CN108862488B - Preparation method of graphene sponge structure electrode for CDI - Google Patents
Preparation method of graphene sponge structure electrode for CDI Download PDFInfo
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- CN108862488B CN108862488B CN201810694347.9A CN201810694347A CN108862488B CN 108862488 B CN108862488 B CN 108862488B CN 201810694347 A CN201810694347 A CN 201810694347A CN 108862488 B CN108862488 B CN 108862488B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4691—Capacitive deionisation
Abstract
The invention relates to a preparation method of a graphene sponge structure electrode for CDI, which comprises the steps of uniformly mixing carbon nanotubes and a graphene oxide solution to obtain a dispersion liquid, spraying the dispersion liquid on the surface of a support to obtain a spraying film, reducing and expanding the spraying film by adopting a lighting method to obtain a three-dimensional sponge structure, and physically stripping the three-dimensional sponge structure from the support to obtain the graphene sponge structure electrode for CDI. The invention has the beneficial effects that: the graphene and carbon nanotube composite three-dimensional system structure prepared by reduction by the illumination method effectively utilizes the p-p effect, thereby not only avoiding graphene agglomeration, but also keeping the strength of the 3D carbon electrode; the sponge structure provides a good ion transmission channel for electrons, and improves the ion diffusion efficiency; the graphene sponge structure electrode has highly stable electrical and mechanical properties and rich specific surface area, so that the graphene sponge structure electrode has specific advantages in the CDI technology; no binder is added, the adsorption and desorption performance is high, the stability is good, and the service life is long.
Description
Technical Field
The invention belongs to the field of preparation of thin film electrode materials by a capacitive deionization technology, and relates to a preparation method of a graphene sponge structure electrode for CDI.
Background
The Capacitive Deionization (CDI) technology is a stable, energy-saving and efficient desalination technology, under the action of an external electric field, ions in water flow through spacing channels between electrodes and are collected and fixed in pore channels inside a carbon material to form an electric double layer, which is a cornerstone for capacitive energy storage and a mechanism for fixing salt ions and selectively extracting the salt ions from the salt water. When ions enter the internal gap pore canal and are separated from water to reach an adsorption saturation state, the electrode can be regenerated through reverse pressurization. In the circulation process, no new chemical substance is introduced, and the CDI is embodied by a pure physical property, so that the CDI has a longer service life and lower later maintenance cost. Most of CDI electrodes in the prior art use activated carbon as a main body and are formed by coating or rolling under the action of a binder, the electrode obtained by the method has poor conductivity and complex process, and the activated carbon with micropores as the main specific surface area has low ion mobility in a solution and poor adsorption and desorption properties.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: based on the above problems, the invention provides a preparation method of a graphene sponge structure electrode for CDI.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a graphene sponge structure electrode for CDI comprises the steps of uniformly mixing carbon nanotubes and a graphene oxide solution to obtain a dispersion liquid, spraying the dispersion liquid on the surface of a support to obtain a spraying film, reducing and expanding the spraying film by adopting a lighting method to obtain a three-dimensional sponge structure, and physically stripping the three-dimensional sponge structure from the support to obtain the graphene sponge structure electrode for CDI.
Further, the graphene oxide solution is prepared by preparing graphene oxide gel from graphite powder by a hummers oxidation-reduction method and then diluting the graphene oxide gel with water, wherein the concentration of the graphene oxide solution is 2-100 mg/ml.
Further, the mass ratio of the graphene oxide solute to the carbon nanotubes in the dispersion liquid is 100: 1-5: 1.
further, the dispersion liquid is placed into a cell crushing instrument for dispersing for 20-120 min.
Furthermore, the support body is commercial abrasive paper with 100-3000 meshes.
Furthermore, the spraying times are 2-8 times, and the thickness of the sprayed film is 10-500 μm.
Further, the illumination method is near infrared spectrum illumination, the illumination time is 0.5-18 h, and the power of the near infrared light is 50-500W.
Furthermore, the sheet resistance of the electrode with the graphene sponge structure for CDI is 1-80 omega/□.
The invention has the beneficial effects that: the graphene and carbon nanotube composite three-dimensional system structure prepared by reduction by the illumination method effectively utilizes the p-p effect, thereby not only avoiding graphene agglomeration, but also keeping the strength of the 3D carbon electrode; meanwhile, the sponge structure provides a good ion transmission channel for electrons, and improves the ion diffusion efficiency; secondly, the graphene sponge structure electrode has highly stable electrical and mechanical properties and rich specific surface area, so that the graphene sponge structure electrode has specific advantages in the CDI technology; finally, the graphene oxide film sprayed by taking the graphene oxide solution and the carbon nano tube as raw materials is not added with a binder, and the graphene oxide is subjected to a light reduction method to obtain graphene, so that the good conductivity and the proper micro-pore structure of the electrode are ensured, the adsorption and desorption performance is high, the stability is good, and the service life is long.
Drawings
The invention is further described below with reference to the accompanying drawings.
Fig. 1 is a CDI adsorption/desorption performance chart of the electrode membrane sheet in example 3.
Detailed Description
The invention will now be further illustrated by reference to specific examples, which are intended to be illustrative of the invention and are not intended to be a further limitation of the invention.
Example 1
Taking commercial graphite powder, preparing graphene oxide gel by a hummers method for later use, and adding water to dilute the graphene oxide gel to a graphene oxide solution with the concentration of 30 mg/ml. Taking the mass ratio of 20: 1, placing the mixture into a cell crushing instrument for dispersing for 40min, then placing the mixture into a high-pressure spraying tank, repeatedly spraying 3 times on 200-mesh abrasive paper, controlling the thickness of the sprayed film to be 80 mu m, then placing the sprayed film under 200W near infrared light, irradiating for 4h, and carrying out physical stripping to obtain the graphene sponge structure electrode film with the sheet resistance of 40 omega/□.
Example 2
Taking commercial graphite powder, preparing graphene oxide gel by a hummers method for later use, and adding water to dilute the graphene oxide gel to a graphene oxide solution with the concentration of 50 mg/ml. Taking the mass ratio of 10: 1, placing the mixture into a cell crushing instrument to be dispersed for 60min, then placing the mixture into a high-pressure spraying tank, repeatedly spraying the mixture on 500-mesh abrasive paper for 4 times, controlling the thickness of the sprayed film to be 100 mu m, then placing the sprayed film under 200W near infrared light, irradiating for 3h, and physically stripping to obtain the graphene sponge structure with the electrode film square resistance of 20 omega/□.
Example 3
Taking commercial graphite powder, preparing graphene oxide gel by a hummers method for later use, and adding water to dilute the graphene oxide gel to 15mg/ml graphene oxide solution. Taking the mass ratio of 25: 1, placing the mixture into a cell crushing instrument for dispersing for 50min, then placing the mixture into a high-pressure spray tank, repeatedly spraying on 1000-mesh abrasive paper for 6 times, controlling the thickness of a sprayed film to be 200 mu m, then placing the sprayed film under 300W near infrared light, irradiating for 2h, and carrying out physical stripping to obtain the graphene sponge structure with the electrode film square resistance of 10 omega/□.
The electrode membrane prepared in example 3 was placed in a small CDI module (electrode size 8 x 8cm), applied with a voltage of 1.6V, the treated water sample was tap water, the conductivity was 455.1 μ s/cm, and 250ml of the volume was taken for electrode CDI desorption cycle performance detection, with the following results: as shown in figure 1, in the 135min adsorption process, the conductivity is reduced from initial 455.1 mus/cm to 145.8 mus/cm, the removal efficiency is 67.96%, and the desorption equilibrium is basically reached after reverse pressure desorption for 60 min.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (6)
1. A preparation method of a graphene sponge structure electrode for CDI is characterized by comprising the following steps: uniformly mixing carbon nanotubes and a graphene oxide solution to obtain a dispersion liquid, spraying the dispersion liquid on the surface of a support to obtain a spraying film, reducing and expanding the spraying film by adopting a lighting method to obtain a three-dimensional sponge structure, physically stripping the three-dimensional sponge structure from the support to obtain the graphene sponge structure electrode for CDI, wherein the spraying frequency is 2-8 times, the thickness of the spraying film is 200-500 mu m, and the support is 100-3000-mesh commercial sand paper.
2. The method for preparing the electrode with the graphene sponge structure for CDI according to claim 1, which is characterized in that: the concentration of the graphene oxide solution is 2-100 mg/ml.
3. The method for preparing the electrode with the graphene sponge structure for CDI according to claim 1, which is characterized in that: the mass ratio of the graphene oxide solute to the carbon nano tubes in the dispersion liquid is 100: 1-5: 1.
4. the method for preparing the electrode with the graphene sponge structure for CDI according to claim 1, which is characterized in that: and (3) dispersing the dispersion liquid in a cell crushing instrument for 20-120 min.
5. The method for preparing the electrode with the graphene sponge structure for CDI according to claim 1, which is characterized in that: the illumination method is near infrared spectrum illumination, the illumination time is 0.5-18 h, and the power of near infrared light is 50-500W.
6. The method for preparing the electrode with the graphene sponge structure for CDI according to claim 1, which is characterized in that: the sheet resistance of the electrode with the graphene sponge structure for CDI is 1-80 omega/□.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103077766A (en) * | 2013-02-06 | 2013-05-01 | 青岛中科昊泰新材料科技有限公司 | Graphene conducting film and application of graphene conducting film to electrochemical capacitor |
| CN104183832A (en) * | 2014-08-13 | 2014-12-03 | 东南大学 | Preparation method and application of FeF3 flexible electrode based on carbon nano tube-graphene composite three-dimensional network |
| CN107565140A (en) * | 2017-10-31 | 2018-01-09 | 武汉理工大学 | Preparation method for the three-dimensional porous graphene carbon nanotube electrode of enzymatic |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103077766A (en) * | 2013-02-06 | 2013-05-01 | 青岛中科昊泰新材料科技有限公司 | Graphene conducting film and application of graphene conducting film to electrochemical capacitor |
| CN104183832A (en) * | 2014-08-13 | 2014-12-03 | 东南大学 | Preparation method and application of FeF3 flexible electrode based on carbon nano tube-graphene composite three-dimensional network |
| CN107565140A (en) * | 2017-10-31 | 2018-01-09 | 武汉理工大学 | Preparation method for the three-dimensional porous graphene carbon nanotube electrode of enzymatic |
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