquor of deionized water dilution step (3), the liquor capacity after dilution are 500mL, and addition concentration is
5% hydrogen peroxide is to solution no longer effervescent.
(5) with the pH value of pH test paper survey step (4) solution, the amount of required acid is estimated, good rear addition dilute sulfuric acid is calculated, and with greatly
Amount deionized water rinsing, until neutral, finally filter and graphene oxide is obtained.
(6) graphene oxide for obtaining step (5) adds deionized water and graphene oxide suspension is obtained, and aoxidizes stone
Black alkene suspension stirs 10min with dispersion homogenizer at a high speed under ultrasound field, and rotating speed is 6000 revs/min, adds modification liquid (second
Glycol) 50mL obtain disperse mother liquor, will dispersion mother liquor be centrifuged after modified graphene oxide microplate is obtained.
(6) graphene oxide for obtaining step (5) adds deionized water and graphene oxide suspension is obtained, and aoxidizes stone
Black alkene suspension stirs 30min with dispersion homogenizer at a high speed under ultrasound field, and rotating speed is 8000 revs/min, adds modification liquid (second
Glycol) 100mL, disperses mother liquor modified graphene oxide microplate to be obtained after being centrifuged.
2. application of the modified graphene oxide microplate in SBS modified pitch, modified graphene oxide microplate is put into work(
For etching 10min under the argon-arc plasma field of 400w, etching is added it in SBS modified pitch after terminating rate, with 2000 revs/min
Speed stirring, temperature be 180 DEG C；Stirring obtains the SBS modified pitch of modified graphene oxide microplate after 40 minutes.
The specific surface of the Graphene (microplate) of the different preparation methods of table 3
The oxygen-containing functional group content of the Graphene (microplate) of the different preparation methods of table 4
Embodiment 3
1., to the modified method of graphene oxide microplate under many kinds of external force fields, comprise the steps：
(1) by carbon content 99%, it is raw material 1g that granularity is the graphite of 300 mesh, and graphite is added to the dense of 98% concentration
In sulfuric acid, 240min, 3000 revs/min of rotating speed is stirred.
(2) transfer in ultrasonic generator after the solution obtained in step (1) stirring, ultrasonic power 400w,
Obtain ultrasonically treated rear solution.
(3) by step (2) obtain ultrasonically treated after solution add potassium permanganate 5g, at 50 DEG C continue stirring 240min,
Obtain reactant liquor.
(4) reactant liquor of deionized water dilution step (3), the liquor capacity after dilution are 500mL, and addition concentration is
10% hydrogen peroxide is to solution no longer effervescent.
(5) with the pH value of pH test paper survey step (4) solution, the amount of required acid is estimated, good rear addition watery hydrochloric acid is calculated, and with greatly
Amount deionized water rinsing, until neutral, finally filter and graphene oxide is obtained.
(6) graphene oxide for obtaining step (5) adds deionized water and graphene oxide suspension is obtained, and aoxidizes stone
Black alkene suspension stirs 60min with dispersion homogenizer at a high speed under ultrasound field, and rotating speed is 10000 revs/min, adds modification liquid
(ethylene glycol) 200mL, dispersion mother liquor are obtained modified graphene oxide microplate after being centrifuged.
2. application of the modified graphene oxide microplate in SBS modified pitch, modified graphene oxide microplate is put into work(
For etching 20min under the argon-arc plasma field of 800w, etching is added it in SBS modified pitch after terminating rate, with 3000 revs/min
Speed stirring, temperature be 190 DEG C；Stirring obtains the SBS modified pitch of modified graphene oxide microplate after 60 minutes.
The specific surface of the Graphene (microplate) of the different preparation methods of table 5
The oxygen-containing functional group content of the Graphene (microplate) of the different preparation methods of table 6
Claims (2)
1. to the modified method of graphene oxide microplate under many kinds of external force fields, it is characterised in that comprise the steps：
(1) with carbon content 90%～99%, it is raw material 1g that granularity is the graphite of 10～300 mesh, graphite is added to quality dense
Spend in the concentrated sulfuric acid for 98%, with rotating speed as 3000 revs/min of 60～240min of stirring；
(2) it is transferred in ultrasonic generator after the solution obtained in step (1) stirring, ultrasonic power is 100～400w,
Obtain ultrasonically treated rear solution；
(3) the ultrasonically treated rear solution for obtaining step (2) adds 0.5～5g of potassium permanganate, in 30 DEG C～50 DEG C temperature conditionss
Lower 60～240min of continuation stirring, obtains reactant liquor；
(4) reactant liquor of deionized water dilution step (3), the liquor capacity after dilution are 500mL, and addition mass concentration is
1%～10% hydrogen peroxide is to solution no longer effervescent；
(5) with the pH value of pH test paper survey step (4) solution, the amount of acid needed for estimating, good rear addition watery hydrochloric acid or dilute sulfuric acid is calculated, and
A large amount of deionized water rinsings are used, until neutral, finally filter and graphene oxide is obtained；
(6) graphene oxide for obtaining step (5) adds deionized water and graphene oxide suspension, graphene oxide is obtained
Suspension stirs 10～60min with dispersion homogenizer at a high speed under ultrasound field, and rotating speed is 6000 revs/min～10000 revs/min,
Add modification liquid 50～200mL of ethylene glycol to obtain disperseing mother liquor, be obtained after dispersion mother liquor is centrifuged modified oxidized
Graphene microchip.
2. application of the modified graphene oxide microplate in SBS modified pitch, it is characterised in that by modified graphene oxide microplate
Power is put into for 1～20min is etched under the argon-arc plasma field of 100w～800w, etching adds it to SBS modified pitch after terminating
In, being stirred with 1500 revs/min～3000 revs/min of speed, temperature is 170 DEG C～190 DEG C；Stirring was obtained after 30～60 minutes
To the SBS modified pitch for having modified graphene oxide microplate；
This modified graphene oxide microplate has more preferable surface roughness and oxygen-containing functional group, makes SBS modified pitch and gathers materials
Between combination more firm, this is by the long durability of road improvement.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610862441.1A CN106477571A (en) | 2016-09-29 | 2016-09-29 | To the modified method of graphene oxide microplate under multiple external force fields |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610862441.1A CN106477571A (en) | 2016-09-29 | 2016-09-29 | To the modified method of graphene oxide microplate under multiple external force fields |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106477571A true CN106477571A (en) | 2017-03-08 |
Family
ID=58268970
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610862441.1A Pending CN106477571A (en) | 2016-09-29 | 2016-09-29 | To the modified method of graphene oxide microplate under multiple external force fields |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106477571A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832977A (en) * | 2017-03-03 | 2017-06-13 | 广西大学 | A kind of composite asphalt modifier containing modified graphene microplate and its preparation method and application |
| CN108117714A (en) * | 2017-12-22 | 2018-06-05 | 广西大学 | A kind of composite asphalt modifier based on modified graphene and its preparation method and application |
| CN110550919A (en) * | 2019-09-29 | 2019-12-10 | 北京工业大学 | method for improving chloride ion permeation resistance of cement-based material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530935A (en) * | 2012-01-09 | 2012-07-04 | 苏州大学 | Polyethylene glycol and polyethyleneimine modified graphene oxide and preparation method thereof |
| CN104448868A (en) * | 2015-01-06 | 2015-03-25 | 山西省交通科学研究院 | SBS modified asphalt based on graphene oxide and preparing method thereof |
| US20150133568A1 (en) * | 2013-11-12 | 2015-05-14 | Shanghai Switchdiy Digital Technology Co., Ltd. | Method for preparing graphene from biomass-derived carbonaceous mesophase |
| CN104961122A (en) * | 2015-05-06 | 2015-10-07 | 深圳高远通新材料科技有限公司 | Graphene organic functional modification methods and application |
| CN105602649A (en) * | 2015-12-21 | 2016-05-25 | 中国科学院兰州化学物理研究所 | Graphene oxide modified nano additive and application thereof to lubricating oil |
-
2016
- 2016-09-29 CN CN201610862441.1A patent/CN106477571A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530935A (en) * | 2012-01-09 | 2012-07-04 | 苏州大学 | Polyethylene glycol and polyethyleneimine modified graphene oxide and preparation method thereof |
| US20150133568A1 (en) * | 2013-11-12 | 2015-05-14 | Shanghai Switchdiy Digital Technology Co., Ltd. | Method for preparing graphene from biomass-derived carbonaceous mesophase |
| CN104448868A (en) * | 2015-01-06 | 2015-03-25 | 山西省交通科学研究院 | SBS modified asphalt based on graphene oxide and preparing method thereof |
| CN104961122A (en) * | 2015-05-06 | 2015-10-07 | 深圳高远通新材料科技有限公司 | Graphene organic functional modification methods and application |
| CN105602649A (en) * | 2015-12-21 | 2016-05-25 | 中国科学院兰州化学物理研究所 | Graphene oxide modified nano additive and application thereof to lubricating oil |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832977A (en) * | 2017-03-03 | 2017-06-13 | 广西大学 | A kind of composite asphalt modifier containing modified graphene microplate and its preparation method and application |
| CN106832977B (en) * | 2017-03-03 | 2019-06-04 | 广西大学 | A kind of composite asphalt modifier of the microplate containing modified graphene and its preparation method and application |
| CN108117714A (en) * | 2017-12-22 | 2018-06-05 | 广西大学 | A kind of composite asphalt modifier based on modified graphene and its preparation method and application |
| CN108117714B (en) * | 2017-12-22 | 2020-01-31 | 广西大学 | modified graphene-based composite asphalt modifier and preparation method and application thereof |
| CN110550919A (en) * | 2019-09-29 | 2019-12-10 | 北京工业大学 | method for improving chloride ion permeation resistance of cement-based material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106477571A (en) | To the modified method of graphene oxide microplate under multiple external force fields | |
| Chen et al. | Graphene oxide-deposited carbon fiber/cement composites for electromagnetic interference shielding application | |
| Wang et al. | Comparative studies on electrochemical activity of graphene nanosheets and carbon nanotubes | |
| US20150064463A1 (en) | Graphene fiber and method of manufacturing the same | |
| Lee et al. | Partially reduced graphene oxide as a multi-functional sizing agent for carbon fiber composites by electrophoretic deposition | |
| CN104403275B (en) | A kind of modified graphene/thermoset ting resin composite and preparation method thereof | |
| CN103072980B (en) | The method quickly preparing graphene platelet | |
| Lei et al. | Excellent dielectric properties of polymer composites based on core-shell structured carbon/silica nanohybrid | |
| CN109401349A (en) | A kind of graphene oxide modified pitch and preparation method thereof | |
| CN106477578A (en) | A kind of MXene two-dimensional material preparation method based on acid deep co-melting solvent | |
| Wu et al. | Novel high-hydrophilic carbon dots from petroleum coke for boosting injection pressure reduction and enhancing oil recovery | |
| Habib et al. | Use of graphene oxide as a bitumen modifier: an innovative process optimization study | |
| CN107759809A (en) | A kind of preparation method of stretchable organic/inorganic composite aquogel | |
| KR101572671B1 (en) | Method of manufacturing of large-area graphene oxide and the large-area graphene oxide thereby | |
| CN103408001A (en) | Method for preparing graphene with large specific surface area through microwave digestion | |
| CN107500275A (en) | A kind of method for producing different Oil repellent fluorinated graphenes in enormous quantities | |
| Wang et al. | Effects of vacancy-carboxyl pair functionalization on electronic properties of carbon nanotubes | |
| CN106241781B (en) | The removing method of metal ion in graphite oxide | |
| CN105199212A (en) | Preparation method of graphene/PVA composite material | |
| Conrado et al. | A continuous 3D-graphene network to overcome threshold issues and contact resistance in thermally conductive graphene nanocomposites | |
| Banerjee et al. | 1‐Aza‐15‐Crown‐5 Functionalized Graphene Oxide for 2D Graphene‐Based Li+‐ion Conductor | |
| CN106832718A (en) | A kind of conducting polymer composite graphite alkene material and preparation method thereof | |
| CN104091932B (en) | WS2nanometer sheet/graphene composite nano material with holes and preparation method | |
| Qiao et al. | Multi-scale carbon-admixtures enhanced cementitious anodic materials for the impressed current cathodic protection of RC structures | |
| KR102212288B1 (en) | Exothermic Concrete using Liquid Carbon Nanotubes and Manufacturing Method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170308 |
|
| WD01 | Invention patent application deemed withdrawn after publication |