CN105819438A - Method for preparing nanometer graphene materials in large scale mode through hydraulic shearing - Google Patents
Method for preparing nanometer graphene materials in large scale mode through hydraulic shearing Download PDFInfo
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention provides a method for preparing nanometer graphene materials in a large scale mode through hydraulic shearing. The method includes the steps that graphite powder is added into liquid, a small number of oxidizing agents are added, oxidizing agent molecules rapidly and alternately enter graphite through a multifunctional grinding dispersion machine in an inserted mode, a high shear emulgator and a high-pressure homogenizer which are connected in series, and the materials are sheared and peeled under the hydraulic effect through continuous mechanical force, and are rapidly layered. The problem that graphene can not be prepared in a large scale mode with high quality and low cost at present is solved, it is guaranteed that the graphene structure is not damaged, and the obtained graphene can be widely applied to the lithium battery field, the super capacitor field, the polymer composite material field, the heat-conduction and heat-radiation film field, the functional coating field, the national-defense and military-industry field and the like.
Description
Technical field
The present invention relates to technical field of nano material, relate generally to a kind of method utilizing aquashear scale to prepare nano-graphene material.
Background technology
Since grapheme material in 2004 is found, researcher has carried out long-time further investigation to it, and drawn, from research, the hexagonal structure that Graphene is made up of SP2 hybrid orbital, owing to the existence of SP2 hybrid orbital makes Graphene have good electric conductivity, can apply at opto-electronic device and electrochemical energy source domain as good conductor.Along with research deeply, the optical property of Graphene, mechanical property, catalytic performance etc. are found in succession so that it have also been obtained in fields such as electromagnetic shielding material, microwave absorbing material, gas sensor, catalyst and is widely applied.
Graphene has the performance of excellence and is widely applied prospect, but the technology of preparing of Graphene is the most ripe, and product quality is the highest, unstable properties and large-scale production cannot all limit its extensive application in every field.It is of a great variety to prepare preparing of Graphene at present, mainly has physical method and the big class of chemical method two, but more or less there is corresponding problem, causes the needs that cannot meet industrial mass production.Graphene prepared by physical method is mainly based on mechanical stripping, but properties of product are unstable, and distribution of sizes cannot accurately control, and Graphene size is the key factor affecting its performance.Advantage is that energy consumption is little, pollutes little, and safety can large-scale continuous production.Chemical method prepares Graphene mainly the method such as catalytic decomposition and organic synthesis, additionally can also notify that graphite carries out preparing grapheme through oxidation reduction.It is controlled that Graphene prepared by chemical method has size, steady performance, but in chemical method preparation process, energy consumption is relatively big, unsuitable large-scale continuous production, and relatively physical method has higher danger.And preparation process can use a large amount of inorganic matter and soda acid, the subsequent treatment causing technique is complex, the most indirectly adds production cost；Oxidation in chemical process can cause the hydraulic performance decline of Graphene.
Chinese invention patent application number 201310750433.4 discloses a kind of method for preparing super capacitor slurry, after it is by tentatively mixing Graphene, binding agent, solvent and other auxiliary additives, uses high-shear emulsifying device that mixed liquor is carried out mechanical mixture.Can get the preferable graphene dispersing solution of dispersibility by the method, and jitter time can be shortened.
Chinese invention patent application number 201510073825.0 discloses a kind of tonne of class mechanical stripping device producing Graphene and production method thereof, it is made up of one-level or multi-stage mechanical peel-off device its mechanical stripping segregation apparatus, by mutually colliding stripping between rotor and graphite, between graphite granule, and achieve multistage continuous processing, can on a large scale, persistence prepare Graphene and dispersion liquid thereof.
Chinese invention patent application 201511007072.X discloses a kind of method utilizing lignin to prepare Graphene, it is by carrying out pretreatment with acid-base pair lignin, then mixed by high pressure homogenizer, homogenizing, and decompose under the effect of catalyst, then entered pyrolytic and prepare Graphene.
Chinese invention patent application number 201010179119.1 discloses the method that high-efficiency and low-cost mechanical stripping prepares Graphene or graphene oxide, and it, by being mixed in a solvent with other larger particles by graphite, is then by mechanically pulling off and prepares Graphene.The charge stripping efficiency of graphite can be improved by the method, and large-scale production can be realized.
From above-mentioned analysis it appeared that, the current method using mechanical stripping to prepare Graphene is more, but these methods are substantially and carry out based on a kind of mechanical stripping method, the Graphene prepared has that quality is unstable, size is uneven, cannot some problems such as large-scale continuous production.The present invention by by grinding distribution agent, high-shear emulsion machine, high pressure homogenizer connect, graphite mixed liquor passes sequentially through three kinds of mechanical stripping devices to carry out continuing repeatedly to peel off mixing, prepared be uniformly dispersed, the graphite of size uniformity.Both ensure that shearing was peeled off, by ensure that graphene-structured is injury-free, the Graphene obtained can be widely applied to the fields such as lithium battery, ultracapacitor, polymer composite, heat conduction and heat radiation film, functional paint, defence and military.
Summary of the invention
For use at present mechanical stripping equipment cannot prepare size uniform, be uniformly dispersed, the problem of steady quality Graphene, the present invention proposes to use the multiple mechanical stripping equipment of series connection and mixing apparatus to carry out Graphene peeling off mixing, to solve currently to prepare Graphene process problem encountered.Especially by fluid power, graphite being carried out lift-off processing step by step and obtain nano-graphene material, concrete technical scheme is as follows:
(1) being dissolved in solvent by oxidant, then will form graphite powder mixed liquor in graphite dispersion to solution, the concentration of graphite mixed liquor is 10-100g/L；
(2) it is sent to the graphite powder mixed liquor that step (1) prepares in grinding distribution machine carry out grinding for the first time, obtains the graphene suspension of certain size；
(3) graphene suspension obtained in step (2) is continued to be fed into high-shear emulsifying device carries out second time mechanical shearing and mixing, obtain that particle diameter is less, the more preferable graphene dispersing solution of dispersibility；
(4) graphene dispersing solution obtained in step (3) is continued to be fed in high pressure homogenizer, utilize high pressure homogenizer that graphene dispersing solution is mixed again, then there is mutually collision by the ejection of high pressure homogenize machine nozzle in material, realize third time mechanical stripping, obtain the graphene dispersing solution of size uniform；
(5) carry out the graphene dispersing solution obtained in step (4) filtering, be centrifuged, be dried, obtain nano-graphene material.
Preferably, the one during described graphite raw material chooses natural flake graphite, graphite powder, expanded graphite, highly oriented graphite, agraphitic carbon.
Preferably, described oxidant is one or more the mixture in Ammonium persulfate., potassium dichromate, chromic acid, potassium permanganate, potassium ferrate, concentrated sulphuric acid, concentrated hydrochloric acid, concentrated nitric acid, perchloric acid, strong phosphoric acid or glacial acetic acid, and graphite and oxidizer mass ratio are 1:0.1-0.3.
Preferably, the described solvent combination of any one or more in butyl acetate, benzyl oxide, diethyl carbonate, DBE, ethyl carbitol acetate, Ethyl methyl carbonate, butyl carbitol acetate, butyl cellosolve acetate, Allyl carbonate, ethanolamine, DMSO, dimethyl succinate, N-dodecylpyrrolidone, propylene glycol methyl ether acetate, NMP, ethyl phthalate, dimethylbenzene, pyridine, dibutyl phthalate, benzaldehyde, dimethyl carbonate, NOP, diphenyl carbonate and deionized water.
Preferably, the rotating speed of described mechanical lapping is 100-1500rpm, and splitting time is 1-5h.
Preferably, the shearing force of described high-shear emulsifying is 1000-5000ips, and emulsification times is 0.5-3h.
Preferably, the described operating pressure higher than homogenizer is 10-80MPa.
Compared with the technology of existing preparation graphene microchip, the multistage aquashear of employing that the present invention proposes is prepared nano-graphene material and is had the advantage that
1. present invention firstly provides employing multiple aquashear equipment tandem compound Graphene is repeatedly peeled off mixed processing to prepare nano-graphene material；
2. owing to present invention employs grinding distribution machine, high-shear emulsion machine, high pressure homogenizer are combined, achieve the mixing of stripping step by step of Graphene, the Graphene size prepared is more uniformly distributed, and due to during add oxidant and carry out showing processing, Graphene is less likely to occur to reunite；
3. it is in series due to three devices of the present invention, it is possible to achieve large-scale continuous production, and safe and pollution-free.
Accompanying drawing explanation
For further illustrating a kind of method utilizing aquashear scale to prepare nano-graphene material, illustrated by accompanying drawing.
1 one kinds of accompanying drawing utilizes the flow chart that nano-graphene material is prepared in aquashear scale.
Specific embodiments:
By detailed description of the invention, the present invention is described in further detail, but this should not being interpreted as, the scope of the present invention is only limitted to Examples below.In the case of without departing from said method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or change, should be included in the scope of the present invention.
Embodiment 1
Weigh 5g potassium ferrate, be dissolved in 1L deionized water, then weigh 50g graphite powder, it is the most tentatively mixed with potassium ferrate solution, obtain graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out for the first time mechanical stripping, rotating speed is 500rpm, and milling time is 2h；Obtain the graphene suspension that grain size is bigger；
By stepThe middle graphene suspension prepared through for the first time mechanical stripping is sent directly in high-shear emulsifying device by pipeline, mechanical stripping dispersion 0.5h under shearing force is 2000ips, obtain smaller, disperse the graphene dispersing solution that is more uniformly distributed；
By stepThe middle graphene dispersion being mixed to prepare through second time mechanical stripping is sent directly in high pressure homogenizer by pipeline, material is carried out pressurization mixing, after reaching 50MPa, material is clashed with higher speed ejection by the nozzle of high pressure homogenizer, it is achieved third time peels off mixing；
By stepThe dispersion liquid prepared carries out filtration treatment, remove larger-size Graphene granule in dispersion liquid so as to get product cut size be more uniformly distributed；
By stepThe graphene dispersing solution of middle filtration gained is centrifuged, dried, obtains nano-graphene material.
Embodiment 2
Weigh 10g potassium ferrate, be dissolved in 1L deionized water, then weigh 50g graphite powder, it is the most tentatively mixed with potassium ferrate solution, obtain graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out for the first time mechanical stripping, rotating speed is 500rpm, and milling time is 2h；Obtain the graphene suspension that grain size is bigger；
By stepThe middle graphene suspension prepared through for the first time mechanical stripping is sent directly in high-shear emulsifying device by pipeline, mechanical stripping dispersion 0.5h under shearing force is 2000ips, obtain smaller, disperse the graphene dispersing solution that is more uniformly distributed；
By stepThe middle graphene dispersion being mixed to prepare through second time mechanical stripping is sent directly in high pressure homogenizer by pipeline, material is carried out pressurization mixing, after reaching 50MPa, material is clashed with higher speed ejection by the nozzle of high pressure homogenizer, it is achieved third time peels off mixing；
By stepThe dispersion liquid prepared carries out filtration treatment, remove larger-size Graphene granule in dispersion liquid so as to get product cut size be more uniformly distributed；
By stepThe graphene dispersing solution of middle filtration gained is centrifuged, dried, obtains nano-graphene material.
Embodiment 3
Weigh 10g potassium ferrate, be dissolved in 1L deionized water, then weigh 50g graphite powder, it is the most tentatively mixed with potassium ferrate solution, obtain graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out for the first time mechanical stripping, rotating speed is 1000rpm, and milling time is 2h；Obtain the graphene suspension that grain size is bigger；
By stepThe middle graphene suspension prepared through for the first time mechanical stripping is sent directly in high-shear emulsifying device by pipeline, mechanical stripping dispersion 0.5h under shearing force is 2000ips, obtain smaller, disperse the graphene dispersing solution that is more uniformly distributed；
By stepThe middle graphene dispersion being mixed to prepare through second time mechanical stripping is sent directly in high pressure homogenizer by pipeline, material is carried out pressurization mixing, after reaching 50MPa, material is clashed with higher speed ejection by the nozzle of high pressure homogenizer, it is achieved third time peels off mixing；
By stepThe dispersion liquid prepared carries out filtration treatment, remove larger-size Graphene granule in dispersion liquid so as to get product cut size be more uniformly distributed；
By stepThe graphene dispersing solution of middle filtration gained is centrifuged, dried, obtains nano-graphene material.
Embodiment 4
Weigh 10g potassium ferrate, be dissolved in 1L deionized water, then weigh 50g graphite powder, it is the most tentatively mixed with potassium ferrate solution, obtain graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out for the first time mechanical stripping, rotating speed is 1000rpm, and milling time is 4h；Obtain the graphene suspension that grain size is bigger；
By stepThe middle graphene suspension prepared through for the first time mechanical stripping is sent directly in high-shear emulsifying device by pipeline, mechanical stripping dispersion 0.5h under shearing force is 2000ips, obtain smaller, disperse the graphene dispersing solution that is more uniformly distributed；
By stepThe middle graphene dispersion being mixed to prepare through second time mechanical stripping is sent directly in high pressure homogenizer by pipeline, material is carried out pressurization mixing, after reaching 50MPa, material is clashed with higher speed ejection by the nozzle of high pressure homogenizer, it is achieved third time peels off mixing；
By stepThe dispersion liquid prepared carries out filtration treatment, remove larger-size Graphene granule in dispersion liquid so as to get product cut size be more uniformly distributed；
By stepThe graphene dispersing solution of middle filtration gained is centrifuged, dried, obtains nano-graphene material.
Embodiment 5
Weigh 10g potassium ferrate, be dissolved in 1L deionized water, then weigh 50g graphite powder, it is the most tentatively mixed with potassium ferrate solution, obtain graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out for the first time mechanical stripping, rotating speed is 1000rpm, and milling time is 4h；Obtain the graphene suspension that grain size is bigger；
By stepThe middle graphene suspension prepared through for the first time mechanical stripping is sent directly in high-shear emulsifying device by pipeline, mechanical stripping dispersion 0.5h under shearing force is 5000ips, obtain smaller, disperse the graphene dispersing solution that is more uniformly distributed；
By stepThe middle graphene dispersion being mixed to prepare through second time mechanical stripping is sent directly in high pressure homogenizer by pipeline, material is carried out pressurization mixing, after reaching 50MPa, material is clashed with higher speed ejection by the nozzle of high pressure homogenizer, it is achieved third time peels off mixing；
By stepThe dispersion liquid prepared carries out filtration treatment, remove larger-size Graphene granule in dispersion liquid so as to get product cut size be more uniformly distributed；
By stepThe graphene dispersing solution of middle filtration gained is centrifuged, dried, obtains nano-graphene material.
Embodiment 6
Weigh 10g potassium ferrate, be dissolved in 1L deionized water, then weigh 50g graphite powder, it is the most tentatively mixed with potassium ferrate solution, obtain graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out for the first time mechanical stripping, rotating speed is 1000rpm, and milling time is 3h；Obtain the graphene suspension that grain size is bigger；
By stepThe middle graphene suspension prepared through for the first time mechanical stripping is sent directly in high-shear emulsifying device by pipeline, mechanical stripping dispersion 1.5h under shearing force is 5000ips, obtain smaller, disperse the graphene dispersing solution that is more uniformly distributed；
By stepThe middle graphene dispersion being mixed to prepare through second time mechanical stripping is sent directly in high pressure homogenizer by pipeline, material is carried out pressurization mixing, after reaching 50MPa, material is clashed with higher speed ejection by the nozzle of high pressure homogenizer, it is achieved third time peels off mixing；
By stepThe dispersion liquid prepared carries out filtration treatment, remove larger-size Graphene granule in dispersion liquid so as to get product cut size be more uniformly distributed；
By stepThe graphene dispersing solution of middle filtration gained is centrifuged, dried, obtains nano-graphene material.
Embodiment 7
Weigh 10g potassium ferrate, be dissolved in 1L deionized water, then weigh 50g graphite powder, it is the most tentatively mixed with potassium ferrate solution, obtain graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out for the first time mechanical stripping, rotating speed is 1000rpm, and milling time is 4h；Obtain the graphene suspension that grain size is bigger；
By stepThe middle graphene suspension prepared through for the first time mechanical stripping is sent directly in high-shear emulsifying device by pipeline, mechanical stripping dispersion 1.5h under shearing force is 5000ips, obtain smaller, disperse the graphene dispersing solution that is more uniformly distributed；
By stepThe middle graphene dispersion being mixed to prepare through second time mechanical stripping is sent directly in high pressure homogenizer by pipeline, material is carried out pressurization mixing, after reaching 80MPa, material is clashed with higher speed ejection by the nozzle of high pressure homogenizer, it is achieved third time peels off mixing；
By stepThe dispersion liquid prepared carries out filtration treatment, remove larger-size Graphene granule in dispersion liquid so as to get product cut size be more uniformly distributed；
By stepThe graphene dispersing solution of middle filtration gained is centrifuged, dried, obtains nano-graphene material.
Claims (7)
1. one kind utilizes the method that nano-graphene material is prepared in aquashear scale, it is characterised in that connected by the mechanical stripping equipment of difference in functionality, by fluid power, graphite is carried out lift-off processing step by step and obtains nano-graphene material, and concrete grammar is as follows:
(1) being dissolved in solvent by oxidant, then will form graphite powder mixed liquor in graphite dispersion to solution, the concentration of graphite mixed liquor is 10-100g/L；
(2) it is sent to the graphite powder mixed liquor that step (1) prepares in grinding distribution machine carry out grinding for the first time, obtains the graphene suspension of certain size；
(3) graphene suspension obtained in step (2) is continued to be fed into high-shear emulsifying device carries out second time mechanical shearing and mixing, obtain that particle diameter is less, the more preferable graphene dispersing solution of dispersibility；
(4) graphene dispersing solution obtained in step (3) is continued to be fed in high pressure homogenizer, utilize high pressure homogenizer that graphene dispersing solution is mixed again, then there is mutually collision by the ejection of high pressure homogenize machine nozzle in material, realize third time mechanical stripping, obtain the graphene dispersing solution of size uniform；
(5) carry out the graphene dispersing solution obtained in step (4) filtering, be centrifuged, be dried, obtain nano-graphene material.
A kind of method utilizing aquashear scale to prepare nano-graphene material, it is characterised in that described graphite raw material chooses the one in natural flake graphite, graphite powder, expanded graphite, highly oriented graphite, agraphitic carbon.
A kind of method utilizing aquashear scale to prepare nano-graphene material; it is characterized in that; described oxidant is one or more the mixture in Ammonium persulfate., potassium dichromate, chromic acid, potassium permanganate, potassium ferrate, concentrated sulphuric acid, concentrated hydrochloric acid, concentrated nitric acid, perchloric acid, strong phosphoric acid or glacial acetic acid, and graphite and oxidizer mass ratio are 1:0.1-0.3.
A kind of method utilizing aquashear scale to prepare nano-graphene material, it is characterized in that, described solvent is selected from butyl acetate, benzyl oxide, diethyl carbonate, DBE, ethyl carbitol acetate, Ethyl methyl carbonate, butyl carbitol acetate, butyl cellosolve acetate, Allyl carbonate, ethanolamine, DMSO, dimethyl succinate, N-dodecylpyrrolidone, propylene glycol methyl ether acetate, NMP, ethyl phthalate, dimethylbenzene, pyridine, dibutyl phthalate, benzaldehyde, dimethyl carbonate, NOP, the combination of any one or more in diphenyl carbonate and deionized water.
A kind of method utilizing aquashear scale to prepare nano-graphene material, it is characterised in that the rotating speed of described mechanical lapping is 100-1500rpm, splitting time is 1-5h.
A kind of method utilizing aquashear scale to prepare nano-graphene material, it is characterised in that the shearing force of described high-shear emulsifying is 1000-5000ips, emulsification times is 0.5-3h.
A kind of method utilizing aquashear scale to prepare nano-graphene material, it is characterised in that the described operating pressure higher than homogenizer is 10-80MPa.
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