CN106185880A - A kind of method that porous graphene directly prepared by graphene oxide slurry utilizing pre-purification - Google Patents
A kind of method that porous graphene directly prepared by graphene oxide slurry utilizing pre-purification Download PDFInfo
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- CN106185880A CN106185880A CN201610435263.4A CN201610435263A CN106185880A CN 106185880 A CN106185880 A CN 106185880A CN 201610435263 A CN201610435263 A CN 201610435263A CN 106185880 A CN106185880 A CN 106185880A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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
Abstract
The invention discloses the preparation method of a kind of porous graphene.Concrete grammar is to utilize oxidation stripping method (hummers method) first to prepare graphite oxide, the graphene oxide dispersion of the pre-purification of thickness is prepared again through natural subsidence ablution and ultrasonic agitation, then dried high-temperature calcination, thus prepare oxide carried porous graphene, remove oxide finally by acid treatment, obtain porous graphene dusty material.The invention provides a kind of impurity method that porous graphene is prepared in auxiliary surface perforate in high-temperature burning process of surface of graphene oxide remnants directly utilizing pre-purification, preparation process has been abandoned the process of long-time cleaning graphite oxide, and prepare raw material without being re-introduced into other, manufacturing cycle simple to operate is short and aperture and hole number can be regulated and controled by the temperature of calcining and the impurity level carried so that controlled the being possibly realized property of industrialization preparing porous graphene.
Description
Technical field
The present invention relates to the technology of preparing of a kind of porous graphene, prepare the side of porous graphene particularly to a kind of magnanimity
Method.
Background technology
The fast development of national economy and the urgent needs of energy source and power resource, necessarily cause the oil and natural gas etc. can not
The day by day exhaustion of regenerated resources, increases the continuous deterioration of the global environmental problems such as air pollution.Therefore, increase for balanced economy
Length, environmental conservation and energy supply relation, the energy technology finding environmentally friendly sustainable development has become scientist's
One of top priority.High-efficiency cleaning energy storage carrier develop into the important directions leading energy-conserving and environment-protective technology, lithium/air cell
Being made up of cathode of lithium, electrolyte and air cathode, wherein air cathode is with the oxygen (O in air2) as active substance, due to
O2Can obtain from surrounding continuously, be not take up the weight of battery itself, thus lithium/air cell has high
Theoretical specific capacity and advantages of environment protection, demonstrate good application prospect.Theoretical specific energy up to 11140Wh/kg, with
Internal combustion engine petroleum system is suitable, promotes, by energy storage field if lithium/air cell can be researched and developed successfully and obtain commercialization
Development produce great progradation [L.Grande, E.Paillard, J.Hassoun, J.B.Park, Y.J.Lee,
Y.K.Sun, S.Passerini, B.Scrosati.The lithium/air battery:still an emerging
System or a practical reality.Adv.Mater., 2015,27,784-800.].But, lithium/air cell is wanted
Thinking practical, the most many obstacles need to overcome, and there is also some problems needing solution badly.From organic system lithium/air cell
Structural analysis, the O in positive electrode surface and air2Contact, reaction generates the Li being insoluble in organic electrolyte2O2With Li2O,
Cause it constantly to deposit at positive electrode surface, thus increase O2Diffusion internal resistance and the electron transfer impedance of electrochemical reaction, cause
Final battery capacity decay and the shortening of cycle life, thus terminate reaction [J.J.Xu, Z.L.Wang, D.Xu,
L.L.Zhang, X.B.Zhang.Tailoring deposition and morphology of discharge products
Towards high-rate and long-life lithium-oxygen batteries.Nat.Commun., 2013,4,
2438.].Therefore, positive pole reaction decides the major part transmission of the energy content of battery, assume responsibility for the voltage drop of whole battery, lithium/air
The structure and properties of cell positive material is the key factor determining battery performance.Positive electrode should have good conductivity, be prone to
The features such as pore-creating, low cost, oxygen reduction activity be good and oxygen absorption affinity is strong.
Porous graphene not only surface has abundant pore structure, and has Graphene light weight, specific surface area height, leads
The features such as the most excellent and abundant boundary effect, are lithium/optimal structures of O for cathode of air battery material, and this kind of material is permissible
Meet the electrode material demand for the aspect such as deposition of the diffusion of gas, the infiltration of electrolyte and discharging product simultaneously.Stone
The boring method of ink alkene mainly has Physical and chemical method two kinds, and Physical often utilizes high precision apparatus little at graphenic surface
Scope output controlled hole.But the expensive industrialized production that is unfavorable for of Physical, and utilize the oxidation that chemical method produces
The defect pore-creating of graphenic surface, prepares porous graphene and has made scale preparation become probability.Peng of Zhejiang University
New life et al. it is also proposed that be mixed with the side preparing porous graphene by soluble metal saline solution and graphene oxide water solution
[Peng is newborn for method；Answer Yulong；A kind of porous graphene and its preparation method and application CN104743548A].
But, the root problem that the scale preparation of graphene oxide exists is that surface of graphene oxide is with hydroxyl, carboxylic
The hydrophilic functional groups such as base and epoxy radicals, shows strong hydrophilic.Utilize the oxidation graphite oxide for preparing of stripping method with
Going deep into of purification, form water-setting (molten) glue with water, it is difficult to dispersion precipitation.No matter use sucking filtration or centrifugal technology, the most very
Difficult separation graphite oxide and aqueous solution, ultimately cause product impurity and cannot obtain basic removal, prepare highly purified in industry
Graphene oxide then needs the equipment of costliness and macrocyclic dialysis work.Our work then utilizes early stage highly acidity
The hydrophobicity that graphite oxide is special, uses repeatedly the simple procedure that natural subsidence is cleaned, at the oxygen obtaining the strong thickness of hydrophilic
Stop the degree of depth after graphite slurry to clean, thus avoid macrocyclic preparation process, but by simple ultrasonic disperse or
The pre-graphene oxide dispersed paste purified of stirring technique preparation, obtains powder sample after dried, utilize the pre-oxygen purified
The impurity of functionalized graphene surface remaining, under hot environment, etching auxiliary perforate prepares porous graphene.This method avoid
The follow-up difficult cleaning problem of graphene oxide, and the problem that porous graphene surface impurity utilizes, such that it is able to realize porous
Prepared by the quick magnanimity of Graphene.Additionally, we introduce kind also by the raw material limiting oxidation stripping method, can be follow-up
The unicity of control oxide and the consistency problem of pore structure in preparation process.
Summary of the invention
The invention provides a kind of method that porous graphene directly prepared by graphene oxide slurry utilizing pre-purification, should
Method has the advantages such as low cost, manufacturing cycle be short, therefore can prepare the ideal side of porous graphene as a kind of magnanimity that is suitable to
Method.
A kind of method of porous graphene, it is characterised in that comprise the following steps:
A oxidation stripping method prepares graphite oxide: using different size natural flake graphite is raw material, by a certain amount of dense sulfur
Acid and potassium permanganate stir successively and are added thereto, and aoxidize graphite, thus obtain graphite oxide.
The pre-graphene oxide slurry purified of B preparation；Deionized water stirring is added in the graphite oxide slurry of highly acidity
Uniformly, after graphite to be oxidized is separated from the water, remove the aqueous phase on upper strata, retain lower sediment, again add deionized water and stir evenly,
Repeated multiple times natural subsidence cleans graphite oxide, until graphite oxide solution is become after dark-brown and natural subsidence not from glassy yellow
It is layered again, collects the pre-purification graphite oxide slurry regulation concentration of lower floor's thickness, then by mechanical agitation or ultrasonic disperse
The pre-graphene oxide slurry purified of preparation, finally utilizes Freeze Drying Technique, the pre-graphene oxide powder purified of preparation.
C prepares oxide carried porous graphene powder: utilize high temperature sintering furnace, and gas shield is to the pre-oxidation purified
Graphene powder carries out high-temperature calcination process, prepares oxide carried porous graphene powder.
D prepares porous graphene powder: oxide carried porous graphene powder high-temperature calcination obtained carries out room
Temperature dilute hydrochloric acid soaking and stirring a few hours, removing the oxide on surface, sucking filtration is cleaned multiple times PH=7, vacuum drying preparation afterwards
Porous graphene powder.
Described natural graphite starting material a size of 45～180 μm, purity is mass fraction 80%-99%, and the sulphuric acid of selection is dense
Degree is 98%, and adding graphite, potassium permanganate is 1: 3: 30-1: 6: 70 with the mass ratio of sulphuric acid.
In the cleaning of described natural subsidence when solution cleans to PH=1.5-2.5, and the volume of slurry increases to original
When 3-6 times, graphite oxide can be purified in advance as early stage product prepared by porous graphene and collect, adjust concentration the most again to 8-
20mg/ml utilizes ultrasonic 400-800W or stirring 100-350r/min, time 30min-3h, peels off the pre-oxidation purified of preparation
Graphene solution, last lyophilization, prepare the graphene oxide powder of pre-purification.
In described step, the temperature of high temperature sintering furnace is set in 800-1100 DEG C, and protective gas is noble gas (argon, nitrogen
Gas), during high temperature sintering 30min-4h, the pre-surface of graphene oxide impurity growing movement purified will be driven and synchronize reduction-oxidation
Graphene, thus prepare oxide carried porous graphene, wherein the floristic analysing of oxide is manganese monoxide, remaining
Element sulphur with waste gas discharge surface deposit.
In described step, the concentration of dilute hydrochloric acid is 5-15%, stirring dip time be 30min～2h, be dried prepare many
Hole Graphene.
The present invention compared with prior art has the advantage that
1, the present invention uses the graphene oxide slurry of pre-purification directly to prepare porous graphene, it is to avoid graphene oxide
The problems such as the cleaning frequency of itself is long, water resource waste, and utilize the impurity of surface of graphene oxide remnants cleverly, at high temperature
The lower preparation realizing porous graphene.
2, present invention optimizes graphite and prepare the raw material introducing of graphene oxide, only with graphite, potassium permanganate and sulfur
Raw material is prepared in acid three kinds, and in high temperature environments, sulfur oxygen element overflows, prepared by the etching achieving a kind of residual impurity cleverly,
Etching prepares Mn oxide porous graphene in high temperature environments, and this product shows the property of excellence in lithium-air battery
Energy.
3, manufacturing cycle of the present invention is short, and all preparation processes can realize industrialization and amplify, and technological process is simple, system
Standby low cost, it is possible to achieve prepared by the scale of porous graphene.
Accompanying drawing explanation
Fig. 1 is the XRD data of manganese monoxide porous graphene.
Fig. 2 is the stereoscan photograph of manganese monoxide porous graphene.
Fig. 3 is the stereoscan photograph of manganese monoxide porous graphene.
Fig. 4 is the stereoscan photograph of porous graphene.
Detailed description of the invention
Embodiment 1
Utilizing the Hummers method improved, using 100g purity is that the 45um natural flake graphite of 90wt% is at 3000ml
The concentrated sulphuric acid of 98wt% and the KMnO of 300g4Graphite oxide is prepared in middle reaction, and sucking filtration removes acid pickle too much in reaction, collects
Graphite oxide slurry, adds the water of 5L, regulates graphite oxide slurry PH=1.0, natural subsidence after placing half, removes upper strata acid
Waste liquid, more repeatedly add high purity water, until graphite oxide slurry PH=2.0 and color are become dark-brown from glassy yellow, now oxygen
Graphite precipitation volume increases to about original 3 times, adjusts the pre-graphite oxide slurry concentration purified and exists to 20mg/ml
Stir 1h under the mechanical stirring device of 350rpm/min, peel off the pre-graphene oxide slurry purified of preparation, then through freezing
Dry technology prepares the graphene oxide powder of pre-purification, by the graphene oxide powder that purifies in advance at high temperature sintering furnace
In, under argon shield, it is warming up to 850 DEG C with 5 DEG C/min, prepares manganese monoxide porous graphene powder after insulation 3h, use
The dilute hydrochloric acid of 15% soaks 30min removal manganese monoxide and prepares porous graphene material.
Embodiment 2
Utilizing the Hummers method improved, using 50g purity is that the 80um natural flake graphite of 95wt% is at 3000ml
The concentrated sulphuric acid of 98wt% and the KMnO of 300g4Graphite oxide, centrifugal segregation reaction acid pickle are prepared in middle reaction, collect graphite oxide
Slurry, addition 2L water, regulation graphite oxide slurry PH=0.5, natural subsidence after placing half, removal upper strata acid waste liquid, more instead
It is added with into high purity water, until graphite oxide slurry PH=2.5 and color are become dark-brown from glassy yellow, now graphite oxide precipitation
Volume increases to about original 6 times, then adjusts the pre-graphite oxide slurry concentration purified to 10mg/ml 250rpm/min's
Stir 2h under mechanical stirring device, peel off the pre-graphene oxide slurry purified of preparation, then prepare through Freeze Drying Technique
Obtain the graphene oxide powder of pre-purification, by the graphene oxide powder that purifies in advance in high temperature sintering furnace, under nitrogen protection,
Being warming up to 900 DEG C with 10 DEG C/min, prepare manganese monoxide porous graphene powder after insulation 2h, the dilute hydrochloric acid with 10% soaks
Bubble 1h removes manganese monoxide and prepares porous graphene material.
Embodiment 3
Utilizing the Hummers method improved, using 80g purity is that the 180um natural flake graphite of 99wt% is at 4000ml
The concentrated sulphuric acid of 98wt% and the KMnO of 320g4Graphite oxide, centrifugal segregation reaction acid pickle are prepared in middle reaction, collect graphite oxide
Slurry, adds 1.5L water, regulates graphite oxide slurry PH=0.5, natural subsidence after placing half, removes upper strata acid waste liquid, then
Repeatedly adding high purity water, until graphite oxide slurry PH=2.5 and color are become dark-brown from glassy yellow, now graphite oxide sinks
Shallow lake volume increases to about original 4 times, adds water mechanical agitation 3h being diluted to 15mg/ml at 100rpm/min, peels off system
The standby pre-graphene oxide slurry purified, then prepares the graphene oxide powder of pre-purification through Freeze Drying Technique,
By the graphene oxide powder that purifies in advance in high temperature sintering furnace, under argon shield, it is warming up to 1000 DEG C with 8 DEG C/min, insulation
Preparing manganese monoxide porous graphene powder after 1h, the dilute hydrochloric acid with 5% soaks 2h removal manganese monoxide and prepares many
Hole grapheme material.
Embodiment 4
Utilizing the Hummers method improved, using 10g purity is that the 150um natural flake graphite of 80wt% is at 700ml
The concentrated sulphuric acid of 98wt% and the KMnO of 60g4Graphite oxide, centrifugal segregation reaction acid pickle are prepared in middle reaction, collect graphite oxide
Slurry, adds 0.5L water, regulates graphite oxide slurry PH=0.5, natural subsidence after placing half, removes upper strata acid waste liquid, then
Repeatedly adding high purity water, until graphite oxide slurry PH=2.0 and color are become dark-brown from glassy yellow, now graphite oxide sinks
Shallow lake volume increases to about original 6 times, adds water and is diluted to the 8mg/ml ultrasonic 30min of 800w in supersonic cleaning machine, peels off
The pre-graphene oxide slurry purified of preparation, then prepares the graphene oxide powder of pre-purification through Freeze Drying Technique
End, by the graphene oxide powder that purifies in advance in high temperature sintering furnace, under argon shield, is warming up to 1100 DEG C with 8 DEG C/min, protects
Preparing manganese monoxide porous graphene powder after temperature 30min, the dilute hydrochloric acid with 15% soaks 30min and removes manganese monoxide system
For obtaining porous graphene material.
Embodiment 5
Utilizing the Hummers method improved, using 30g purity is that the 75um natural flake graphite of 85wt% is at 1800ml
The concentrated sulphuric acid of 98wt% and the KMnO of 150g4Graphite oxide, centrifugal segregation reaction acid pickle are prepared in middle reaction, collect graphite oxide
Slurry, addition 3L water, regulation graphite oxide slurry PH=1.0, natural subsidence after placing, removal upper strata acid waste liquid, more instead
It is added with into high purity water, until graphite oxide slurry PH=2.5 and color are become dark-brown from glassy yellow, now graphite oxide precipitation
Volume increases to about original 5 times, adds water and is diluted to the 10mg/ml ultrasonic 1.5h of 400w in supersonic cleaning machine, peels off system
The standby pre-graphene oxide slurry purified, then prepares the graphene oxide powder of pre-purification through Freeze Drying Technique,
By the graphene oxide powder that purifies in advance in high temperature sintering furnace, under argon shield, it is warming up to 950 DEG C with 10 DEG C/min, insulation
Preparing manganese monoxide porous graphene powder after 1.5h, the dilute hydrochloric acid with 10% soaks 1h removal manganese monoxide and prepares
Porous graphene material.
Claims (5)
1. one kind utilizes the method that porous graphene directly prepared by the pre-graphene oxide slurry purified, it is characterised in that concrete
Step is as follows:
(1) oxidation stripping method prepares graphite oxide: using different size natural flake graphite is raw material, by a certain amount of concentrated sulphuric acid
Stir successively with potassium permanganate and be added thereto, graphite is aoxidized, thus obtains graphite oxide；
(2) the pre-graphene oxide slurry purified of preparation: add deionized water stirring in the graphite oxide slurry of highly acidity all
Even, after graphite to be oxidized is separated from the water, remove the aqueous phase on upper strata, retain lower sediment, again add deionized water and stir evenly, instead
Multiple the most repeatedly natural subsidence cleans graphite oxide, until graphite oxide solution is become after dark-brown and natural subsidence no longer from glassy yellow
Layering, collects the pre-purification graphite oxide slurry regulation concentration of lower floor's thickness, then by mechanical agitation or ultrasonic disperse system
The standby pre-graphene oxide slurry purified, finally utilizes Freeze Drying Technique, the pre-graphene oxide powder purified of preparation；
(3) preparing oxide carried porous graphene powder: utilize high temperature sintering furnace, gas shield is to the pre-oxidation stone purified
Ink alkene powder carries out high-temperature calcination process, prepares oxide carried porous graphene powder；
(4) porous graphene powder is prepared: oxide carried porous graphene powder high-temperature calcination obtained carries out room temperature
Dilute hydrochloric acid soaking and stirring a few hours, removing the oxide on surface, sucking filtration is cleaned multiple times PH=7 afterwards, and vacuum drying preparation is many
Hole graphene powder.
2. the side of porous graphene is directly prepared according to a kind of graphene oxide slurry utilizing pre-purification described in claim 1
Method, it is characterised in that: in described step (1), the method for synthesis graphite oxide is with graphite, concentrated sulphuric acid and potassium permanganate as raw material,
The method utilizing chemical oxidation prepares graphite oxide, and the method equipment is simple, with low cost, can realize the magnanimity system of graphite oxide
Standby, and the raw material type introduced in preparation process is less, and in the pre-purified product therefore obtained, the kind of impurity is single,
Be conducive to controlling hole number and the hole dimension of porous graphene；Natural graphite starting material a size of 45～180 μm, purity is that quality is divided
Number 80%-99%, the sulfuric acid concentration of selection is 98%, and adding graphite, potassium permanganate is 1: 3: 30-1 with the mass ratio of sulphuric acid:
6: 70, utilize the reaction of Hummers method to obtain graphite oxide.
3. the side of porous graphene is directly prepared according to a kind of graphene oxide slurry utilizing pre-purification described in claim 1
Method, it is characterised in that: step (2) utilizes the hydrophobicity of the graphite oxide slurry of highly acidity, clear by simple natural subsidence
The method of washing obtains the graphene oxide powder of pre-purification, is become dark-brown when graphite oxide slurry from glassy yellow in natural subsidence cleaning
After solution, the layering of natural subsidence then can become more and more difficult, becomes the graphite oxide slurry of thickness, when solution cleans to PH
During=1.5-2.5, and when the volume of slurry increases to original 3-6 times, the early stage product can prepared as porous graphene
The pre-graphite oxide that purifies is collected, and adjusts concentration the most again and utilizes ultrasonic 400-800W or stirring 100-350r/ to 8-20mg/ml
Min, time 30min-3h, peel off the pre-graphene oxide solution purified of preparation, last lyophilization, prepare pre-purification
Graphene oxide powder.
4. the side of porous graphene is directly prepared according to a kind of graphene oxide slurry utilizing pre-purification described in claim 1
Method, it is characterised in that: in step (3), the temperature of high temperature sintering furnace is set in 800-1100 DEG C, and protective gas is noble gas (argon
Gas, nitrogen), during high temperature sintering 30min-4h, obtain driving the pre-surface of graphene oxide impurity growing movement purified etching
Porous pattern and synchronize redox graphene, thus prepare oxide carried porous graphene, wherein oxide
Kind phenetic analysis is manganese monoxide, and remaining element sulphur is discharged with waste gas under the high temperature conditions and do not deposited on surface.
5. according to the preparation method of the porous graphene described in claim 1, it is characterised in that: in step (4), dilute hydrochloric acid is dense
Degree is 5-15%, and stirring dip time is 30min～2h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324318A (en) * | 2017-07-10 | 2017-11-07 | 黑龙江省宝泉岭农垦帝源矿业有限公司 | The method of the preparation of porous graphene and manganese oxide porous graphene composite |
| CN108892123A (en) * | 2018-06-08 | 2018-11-27 | 深圳新恒业电池科技有限公司 | A kind of preparation method of porous graphene |
| CN109231196A (en) * | 2018-11-21 | 2019-01-18 | 中国科学院兰州化学物理研究所 | The method for preparing graphene oxide based on non-polar organic solvent transfer purification technique |
| CN109368621A (en) * | 2018-12-24 | 2019-02-22 | 中国科学院兰州化学物理研究所 | The method of porous graphene is directly prepared by graphite |
| CN113120912A (en) * | 2021-04-22 | 2021-07-16 | 福建师范大学泉港石化研究院 | Method for preparing graphene-loaded silicon dioxide by using graphene oxide waste liquid |
| CN113697803A (en) * | 2021-08-23 | 2021-11-26 | 华南理工大学 | Graphite oxide material and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324318A (en) * | 2017-07-10 | 2017-11-07 | 黑龙江省宝泉岭农垦帝源矿业有限公司 | The method of the preparation of porous graphene and manganese oxide porous graphene composite |
| CN108892123A (en) * | 2018-06-08 | 2018-11-27 | 深圳新恒业电池科技有限公司 | A kind of preparation method of porous graphene |
| CN109231196A (en) * | 2018-11-21 | 2019-01-18 | 中国科学院兰州化学物理研究所 | The method for preparing graphene oxide based on non-polar organic solvent transfer purification technique |
| CN109231196B (en) * | 2018-11-21 | 2021-04-27 | 中国科学院兰州化学物理研究所 | Method for preparing graphene oxide based on nonpolar organic solvent transfer purification technology |
| CN109368621A (en) * | 2018-12-24 | 2019-02-22 | 中国科学院兰州化学物理研究所 | The method of porous graphene is directly prepared by graphite |
| CN113120912A (en) * | 2021-04-22 | 2021-07-16 | 福建师范大学泉港石化研究院 | Method for preparing graphene-loaded silicon dioxide by using graphene oxide waste liquid |
| CN113120912B (en) * | 2021-04-22 | 2022-05-27 | 福建师范大学泉港石化研究院 | Method for preparing graphene-loaded silicon dioxide by using graphene oxide waste liquid |
| CN113697803A (en) * | 2021-08-23 | 2021-11-26 | 华南理工大学 | Graphite oxide material and preparation method and application thereof |
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