CN108147394A - A kind of method for preparing diverse microcosmic size graphite alkene aeroge - Google Patents
A kind of method for preparing diverse microcosmic size graphite alkene aeroge Download PDFInfo
- Publication number
- CN108147394A CN108147394A CN201810068086.XA CN201810068086A CN108147394A CN 108147394 A CN108147394 A CN 108147394A CN 201810068086 A CN201810068086 A CN 201810068086A CN 108147394 A CN108147394 A CN 108147394A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- graphene
- size
- gained
- graphite alkene
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention provides a kind of method for preparing diverse microcosmic size graphite alkene aeroge, with deionized water or organic solvent diluting graphene oxide solution so that a concentration of 0.01mg/ml 20mg/ml of graphene oxide solution；Regulated and controled by the method centrifuged and ultrasound is combined, so as to obtain various sizes of graphene oxide, be subsequently added into reducing agent, graphene aerogel is prepared by the method for heating water bath.Gained graphene aerogel microscopic dimensions are controllable, and preparation method is simple and practicable, and reaction condition is mild, and product is nontoxic and environmental-friendly, easily realize batch production, are expected to be used for the fields such as environmental improvement, sensor.
Description
Technical field
The invention belongs to materialogy fields, are related to a kind of graphene, specifically a kind of to prepare diverse microcosmic size stone
The method of black alkene aeroge.
Background technology
Graphene is single layer of carbon atom with SP2The nano material of hexagonal structure existing for hydridization form, be it is most thin,
The two-dimensional material of maximum intensity.Graphene has excellent pyroconductivity, higher carrier mobility, larger specific surface area
With excellent mechanical performance, have broad application prospects in fields such as energy stores, environmental protection, sensor and catalysis.
Graphene aerogel is that the three-dimensional assembly formed is built by two-dimensional graphene by overcritical or freeze-drying skill
The art light porous material with spacial framework obtained.Graphene aerogel has higher compared with common graphite alkene
Porosity and larger specific surface area, while the characteristics of have both the excellent physicochemical properties of graphene and aerogel structure,
One of hot spot as current graphene-based investigation of materials.The size of graphene and its performance are closely related, the different oxygen of size
Graphite alkene and graphene have different property in mechanical strength, surface-active and photo-thermal etc., and microscopic dimensions are different
Its porosity of graphene aerogel and specific surface area are also different, thus carry out controllable size point to graphene oxide and graphene
Grade is significant.
Common graphene oxide size classification such as introduces exogenous agent staging, is difficult to remove there are impurity, environment
Pollute big, of high cost, the problems such as being difficult to produce in enormous quantities；Simple physics centrifugal classification, there are size it is uneven the problem of.System
The method of standby graphene aerogel mainly has chemical gas-phase method, hydro-thermal method and chemical reduction method etc.；Wherein chemical reduction method reacts
Device is simple, reaction condition is mild, is more easy to realize large-scale production, so the method pair that we are combined using centrifugation and ultrasound
Its size is regulated and controled and is classified, and the different graphene aerogel of microscopic dimensions is prepared in conjunction with chemical reduction method.
Invention content
For above-mentioned technical problem of the prior art, diverse microcosmic size graphite alkene gas is prepared the present invention provides a kind of
The method of gel, this method for preparing diverse microcosmic size graphite alkene aeroge will solve what is prepared in the prior art
Graphene aerogel impurity is difficult to remove, environmental pollution is big, of high cost, the technical issues of being difficult to produce in enormous quantities.
The present invention provides a kind of methods for preparing diverse microcosmic size graphite alkene aeroge, it is characterised in that including following
Step：
1) graphene oxide solution is diluted with solvent so that a concentration of 0.01mg/ml-20mg/ml of graphene oxide solution；
2) graphite oxide dispersion is centrifuged into 10 ~ 600min, gained deposition fraction under room temperature in 1000 ~ 5000rpm rotating speeds
It collects up to large scale graphene oxide；
3) by step 2）Supernatant liquid centrifuge 10 ~ 600min, gained deposition portion under room temperature in 5000 ~ 8000rpm rotating speeds
Divide and collect as middle size graphene oxide；
4) by step 3）Supernatant liquid centrifuge 10 ~ 600min under room temperature in 8000 ~ 15000rpm rotating speeds, by deposition fraction
It collects as reduced size graphene oxide；Supernatant liquid is the graphene oxide of small size；
5) to step 4）Small size graphene oxide by be ultrasonically treated, ultrasonic power be 10W ~ 10000W, ultrasonic time
For 10 ~ 600min, obtain than step 4）Smaller szie and the graphene oxide being more uniformly distributed；
6) to step 2）、3）、4)、5）Ascorbic acid is added in obtained various sizes of graphene oxide solution, according to oxidation
The mass ratio 1 of graphene and ascorbic acid:1~1:Then 1000 additions stir 1 ~ 360min or 1 ~ 360min of ultrasound to mixing
Object uniformly mixes；
7) by step 6）The mixed liquor of gained is quantitatively adding in mold, and then mold is put into water-bath and is warming up to 60 ~ 100
DEG C, and heat preservation 1 ~ for 24 hours, obtain graphene hydrogel；
8) by step 7）Gained graphene hydrogel removes contained humidity by the method for freeze-drying, obtains porous graphene gas
Gel.
Further, the solvent for water, methanol, ethyl alcohol, ethylene glycol, propyl alcohol, acetone, tetrahydrofuran, isopropanol, N,
It is any in N- dimethylformamides or N- methyl pyrrolidones.
Further, the size range of different size graphene oxides obtained is 0.01 μm2To 990 μm2。
The present invention obtains graphene oxide dispersion with deionized water or organic solvent diluting, passes through centrifugation and ultrasonic phase
With reference to method regulated and controled, so as to obtain various sizes of graphene oxide, be subsequently added into reducing agent, under water bath condition lead to
It crosses self assembly reduction method and prepares graphene aerogel.
The present invention is compared with prior art, and technological progress is significant.The gained microcosmic ruler of graphene aerogel of the invention
Very little controllable, preparation method is simple and practicable, and reaction condition is mild, and product is nontoxic and environmental-friendly, easily realizes batch production, is expected to use
In fields such as environmental improvement, sensors.
Description of the drawings
Fig. 1 is the scanning electron microscopic picture of large-size graphene oxide sheet layer.
Fig. 2 is the scanning electron microscopic picture of small size graphene oxide layer.
Fig. 3 is the scanning electron microscopic picture of the smaller szie graphene oxide layer of ultrasound 60min.
Fig. 4 be different size graphene oxides prepare graphene aerogel picture, 1 be big size graphene aeroge, 2
It is smaller szie graphene aerogel for small size graphene aerogel, 3.
Specific embodiment
The method of the present invention is illustrated, but it is not intended that the scope of the present invention below by specific embodiment
Limitation, any modifications, equivalent replacements and improvementsmade within the spirit and principles of the invention, etc. should be included in this
Within the protection domain of invention.
Experimental method described in following example is conventional method unless otherwise specified；The reagent and material, such as
Without specified otherwise, can be obtained by commercial sources.
Embodiment 1 prepares the different graphene aerogel of microscopic dimensions：
The preparation of graphene oxide：Graphite powder 5.0g, sodium nitrate 2.5g are weighed, the dense H of 115ml are added under the conditions of ice-water bath2SO4It stirs
Mix 25min.15g potassium permanganate is then slowly added under conditions of less than 10 DEG C, stirs 25min.35 DEG C are then heated to, is stirred
Mix 45min.Then 230ml deionized waters are slowly added to, 98 DEG C of stirring 45min is then heated to, brown liquid is made to become shallow
Glassy yellow.Mixing liquid is diluted to 750ml with deionized water, adds in 30ml H2O2(mass fraction 30%) terminates reaction；
Add in hydrochloric acid 50ml（Hydrochloric acid：Water=1:9）.Obtained solid dilutes after drying in air, and dialysis is until pH is in deionized water
7, obtain graphene oxide solution.
The size classification of graphene oxide：
1）With the prepared graphene oxide solution of deionized water dilution, wherein a concentration of 6mg/ml of graphene oxide dispersion.
2）Graphite oxide dispersion centrifuges 30min under room temperature in 4000rpm rotating speeds, and deposition fraction collects to obtain the final product
Large scale graphene oxide, supernatant liquid centrifuge 30min under room temperature in 7000rpm rotating speeds, and deposition fraction collects i.e.
For middle size graphene oxide, supernatant liquid centrifuges 30min under room temperature in 10000rpm rotating speeds, and deposition fraction collects
Extremely reduced size graphene oxide, supernatant liquid are the graphene oxide of small size.
3）By ultrasonic method prepared by graphene oxide that is smaller and being more uniformly distributed to the graphene oxide of small size, is surpassed
Acoustical power is that 325W ultrasonic times are 180min.
4）Ascorbic acid is added in into the various sizes of graphene oxide solution of gained, it is worse than anti-according to graphene oxide
Hematic acid 1:4 mass ratio adds in；Magnetic agitation 30min is uniformly mixed liquid, and 2ml mixed liquors is taken to add in phase respectively with liquid-transfering gun
With in the Teflon mould of size, mold is placed in water-bath and keeps the temperature 3h under the conditions of 95 DEG C, by gained graphene gas
Gel refrigeration drying obtains graphene aerogel in 1 day.
Embodiment 2 prepares the different graphene aerogel of microscopic dimensions：
The preparation of graphene oxide：Preparation method is same as above.
The size classification of graphene oxide：
1）Graphene oxide solution, wherein a concentration of 6mg/ml of graphene oxide dispersion are diluted with deionized water.
2）Graphite oxide dispersion centrifuges 30min under room temperature in 5000rpm rotating speeds, and gained deposition fraction collects
Up to large scale graphene oxide, supernatant liquid centrifuges 30min under room temperature in 8000rpm rotating speeds, and gained deposition fraction is received
Collection gets up as middle size graphene oxide, and supernatant liquid centrifuges 30min under room temperature in 11000rpm rotating speeds, will deposit portion
Divide and collect as reduced size graphene oxide, supernatant liquid is the graphene oxide of small size.
3）By ultrasonic method prepared by graphene oxide that is smaller and being more uniformly distributed to the graphene oxide of small size, is surpassed
Acoustical power is that 1000W ultrasonic times are 60min.
4）Ascorbic acid is added in into the various sizes of graphene oxide solution of gained, it is worse than anti-according to graphene oxide
Hematic acid 1:6 mass ratio adds in；Magnetic agitation 30min is uniformly mixed liquid, 2ml mixed liquors is taken to add in respectively with liquid rifle identical
In the Teflon mould of size, mold is placed in water-bath and keeps the temperature 2h under the conditions of 80 DEG C, by gained graphene airsetting
Glue is freeze-dried 2 days and obtains graphene aerogel.
Embodiment 3 prepares the different graphene aerogel of microscopic dimensions：
The preparation of graphene oxide：Preparation method is same as above.
The size classification of graphene oxide：
1）A concentration of 8mg/ml graphene oxide dispersions are obtained with deionized water dilution graphene oxide solution.
2）Graphite oxide dispersion centrifuges 30min under room temperature in 3000rpm rotating speeds, and deposition fraction collects to obtain the final product
Large scale graphene oxide, supernatant liquid centrifuge 30min under room temperature in 6000rpm rotating speeds, and deposition fraction collects i.e.
For middle size graphene oxide, supernatant liquid centrifuges 30min under room temperature in 9000rpm rotating speeds, and deposition fraction collects
As reduced size graphene oxide, supernatant liquid are the graphene oxide of small size.
3）By ultrasonic method prepared by graphene oxide that is smaller and being more uniformly distributed to the graphene oxide of small size, is surpassed
Acoustical power is that 2000W ultrasonic times are 120min.
4）Dopamine is added in into the various sizes of graphene oxide solution of gained, compares dopamine according to graphene oxide
1:10 mass ratio adds in；Magnetic agitation 60min is uniformly mixed liquid, 4ml mixed liquors is taken to add in respectively with liquid-transfering gun identical
In the Teflon mould of size, mold is placed in water-bath and keeps the temperature 4h under the conditions of 90 DEG C, by gained graphene airsetting
Glue is freeze-dried 2 days and obtains graphene aerogel.
The scanning electron microscopic picture of 1000 times of large scale graphene oxide made from this example is as schemed（1）It is shown, it can from figure
It is larger with the graphene oxide size for seeing prepared.The scanning electron microscope (SEM) photograph of 1000 times obtained of reduced size graphene oxide
Piece is as schemed（2）It is shown, the graphene oxide of large-size is wherein remained as we can see from the figure, and Size Distribution is uneven
It is even.By the scanning electron microscopic picture of 1000 times of small size graphene oxide obtained after supersound process as schemed（3）It is shown, from figure
It can see more smaller and distribution uniform.
Small column with diverse microcosmic size graphite alkene aeroge prepared by this example is as schemed（4）It is shown, find them
Dimensional contraction rate it is different, illustrate that the different graphene oxide of microscopic dimensions can influence the macroscopic view of made graphene aerogel
Pattern.
The present invention can also optimize the Size Distribution of graphene oxide while different size graphene oxides are obtained, can
Control obtains various sizes of graphene oxide, and size is then made and is more uniformly distributed and controllable graphene aerogel.Preparation side
Method is simple and practicable, and reaction condition is mild, and product is nontoxic and environmental-friendly, easily realizes batch production, is expected to be used for environmental improvement, passes
The fields such as sensor.
Claims (2)
- A kind of 1. method for preparing diverse microcosmic size graphite alkene aeroge, it is characterised in that include the following steps：1）Graphene oxide solution is diluted with solvent so that a concentration of 0.01mg/ml-20mg/ml of graphene oxide solution；2）Graphite oxide dispersion is centrifuged into 10 ~ 600min, gained deposition fraction under room temperature in 1000 ~ 5000rpm rotating speeds It collects up to large scale graphene oxide；3）By step 2）Supernatant liquid centrifuge 10 ~ 600min, gained deposition portion under room temperature in 5000 ~ 8000rpm rotating speeds Divide and collect as middle size graphene oxide；4）By step 3）Supernatant liquid centrifuge 10 ~ 600min under room temperature in 8000 ~ 15000rpm rotating speeds, by deposition fraction It collects as reduced size graphene oxide；Supernatant liquid is the graphene oxide of small size；5）To step 4）Small size graphene oxide by be ultrasonically treated, ultrasonic power be 10W ~ 10000W, ultrasonic time For 10 ~ 600min, obtain than step 4）Smaller szie and the graphene oxide being more uniformly distributed；6）To step 2）、3）、4)、5）Ascorbic acid is added in obtained various sizes of graphene oxide solution, according to oxidation The mass ratio 1 of graphene and ascorbic acid:1~1:Then 1000 additions stir 1 ~ 360min or 1 ~ 360min of ultrasound to mixing Object uniformly mixes；7）By step 6）The mixed liquor of gained is quantitatively adding in mold, and then mold is put into water-bath and is warming up to 60 ~ 100 DEG C, and heat preservation 1 ~ for 24 hours, obtain graphene hydrogel；8）By step 7）Gained graphene hydrogel removes contained humidity by the method for freeze-drying, obtains porous graphene gas Gel.
- 2. a kind of method for preparing diverse microcosmic size graphite alkene aeroge according to claim 1, it is characterised in that：Institute The solvent stated for water, methanol, ethyl alcohol, ethylene glycol, propyl alcohol, acetone, tetrahydrofuran, isopropanol, N, N- dimethylformamides or It is any in N- methyl pyrrolidones.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810068086.XA CN108147394A (en) | 2018-01-24 | 2018-01-24 | A kind of method for preparing diverse microcosmic size graphite alkene aeroge |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810068086.XA CN108147394A (en) | 2018-01-24 | 2018-01-24 | A kind of method for preparing diverse microcosmic size graphite alkene aeroge |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108147394A true CN108147394A (en) | 2018-06-12 |
Family
ID=62458979
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810068086.XA Pending CN108147394A (en) | 2018-01-24 | 2018-01-24 | A kind of method for preparing diverse microcosmic size graphite alkene aeroge |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108147394A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109925981A (en) * | 2019-03-13 | 2019-06-25 | 太原理工大学 | A kind of preparation method of the graphene composite aerogel of high compression-strength |
| CN110002433A (en) * | 2019-03-13 | 2019-07-12 | 太原理工大学 | A kind of preparation method of high-specific surface area high compression-strength graphene aerogel |
| CN114082273A (en) * | 2020-07-29 | 2022-02-25 | 广东美的制冷设备有限公司 | Gas purification assembly and air treatment device |
| WO2022262349A1 (en) * | 2021-06-15 | 2022-12-22 | 山东理工大学 | Multifunctional bio-based wearable sensing gel and preparation method therefor |
| CN115784217A (en) * | 2020-12-28 | 2023-03-14 | 中国科学技术大学先进技术研究院 | Method for preparing monolayer graphene oxide with controllable sheet diameter size |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941693A (en) * | 2010-08-25 | 2011-01-12 | 北京理工大学 | Graphene aerogel and preparation method thereof |
| CN106082202A (en) * | 2016-06-29 | 2016-11-09 | 北京化工大学 | A kind of preparation method and application of graphene aerogel |
| CN107128907A (en) * | 2017-05-04 | 2017-09-05 | 上海理工大学 | A kind of size classification method of improved graphene oxide and graphene |
-
2018
- 2018-01-24 CN CN201810068086.XA patent/CN108147394A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941693A (en) * | 2010-08-25 | 2011-01-12 | 北京理工大学 | Graphene aerogel and preparation method thereof |
| CN106082202A (en) * | 2016-06-29 | 2016-11-09 | 北京化工大学 | A kind of preparation method and application of graphene aerogel |
| CN107128907A (en) * | 2017-05-04 | 2017-09-05 | 上海理工大学 | A kind of size classification method of improved graphene oxide and graphene |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109925981A (en) * | 2019-03-13 | 2019-06-25 | 太原理工大学 | A kind of preparation method of the graphene composite aerogel of high compression-strength |
| CN110002433A (en) * | 2019-03-13 | 2019-07-12 | 太原理工大学 | A kind of preparation method of high-specific surface area high compression-strength graphene aerogel |
| CN110002433B (en) * | 2019-03-13 | 2022-09-06 | 太原理工大学 | Preparation method of graphene aerogel with high specific surface area and high compressive strength |
| CN114082273A (en) * | 2020-07-29 | 2022-02-25 | 广东美的制冷设备有限公司 | Gas purification assembly and air treatment device |
| CN115784217A (en) * | 2020-12-28 | 2023-03-14 | 中国科学技术大学先进技术研究院 | Method for preparing monolayer graphene oxide with controllable sheet diameter size |
| WO2022262349A1 (en) * | 2021-06-15 | 2022-12-22 | 山东理工大学 | Multifunctional bio-based wearable sensing gel and preparation method therefor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108147394A (en) | A kind of method for preparing diverse microcosmic size graphite alkene aeroge | |
| CN106082202B (en) | A kind of preparation method and application of graphene aerogel | |
| CN104445215B (en) | The preparation method of hollow silica nano material | |
| CN104401979B (en) | The phase transfer preparation method of graphene-based composite aerogel | |
| CN102580716B (en) | Method for synthesizing zinc oxide/graphene composite by solvothermal method | |
| CN106744744B (en) | A kind of preparation method and products therefrom of cobalt doped honeycomb graphite phase carbon nitride nano material | |
| CN105217622A (en) | A kind of preparation method of controlled three-dimensional grapheme microballoon | |
| CN105397103A (en) | Nano-silver/graphene composite material and preparation method thereof | |
| CN105174249B (en) | High-performance graphene film and fiber and its gel conversion preparation method | |
| CN107922210A (en) | The preparation method of magnetic iron oxide graphene composite material | |
| CN106975489A (en) | A kind of preparation method of nickel oxide in-stiu coating graphene nanocomposite material | |
| CN113929105A (en) | Preparation method of metal organic framework derived nickel silicate | |
| CN106673058A (en) | Preparation method of titanium dioxide nano-particles based on nano gold solution glow discharge | |
| CN108529609A (en) | A kind of graphene aqueous solution and preparation method thereof | |
| CN107128907A (en) | A kind of size classification method of improved graphene oxide and graphene | |
| CN105967176A (en) | Preparation method of cellular three-dimensional graphene | |
| CN106115779B (en) | A kind of hollow nano-TiO2The preparation method of bag carbon Yolk shell structures | |
| CN107460021B (en) | Preparation method of low-temperature graphene-based nano borate composite material | |
| CN111943166B (en) | Preparation of solvent-free hydrothermal carbon material | |
| CN109399655A (en) | A kind of method that high efficiency, low cost prepares kaolin nanotube and its composite material | |
| CN106044748A (en) | Method for preparing boron-doped graphene | |
| CN113745542A (en) | High platinum loading platinum/carbon catalyst for fuel cell and preparation method thereof | |
| CN108358192A (en) | A kind of preparation method of silicon doping High-performance graphene material | |
| CN106744899A (en) | Preparation method of two-dimensional material nano roll | |
| CN106693963A (en) | Preparation method of novel gold nanoparticle-modified silicon dioxide nanosheet catalyst |
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 | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180612 |