CN108172408B - NH (hydrogen sulfide)2-rGO/MnO2Composite material, preparation method and application - Google Patents
NH (hydrogen sulfide)2-rGO/MnO2Composite material, preparation method and application Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims description 4
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 27
- 239000002131 composite material Substances 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 22
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 21
- 239000010439 graphite Substances 0.000 claims abstract description 21
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 21
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000006228 supernatant Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005576 amination reaction Methods 0.000 claims abstract description 6
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 239000000376 reactant Substances 0.000 claims abstract description 4
- 230000009467 reduction Effects 0.000 claims abstract description 4
- 238000010992 reflux Methods 0.000 claims abstract description 4
- 239000003990 capacitor Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000003792 electrolyte Substances 0.000 abstract description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 2
- 239000003575 carbonaceous material Substances 0.000 description 5
- 229920001940 conductive polymer Polymers 0.000 description 5
- 238000011160 research Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000002077 nanosphere Substances 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
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- 239000006229 carbon black Substances 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
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- 230000001351 cycling effect Effects 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
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- 239000002245 particle Substances 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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Abstract
The invention discloses NH2‑rGO/MnO2The composite material, the preparation method and the application thereof are characterized in that graphite oxide GO is prepared, and the prepared graphite oxide is prepared into an aqueous solution for later use; stirring a graphite oxide aqueous solution and dimethylformamide in a water bath, then adding a p-phenylenediamine solution into the reaction, raising the temperature, carrying out reflux stirring, washing the obtained reactant with ethanol and deionized water until the supernatant is colorless and neutral, and dispersing the obtained precipitate into the deionized water to obtain amination reduction graphene oxide NH2-an aqueous rGO solution; adopts a hydrothermal method to prepare potassium permanganate KMnO4With the NH obtained2Mixing and stirring the-rGO aqueous solution, performing ultrasonic treatment, and then transferring the mixture into a reaction kettle to prepare NH2‑rGO/MnO2A material. The prepared aminated graphene can improve the conductivity of manganese dioxide, the existence of amino can improve the electrochemical activity of the material, increase the wettability of the material and electrolyte, and simultaneously can regulate and control the micro-morphology of the manganese dioxide, increase the specific surface area and improve the dispersibility of the material, thereby integrally improving the performance of the supercapacitor.
Description
Technical Field
The invention relates to a preparation method of a capacitor material, in particular to NH2-rGO/MnO2Composite material, preparation method and application.
Background
Energy is a precious resource on which people live, and with the continuous increase of population and the accelerated consumption of energy, the search for new energy and energy storage devices is one of effective ways for people to solve the problem of energy exhaustion. In the process of researching new energy devices for replacing internal combustion engines, research and development on hybrid power, fuel cells, chemical battery products and application are carried out, and certain effect is achieved. But they have not been well solved because of their inherent fatal weaknesses such as short service life, poor temperature characteristics, environmental pollution of chemical batteries, complex system, high cost, etc. The super capacitor as a new energy storage device has the advantages of high energy density, long cycle life, short charging time and the like, can partially or completely replace the traditional chemical battery to be used as a traction power supply and a starting energy source of a vehicle, and has wider application compared with the traditional chemical battery.
The materials of the super capacitor mainly comprise three types of carbon materials, conductive polymers and transition metal oxides. The carbon material has the advantages of large specific surface area, small internal resistance, low price and good stability. Common carbon materials include: carbon black, carbon nanotubes, carbon nanofibers, and the like, but carbon materials have a small specific capacitance and a low energy density. The focus of current research is mainly composite materials of ordered carbon nanotube arrays and graphene.
The conductive polymer mainly comprises polypyrrole, polyaniline and polythiophene. The specific capacitance of the conductive polymer is large, and the cost is low; the defects are that the variety is less, the internal resistance is higher when the conductive polymer is directly used as the electrode material of the super capacitor, and the service life of the electrode is short. The current research direction is to develop new conductive polymers to make composites to improve overall performance.
The transition metal oxide has high specific capacitance (10-100 times of that of a carbon material) and good stability, but the overall performance of the transition metal oxide is poor due to the defects of poor conductivity and compact structure. A representative material is MnO2、Co3O4NiO, etc. At present, the research direction is to regulate and control the microscopic appearance of the nano-spheres, nano-flowers, nano-rods and the like by different preparation methods so as to increase the specific surface area and be beneficial to the transmission of ions.
The manganese oxide is low in price, has ultrahigh theoretical specific capacitance and is good in stability. Considerable research has been carried out and researchers are trying to improve their specific capacitance performance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides NH2-rGO/MnO2The composite material, the preparation method and the application can improve the conductivity and the dispersibility of the whole composite material.
The invention is realized by the following technical scheme, namely NH of the invention2-rGO/MnO2The preparation method of the composite material comprises the following steps:
(1) preparing graphite oxide GO by a Hummers method, and preparing the prepared graphite oxide into an aqueous solution for later use;
(2) stirring a graphite oxide aqueous solution and dimethylformamide in a water bath at the temperature of 30-40 ℃ for 1-1.5 hours, then adding a p-phenylenediamine solution into the reaction, raising the temperature to 70-90 ℃, carrying out reflux stirring for 9-11 hours, washing the obtained reactant with ethanol and deionized water until the supernatant is colorless and neutral, dispersing the obtained precipitate into the deionized water, and obtaining amination reduction graphene oxide NH with the concentration of 0.1-1 g/L2-an aqueous rGO solution;
(3) adopts a hydrothermal method to prepare potassium permanganate KMnO4With the NH obtained2Mixing and stirring the-rGO aqueous solution, performing ultrasonic treatment, and then transferring the mixture into a reaction kettle to prepare NH2-rGO/MnO2A material.
In the step (1), graphite oxide is prepared by a Hummers method, the obtained graphite oxide solution is washed by ethanol and deionized water in a ratio of 1:1 until the supernatant is colorless, and the graphite oxide solution is dispersed in the deionized water to obtain 0.5-1.0 g/L of graphite oxide aqueous solution.
In the step (2), the concentration of the p-phenylenediamine solution is 3g/L, and the ultrasonic treatment is carried out for 30-60 minutes in an ultrasonic environment.
In the step (3), potassium permanganate is added into deionized water to prepare 0.025mol/L potassium permanganate aqueous solution, and 10mL of NH is taken2Mixing the-rGO aqueous solution with 40mL of potassium permanganate aqueous solution, performing ultrasonic treatment for more than 30 minutes, transferring the mixture into a reaction kettle for hydrothermal reaction to obtain the final productWashing the precipitate with deionized water and ethanol solution until the supernatant is colorless, vacuum drying the precipitate at 60 deg.C, and grinding to obtain NH2-rGO/MnO2And (3) powder.
In the step (3), the temperature of the hydrothermal reaction is 180 ℃ and the time is 15 hours.
NH prepared by the preparation method2-rGO/MnO2A composite material.
NH (hydrogen sulfide)2-rGO/MnO2Use of a composite material for the preparation of a capacitor material.
Compared with the prior art, the invention has the following advantages: the prepared aminated graphene can improve the conductivity of manganese dioxide, the existence of amino can improve the electrochemical activity of the material, increase the wettability of the material and electrolyte, regulate and control the micro morphology of the manganese dioxide, increase the specific surface area and improve the dispersibility of the material, thereby integrally improving the supercapacitance performance and NH2-rGO/MnO2XRD and SEM analysis shows that the composite material is a composite material of manganese dioxide and aminated graphene, has high specific capacitance and good micro morphology, and shows excellent cycling stability in multiple charge and discharge experiments. The aminated graphene in the composite material has a regulating effect on the growth of manganese dioxide, so that the agglomeration of manganese dioxide particles is reduced, the conductivity of the material is improved, the advantages are complementary, compared with the common graphene and manganese dioxide composite material, the composite material has the advantages of higher specific capacitance, more regular appearance and simple manufacturing process.
Drawings
FIG. 1 is an SEM picture of a composite material prepared by the present invention;
FIG. 2 is an XRD pattern of a composite material made in accordance with the present invention;
FIG. 3 is a graph of the capacitive performance of the composite material made in accordance with the present invention.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The preparation process of this example is as follows:
(1) preparing graphite oxide by a Hummers method, washing the obtained graphite oxide solution with 1:1 ethanol and deionized water until the supernatant is colorless, and dispersing the graphite oxide solution into the deionized water to obtain 0.5-1.0 g/L of graphite oxide aqueous solution;
(2) stirring 1g/L graphite oxide aqueous solution 20mL and dimethylformamide 50mL in 35 ℃ water bath for 1 hour, then adding 100mL p-phenylenediamine solution into the reaction, raising the temperature to 80 ℃, refluxing and stirring for 10 hours, washing the obtained reactant with ethanol and deionized water until the supernatant is colorless and neutral, dispersing the obtained precipitate into deionized water, and obtaining amination reduction graphene oxide NH with the concentration of 1g/L2-an aqueous rGO solution; the concentration of the p-phenylenediamine solution is 3g/L, and the p-phenylenediamine solution is subjected to ultrasonic treatment for 30-60 minutes in an ultrasonic environment;
(3) 0.395g of potassium permanganate is added into 100mL of deionized water to prepare 0.025mol/L potassium permanganate aqueous solution, and 10mL of NH is taken2Mixing the-rGO aqueous solution with 40mL of potassium permanganate aqueous solution, performing ultrasonic treatment for more than 30 minutes, transferring the mixture into a reaction kettle for hydrothermal reaction at the temperature of 180 ℃ for 15 hours, washing the obtained precipitate with deionized water and ethanol solution respectively until the supernatant is colorless, performing vacuum drying on the precipitate at the temperature of 60 ℃, and grinding to obtain NH2-rGO/MnO2And (3) powder.
Example 2
In this example, 0.395g of potassium permanganate is added into 100mL of deionized water to prepare 0.025mol/L potassium permanganate aqueous solution, and 10mL of amination reduced graphene oxide NH with a concentration of 0.1g/L is taken2Mixing the-rGO aqueous solution with 40mL of potassium permanganate aqueous solution, performing ultrasonic treatment for more than 30 minutes, transferring the mixture into a reaction kettle for hydrothermal reaction at the temperature of 180 ℃ for 15 hours, washing the obtained precipitate with deionized water and ethanol solution respectively until the supernatant is colorless, and circulating the precipitate at the temperature of 60 DEG CVacuum drying and grinding under ambient conditions to obtain NH2-rGO/MnO2And (3) powder.
Other embodiments are the same as example 1.
Example 3
In this example, 0.395g of potassium permanganate is added into 100mL of deionized water to prepare 0.025mol/L potassium permanganate aqueous solution, and 10mL of amination reduced graphene oxide NH with a concentration of 0.5g/L is taken2Mixing the-rGO aqueous solution with 40mL of potassium permanganate aqueous solution, performing ultrasonic treatment for more than 30 minutes, transferring the mixture into a reaction kettle for hydrothermal reaction at the temperature of 180 ℃ for 15 hours, washing the obtained precipitate with deionized water and ethanol solution respectively until the supernatant is colorless, performing vacuum drying on the precipitate at the temperature of 60 ℃, and grinding to obtain NH2-rGO/MnO2And (3) powder.
Other embodiments are the same as example 1.
SEM analysis of the composite material prepared in example 1 is shown in figure 1, and it can be seen from the figure that the composite material has good microscopic morphology, uniformity and order, and better dispersibility of manganese dioxide, and shown in the figure is a flower ball formed by MnO2 nanosheets attached to aminated graphene and growing, which can be called manganese dioxide nanospheres for short.
XRD analysis of the composite materials prepared in examples 1-3 is shown in figure 2, and it can be seen from the figure that the obtained composite materials are manganese dioxide and aminated graphene composites, a manganese dioxide diffraction peak is obvious in the figure, and the graphene content is low, so that the manganese dioxide diffraction peak is covered.
The capacitance test of the composite material prepared in example 1 is shown in fig. 3, and it can be seen from the figure that the charging and discharging time of the supercapacitor reaches 300s when the current density is 1A/g.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. NH (hydrogen sulfide)2-rGO/MnO2The preparation method of the composite material is characterized by comprising the following steps:
(1) preparing graphite oxide GO by a Hummers method, and preparing the prepared graphite oxide into an aqueous solution for later use;
(2) stirring 1g/L graphite oxide aqueous solution 20mL and dimethylformamide in a water bath at 30-40 ℃ for 1-1.5 hours, then adding 100mL of p-phenylenediamine solution with the concentration of 3g/L, carrying out ultrasonic treatment for 30-60 minutes in an ultrasonic environment, raising the temperature to 70-90 ℃, carrying out reflux stirring for 9-11 hours, washing the obtained reactant with ethanol and deionized water until the supernatant is colorless and neutral, dispersing the obtained precipitate into deionized water, and obtaining amination reduction graphene oxide NH with the concentration of 0.1-1 g/L2-an aqueous rGO solution;
(3) adopts a hydrothermal method to prepare potassium permanganate KMnO4With the NH obtained2Mixing and stirring the-rGO aqueous solution, performing ultrasonic treatment, and then transferring the mixture into a reaction kettle to prepare NH2-rGO/MnO2A material; in the step (3), potassium permanganate is added into deionized water to prepare 0.025mol/L potassium permanganate aqueous solution, and 10mL of NH is taken2Mixing the-rGO aqueous solution with 40mL of potassium permanganate aqueous solution, performing ultrasonic treatment for more than 30 minutes, transferring the mixture into a reaction kettle for hydrothermal reaction, washing obtained precipitates respectively with deionized water and ethanol solution until the supernatant is colorless, performing vacuum drying on the precipitates at the temperature of 60 ℃, and grinding to obtain NH2-rGO/MnO2And (3) powder.
2. NH according to claim 12-rGO/MnO2The preparation method of the composite material is characterized in that in the step (1), graphite oxide is prepared by a Hummers method, the obtained graphite oxide solution is washed by ethanol and deionized water in a ratio of 1:1 until the supernatant is colorless, and the graphite oxide solution is dispersed in the deionized water.
3. NH according to claim 12-rGO/MnO2The preparation method of the composite material is characterized in that in the step (3), the hydrothermal reaction is carried outThe temperature should be 180 ℃ and the time 15 hours.
4. NH prepared by the preparation method of any one of claims 1 to 32-rGO/MnO2A composite material.
5. The NH of claim 42-rGO/MnO2Use of a composite material for the preparation of a capacitor material.
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| CN109817471A (en) * | 2018-12-26 | 2019-05-28 | 中国电子科技集团公司第十八研究所 | Modification method of graphene-based lithium ion capacitor positive electrode material |
| CN110108670B (en) * | 2019-05-31 | 2021-07-02 | 重庆理工大学 | Manufacturing method of hydrogen sulfide sensor based on film-coated thin-core optical fiber, sensor thereof and detection method of hydrogen sulfide gas concentration |
| CN110354282B (en) * | 2019-08-23 | 2021-11-09 | 东华大学 | Manganese dioxide and adriamycin loaded nano hydrogel and preparation and application thereof |
| CN113053676B (en) * | 2021-03-18 | 2022-07-29 | 合肥工业大学 | Preparation method of NH 2-rGO/CNT/alpha-MnO 2NWs composite film electrode material and electrode |
| CN113603205B (en) * | 2021-07-06 | 2022-10-04 | 山东大学 | Method for accelerating degradation of organic pollutants by potassium permanganate |
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