CN104118872A - Method and device for purifying oxidized graphene/graphene solution - Google Patents
Method and device for purifying oxidized graphene/graphene solution Download PDFInfo
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- CN104118872A CN104118872A CN201410377639.1A CN201410377639A CN104118872A CN 104118872 A CN104118872 A CN 104118872A CN 201410377639 A CN201410377639 A CN 201410377639A CN 104118872 A CN104118872 A CN 104118872A
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Abstract
The invention discloses a method and a device for purifying an oxidized graphene/graphene solution. The method comprises the following steps: pumping the oxidized graphene/graphene solution to be purified into a channel consisting of at least one filtering and discharging pipe, arranging the at least one filtering and discharging pipe between at least one group of negative and positive electrodes of an electrolytic tank, and forming auxiliary liquid channels between the negative and positive electrodes and the at least one filtering and discharging pipe; performing electrode migration on ions and charged particles in the oxidized graphene/graphene solution to be purified under the action of an electrical field between the negative and positive electrodes, filtering impurities out of the filtering and discharging pipes, taking away the impurities by auxiliary liquid, and pumping the residual purified oxidized graphene/graphene solution into another water tank from the at least one filtering and discharging pipe to form filtering circulation. According to the method and the device, the process is simple, the cost is low, the speed that the impurities are filtered out of the at least one filtering and discharging pipe can be increased, efficient purification of the oxidized graphene/graphene solution is realized, and the method is very suitable for industrial production.
Description
Technical field
The present invention relates to a kind of method of purification and device of graphene oxide/graphene solution, specifically a kind of method of purification and device of the graphene oxide/graphene solution based under electrolysis and filtration dual function.
Background technology
Graphene (Graphene) is that a kind of by the tightly packed Two-dimensional Carbon atomic crystal forming of monolayer carbon atom, its thickness is about 0.335nm, and wherein C-C passes through SP
2hydridization forms, and bond distance is about 0.142nm, and in Graphene plane, each carbon atom is connected with σ key with three adjacent carbon atoms, makes whole lamella have high structural strength.Meanwhile, each carbon atom has a not π-electron of Cheng Jian, therefore can form π track in vertical direction.Due to the existence of π track, make the electronics can free movement in Graphene crystal, make Graphene there is excellent electronic transmission performance, the electronic mobility on room temperature lower plane is 15000 cm
2v
-1s
-1, the resistivity corresponding with this numerical value is 10
-6Ω cm, is slightly smaller than silver-colored resistivity 1.59 * 10
-6Ω cm, so Graphene has excellent electroconductibility.Meanwhile, the specific surface area (2630m of Graphene
2/ g) very large, tensile modulus (1.01TPa) is suitable with single-walled nanotube with ultimate strength (116GPa).Compare with carbon nanotube with expensive soccerballene, Graphene is cheap, and raw material is easy to get, and is expected to the final application in fields such as electronic material, matrix material, medicine, aerospace.
Graphene since being found for 2004, and its main preparation method has: tape stripping method (or micromechanics stripping method), silicon carbide (SiC) epitaxial growth method, chemical vapour deposition (CVD) method and chemical stripping method.Wherein, first three plants big area and mass-producing preparation that preparation method is difficult to realize Graphene, and preparation cost is high.Chemical stripping method is current most widely used a kind of synthetic method.At present, the Graphene size obtaining based on micromechanics stripping method is wayward, is only suitable for pursuing fundamental studies; And all cannot obtain uniform big area Graphene by epitaxial growth method and chemical Vapor deposition process, low preparation efficiency and high preparation cost have also limited the application of these two kinds of methods simultaneously.The graphene oxide preparing by these ways, Graphene contain a large amount of foreign ions, conventionally adopt filtration, electrolysis and the method purifying such as centrifugal, and process is complicated.Take wherein low, the consuming time length of single method of purification efficiency, yield poorly, cannot go on industrialization road.
CN 102626591 A disclose a kind of purification process and device of graphene oxide/graphene solution, the method is by graphene oxide to be purified/graphene solution input dialysis chamber, dialysis chamber is placed between anodic-cathodic, in the middle of dialysis chamber, it is graphene oxide/graphene solution passage, between dialysis chamber and anodic-cathodic, be provided with solvent streams passage, graphene oxide/graphene solution to be purified enters from one end of dialysis chamber, be subject to the electric field action between anodic-cathodic, ion in graphene oxide/graphene solution to be purified and charged particle see through respectively dialysis chamber wall to the electrode migration of oppositely charged, and taken away by solvent streams, graphene oxide/the graphene solution of residue purifying flows out from dialysis chamber.Yet the purifying that carries out graphene oxide/graphene solution under the effect of electrolysis and dialysis can cause length consuming time, efficiency is low, and comprehensive cost is high, troublesome poeration.
Summary of the invention
The object of the invention is to overcome the above-mentioned deficiency of prior art and method of purification and the device of a kind of high-level efficiency, low cost, short, the simple graphene oxide/graphene solution of technique consuming time are provided.
Technical scheme of the present invention is:
The method of purification of graphene oxide/graphene solution of the present invention, graphene oxide/graphene solution to be purified is pumped in the passage of at least one filtration comb, by filtering comb, be placed between at least one group of anodic-cathodic of electrolyzer, between anodic-cathodic and filtration comb, be provided with auxiliary liquid passage; Be subject to the electric field action between anodic-cathodic, ion in graphene oxide/graphene solution to be purified and charged particle carry out electrode migration, impurity is leached and filtered outside comb, by auxiliary liquid, taken away, graphene oxide/graphene solution after residue is purified is pumped into another tank from filtering comb, forms filtration cycle.
Further, the aperture of described filtration comb is 1.0 ~ 5.0 μ m, filters the aperture of comb and also can adjust according to the size of graphene film.
Further, the aqueous solution that the concentration of described graphene oxide/graphene solution is 0.5% ~ 18%.
Further, the flow velocity of described graphene oxide/graphene solution passage is 10 ~ 250cm/s.
Further, anodic-cathodic and the auxiliary liquid filtering between comb are water or other solvent, without particular requirement; Impurity leaches and filters outside comb, when impurity concentration outside pipe is higher, needs to change auxiliary liquid.
The purifying plant of graphene oxide/graphene solution of the present invention, for electrolysis and filtration, comprise at least one group of anodic-cathodic of being located in electrolyzer and filter comb, described anodic-cathodic is located at respectively the both sides of filtering comb, the inner chamber that filters comb is graphene oxide/graphene solution passage, filters between comb and anodic-cathodic and is provided with and assists liquid passage.
Further, described filtration comb is connected in series water pump, valve and tank successively; Described anodic-cathodic is electrically connected to rectifier.
Further, described filtration comb has one at least, and described anodic-cathodic is arranged at respectively every both sides of filtering comb.
Further, the surface of described filtration comb is provided with some apertures, and the aperture of described aperture is 1.0 ~ 5.0 μ m.
Further, the voltage of described rectifier is 0.1 ~ 36V.
Further, described anodic-cathodic is comprised of titanium plate and graphite cake, can be also other electro-conductive material.
Principle of work of the present invention is: utilize the principle of foreign ion/charged particle in charged anodic-cathodic surface adsorption solution, foreign ion in solution/charged particle is reunited on anodic-cathodic surface, thereby realize the purifying of graphene oxide/graphene solution.Be specially: when the graphene oxide/graphene solution of not purifying is mobile in filtering comb, be subject to the impact of electric field action between anodic-cathodic, foreign ion/charged particle in the graphene oxide/graphene solution of not purifying is subject to the effect of electronic migration, concentration reduces greatly, by filtering comb, contaminant filter is gone out outside pipe, obtain the graphene oxide/graphene solution of purifying; By controlling the concentration of graphene oxide/graphene solution and the aperture of filtering comb, the content of conducting particles in capable of regulating final product.
The present invention compared with prior art has following features:
(1) the filtration comb that graphene oxide/graphene solution is housed is placed in to electric field, by electric field, accelerate ion in solution toward the migration of anode and cathode, regulating YIN and YANG electrode and the quantity of filtering comb as requested, thus the speed that comb leaches impurity of filtering improved;
(2) by controlling the concentration of graphene oxide/graphene solution and the aperture of filtering comb, the content of conducting particles in capable of regulating final product, realizes the high-level efficiency of graphene oxide/graphene solution and purifies; Wherein, the aperture of filtering comb is 1.0 ~ 5.0 μ m, and compared with the prior art, efficiency improves 2 ~ 5 times; The concentration of graphene oxide/graphene solution is 0.5% ~ 18% the aqueous solution, and compared with the prior art, purity improves 2 ~ 3 times;
(3) without the flow velocity of controlling auxiliary liquid in electrolyzer, easy and simple to handle, and cost is low, and refining effect is good, is highly suitable for industrial production.
Accompanying drawing explanation
Fig. 1 is the structural representation of graphene oxide/graphene solution purifying plant of the present invention;
Fig. 2 is the structural representation of the purification process of graphene oxide/graphene solution of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, detailed structure of the present invention is further described.
Embodiment 1
As shown in Figure 1: a kind of purifying plant of graphene oxide/graphene solution, for the graphene oxide/graphene solution of not purifying is carried out to electrolysis and filtration, comprise one group of anodic-cathodic and the filtration comb 6 be located in electrolyzer 4, anodic-cathodic is located at respectively the both sides of filtering comb 6, the inner chamber that filters comb 6 is graphene oxide/graphene solution passage, filters between comb 6 and anodic-cathodic and is provided with and assists liquid passage.
Filter comb 6 and be connected in series successively water pump 1, valve 2 and tank 3, water pump 1 is for the graphene oxide/graphene solution of not purifying is inputed in the bore passages of filtering comb 6 from filtering one end of comb 6, and the graphene oxide/graphene solution after purifying is drawn to tank 3 from filtering the other end of comb 6; Water pump 1 carries out opening and closing under the effect of valve 2; Anodic-cathodic is electrically connected to rectifier 7, and rectifier 7 is used to and provides constant operating voltage, the scope of voltage between anodic-cathodic is 0.1 ~ 36V.
In the present embodiment, water pump 1 is anticorrosion water pump; Negative electrode 8 is titanium plate, and anode 5 is graphite cake; The surface of filtering comb 6 is provided with the aperture that some apertures are 1.0 μ m, for controlling the content of final product conducting particles.
Embodiment 2
As shown in Figure 2: a kind of method of purification of graphene oxide/graphene solution, graphene oxide/the graphene solution to be purified that is 10mg/mL by concentration pumps into respectively in the passage of three filtration combs 6, by three, filter comb 6 and be placed between one group of anodic-cathodic in electrolyzer 4, between anodic-cathodic and filtration comb 6 and between every adjacent two filtration combs 6, be provided with aqueous solution channel; Voltage between anodic-cathodic is 3.5V; Be subject to the electric field action between anodic-cathodic, foreign ion/charged particle in graphene oxide/graphene solution to be purified carries out electrode migration, impurity is leached and filtered outside comb 6, by the aqueous solution, taken away, graphene oxide/graphene solution after residue is purified is pumped into another tank from filtering comb 6, forms filtration cycle.
In the present embodiment, the flow velocity of graphene oxide/graphene solution passage is 10cm/s, the speed that filtration comb 6 leaches impurity is 0.5cm/s, and by controlling the concentration of graphene oxide/graphene solution, be that 10mg/mL and the aperture of filtering comb 6 are 5.0 μ m, the content that obtains conducting particles in final product is 0.3ppm.
Embodiment 3
A kind of method of purification of graphene oxide/graphene solution, graphene oxide/the graphene solution to be purified that is 2mg/mL by concentration pumps into respectively in the passage of three filtration combs, in electrolyzer, be provided with three groups of anodic-cathodics, three groups of anodic-cathodics are arranged at respectively every both sides of filtering comb, between anodic-cathodic and filtration comb, are provided with aqueous solution channel; Voltage between every group of anodic-cathodic is 10V; Be subject to the electric field action between anodic-cathodic, foreign ion/charged particle in graphene oxide/graphene solution to be purified carries out electrode migration, by filtration comb, the electrode to oppositely charged moves charged foreign ion respectively, charged foreign ion is gathered in anodic-cathodic surface, impurity is leached and filtered outside comb, concentration impurity ion in strainer tube is reduced greatly, by the aqueous solution, taken away, graphene oxide/graphene solution after residue is purified is pumped into another tank from filtering comb, forms filtration cycle.
In the present embodiment, the flow velocity of graphene oxide/graphene solution passage is 250cm/s, the speed that filtration comb leaches impurity is 10cm/s, and by controlling the concentration of graphene oxide/graphene solution, be that 2mg/mL and the aperture of filtering comb are 1.0 μ m, the content that obtains conducting particles in final product is 0.1ppm.
These are only the preferred embodiments of the present invention, be not limited to the present invention, obviously, those skilled in the art can carry out various changes, modification and not depart from the spirit and scope of the present invention the present invention.If of the present invention these are revised and within modification belongs to the scope of the claims in the present invention and equivalent technologies thereof, are all belonged to protection scope of the present invention.
Claims (10)
1. the method for purification of a graphene oxide/graphene solution, it is characterized in that: graphene oxide/graphene solution to be purified is pumped in the passage of at least one filtration comb, by filtering comb, be placed between at least one group of anodic-cathodic of electrolyzer, between anodic-cathodic and filtration comb, be provided with auxiliary liquid passage; Be subject to the electric field action between anodic-cathodic, ion in graphene oxide/graphene solution to be purified and charged particle carry out electrode migration, impurity is leached and filtered outside comb, by auxiliary liquid, taken away, graphene oxide/graphene solution after residue is purified is pumped into another tank from filtering comb, forms filtration cycle.
2. the method for purification of graphene oxide/graphene solution according to claim 1, is characterized in that: the aperture of described filtration comb is 1.0 ~ 5.0 μ m.
3. according to the method for purification of graphene oxide/graphene solution described in claim 1 or 2, it is characterized in that: the aqueous solution that the concentration of described graphene oxide/graphene solution is 0.5% ~ 18%.
4. according to the method for purification of graphene oxide/graphene solution described in claim 1 or 2, it is characterized in that: the flow velocity of described graphene oxide/graphene solution passage is 10 ~ 250cm/s.
5. the purifying plant of graphene oxide/graphene solution according to claim 1, for electrolysis and filtration, it is characterized in that: comprise at least one group of anodic-cathodic of being located in electrolyzer and filter comb, described anodic-cathodic is located at respectively the both sides of filtering comb, the inner chamber that filters comb is graphene oxide/graphene solution passage, filters between comb and anodic-cathodic and is provided with solvent streams passage.
6. the purifying plant of graphene oxide/graphene solution according to claim 5, is characterized in that: described filtration comb is connected in series water pump, valve and tank successively; Described anodic-cathodic is electrically connected to rectifier.
7. the purifying plant of graphene oxide/graphene solution according to claim 6, is characterized in that: described filtration comb has one at least, and described anodic-cathodic is arranged at respectively every both sides of filtering comb.
8. according to the purifying plant of graphene oxide/graphene solution described in claim 5 ~ 7 any one, it is characterized in that: the surface of described filtration comb is provided with some apertures, the aperture of described aperture is 1.0 ~ 5.0 μ m.
9. according to the purifying plant of graphene oxide/graphene solution described in claim 5 ~ 7 any one, it is characterized in that: the voltage of described rectifier is 0.1 ~ 36V.
10. according to the purifying plant of graphene oxide/graphene solution described in claim 5 ~ 7 any one, it is characterized in that: described anodic-cathodic is comprised of titanium plate and graphite cake.
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| CN107631972A (en) * | 2017-08-03 | 2018-01-26 | 同济大学 | The experimental system that a kind of graphene particles are permeated in GCL |
| CN108910871A (en) * | 2018-08-02 | 2018-11-30 | 无锡泰科纳米新材料有限公司 | A kind of purifying plant and method of the liquid containing graphene |
| CN109485039A (en) * | 2018-11-19 | 2019-03-19 | 大同新成新材料股份有限公司 | A kind of purification devices and its method of graphene oxide |
| CN109721051A (en) * | 2019-02-28 | 2019-05-07 | 武淑敏 | A kind of graphene solution clarification equipment |
| CN111204758A (en) * | 2020-01-21 | 2020-05-29 | 王佳友 | Single crystal graphite material preparation purification equipment |
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| CN109485039A (en) * | 2018-11-19 | 2019-03-19 | 大同新成新材料股份有限公司 | A kind of purification devices and its method of graphene oxide |
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| CN111204758A (en) * | 2020-01-21 | 2020-05-29 | 王佳友 | Single crystal graphite material preparation purification equipment |
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| CN104118872B (en) | 2017-03-22 |
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