CN109192541B - Preparation method of doped modified graphene oxide special for super capacitor - Google Patents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method of doped modified graphene oxide special for a super capacitor, and belongs to the technical field of new energy materials. The method comprises the steps of stirring and mixing water, normal hexane, nano graphene oxide and polyallylamine uniformly, and introducing carbon dioxide in the stirring process to prepare a self-made emulsion; then stirring and mixing the self-made emulsion, cerium salt and manganese salt uniformly, slowly dripping a precipitator in a stirring state, adjusting the pH value, continuously stirring for reaction, standing and aging to obtain an aged material; transferring the aged material into a reaction kettle, continuously introducing inert gas into the reaction kettle, heating and raising the temperature under the protection of the inert gas, carrying out heat preservation reaction, cooling, discharging, standing for layering, and collecting an oil phase; and (3) carrying out centrifugal separation on the oil phase, collecting the lower-layer precipitate, and then washing and drying to obtain the special doped modified graphene oxide for the super capacitor. The doped modified graphene oxide special for the super capacitor has excellent electrochemical performance.
Description
Technical Field
The invention discloses a preparation method of doped modified graphene oxide special for a super capacitor, and belongs to the technical field of new energy materials.
Background
Energy problems are one of the most serious problems facing today's society. Therefore, development of new energy conversion and storage devices with low cost and environmental friendliness is one of the effective approaches to solving the energy problem. In all devices, compared with the traditional capacitor and secondary battery, the specific power of the super capacitor is more than 10 times of that of the battery, the capacity of storing electric charge is higher than that of a common capacitor, and the super capacitor has the characteristics of high charging and discharging speed, no pollution to the environment, long cycle life, wide use temperature range and the like, and becomes one of the most potential electrochemical energy storage devices. And has wide application prospect in the fields of hybrid electric vehicles, mobile communication and the like.
As is well known, supercapacitor electrode materials basically comprise 3 major classes: carbon with electric double layer capacitance, metal hydroxides with pseudo capacitance, oxides and conductive polymers. In recent years, binary or even multi-element composite electrode materials have attracted much attention because single electrode materials have some defects of the single electrode materials. Among them, NiO/reduced graphene oxide (rGO) composite electrode materials are one of the topics of interest to many researchers, mainly due to: NiO has higher theoretical specific capacitance, and rGO nano-sheets have higher conductivity. The synergistic effect of the two materials greatly improves the electrochemical performance of the composite material compared with that of a pure electrode material. For example, a NiO/rGO composite electrode material is synthesized through microwave assistance, and the composite material shows higher specific capacitance (the specific capacitance reaches 799F/g at 0.3A/g); obtaining a NiO and graphene composite film by adopting electrophoretic deposition and electrochemical deposition methods, wherein the specific capacitance of the film reaches 400F/g when the film is 2A/g; the novel porous graphene/NiO nano composite material is prepared by a reflux method, and the specific capacitance of the electrode material reaches 429.7F/g at 200 mA/g. The electrochemical performance of graphene oxide used in the conventional supercapacitor cannot be further improved, and when inorganic metal oxide is adopted for doping, inorganic metal oxide powder cannot effectively permeate into an interlayer structure of graphene layers, and the powder is easy to agglomerate in the preparation process, so that the electrochemical performance of the graphene oxide cannot be improved or reduced, and therefore the research on the electrochemical performance of the graphene oxide is required.
Disclosure of Invention
The invention mainly solves the technical problems that: aiming at the defects that the electrochemical performance of graphene oxide used by a traditional super capacitor cannot be further improved, and inorganic metal oxide powder is difficult to effectively permeate into an interlayer structure of graphene layers when being doped by the inorganic metal oxide, and the powder is easy to agglomerate in the preparation process, so that the electrochemical performance of the graphene oxide is not improved and reduced, the preparation method of the doped modified graphene oxide special for the super capacitor is provided.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
(1) according to the weight parts, 60-80 parts of water, 80-120 parts of n-hexane, 15-20 parts of nano graphene oxide and 4-8 parts of polyallylamine are sequentially taken, stirred and mixed uniformly, and carbon dioxide is continuously introduced in the stirring process to obtain an emulsion;
(2) according to the weight parts, 200-300 parts of self-made emulsion, 1-3 parts of cerium salt and 10-20 parts of manganese salt are sequentially taken, stirred and mixed uniformly, then a precipitator is slowly dripped under the stirring state, the pH value is adjusted to 8.5-9.0, and after the stirring reaction is continued, standing and aging are carried out to obtain an aging material;
(3) transferring the aged material into a reaction kettle, continuously introducing inert gas into the reaction kettle, heating to 55-60 ℃ under the protection of the inert gas, keeping the temperature for reaction for 30-40 min, cooling, discharging, standing for layering, and collecting an oil phase;
(4) and (3) carrying out centrifugal separation on the oil phase, collecting the lower-layer precipitate, and then washing and drying to obtain the special doped modified graphene oxide for the super capacitor.
The step (1) of continuously introducing carbon dioxide comprises the following steps: continuously introducing carbon dioxide gas at a rate of 60-80 mL/min.
The cerium salt in the step (2) is any one of cerium nitrate, cerium chloride and cerium sulfate.
The manganese salt in the step (2) is any one of manganese chloride, manganese sulfate and manganese nitrate.
And (3) the slow dripping is carried out at the speed of 2-4 mL/min.
And (3) the precipitator in the step (2) is any one of ammonia water with the mass fraction of 8-10% or urea solution with the mass fraction of 8-10%.
And (3) continuously introducing inert gas: continuously introducing inert gas at the rate of 80-100 mL/min for 30-45 min.
And (4) the inert gas in the step (3) is any one of nitrogen or argon.
The invention has the beneficial effects that:
(1) according to the technical scheme, firstly, water is used as a water phase, normal hexane is used as an oil phase, a certain emulsification effect is exerted by utilizing good hydrophilic and oleophilic surface activity of graphene oxide, a microemulsion system is formed in the stirring and mixing process, polyallylamine and carbon dioxide are matched to realize the stability of the microemulsion system, and the phase separation in the subsequent preparation process is avoided;
(2) the technical scheme of the invention introduces cerium salt and manganese salt into the self-made microemulsion system, on one hand, the two metal salts can be ionized in aqueous solution to generate corresponding metal ions, on the other hand, the metal ions generated by ionization can generate electrostatic adsorption by carboxyl at the edge of oxidized graphene, thereby fixing the metal ions at the oil/water interface, after the precipitant is added, the balance is destroyed, the metal ions and the hydroxide ions are combined at the interface to form corresponding hydroxide, and once hydroxide crystal nuclei are generated, the hydroxide crystal nuclei are wrapped by graphene oxide and enter the oil drop core, so that the further growth and agglomeration of the crystal nuclei are effectively avoided, and after the oil phase is removed through the subsequent separation and separation of oil and water phases, obtaining the graphene oxide doped with the metal oxide with good dispersibility, so that the electrochemical performance of the graphene oxide is effectively improved on the original basis;
(3) according to the technical scheme, the manganese oxide is doped by adopting the rare earth cerium element, so that the unit cell parameters of the prepared manganese oxide are subjected to anisotropic expansion, the tunnel size is changed, the electrochemical performance of the material is effectively improved, and the electrochemical performance of the doped graphene oxide is further improved.
Detailed Description
According to the weight parts, 60-80 parts of water, 80-120 parts of n-hexane, 15-20 parts of nano graphene oxide and 4-8 parts of polyallylamine are poured into a No. 1 beaker in sequence, a stirrer is used for stirring and mixing at the rotating speed of 400-600 r/min for 30-60 min, carbon dioxide gas is continuously introduced into the material in the No. 1 beaker through a guide pipe in the stirring process, the introduction rate of the carbon dioxide gas is adjusted to be 60-80 mL/min, and the introduction of the carbon dioxide gas is stopped after the stirring and mixing are finished, so that emulsion is prepared; according to the weight parts, 200-300 parts of self-made emulsion, 1-3 parts of cerium salt and 10-20 parts of manganese salt are sequentially added into a four-mouth flask with a stirrer, under the condition that the stirring rotating speed is 600-800 r/min, a precipitator is added into the four-mouth flask at the speed of 2-4 mL/min through a dropping funnel while stirring, the pH value of the material in the four-mouth flask is adjusted to 8.5-9.0, after the pH value is adjusted, the stirring reaction is continued for 2-3 hours at the rotating speed of 400-500 r/min, after the reaction is finished, the stirring is stopped, standing and aging are carried out for 2-3 hours, and an aged material is obtained; and transferring the obtained aged material into a reaction kettle, continuously introducing inert gas into the reaction kettle at a speed of 80-100 mL/min for 30-45 min, then sealing the reaction kettle, heating to 55-60 ℃ under the protection of the inert gas, keeping the temperature for reaction for 30-40 min, opening the reaction kettle, naturally cooling the materials in the reaction kettle to room temperature, discharging, standing for layering, removing a water phase, collecting an oil phase, transferring the oil phase into a centrifuge, centrifugally separating for 10-20 min at a rotation speed of 8000-12000 r/min, removing a supernatant, collecting a lower-layer precipitate, washing the obtained lower-layer precipitate with absolute ethyl alcohol for 3-5 times, transferring into a vacuum drying box, vacuum drying to constant weight under the conditions of a temperature of 95-105 ℃ and a pressure of 80-120 Pa, and discharging to obtain the doped modified graphene oxide special for the supercapacitor. The cerium salt is any one of cerium nitrate, cerium chloride and cerium sulfate. The manganese salt is any one of manganese chloride, manganese sulfate and manganese nitrate. The precipitator is any one of 8-10% by mass of ammonia water or 8-10% by mass of urea solution. The inert gas is any one of nitrogen or argon.
According to the weight parts, 80 parts of water, 120 parts of n-hexane, 20 parts of nano graphene oxide and 8 parts of polyallylamine are sequentially poured into a No. 1 beaker, stirred and mixed for 60min at the rotating speed of 600r/min by a stirrer, carbon dioxide gas is continuously introduced into the material in the No. 1 beaker through a conduit in the stirring process, the introduction rate of the carbon dioxide gas is adjusted to 80mL/min, and the introduction of the carbon dioxide gas is stopped after the stirring and mixing are finished, so that the emulsion is prepared; according to the weight parts, 300 parts of self-made emulsion, 3 parts of cerium salt and 20 parts of manganese salt are sequentially added into a four-mouth flask with a stirrer, under the condition that the stirring speed is 800r/min, a precipitator is added into the four-mouth flask at the speed of 4mL/min through a dropping funnel while stirring, the pH of the material in the four-mouth flask is adjusted to 9.0, after the pH is adjusted, the stirring reaction is continued at the speed of 500r/min for 3 hours, after the reaction is finished, the stirring is stopped, the standing and aging are carried out for 3 hours, and the aging material is discharged to obtain the aging material; and transferring the obtained aged material into a reaction kettle, continuously introducing inert gas into the reaction kettle at the speed of 100mL/min for 45min, then sealing the reaction kettle, heating to 60 ℃ under the protection of the inert gas, keeping the temperature for reaction for 40min, then opening the reaction kettle, naturally cooling the materials in the reaction kettle to room temperature, discharging, standing for layering, removing a water phase, collecting an oil phase, transferring the oil phase into a centrifuge, centrifugally separating for 20min at the rotation speed of 12000r/min, removing a supernatant, collecting a lower-layer precipitate, washing the obtained lower-layer precipitate with absolute ethyl alcohol for 5 times, transferring into a vacuum drying oven, vacuum drying at the temperature of 105 ℃ and the pressure of 120Pa to constant weight, and discharging to obtain the doped modified graphene oxide special for the supercapacitor. The cerium salt is cerium nitrate. The manganese salt is manganese chloride. The precipitator is ammonia water with the mass fraction of 10%. The inert gas is nitrogen.
According to the weight parts, 80 parts of water, 120 parts of n-hexane and 20 parts of nano graphene oxide are sequentially taken and poured into a No. 1 beaker, a stirrer is used for stirring and mixing for 60min at the rotating speed of 600r/min, carbon dioxide gas is continuously introduced into the material in the No. 1 beaker through a guide pipe in the stirring process, the introduction rate of the carbon dioxide gas is adjusted to be 80mL/min, and the introduction of the carbon dioxide gas is stopped after the stirring and mixing are finished, so that the emulsion is prepared; according to the weight parts, 300 parts of self-made emulsion, 3 parts of cerium salt and 20 parts of manganese salt are sequentially added into a four-mouth flask with a stirrer, under the condition that the stirring speed is 800r/min, a precipitator is added into the four-mouth flask at the speed of 4mL/min through a dropping funnel while stirring, the pH of the material in the four-mouth flask is adjusted to 9.0, after the pH is adjusted, the stirring reaction is continued at the speed of 500r/min for 3 hours, after the reaction is finished, the stirring is stopped, the standing and aging are carried out for 3 hours, and the aging material is discharged to obtain the aging material; and transferring the obtained aged material into a reaction kettle, continuously introducing inert gas into the reaction kettle at the speed of 100mL/min for 45min, then sealing the reaction kettle, heating to 60 ℃ under the protection of the inert gas, keeping the temperature for reaction for 40min, then opening the reaction kettle, naturally cooling the materials in the reaction kettle to room temperature, discharging, standing for layering, removing a water phase, collecting an oil phase, transferring the oil phase into a centrifuge, centrifugally separating for 20min at the rotation speed of 12000r/min, removing a supernatant, collecting a lower-layer precipitate, washing the obtained lower-layer precipitate with absolute ethyl alcohol for 5 times, transferring into a vacuum drying oven, vacuum drying at the temperature of 105 ℃ and the pressure of 120Pa to constant weight, and discharging to obtain the doped modified graphene oxide special for the supercapacitor. The cerium salt is cerium nitrate. The manganese salt is manganese chloride. The precipitator is ammonia water with the mass fraction of 10%. The inert gas is nitrogen.
According to the weight parts, 80 parts of water, 120 parts of n-hexane, 20 parts of nano graphene oxide and 8 parts of polyallylamine are sequentially poured into a No. 1 beaker, stirred and mixed for 60min at the rotating speed of 600r/min by a stirrer, carbon dioxide gas is continuously introduced into the material in the No. 1 beaker through a conduit in the stirring process, the introduction rate of the carbon dioxide gas is adjusted to 80mL/min, and the introduction of the carbon dioxide gas is stopped after the stirring and mixing are finished, so that the emulsion is prepared; according to the weight parts, 300 parts of self-made emulsion and 20 parts of manganese salt are sequentially added into a four-mouth flask with a stirrer, under the condition that the stirring rotating speed is 800r/min, a precipitator is added into the four-mouth flask at the speed of 4mL/min through a dropping funnel while stirring, the pH of materials in the four-mouth flask is adjusted to 9.0, after the pH adjustment is finished, the materials are continuously stirred and reacted at the rotating speed of 500r/min for 3 hours, after the reaction is finished, the stirring is stopped, standing and aging are carried out for 3 hours, and discharging is carried out to obtain an aged material; and transferring the obtained aged material into a reaction kettle, continuously introducing inert gas into the reaction kettle at the speed of 100mL/min for 45min, then sealing the reaction kettle, heating to 60 ℃ under the protection of the inert gas, keeping the temperature for reaction for 40min, then opening the reaction kettle, naturally cooling the materials in the reaction kettle to room temperature, discharging, standing for layering, removing a water phase, collecting an oil phase, transferring the oil phase into a centrifuge, centrifugally separating for 20min at the rotation speed of 12000r/min, removing a supernatant, collecting a lower-layer precipitate, washing the obtained lower-layer precipitate with absolute ethyl alcohol for 5 times, transferring into a vacuum drying oven, vacuum drying at the temperature of 105 ℃ and the pressure of 120Pa to constant weight, and discharging to obtain the doped modified graphene oxide special for the supercapacitor. The manganese salt is manganese chloride. The precipitator is ammonia water with the mass fraction of 10%. The inert gas is nitrogen.
According to the weight parts, 80 parts of water, 120 parts of absolute ethyl alcohol, 20 parts of nano graphene oxide and 8 parts of polyallylamine are sequentially poured into a No. 1 beaker, stirred and mixed for 60min at the rotating speed of 600r/min by a stirrer, carbon dioxide gas is continuously introduced into the material in the No. 1 beaker through a guide pipe in the stirring process, the introduction rate of the carbon dioxide gas is adjusted to be 80mL/min, and the introduction of the carbon dioxide gas is stopped after the stirring and mixing are finished, so that emulsion is prepared; according to the weight parts, 300 parts of self-made emulsion, 3 parts of cerium salt and 20 parts of manganese salt are sequentially added into a four-mouth flask with a stirrer, under the condition that the stirring speed is 800r/min, a precipitator is added into the four-mouth flask at the speed of 4mL/min through a dropping funnel while stirring, the pH of the material in the four-mouth flask is adjusted to 9.0, after the pH is adjusted, the stirring reaction is continued at the speed of 500r/min for 3 hours, after the reaction is finished, the stirring is stopped, the standing and aging are carried out for 3 hours, and the aging material is discharged to obtain the aging material; and transferring the obtained aged material into a reaction kettle, continuously introducing inert gas into the reaction kettle at the speed of 100mL/min for 45min, then sealing the reaction kettle, heating to 60 ℃ under the protection of the inert gas, keeping the temperature for reaction for 40min, then opening the reaction kettle, naturally cooling the materials in the reaction kettle to room temperature, discharging, standing for layering, removing a water phase, collecting an oil phase, transferring the oil phase into a centrifuge, centrifugally separating for 20min at the rotation speed of 12000r/min, removing a supernatant, collecting a lower-layer precipitate, washing the obtained lower-layer precipitate with absolute ethyl alcohol for 5 times, transferring into a vacuum drying oven, vacuum drying at the temperature of 105 ℃ and the pressure of 120Pa to constant weight, and discharging to obtain the doped modified graphene oxide special for the supercapacitor. The cerium salt is cerium nitrate. The manganese salt is manganese chloride. The precipitator is ammonia water with the mass fraction of 10%. The inert gas is nitrogen.
Comparative example: modified graphene oxide from Changzhou materials science and technology Limited.
The modified graphene oxides obtained in examples 1 to 4 and comparative example products were subjected to performance testing, and the specific testing method was as follows:
and carrying out constant current charge and discharge test on the modified graphene oxide material.
The calculation formula of the specific capacity is as follows:
Cm=IΔt/mΔV
in the formula: cm is specific capacitance, F/g; i is a discharge current, A; Δ t is the discharge time, s; m is the mass of the active material in the electrode material, g; Δ V is the discharge voltage range, V.
Specific detection results are shown in table 1:
table 1: performance test meter
| Detecting content | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| Specific capacitance F/g | 770 | 732 | 659 | 696 | 527 |
The detection results in table 1 show that the doped modified graphene oxide specially used for the super capacitor has excellent electrochemical properties.
Claims (7)
1. A preparation method of doped modified graphene oxide special for a super capacitor is characterized by comprising the following specific preparation steps:
(1) according to the weight parts, 60-80 parts of water, 80-120 parts of n-hexane, 15-20 parts of nano graphene oxide and 4-8 parts of polyallylamine are sequentially taken, stirred and mixed uniformly, and carbon dioxide is continuously introduced in the stirring process to obtain an emulsion;
(2) according to the weight parts, 200-300 parts of self-made emulsion, 1-3 parts of cerium salt and 10-20 parts of manganese salt are sequentially taken, stirred and mixed uniformly, a precipitator is added dropwise at the speed of 2-4 mL/min under the stirring state, the pH value is adjusted to 8.5-9.0, and after the stirring reaction is continued, standing and aging are carried out to obtain an aging material;
(3) transferring the aged material into a reaction kettle, continuously introducing inert gas into the reaction kettle, heating to 55-60 ℃ under the protection of the inert gas, keeping the temperature for reaction for 30-40 min, cooling, discharging, standing for layering, and collecting an oil phase;
(4) and (3) carrying out centrifugal separation on the oil phase, collecting the lower-layer precipitate, and then washing and drying to obtain the special doped modified graphene oxide for the super capacitor.
2. The preparation method of the doped modified graphene oxide special for the supercapacitor according to claim 1, wherein the continuous introduction of carbon dioxide in the step (1) is: continuously introducing carbon dioxide gas at a rate of 60-80 mL/min.
3. The method for preparing the doped modified graphene oxide special for the supercapacitor according to claim 1, wherein the cerium salt in the step (2) is any one of cerium nitrate, cerium chloride and cerium sulfate.
4. The preparation method of the doped modified graphene oxide special for the supercapacitor according to claim 1, wherein the manganese salt in the step (2) is any one of manganese chloride, manganese sulfate and manganese nitrate.
5. The preparation method of the doped modified graphene oxide special for the supercapacitor according to claim 1, wherein the precipitator in the step (2) is any one of ammonia water with a mass fraction of 8-10% or urea solution with a mass fraction of 8-10%.
6. The preparation method of the doped modified graphene oxide special for the supercapacitor according to claim 1, wherein the continuous inert gas introduction in the step (3) is: continuously introducing inert gas at the rate of 80-100 mL/min for 30-45 min.
7. The preparation method of the doped modified graphene oxide special for the supercapacitor according to claim 1, wherein the inert gas in the step (3) is any one of nitrogen and argon.
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