CN106145102B - A method of preparing expanded graphite or graphene - Google Patents
A method of preparing expanded graphite or graphene Download PDFInfo
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- CN106145102B CN106145102B CN201610587608.8A CN201610587608A CN106145102B CN 106145102 B CN106145102 B CN 106145102B CN 201610587608 A CN201610587608 A CN 201610587608A CN 106145102 B CN106145102 B CN 106145102B
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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
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Abstract
The invention discloses a kind of method preparing expanded graphite or graphene, this method technical process is as follows：After graphite and swelling agent are uniformly mixed, pretreated solid mixture is added in suitable chlorosulfonic acid, expanded graphite and graphene are quickly prepared under room temperature.The present invention prepares expanded graphite and is not related to any high temperature and pressure process, and safe operation is of low cost, environmental-friendly.The expanded graphite that the present invention obtains can realize 50-1000 times of volume expansion, and maintain the integrality of graphite platelet structure.Expanded graphite prepared by the present invention can be widely applied to the various fields such as energy storage, opto-electronic device, solar cell, anticorrosive paint.Expanded graphite prepared by the present invention also can be used as the presoma for preparing high-quality graphene, and expanded graphite is carried out mechanics stripping, can get the high-quality graphene for being substantially free of defect.
Description
【Technical field】
The invention belongs to technical field of material, more particularly, to a kind of side preparing expanded graphite or graphene
Method.
【Background technology】
Graphene has been concerned as a kind of novel carbon material since being found from 2004；It has high light transmission
Property, electric conductivity and specific surface area and excellent mechanical property, in composite material, energy and material, the fields such as communication have wide
Application prospect and huge commercial value.
How highly effective and safe, low cost, a large amount of prepare realize one that industrialized production is still graphene application study
Important essential precondition.
In disclosed expanded graphite preparation method, Behabtu[ in 2010;Behabtu et al.,Nat
Nanotechnol,2010,5,406]Deng the new method for proposing prepared by graphene, specially：Under vacuum condition, graphite powder drying
Dehumidifying, hot wind continuously blows 12h processing later, and then treated graphite powder is added in chlorosulfonic acid and continuously stirs 48h, long-time
Centrifugation obtains graphene.This method prepares graphene process complexity, and the period is long, and preparation method is limited by all many conditions, uncomfortable
For mass producing.Wherein improvement of the Changchun Inst. of Applied Chemistry, Chinese Academy of Sciences to the experiment, (patent No.：
CN102627272A) it uses chlorosulfonic acid and hydrogen peroxide complex system is i.e. peelable prepares graphene, and entire reaction is rendered as
Explosive, chlorosulfonic acid meets water and vigorous reaction occurs so that this method is difficult to scale industrial production.Chinese patent《It is a kind of normal
The method that expanded graphite or graphene are directly prepared under normal temperature and pressure》It is dense by the way that graphite to be added in (105253878 A of CN)
Sulfuric acid prepares expanded graphite or graphene with the system of combining of oxidant ammonium persulfate etc., but this method discharges in preparation process
The toxic gases such as a large amount of sulfur dioxide, and at 3 hours or more under reaction time normal temperature and pressure.In the presence of discharge a large amount of toxic gases and
Long preparation period problem.Chinese patent《The graphene for preparing the method for graphene and being prepared by this method》(CN
105084344 A) by using graphite powder is mixed with chlorosulfonic acid and is put into reactor, it is 110 DEG C~130 DEG C in temperature
Under the conditions of heat 4~6 hours, pretreating graphite is mixed with the concentrated sulfuric acid, stir and be added dropwise hydrogenperoxide steam generator cause expansion reaction,
Obtain expanded graphite.Although the expanded graphite of high quality is prepared in this method, but this method pretreatment reaction time is long, and
Long-time heating is needed, it is not only cumbersome, and also the production cycle is too long.Therefore, a kind of extensive, low cost of exploitation and environment
Close friend, simple and easy to control, the method for a large amount of preparation high quality expanded graphites or graphene is imperative.
【Invention content】
The object of the present invention is to provide a kind of methods preparing expanded graphite or graphene, can extensive, low cost
High quality expanded graphite or graphene are prepared, and environmental-friendly, it is simple and easy to control.
To achieve the goals above, the present invention adopts the following technical scheme that：
A method of expanded graphite is prepared, is achieved by the steps of：
(a) under normal temperature and pressure, graphite is slowly stirred with solid inorganic salt swelling agent in open-top receptacle appropriate and is mixed
Uniformly, pre-treated solid mixture is obtained；Wherein, the dosage of solid inorganic salt swelling agent is 1-50 times of graphite weight；
(b) under normal temperature and pressure, the pre-treated solid mixture is added in chlorosulfonic acid and is reacted, wait for that reaction is completed
Afterwards, highly expanded graphite is obtained；Wherein, the mass ratio of the chlorosulfonic acid and the pre-treated solid mixture is 5:1-30:1；
(c) after the obtained highly expanded graphite being washed with deionized, the high power expansion stone of hygrometric state is obtained by filtration
Ink.
Further, the highly expanded graphite of the hygrometric state obtained by step (c) is sprayed or is freeze-dried, obtain high power
Expanded graphite.
In the step (a), the solid inorganic salt swelling agent using sodium perborate, carbamide percarbonate, SODIUM PERCARBONATE and
One or more of adduct sodium sulphate-hydrogen peroxide-sodium chloride, sodium carbonate, sodium bicarbonate and ammonium hydrogen carbonate.
In the step (a), the time being stirred is 1min-3h, mixing speed 10rpm-1000rpm.
In the step (a) and the step (b), the normal pressure is 1atm, and the room temperature is 10 DEG C -40
℃。
A method of graphene is prepared, is achieved by the steps of：
(a) under normal temperature and pressure, graphite is slowly stirred with solid inorganic salt swelling agent in open-top receptacle appropriate and is mixed
Uniformly, pre-treated solid mixture is obtained；Wherein, the dosage of solid inorganic salt swelling agent is 1-50 times of graphite weight；
(b) under normal temperature and pressure, the pre-treated solid mixture is added in chlorosulfonic acid and is reacted；Wherein, described
The mass ratio of chlorosulfonic acid and the pre-treated solid mixture is 5:1-30:1；
(c) ultrasonic remover is directly added into the mixed liquor after step (b) reaction, ultrasound stripping obtains graphene dispersion
Liquid；Wherein, the quality of ultrasonic remover is 1-50 times of graphite quality；
(d) graphene dispersing solution is filtered, distilled water washs repeatedly repeatedly obtains the graphene of hygrometric state；
(e) graphene of the hygrometric state is sprayed or is freeze-dried, obtain graphene powder.
In the step (a), the solid inorganic salt swelling agent using sodium perborate, carbamide percarbonate, SODIUM PERCARBONATE and
One or more of adduct sodium sulphate-hydrogen peroxide-sodium chloride, sodium carbonate, sodium bicarbonate and ammonium hydrogen carbonate.
In the step (a), the time being stirred is 1min-3h, mixing speed 10rpm-1000rpm.
In the step (a) and the step (b), the normal pressure is 1atm, and the room temperature is 10 DEG C -40 DEG C.
In the step (c), the ultrasonic remover is pure water solution, N-Methyl pyrrolidone, N, N- dimethyl methyls
One or more of amide, DMAC N,N' dimethyl acetamide, ethyl alcohol；Ultrasonic time is 0.5h-2h, ultrasonic power 20-
80KHz。
Using the above scheme, the advantage of the invention is that：
(1) it is not necessarily to high temperature and pressure to operate, entire reaction process discharges a small amount of sulfur dioxide, and expansion process is to discharge titanium dioxide
It is environmentally protective based on carbon.
(2) intumescent system that this method uses selects cheap chlorosulfonic acid, carbonate or percarbonate system, anyway the period
Short, whole manufacturing cost is cheap, is convenient for industrialized production.
(3) percarbonate or carbonate substance also have the effect for neutralizing acid reaction medium in this method reaction process
Fruit reduces the processing cost of waste reaction solution.
(4) although it is reaction dissolvent that the present invention, which uses chlorosulfonic acid, it is not introduced into water, avoids the violent of chlorosulfonic acid and water
Reaction.
The expanded graphite obtained by the method for the invention can realize 50-1000 times of volume expansion, and maintain graphite
The integrality of lamellar structure.Expanded graphite prepared by the present invention can be widely applied to energy storage, opto-electronic device, solar cell,
The various fields such as anticorrosive paint.Expanded graphite prepared by the present invention also can be used as the presoma for preparing high-quality graphene, will be swollen
Swollen graphite carries out mechanics stripping, can get the high-quality graphene for being substantially free of defect.
【Description of the drawings】
Fig. 1 is the surface topography map of the highly expanded graphite scanning electron microscopic observation of 4 gained of the embodiment of the present invention；
Fig. 2 is the surface topography map of the graphene scanning electron microscopic observation of 5 gained of the embodiment of the present invention；
Fig. 3 is the X-ray diffracting spectrum and Raman collection of illustrative plates of the graphene and raw graphite powder of 5 gained of the embodiment of the present invention.
【Specific implementation mode】
It is further illustrated the present invention below by way of specific implementation mode.It should be understood that specific implementation example is not used in limitation
The scope of the present invention.Under conditions of no substantial technological content alteration, be also considered as the present invention can practical range, in the present invention
It is required that protection domain in.
Embodiment 1：
A kind of method preparing expanded graphite of the present invention, is achieved by the steps of：
(1) by graphite 10g and carbamide percarbonate 200g, 0.5h is stirred with the rotating speed of 100rmp in iron ware,
The solid mixture stirred evenly.
(2) in conical flask, the chlorosulfonic acid of 20ml and solid mixture 2g are sequentially added, magnetic agitation 5min, is stirred
Above-mentioned solid mixture rapid spatial expansion in the process, correspondingly the rotating speed of magnetic agitation to improve 10%-50%, make bulge
The reaction heat divided is quickly discharged into ambient enviroment.After the completion of reaction, detaches upper layer expanded graphite and acid solution, deionized water are more
Secondary washing filtering obtains the highly expanded graphite of hygrometric state to neutrality.
Embodiment 2：
A kind of method preparing expanded graphite of the present invention, is achieved by the steps of：
(1) by graphite 10g and sodium perborate 200g, 0.5h is stirred with the rotating speed of 100rmp in iron ware, is obtained
To the solid mixture stirred evenly.
(2) in conical flask, the chlorosulfonic acid of 20ml and solid mixture 2g are sequentially added, magnetic agitation 5min, is stirred
Above-mentioned solid mixture rapid spatial expansion in the process, correspondingly the rotating speed of magnetic agitation to improve 10%-50%, make bulge
The reaction heat divided is quickly discharged into ambient enviroment.After the completion of reaction, detaches upper layer expanded graphite and acid solution, deionized water are more
Secondary washing filtering obtains the highly expanded graphite of hygrometric state to neutrality.
Embodiment 3：
A kind of method preparing expanded graphite of the present invention, is achieved by the steps of：
(1) by graphite 10g and SODIUM PERCARBONATE 200g, 2h is stirred with the rotating speed of 50rmp in iron ware, is stirred
Mix uniform solid mixture.
(2) in conical flask, the chlorosulfonic acid of 20ml and solid mixture 2g are sequentially added, magnetic agitation 5min, is stirred
Above-mentioned solid mixture rapid spatial expansion in the process, correspondingly the rotating speed of magnetic agitation to improve 10%-50%, make bulge
The reaction heat divided is quickly discharged into ambient enviroment.After the completion of reaction, detaches upper layer expanded graphite and acid solution, deionized water are more
Secondary washing filtering obtains the highly expanded graphite of hygrometric state to neutrality.
(3) it is freeze-dried the highly expanded graphite of hygrometric state to obtain highly expanded graphite.
Embodiment 4：
A kind of method preparing expanded graphite of the present invention, is achieved by the steps of：
(1) by graphite 10g and sodium bicarbonate 200g, 1h is stirred with the rotating speed of 100rmp in iron ware, is obtained
The solid mixture stirred evenly.
(2) in conical flask, the chlorosulfonic acid of 20ml and solid mixture 2g are sequentially added, magnetic agitation 5min, is stirred
Above-mentioned solid mixture rapid spatial expansion in the process, correspondingly the rotating speed of magnetic agitation to improve 10%-50%, make bulge
The reaction heat divided is quickly discharged into ambient enviroment.After the completion of reaction, detaches upper layer expanded graphite and acid solution, deionized water are more
Secondary washing filtering obtains the highly expanded graphite of hygrometric state to neutrality.
(3) it is freeze-dried the highly expanded graphite of hygrometric state to obtain highly expanded graphite.
The surface topography of highly expanded graphite scanning electron microscopic observation obtained by the present embodiment is as shown in Figure 1.
Embodiment 5：
A kind of method preparing graphene of the present invention, is achieved by the steps of：
(1) mixed with the stirring of the rotating speed of 100rmp in iron ware by graphite 10g and carbamide percarbonate or Boratex 200g
Close 0.5h, the solid mixture stirred evenly.
(2) in conical flask, the chlorosulfonic acid of 20ml and solid mixture 2g are sequentially added, magnetic agitation 5min, is stirred
Above-mentioned solid mixture rapid spatial expansion in the process, correspondingly the rotating speed of magnetic agitation to improve 10%-50%, make bulge
The reaction heat divided is quickly discharged into ambient enviroment.After the completion of reaction, hygrometric state expanded graphite and the mixture of acid solution are obtained；Again
(it is 4 by the volume ratio of water and N-Methyl pyrrolidone by 100g ultrasounds remover:1 is prepared) it is added to hygrometric state expanded graphite
With the mixture of acid solution, is handled 30 minutes at 25 DEG C by the Probe Ultrasonic Searching of 80kHz, obtain graphene dispersing solution.
(3) graphene dispersing solution is filtered, is washed with distilled water, again water-dispersible, then freeze-drying obtains graphite
Alkene powder.
(a), (b) are shown in the surface topography such as Fig. 2 of graphene scanning electron microscopic observation obtained by the present embodiment；The present embodiment
The graphene of gained and the X-ray diffracting spectrum of raw graphite powder and Raman collection of illustrative plates are as shown in Figure 3.
Embodiment 6：
A kind of method preparing graphene of the present invention, embodiment 6 are differed only in embodiment 5：Ultrasonic remover is pressed
The volume ratio of water and DMAC N,N' dimethyl acetamide is 4:1 is formulated.
Embodiment 7：
A kind of method preparing expanded graphite of the present invention, is achieved by the steps of：
(1) by graphite 1g and ammonium hydrogen carbonate 49g, 30min is stirred with the speed of 500rmp in iron ware, is obtained
The solid mixture stirred evenly.
(2) in beaker, the chlorosulfonic acid of 30ml and solid mixture 5g are sequentially added, magnetic agitation 5min is stirred
Above-mentioned solid mixture rapid spatial expansion in journey, correspondingly the rotating speed of magnetic agitation to improve 10%-50%, make dilation
Reaction heat be quickly discharged into ambient enviroment.After the completion of reaction, detaches upper layer expanded graphite and acid solution, deionized water are multiple
Washing filtering obtains the highly expanded graphite of hygrometric state to neutrality.
Embodiment 8：
A kind of method preparing graphene of the present invention, is achieved by the steps of：
(1) by graphite 1g and ammonium hydrogen carbonate 49g, 30min is stirred with the speed of 500rmp in iron ware, is obtained
The solid mixture stirred evenly.
(2) in beaker, the chlorosulfonic acid of 30ml and solid mixture 5g are sequentially added, magnetic agitation 5min is stirred
Above-mentioned solid mixture rapid spatial expansion in journey, correspondingly the rotating speed of magnetic agitation to improve 10%-50%, make dilation
Reaction heat be quickly discharged into ambient enviroment.After the completion of reaction, hygrometric state expanded graphite and the mixture of acid solution are obtained；
(3) (it is 4 by the volume ratio of water and ethyl alcohol by 50g ultrasounds remover:1 is prepared) it is added to hygrometric state expanded graphite
With the mixture of acid solution, is handled 60 minutes at 25 DEG C by the Probe Ultrasonic Searching of 20kHz, obtain graphene dispersing solution.
(4) graphene dispersing solution is filtered, distills water washing, again water-dispersible, then freeze-drying obtains graphene
Powder.
Embodiment 9：
A kind of method preparing graphene of the present invention, is achieved by the steps of：
(1) by graphite 10g and SODIUM PERCARBONATE 200g, 2h is stirred with the rotating speed of 50rmp in iron ware, is stirred
Mix uniform solid mixture.
(2) in conical flask, the chlorosulfonic acid of 20ml and solid mixture 2g are sequentially added, magnetic agitation 5min, is stirred
Above-mentioned solid mixture rapid spatial expansion in the process, correspondingly the rotating speed of magnetic agitation to improve 10%-50%, make bulge
The reaction heat divided is quickly discharged into ambient enviroment.After the completion of reaction, detaches upper layer expanded graphite and acid solution, deionized water are more
Secondary washing filtering obtains the highly expanded graphite of hygrometric state to neutrality.
(3) it is freeze-dried the highly expanded graphite of hygrometric state to obtain highly expanded graphite.
(4) it is 4 highly expanded graphite 1g to be added to by the volume ratio of water and DMAC N,N' dimethyl acetamide:1 is formulated
100ml mixed liquors in, handled 30 minutes at 25 DEG C by the Probe Ultrasonic Searching of 80kHz, obtain graphene dispersing solution.
(5) graphene dispersing solution is filtered, distills water washing, again water-dispersible, then freeze-drying obtains graphene
Powder.
Embodiment 10：
A kind of method preparing graphene of the present invention, is achieved by the steps of：
(1) by graphite 10g and sodium bicarbonate 200g, 1h is stirred with the rotating speed of 100rmp in iron ware, is obtained
The solid mixture stirred evenly.
(2) in conical flask, the chlorosulfonic acid of 20ml and solid mixture 2g are sequentially added, magnetic agitation 5min, is stirred
Above-mentioned solid mixture rapid spatial expansion in the process, correspondingly the rotating speed of magnetic agitation to improve 10%-50%, make bulge
The reaction heat divided is quickly discharged into ambient enviroment.After the completion of reaction, detaches upper layer expanded graphite and acid solution, deionized water are more
Secondary washing filtering obtains the highly expanded graphite of hygrometric state to neutrality.
(3) it is freeze-dried the highly expanded graphite of hygrometric state to obtain highly expanded graphite.
(4) it is 4 highly expanded graphite 1g to be added to by the volume ratio of water and DMAC N,N' dimethyl acetamide:1 is formulated
100ml mixed liquors in, handled 30 minutes at 25 DEG C by the Probe Ultrasonic Searching of 80kHz, obtain graphene dispersing solution.
(5) graphene dispersing solution is filtered, distills water washing, again water-dispersible, then freeze-drying obtains graphene
Powder.
Claims (6)
1. a kind of method preparing expanded graphite, which is characterized in that be achieved by the steps of：
(a) under normal temperature and pressure, graphite is slowly stirred with solid inorganic salt swelling agent in open-top receptacle appropriate and is uniformly mixed,
Obtain pre-treated solid mixture；Wherein, the dosage of solid inorganic salt swelling agent is 1-50 times of graphite weight；The solid without
Machine salt swelling agent is using sodium perborate, carbamide percarbonate, SODIUM PERCARBONATE and adduct sodium sulphate-hydrogen peroxide-sodium chloride, carbon
One or more of sour sodium, sodium bicarbonate and ammonium hydrogen carbonate；Specifically, the time being stirred is 1min-3h, mixing speed
For 10rpm-1000rpm；
(b) under normal temperature and pressure, the pre-treated solid mixture is added in chlorosulfonic acid and is reacted, waited after the completion of reacting,
Obtain highly expanded graphite；Wherein, the mass ratio of the chlorosulfonic acid and the pre-treated solid mixture is 5:1-30:1；
(c) after the obtained highly expanded graphite being washed with deionized, the highly expanded graphite of hygrometric state is obtained by filtration.
2. a kind of method preparing expanded graphite according to claim 1, it is characterised in that：It will be wet obtained by step (c)
The highly expanded graphite of state is sprayed or is freeze-dried, and highly expanded graphite is obtained.
3. a kind of method preparing expanded graphite according to claim 1, it is characterised in that：The step (a) and described
In step (b), the normal pressure is 1atm, and the room temperature is 10 DEG C -40 DEG C.
4. a kind of method preparing graphene, which is characterized in that be achieved by the steps of：
(a) under normal temperature and pressure, graphite is slowly stirred with solid inorganic salt swelling agent in open-top receptacle appropriate and is uniformly mixed,
Obtain pre-treated solid mixture；Wherein, the dosage of solid inorganic salt swelling agent is 1-50 times of graphite weight；The solid without
Machine salt swelling agent is using sodium perborate, carbamide percarbonate, SODIUM PERCARBONATE and adduct sodium sulphate-hydrogen peroxide-sodium chloride, carbon
One or more of sour sodium, sodium bicarbonate and ammonium hydrogen carbonate；Specifically, the time being stirred is 1min-3h, mixing speed
For 10rpm-1000rpm；
(b) under normal temperature and pressure, the pre-treated solid mixture is added in chlorosulfonic acid and is reacted；Wherein, the chlorine sulphur
The sour mass ratio with the pre-treated solid mixture is 5:1-30:1；
(c) ultrasonic remover is directly added into the mixed liquor after step (b) reaction, ultrasound stripping obtains graphene dispersing solution；
Wherein, the quality of ultrasonic remover is 1-50 times of graphite quality；
(d) graphene dispersing solution is filtered, distilled water washs repeatedly repeatedly obtains the graphene of hygrometric state；
(e) graphene of the hygrometric state is sprayed or is freeze-dried, obtain graphene powder.
5. a kind of method preparing expanded graphite according to claim 4, it is characterised in that：The step (a) and described
In step (b), the normal pressure is 1atm, and the room temperature is 10 DEG C -40 DEG C.
6. a kind of method preparing expanded graphite according to claim 4, it is characterised in that：It is described in the step (c)
Ultrasonic remover be pure water solution, N-Methyl pyrrolidone, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, ethyl alcohol
One or more of；Ultrasonic time is 0.5h-2h, ultrasonic power 20-80KHz.
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| CN107082425B (en) * | 2017-04-14 | 2018-12-28 | 燕山大学 | A kind of method that one step of room temperature prepares expanded graphite |
| CN107275621A (en) * | 2017-07-07 | 2017-10-20 | 天津巴莫科技股份有限公司 | Graphene-based sulphur composite positive pole and preparation method thereof |
| CN107539973B (en) * | 2017-09-12 | 2020-08-28 | 华侨大学 | Preparation method of graphene powder |
| CN107585761A (en) * | 2017-10-13 | 2018-01-16 | 南京旭羽睿材料科技有限公司 | A kind of expanded graphite alkene preparation method |
| CN108439393A (en) * | 2018-04-25 | 2018-08-24 | 燕山大学 | A kind of method that one step of room temperature prepares expanded graphite |
| CN110117118B (en) * | 2019-04-26 | 2022-01-14 | 浙江龙盛化工研究有限公司 | Method for treating chlorosulfonated acidic wastewater |
| CN111109289A (en) * | 2019-12-31 | 2020-05-08 | 南京福斯特牧业科技有限公司 | Stable solid hydrogen peroxide adduct and application thereof in livestock and poultry and aquaculture fields |
| CN111217367B (en) * | 2020-01-14 | 2021-08-24 | 中国石油大学(华东) | Multi-element composite intercalated low-temperature expandable graphite system for profile control and water shutoff of deep reservoir and preparation method and application thereof |
| CN111960414B (en) * | 2020-07-02 | 2023-01-20 | 天津科技大学 | Wood biomass-based porous carbon material prepared from inorganic molten salt hydrate, and preparation method and application thereof |
| CN115072712A (en) * | 2022-06-21 | 2022-09-20 | 西南科技大学 | Graphene with large sheet diameter and high conductivity and preparation method thereof |
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