CN105819438B - A kind of method using aquashear prepare with scale nano-graphene material - Google Patents
A kind of method using aquashear prepare with scale nano-graphene material Download PDFInfo
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- CN105819438B CN105819438B CN201610295055.9A CN201610295055A CN105819438B CN 105819438 B CN105819438 B CN 105819438B CN 201610295055 A CN201610295055 A CN 201610295055A CN 105819438 B CN105819438 B CN 105819438B
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention proposes a kind of method using aquashear prepare with scale nano-graphene material; graphite powder is added in liquid; add a small amount of oxidant; pass through multi-functional grinding distribution machine, high-shear emulsifying device, the high pressure homogenizer of series connection; oxidizer molecule quickly interts and enters inside graphite; material is peeled off in fluid power effect down cut using continuous mechanical force, make its fast hierarchical.Both solved and be difficult to extensive, high quality, low cost at present and prepare graphene, it in turn ensure that graphene-structured is injury-free, obtained graphene 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.
Description
Technical field
The present invention relates to technical field of nano material, relates generally to one kind and utilizes aquashear prepare with scale nano-graphite
The method of alkene material.
Background technology
Since grapheme material in 2004 is found, researcher has carried out it to further investigate for a long time, and from
The hexagonal structure that graphene is made of SP2 hybridized orbits is drawn in research, since the presence of SP2 hybridized orbits causes stone
Black alkene has good electric conductivity, can be applied as good conductor in opto-electronic device and electrochemical energy source domain.With
Deeply, the optical property of graphene, mechanical property, catalytic performance etc. are found in succession for research so that its electromagnetic shielding material,
The fields such as microwave absorbing material, gas sensor, catalyst are also widely used.
Graphene possesses excellent performance and is widely applied prospect, but the technology of preparing of graphene is not yet ripe, product
It is of low quality, performance is unstable and can not mass produce and all limits its extensive use in every field.Prepare at present
The preparation species of graphene is various, mainly there is two major class of physical method and chemical method, but more or less there are it is corresponding the problem of,
Lead to not the needs for meeting industrial mass production.Graphene prepared by physical method is mainly based on mechanical stripping, but produce
Moral character can be unstable, and Size Distribution can not be controlled accurately, and graphene size is to influence a key factor of its performance.
Advantage is that energy consumption is small, and pollution is small, and safety can large-scale continuous production.Chemical method prepare graphene mainly have catalytic decomposition and
The methods of organic synthesis, in addition can also notify graphite to carry out preparing grapheme through oxidation reduction.Graphene prepared by chemical method
It is controllable with size, steady performance, but energy consumption is larger in chemical method preparation process, unsuitable large-scale continuous production,
And there is higher danger compared with physical method.And a large amount of inorganic matters and soda acid can be used in preparation process, cause technique
Subsequent treatment is complex, also adds production cost indirectly；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, it is logical
Cross after graphene, binding agent, solvent and other auxiliary additives tentatively mixing, mixed liquor is carried out using high-shear emulsifying device
Mechanical mixture.The preferable graphene dispersing solution of dispersiveness can obtain by this method, and jitter time can be shortened.
Chinese invention patent application number 201510073825.0 discloses the class mechanical stripping of a kind of tonne of production graphene
Device and its production method, it is made of level-one or multi-stage mechanical peel-off device its mechanical stripping separator, passes through
Mutual collision between rotor and graphite, between graphite particle is peeled off, and realizes multistage continuous processing, can on a large scale, persistently
Property prepares graphene and its dispersion liquid.
Chinese invention patent application number 201511007072.X discloses a kind of method that graphene is prepared using lignin,
It is pre-processed by using acid-base pair lignin, is then mixed by high pressure homogenizer, homogeneous, and under the action of catalyst
Decompose, then graphene is prepared into pyrolytic is crossed.
Chinese invention patent application number 201010179119.1 discloses high-efficiency and low-cost mechanical stripping and prepares graphene
Or the method for graphene oxide, then it passes through machinery by the way that graphite is mixed in a solvent with other larger particles
Stripping prepares graphene.The charge stripping efficiency of graphite can be improved by this method, and can realize large-scale production.
From above-mentioned analysis it can be found that the method for preparing graphene using mechanical stripping at present is more, but these method bases
Originally it is all based on what a kind of mechanical stripping method carried out, obtained graphene is with quality is unstable, size is uneven, Wu Fa great
Some problems such as scale continuous production.The present invention is by the way that grinding distribution agent, high-shear emulsion machine, high pressure homogenizer are connected, stone
Black mixed liquor, which passes sequentially through three kinds of mechanical stripping devices, to be continued to peel off mixing repeatedly, be made be uniformly dispersed, size uniformity
Graphite.Both it ensure that shearing is peeled off, by ensure that graphene-structured is injury-free, obtained graphene can be widely applied to lithium
The fields such as battery, ultracapacitor, polymer composite, heat conduction and heat radiation film, functional paint, defence and military.
The content of the invention
For at present using mechanical stripping equipment can not prepare size uniform, be uniformly dispersed, stable quality graphene is asked
Topic, the present invention proposes to carry out stripping mixing to graphene using connect a variety of mechanical stripping equipments and mixing apparatus, to solve to work as
Before prepare graphene process problem encountered.Carry out lift-off processing step by step to graphite especially by fluid power and obtain nano-graphite
Alkene material, concrete technical scheme are as follows：
（1）Oxidant is dissolved in solvent, graphite dispersion is then formed into graphite powder mixed liquor into solution, graphite mixes
The concentration for closing liquid is 10-100g/L；
（2）By step（1）Obtained graphite powder mixed liquor is sent to progress first time grinding in grinding distribution machine, obtains one
The graphene suspension being sized；
（3）By step（2）In obtained graphene suspension continue to be fed into high-shear emulsifying device and carry out second of machinery
Shearing and mixing, obtain particle diameter smaller, the more preferable graphene dispersing solution of dispersiveness；
（4）By step（3）In obtained graphene dispersing solution continue to be fed into high pressure homogenizer, utilize high pressure homogenizer pair
Graphene dispersing solution mixes again, and then material is sprayed by high-pressure homogeneous machine nozzle occurs mutually collision, realizes third time machine
Tool is peeled off, and obtains the graphene dispersing solution of size uniform；
（5）By step（4）In obtained graphene dispersing solution filtered, centrifuged, is dry, obtain nano-graphene material
Material.
Preferably, the graphite raw material chooses natural flake graphite, graphite powder, expanded graphite, highly oriented graphite, unformed
One kind in carbon.
Preferably, the oxidant is ammonium persulfate, potassium bichromate, chromium trioxide, potassium permanganate, potassium ferrate, dense sulphur
Mixture more than one or both of acid, concentrated hydrochloric acid, concentrated nitric acid, perchloric acid, concentrated phosphoric acid or glacial acetic acid, graphite and oxidant
Dosage mass ratio is 1:0.1-0.3.
Preferably, the solvent is selected from butyl acetate, benzyl oxide, diethyl carbonate, DBE, ethyl carbitol acetate, carbonic acid
Methyl ethyl ester, butyl carbitol acetate, butyl cellosolve acetate, propene carbonate, monoethanolamine, DMSO, dimethyl succinate,
N- dodecyl pyrrolidones, propylene glycol methyl ether acetate, NMP, ethyl phthalate, dimethylbenzene, pyridine, phthalic acid two
Any of butyl ester, benzaldehyde, dimethyl carbonate, N- octylpyrrolidones, diphenyl carbonate and deionized water or two kinds
Combination above.
Preferably, the rotating speed of the mechanical lapping is 100-1500rpm, splitting time 1-5h.
Preferably, the shearing force of the high-shear emulsifying is 1000-5000ips, emulsification times 0.5-3h.
Preferably, the operating pressure higher than homogenizer is 10-80MPa.
It is proposed by the present invention that nanometer is prepared using multistage aquashear compared with the technology of existing preparation graphene microchip
Grapheme material has the advantage that：
It is 1. mixed present invention firstly provides carrying out repeatedly peeling off to graphene using a variety of aquashear equipment tandem compounds
Conjunction processing prepares nano-graphene material；
2. to be combined since present invention employs grinding distribution machine, high-shear emulsion machine, high pressure homogenizer, realize
The mixing of stripping step by step of graphene, obtained graphene size are more uniformly distributed, and oxidant progress is added due to during
Show to handle, graphene is less likely to occur to reunite；
3. since three devices of the present invention are in series, it is possible to achieve large-scale continuous production, and it is safe and pollution-free.
Brief description of the drawings
For further illustrate a kind of method using aquashear prepare with scale nano-graphene material, by attached drawing into
Row explanation.
A kind of flow chart using aquashear prepare with scale nano-graphene material of attached drawing 1.
Specific embodiment：
By embodiment, the present invention is described in further detail, but this should not be interpreted as to the model of the present invention
Enclose and be only limitted to following example.Without departing from the idea of the above method of the present invention, according to ordinary skill knowledge
The various replacements or change made with customary means, should be included in the scope of the present invention.
Embodiment 1
5g potassium ferrates are weighed, are dissolved in 1L deionized waters, then weigh 50g graphite powders, by itself and high ferro
Sour potassium solution is tentatively mixed under magnetic stirring, obtains graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out first time mechanical stripping, rotating speed is
500rpm, milling time 2h；Obtain the larger graphene suspension of grain size；
By stepGraphene suspension made from middle process first time mechanical stripping is sent directly into height by pipeline and cuts
Cut in emulsifier, in the case where shearing force is 2000ips, mechanical stripping disperses 0.5h, obtains smaller, the scattered stone being more uniformly distributed
Black alkene dispersion liquid；
By stepThe middle graphene dispersion being mixed to prepare by second of mechanical stripping is sent directly into height by pipeline
Press in homogenizer, pressurization mixing is carried out to material, after 50MPa is reached, material is by the nozzle of high pressure homogenizer with higher
Speed sprays head-on collision, realizes that third time peels off mixing；
By stepObtained dispersion liquid carries out filtration treatment, removes larger-size graphene particles in dispersion liquid,
The product cut size made is more uniformly distributed；
By stepGraphene dispersing solution obtained by middle filtering is centrifuged, drying process, obtains nano-graphene material
Material.
Embodiment 2
10g potassium ferrates are weighed, are dissolved in 1L deionized waters, then weigh 50g graphite powders, by itself and high ferro
Sour potassium solution is tentatively mixed under magnetic stirring, obtains graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out first time mechanical stripping, rotating speed is
500rpm, milling time 2h；Obtain the larger graphene suspension of grain size；
By stepGraphene suspension made from middle process first time mechanical stripping is sent directly into height by pipeline and cuts
Cut in emulsifier, in the case where shearing force is 2000ips, mechanical stripping disperses 0.5h, obtains smaller, the scattered stone being more uniformly distributed
Black alkene dispersion liquid；
By stepThe middle graphene dispersion being mixed to prepare by second of mechanical stripping is sent directly into height by pipeline
Press in homogenizer, pressurization mixing is carried out to material, after 50MPa is reached, material is by the nozzle of high pressure homogenizer with higher
Speed sprays head-on collision, realizes that third time peels off mixing；
By stepObtained dispersion liquid carries out filtration treatment, removes larger-size graphene particles in dispersion liquid,
The product cut size made is more uniformly distributed；
By stepGraphene dispersing solution obtained by middle filtering is centrifuged, drying process, obtains nano-graphene material
Material.
Embodiment 3
10g potassium ferrates are weighed, are dissolved in 1L deionized waters, then weigh 50g graphite powders, by itself and high ferro
Sour potassium solution is tentatively mixed under magnetic stirring, obtains graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out first time mechanical stripping, rotating speed is
1000rpm, milling time 2h；Obtain the larger graphene suspension of grain size；
By stepGraphene suspension made from middle process first time mechanical stripping is sent directly into height by pipeline and cuts
Cut in emulsifier, in the case where shearing force is 2000ips, mechanical stripping disperses 0.5h, obtains smaller, the scattered stone being more uniformly distributed
Black alkene dispersion liquid；
By stepThe middle graphene dispersion being mixed to prepare by second of mechanical stripping is sent directly into height by pipeline
Press in homogenizer, pressurization mixing is carried out to material, after 50MPa is reached, material is by the nozzle of high pressure homogenizer with higher
Speed sprays head-on collision, realizes that third time peels off mixing；
By stepObtained dispersion liquid carries out filtration treatment, removes larger-size graphene particles in dispersion liquid,
The product cut size made is more uniformly distributed；
By stepGraphene dispersing solution obtained by middle filtering is centrifuged, drying process, obtains nano-graphene material
Material.
Embodiment 4
10g potassium ferrates are weighed, are dissolved in 1L deionized waters, then weigh 50g graphite powders, by itself and high ferro
Sour potassium solution is tentatively mixed under magnetic stirring, obtains graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out first time mechanical stripping, rotating speed is
1000rpm, milling time 4h；Obtain the larger graphene suspension of grain size；
By stepGraphene suspension made from middle process first time mechanical stripping is sent directly into height by pipeline and cuts
Cut in emulsifier, in the case where shearing force is 2000ips, mechanical stripping disperses 0.5h, obtains smaller, the scattered stone being more uniformly distributed
Black alkene dispersion liquid；
By stepThe middle graphene dispersion being mixed to prepare by second of mechanical stripping is sent directly into height by pipeline
Press in homogenizer, pressurization mixing is carried out to material, after 50MPa is reached, material is by the nozzle of high pressure homogenizer with higher
Speed sprays head-on collision, realizes that third time peels off mixing；
By stepObtained dispersion liquid carries out filtration treatment, removes larger-size graphene particles in dispersion liquid,
The product cut size made is more uniformly distributed；
By stepGraphene dispersing solution obtained by middle filtering is centrifuged, drying process, obtains nano-graphene material
Material.
Embodiment 5
10g potassium ferrates are weighed, are dissolved in 1L deionized waters, then weigh 50g graphite powders, by itself and high ferro
Sour potassium solution is tentatively mixed under magnetic stirring, obtains graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out first time mechanical stripping, rotating speed is
1000rpm, milling time 4h；Obtain the larger graphene suspension of grain size；
By stepGraphene suspension made from middle process first time mechanical stripping is sent directly into height by pipeline and cuts
Cut in emulsifier, in the case where shearing force is 5000ips, mechanical stripping disperses 0.5h, obtains smaller, the scattered stone being more uniformly distributed
Black alkene dispersion liquid；
By stepThe middle graphene dispersion being mixed to prepare by second of mechanical stripping is sent directly into height by pipeline
Press in homogenizer, pressurization mixing is carried out to material, after 50MPa is reached, material is by the nozzle of high pressure homogenizer with higher
Speed sprays head-on collision, realizes that third time peels off mixing；
By stepObtained dispersion liquid carries out filtration treatment, removes larger-size graphene particles in dispersion liquid,
The product cut size made is more uniformly distributed；
By stepGraphene dispersing solution obtained by middle filtering is centrifuged, drying process, obtains nano-graphene material
Material.
Embodiment 6
10g potassium ferrates are weighed, are dissolved in 1L deionized waters, then weigh 50g graphite powders, by itself and high ferro
Sour potassium solution is tentatively mixed under magnetic stirring, obtains graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out first time mechanical stripping, rotating speed is
1000rpm, milling time 3h；Obtain the larger graphene suspension of grain size；
By stepGraphene suspension made from middle process first time mechanical stripping is sent directly into height by pipeline and cuts
Cut in emulsifier, in the case where shearing force is 5000ips, mechanical stripping disperses 1.5h, obtains smaller, the scattered stone being more uniformly distributed
Black alkene dispersion liquid；
By stepThe middle graphene dispersion being mixed to prepare by second of mechanical stripping is sent directly into height by pipeline
Press in homogenizer, pressurization mixing is carried out to material, after 50MPa is reached, material is by the nozzle of high pressure homogenizer with higher
Speed sprays head-on collision, realizes that third time peels off mixing；
By stepObtained dispersion liquid carries out filtration treatment, removes larger-size graphene particles in dispersion liquid,
The product cut size made is more uniformly distributed；
By stepGraphene dispersing solution obtained by middle filtering is centrifuged, drying process, obtains nano-graphene material
Material.
Embodiment 7
10g potassium ferrates are weighed, are dissolved in 1L deionized waters, then weigh 50g graphite powders, by itself and high ferro
Sour potassium solution is tentatively mixed under magnetic stirring, obtains graphite mixed liquor；
By stepIn graphite mixed liquor be injected into grinding distribution machine and carry out first time mechanical stripping, rotating speed is
1000rpm, milling time 4h；Obtain the larger graphene suspension of grain size；
By stepGraphene suspension made from middle process first time mechanical stripping is sent directly into height by pipeline and cuts
Cut in emulsifier, in the case where shearing force is 5000ips, mechanical stripping disperses 1.5h, obtains smaller, the scattered stone being more uniformly distributed
Black alkene dispersion liquid；
By stepThe middle graphene dispersion being mixed to prepare by second of mechanical stripping is sent directly into height by pipeline
Press in homogenizer, pressurization mixing is carried out to material, after 80MPa is reached, material is by the nozzle of high pressure homogenizer with higher
Speed sprays head-on collision, realizes that third time peels off mixing；
By stepObtained dispersion liquid carries out filtration treatment, removes larger-size graphene particles in dispersion liquid,
The product cut size made is more uniformly distributed；
By stepGraphene dispersing solution obtained by middle filtering is centrifuged, drying process, obtains nano-graphene material
Material.
Claims (2)
- A kind of 1. method using aquashear prepare with scale nano-graphene material, it is characterised in that by difference in functionality Mechanical stripping equipment is connected, and is carried out lift-off processing step by step to graphite by fluid power and is obtained nano-graphene material, specific side Method is as follows：（1）Oxidant is dissolved in solvent, graphite dispersion is then formed into graphite powder mixed liquor, graphite mixed liquor into solution Concentration be 10-100g/L；The oxidant is ammonium persulfate, potassium bichromate, chromium trioxide, potassium permanganate, potassium ferrate, dense Mixture more than one or both of sulfuric acid, concentrated hydrochloric acid, concentrated nitric acid, perchloric acid, concentrated phosphoric acid or glacial acetic acid, graphite and oxidation Agent dosage mass ratio is 1:0.1-0.3；The solvent is selected from butyl acetate, benzyl oxide, diethyl carbonate, DBE, ethyl carbitol acetate, methyl ethyl carbonate, fourth Base carbitol acetate, butyl cellosolve acetate, propene carbonate, monoethanolamine, DMSO, dimethyl succinate, N- dodecanes Base pyrrolidones, propylene glycol methyl ether acetate, NMP, ethyl phthalate, dimethylbenzene, pyridine, dibutyl phthalate, rest in peace Any of fragrant aldehyde, dimethyl carbonate, n-octylpyrrolidone, diphenyl carbonate and deionized water or two or more groups Close；（2）By step（1）Obtained graphite powder mixed liquor is sent to progress first time grinding in grinding distribution machine, obtains a scale Very little graphene suspension；The rotating speed of the mechanical lapping is 100-1500rpm, splitting time 1-5h；（3）By step（2）In obtained graphene suspension continue to be fed into second of mechanical shearing carried out in high-shear emulsifying device And mixing, obtain particle diameter smaller, the more preferable graphene dispersing solution of dispersiveness；The shearing force of the high-shear emulsifying is 1000- 5000ips, emulsification times 0.5-3h；（4）By step（3）In obtained graphene dispersing solution continue to be fed into high pressure homogenizer, using high pressure homogenizer to graphite Alkene dispersion liquid mixes again, and then material is sprayed by high-pressure homogeneous machine nozzle occurs mutually collision, realizes third time machinery stripping From obtaining the graphene dispersing solution of size uniform；The operating pressure of the high pressure homogenizer is 10-80MPa；（5）By step（4）In obtained graphene dispersing solution filtered, centrifuged, is dry, obtain nano-graphene material.
- 2. a kind of method using aquashear prepare with scale nano-graphene material according to claim 1, its feature It is, the graphite raw material chooses one in natural flake graphite, graphite powder, expanded graphite, highly oriented graphite, agraphitic carbon Kind.
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| CN103521330B (en) * | 2013-10-17 | 2016-03-02 | 广州派勒机械设备有限公司 | A kind of high-pressure nano homogenizer |
| KR101682007B1 (en) * | 2013-12-26 | 2016-12-02 | 주식회사 엘지화학 | Preparation method of graphene |
| CN105540575A (en) * | 2016-01-28 | 2016-05-04 | 成都新柯力化工科技有限公司 | Method for preparing graphene by using high-pressure homogenizer delamination |
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