CN115394564A - Preparation method and application of triazole copper/polypyrrole composite electrode material - Google Patents
Preparation method and application of triazole copper/polypyrrole composite electrode material Download PDFInfo
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- 229920000128 polypyrrole Polymers 0.000 title claims abstract description 115
- 150000003852 triazoles Chemical class 0.000 title claims abstract description 101
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000007772 electrode material Substances 0.000 title claims abstract description 66
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 63
- 239000010949 copper Substances 0.000 title claims abstract description 63
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- ZXBVATFSHBMXOL-UHFFFAOYSA-N copper;2h-triazole Chemical compound [Cu].C=1C=NNN=1 ZXBVATFSHBMXOL-UHFFFAOYSA-N 0.000 claims abstract description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000000843 powder Substances 0.000 claims abstract description 52
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 11
- 238000004146 energy storage Methods 0.000 claims abstract description 8
- 239000003990 capacitor Substances 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims description 43
- 239000008367 deionised water Substances 0.000 claims description 40
- 229910021641 deionized water Inorganic materials 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 34
- 239000011259 mixed solution Substances 0.000 claims description 31
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 27
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 20
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 19
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 10
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000178 monomer Substances 0.000 claims description 10
- HUUBMTMJIQHAEN-UHFFFAOYSA-N triazole-1,4-diamine Chemical compound NC1=CN(N)N=N1 HUUBMTMJIQHAEN-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 description 15
- 238000001291 vacuum drying Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
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- 238000011065 in-situ storage Methods 0.000 description 1
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
-
- 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
- H01G11/22—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
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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
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- 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 and application of a triazole copper/polypyrrole composite electrode material, wherein triazole copper powder is prepared by a simple room-temperature stirring method; preparing nano granular polypyrrole powder; dissolving copper triazole in ethanol, adding polypyrrole powder into a beaker, placing the beaker into a constant-temperature water bath for magnetic stirring, dropwise adding a copper triazole solution, and drying in an oven to obtain the copper triazole/polypyrrole composite electrode material powder. The preparation process is simple to operate, has the characteristics of low cost and high yield, is easy to scale, and the prepared triazole copper/polypyrrole composite electrode material has the characteristics of good conductivity, excellent electrochemical performance and the like, and can be widely applied to the fields of water-based batteries, super capacitors or energy storage equipment and the like.
Description
Technical Field
The invention relates to a preparation method and application of an electrode material, in particular to a triazole copper/polypyrrole composite electrode material and a preparation method and application thereof.
Background
Since the twenty-first century, human needs for energy have increased, and fossil fuels have been in increasing shortage on earth. Meanwhile, in the process of energy development and utilization, a large amount of greenhouse gases and toxic substances are discharged, and great harm is caused to the environment and the human health. Therefore, in order to solve the above problems, the development of a green, stable and sustainable renewable energy storage system is promoted. Currently, lithium ion batteries are one of the most successful energy storage systems today, which have a higher energy density than other batteries, leading mobile devices and electric vehicles on the market. However, due to the toxic, flammable and explosive organic electrolyte, limited lithium source reserves, uneven distribution on the earth and the like, further deep and large-scale energy storage application of the lithium ion battery is severely limited. In contrast, the electrolyte of the water-based battery is an aqueous solution, which has incomparable cost advantage, and the probability of explosion combustion of the water-based battery is greatly reduced due to the incombustibility and high specific heat capacity of water.
The electrode material is a key factor for determining the performance of the water-based battery, the triazole copper is a metal complex rich in amino, and rich N-H active reaction groups of the triazole copper can reversibly gain and lose electrons in the electrochemical process, so that the triazole copper has high redox activity. In addition, the copper triazole has the advantages of low cost, high yield, environmental friendliness, flexible structural design and the like. However, like most organic compounds, copper triazole has slow ion conduction speed, low conductivity and slow kinetic behavior in the electrochemical reaction process, which limits the practical application of copper triazole as an electrode material in the field of energy storage.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a preparation method of a triazole copper/polypyrrole composite electrode material, so that the composite electrode material with excellent conductivity and chemical stability is obtained. Wherein, the triazole copper is used as an electrode active material, provides abundant redox groups and has higher electrochemical stability; PPY has excellent conductivity and good dynamic performance, and a synergetic heterojunction network is compositely constructed by the triazole copper and the PPY through dropwise adding to prepare the high-performance electrode material.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a triazole copper/polypyrrole composite electrode material comprises the following steps:
step 1: preparing copper triazole powder;
step 2: preparing polypyrrole powder;
and step 3: preparing a triazole copper/polypyrrole composite electrode material: dissolving the triazole copper powder prepared in the step 1 in ethanol to form a triazole copper solution; and (3) adding the polypyrrole powder prepared in the step (2) into a beaker, placing the beaker into a constant-temperature water bath kettle for magnetic stirring, dropwise adding a copper triazole solution to obtain a uniform mixed solution of copper triazole and polypyrrole, and after the solution is completely evaporated, placing the mixed solution into a 60 ℃ oven for drying for 12 hours to obtain the copper triazole/polypyrrole composite electrode material powder.
Preferably, the mass ratio of the copper triazole to the polypyrrole in the mixed solution of the copper triazole/the polypyrrole prepared in the step 3 is as follows: triazole copper: polypyrrole =1-2:1-2.
Preferably, the weight of the triazole copper powder in the step 3 is 10-20 mg.
Preferably, the temperature of the constant-temperature water bath in the step 3 is 40-60 ℃.
Preferably, the preparation of the triazole copper powder in the step 1 comprises the following steps:
step 1-1: 0.3964 g of 3, 5-diamino-1, 2, 3-triazole and 0.4832 g of copper nitrate trihydrate are dissolved in 50 mL of deionized water;
step 1-2: rapidly stirring the mixed solution in the step 1-1 at room temperature for 12 hours;
step 1-3: after the mixed solution in the step 1-2 is reacted, filtering the green precipitate, and washing for several times by using deionized water and ether in sequence;
step 1-4: and finally, drying the mixed solution washed in the step 1-3 in vacuum at the temperature of 60 ℃ to obtain the triazole copper powder.
Preferably, the preparation of polypyrrole powder in step 2 comprises the following steps:
step 2-1: adding 0.6 g of pyrrole monomer with the purity of 99.0% into 50 mL of deionized water, and stirring for 10 min;
step 2-2: 2 g of ammonium persulfate is added into the solution obtained in the step 2-1, and the mixture is stirred for 12 hours at the temperature of 0 ℃;
step 2-3: and collecting precipitates, washing the precipitates respectively by using deionized water and ethanol, and putting the precipitates into an oven to be dried for 12 hours to obtain polypyrrole powder.
Preferably, in the step 3, the copper triazole powder prepared in the step 1 is dissolved in 15mL of ethanol.
The triazole copper/polypyrrole composite electrode material is formed by compounding triazole copper powder and polypyrrole powder.
An application of a triazole copper/polypyrrole composite electrode material in a water system battery, a super capacitor or an energy storage device.
The invention has the following beneficial effects: (1) The method adopts a dropping method to drop the triazole copper solution into the polypyrrole powder, the process is simple, and the prepared composite electrode material is more uniform than that of an in-situ growth method.
(2) According to the invention, the copper triazole is used as an electrode active material, abundant amino electron-withdrawing groups are provided, the electrochemical stability is high, the PPY has excellent conductivity and good dynamic performance, and the problems of low conductivity of the copper triazole, slow dynamic behavior in the electrochemical reaction process and the like are solved; and PPY is uniformly coated on the surface of the triazole copper, so that the prepared triazole copper/polypyrrole composite material constructs a synergistic heterojunction network, and the transmission of electrons is greatly promoted.
(3) The preparation method has the advantages of simple production process, sufficient raw material sources, large yield, low cost, high stability of the prepared composite electrode material and excellent electrochemical performance.
(4) The triazole copper/polypyrrole composite electrode material prepared by the invention can be widely applied to the fields of water-based batteries, super capacitors or energy storage equipment and the like.
Drawings
FIG. 1 is a diagram of a triazole copper material prepared in example 1 of the present invention.
FIG. 2 is a scanning electron microscope image of the triazole copper/polypyrrole composite electrode material prepared in example 1 of the invention.
FIG. 3 is an XPS N1 s spectrum of the triazole copper/polypyrrole composite electrode material prepared in example 1 of the invention.
FIG. 4 is a cyclic voltammetry curve diagram of the triazole copper/polypyrrole composite electrode material prepared in example 1 of the present invention at different scan rates.
FIG. 5 shows that the triazole copper/polypyrrole composite electrode material prepared in example 1 of the invention has a current density of 1A g -1 The following charge-discharge curve.
FIG. 6 is a multiplying power curve diagram of the triazole copper/polypyrrole composite electrode material prepared in example 1 of the invention.
FIG. 7 shows that the triazole copper/polypyrrole composite electrode material prepared in example 1 of the invention has a current density of 20A g -1 Long cycle plot below.
FIG. 8 shows the current density of the triazole copper/polypyrrole composite electrode material prepared in examples 1 to 5 of the invention is 1 Ag -1 Graph comparing the specific capacity of the lower mass.
Detailed Description
In the following description, for purposes of explanation, numerous implementation details are set forth in order to provide a thorough understanding of the embodiments of the present invention. It should be understood, however, that these implementation details are not to be interpreted as limiting the invention. That is, in some embodiments of the invention, such implementation details are not necessary. In addition, some conventional structures and components are shown in simplified schematic form in the drawings for the sake of simplicity.
A preparation method of a triazole copper/polypyrrole composite electrode material comprises the following steps:
step 1: preparing triazole copper powder:
step 1-1: 0.3964 g of 3, 5-diamino-1, 2, 3-triazole and 0.4832 g of copper nitrate trihydrate are dissolved in 50 mL of deionized water;
step 1-2: rapidly stirring the mixed solution in the step 1-1 at room temperature for 12 hours;
step 1-3: after the mixed solution in the step 1-2 is reacted, filtering the green precipitate, and washing for several times by using deionized water and ether in sequence;
step 1-4: finally, vacuum drying the mixed solution washed in the step 1-3 at 60 ℃ to obtain triazole copper powder;
step 2: preparation of polypyrrole powder:
step 2-1: adding 0.6 g of pyrrole monomer with the purity of 99.0% into 50 mL of deionized water, and stirring for 10 min;
step 2-2: 2 g of ammonium persulfate is added into the solution obtained in the step 2-1, and the mixture is stirred for 12 hours at the temperature of 0 ℃;
step 2-3: collecting the precipitate, washing with deionized water and ethanol respectively, and drying in an oven for 12 h to obtain polypyrrole powder;
and 3, step 3: preparing a triazole copper/polypyrrole composite electrode material: dissolving the triazole copper powder prepared in the step 1 in 15mL of ethanol to form a triazole copper solution; and (3) adding the polypyrrole powder prepared in the step (2) into a 50 mL beaker, placing the beaker into a constant-temperature water bath kettle for magnetic stirring, dropwise adding a copper triazole solution to obtain a uniform mixed solution of copper triazole and polypyrrole, and after the solution is completely evaporated, placing the mixed solution into a 60 ℃ oven for drying for 12 hours to obtain copper triazole/polypyrrole composite electrode material powder.
Example 1
The invention relates to a preparation method of a triazole copper/polypyrrole composite electrode material, which specifically comprises the following steps:
Step 3, preparing the triazole copper/polypyrrole composite electrode material: 10 mg of copper triazole powder is dissolved in 15mL of ethanol to form a copper triazole solution. And adding 10 mg of PPY powder into a 50 mL beaker, placing the beaker in a 50 ℃ constant-temperature water bath kettle, performing magnetic stirring for 6 hours, dropwise adding a copper triazole solution to obtain a uniform mixed solution of copper triazole and PPY, and after the solution is completely evaporated, placing the mixed solution into a 60 ℃ oven for drying for 12 hours to obtain the copper triazole/polypyrrole composite electrode material powder.
The triazole copper/polypyrrole composite electrode material prepared by the method has high yield and excellent chemical stability and conductivity. FIG. 1 is a schematic diagram of a triazole copper powder. Fig. 2 is a scanning electron microscope image of the copper triazole/polypyrrole composite electrode material, and it can be observed that PPY is coated on the surface of the copper triazole. FIG. 3 is a spectrum diagram of N1 s of the triazole copper/polypyrrole composite electrode material, and it can be seen that the diffraction peaks at 398.82 eV, corresponding to = N-bond in PPY, and at 399.27 eV and 400.42 eV, respectively, correspond to N-H/C-N-C and C-N-C bonds of the triazole ring in triazole copper. In addition, the characteristic peak at 397.67 eV is attributed to the metal complex bond Cu-N bond in the copper triazole.
Fig. 4 to 7 are the electrochemical performance characterization diagrams of the triazole copper/polypyrrole composite electrode material obtained in this example. Mixing copper triazole/polypyrrole, carbon black and PVDF in a proportion of 5:4:1, coating the carbon paper on the carbon paper, and performing electrochemical test on the carbon paper in sulfuric acid electrolyte, wherein the result shows that the triazole copper/polypyrrole composite electrode has excellent electrochemical performance. It can be seen from the CV curve in fig. 4 that the material has three pairs of distinct redox peaks, corresponding one-to-one to the charge and discharge plateaus of the GCD curve (fig. 5). In addition, the electrode was at 1 Ag -1 At a current density of (2), the initial discharge capacity is as high as 180.8 mAh g -1 . FIG. 6 shows the excellent rate capability of the material, at 50 Ag -1 The discharge capacity is still kept at 72.9 mAh g under the current density of (2) -1 . It is observed from the long cycle curve of fig. 7 that the capacity retention rate exceeds 100% after 7000 charge and discharge cycles. FIG. 8 shows the triazole copper/polypyrrole composite electrode materials with different proportions, which are prepared under the condition of constant temperature water bath at 50 ℃, and the current density is 1A g -1 And comparing specific capacity. As can be seen from the figure, when the copper triazole: when PPY =1, the specific capacity of the obtained triazole copper/polypyrrole composite electrode material is the highest, and the electrochemical performance is the best.
Example 2
The preparation method comprises the following steps:
Step 2: 0.6 g of 99.0% pure pyrrole monomer was added to 50 mL of deionized water and stirred for 10 min. Adding 2 g of ammonium persulfate, and stirring at 0 ℃ for 12 h; and after full reaction, collecting precipitate, washing the precipitate by using deionized water and ethanol in sequence, and drying the precipitate in an oven for 12 hours to obtain PPY powder.
Step 3, preparing the triazole copper/polypyrrole composite electrode material: 10 mg of copper triazole powder is dissolved in 15mL of ethanol to form a copper triazole solution. Adding 15 mg of PPY powder into a 50 mL beaker, placing the beaker in a 50-DEG C constant-temperature water bath kettle, performing magnetic stirring for 6 hours, dropwise adding a copper triazole solution to obtain a uniform mixed solution of copper triazole and PPY, and after the solution is completely evaporated, placing the mixed solution into a 60-DEG C oven for drying for 12 hours to obtain copper triazole/polypyrrole composite electrode material powder.
Example 3
The preparation method comprises the following steps:
Step 2: 0.6 g of 99.0% pure pyrrole monomer was added to 50 mL of deionized water and stirred for 10 min. Adding 2 g of ammonium persulfate, and stirring at 0 ℃ for 12 h; and after full reaction, collecting precipitate, washing the precipitate by using deionized water and ethanol in sequence, and drying the precipitate in an oven for 12 hours to obtain PPY powder.
Step 3, preparing the triazole copper/polypyrrole composite electrode material: 15 mg of copper triazole powder is dissolved in 15mL of ethanol to form a copper triazole solution. And adding 10 mg of PPY powder into a 50 mL beaker, placing the beaker in a 50-DEG C constant-temperature water bath kettle, performing magnetic stirring for 6 hours, dropwise adding a copper triazole solution to obtain a uniform mixed solution of copper triazole and PPY, and after the solution is completely evaporated, placing the mixed solution into a 60-DEG C oven for drying for 12 hours to obtain copper triazole/polypyrrole composite electrode material powder.
Example 4
The preparation method comprises the following steps:
Step 2: 0.6 g of pyrrole monomer having a purity of 99.0% was added to 50 mL of deionized water and stirred for 10 min. Adding 2 g of ammonium persulfate, and stirring at 0 ℃ for 12 h; after sufficient reaction, the precipitate was collected, washed with deionized water and ethanol in order, and dried in an oven overnight to give a PPY powder.
Step 3, preparing the triazole copper/polypyrrole composite electrode material: 10 mg of copper triazole powder is dissolved in 15mL of ethanol to form a copper triazole solution. And adding 20 mg of PPY powder into a 50 mL beaker, placing the beaker in a 50-DEG C constant-temperature water bath kettle, performing magnetic stirring for 6 hours, dropwise adding a copper triazole solution to obtain a uniform mixed solution of copper triazole and PPY, and after the solution is completely evaporated, placing the mixed solution into a 60-DEG C oven for drying for 12 hours to obtain copper triazole/polypyrrole composite electrode material powder.
Example 5
The preparation method comprises the following steps:
Step 2: 0.6 g of 99.0% pure pyrrole monomer was added to 50 mL of deionized water and stirred for 10 min. Adding 2 g of ammonium persulfate, and stirring at 0 ℃ for 12 h; and after full reaction, collecting precipitate, washing the precipitate by using deionized water and ethanol in sequence, and drying the precipitate in an oven for 12 hours to obtain PPY powder.
Step 3, preparing the triazole copper/polypyrrole composite electrode material: 20 mg of copper triazole powder is dissolved in 15mL of ethanol to form a copper triazole solution. And adding 10 mg of PPY powder into a 50 mL beaker, placing the beaker in a 50-DEG C constant-temperature water bath kettle, performing magnetic stirring for 6 hours, dropwise adding a copper triazole solution to obtain a uniform mixed solution of copper triazole and PPY, and after the solution is completely evaporated, placing the mixed solution into a 60-DEG C oven for drying for 12 hours to obtain the copper triazole/polypyrrole composite electrode material powder.
Example 6
The preparation method comprises the following steps:
Step 2: 0.6 g of 99.0% pure pyrrole monomer was added to 50 mL of deionized water and stirred for 10 min. Adding 2 g of ammonium persulfate, and stirring at 0 ℃ for 12 h; and after full reaction, collecting precipitate, washing the precipitate by using deionized water and ethanol in sequence, and drying the precipitate in an oven for 12 hours to obtain PPY powder.
Step 3, preparing the triazole copper/polypyrrole composite electrode material: 10 mg of copper triazole powder is dissolved in 15mL of ethanol to form a copper triazole solution. And adding 10 mg of PPY powder into a 50 mL beaker, placing the beaker in a constant-temperature water bath kettle at 40 ℃ for magnetic stirring for 6 hours, dropwise adding a copper triazole solution to obtain a uniform mixed solution of copper triazole and PPY, and after the solution is completely evaporated, placing the mixed solution into a 60 ℃ oven for drying for 12 hours to obtain the copper triazole/polypyrrole composite electrode material powder.
Example 7
The preparation method comprises the following steps:
Step 2: 0.6 g of 99.0% pure pyrrole monomer was added to 50 mL of deionized water and stirred for 10 min. 2 g of ammonium persulfate is added and stirred for 12 hours at the temperature of 0 ℃; and after full reaction, collecting precipitate, washing the precipitate by using deionized water and ethanol in sequence, and drying the precipitate in an oven for 12 hours to obtain PPY powder.
Step 3, preparing the triazole copper/polypyrrole composite electrode material: 10 mg of copper triazole powder is dissolved in 15mL of ethanol to form a copper triazole solution. And adding 10 mg of PPY powder into a 50 ml beaker, placing the beaker in a constant-temperature water bath kettle at 60 ℃ for magnetic stirring for 6 hours, dropwise adding a copper triazole solution to obtain a uniform mixed solution of copper triazole and PPY, and after the solution is completely evaporated, placing the mixed solution into a 60 ℃ oven for drying for 12 hours to obtain the copper triazole/polypyrrole composite electrode material powder.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. However, the above description is only an example of the present invention, and the technical features of the present invention are not limited thereto, and other embodiments that can be made by those skilled in the art without departing from the technical scope of the present invention should be covered by the claims of the present invention.
Claims (9)
1. A preparation method of a triazole copper/polypyrrole composite electrode material is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1: preparing copper triazole powder;
step 2: preparing polypyrrole powder;
and step 3: preparing a triazole copper/polypyrrole composite electrode material: dissolving the triazole copper powder prepared in the step 1 in ethanol to form a triazole copper solution; and (3) adding the polypyrrole powder prepared in the step (2) into a beaker, placing the beaker into a constant-temperature water bath kettle for magnetic stirring, dropwise adding a copper triazole solution to obtain a uniform mixed solution of copper triazole and polypyrrole, and after the solution is completely evaporated, placing the mixed solution into a 60 ℃ oven for drying for 12 hours to obtain the copper triazole/polypyrrole composite electrode material powder.
2. The preparation method of the triazole copper/polypyrrole composite electrode material according to claim 1, characterized in that: the mass ratio of the triazole copper to the polypyrrole in the triazole copper/polypyrrole mixed solution prepared in the step 3 is as follows: triazole copper: polypyrrole =1-2:1-2.
3. The preparation method of the triazole copper/polypyrrole composite electrode material according to claim 1, characterized in that: the weight of the triazole copper powder in the step 3 is 10-20 mg.
4. The preparation method of the triazole copper/polypyrrole composite electrode material according to claim 1, characterized in that: the temperature of the constant-temperature water bath in the step 3 is 40-60 ℃.
5. The preparation method of the triazole copper/polypyrrole composite electrode material according to claim 1, characterized in that: the preparation of the triazole copper powder in the step 1 comprises the following steps:
step 1-1: 0.3964 g of 3, 5-diamino-1, 2, 3-triazole and 0.4832 g of copper nitrate trihydrate are dissolved in 50 mL of deionized water;
step 1-2: rapidly stirring the mixed solution in the step 1-1 at room temperature for 12 hours;
step 1-3: after the mixed solution in the step 1-2 is reacted, filtering the green precipitate, and washing for several times by using deionized water and ether in sequence;
step 1-4: and finally, drying the mixed solution washed in the step 1-3 in vacuum at the temperature of 60 ℃ to obtain the triazole copper powder.
6. The preparation method of the triazole copper/polypyrrole composite electrode material according to claim 1, characterized by comprising the following steps: the preparation of polypyrrole powder in step 2 comprises the following steps:
step 2-1: adding 0.6 g of pyrrole monomer with the purity of 99.0% into 50 mL of deionized water, and stirring for 10 min;
step 2-2: 2 g of ammonium persulfate is added into the solution obtained in the step 2-1, and the mixture is stirred for 12 hours at the temperature of 0 ℃;
step 2-3: and collecting precipitates, washing the precipitates respectively by using deionized water and ethanol, and putting the precipitates into an oven to be dried for 12 hours to obtain polypyrrole powder.
7. The preparation method of the triazole copper/polypyrrole composite electrode material according to claim 1, characterized in that: and 3, dissolving the triazole copper powder prepared in the step 1 in 15mL of ethanol.
8. The triazole copper/polypyrrole composite electrode material obtained by the preparation method of the triazole copper/polypyrrole composite electrode material according to any one of claims 1-7 is characterized in that: the triazole copper/polypyrrole composite electrode material is formed by compounding triazole copper powder and polypyrrole powder.
9. The application of the triazole copper/polypyrrole composite electrode material according to claim 8 in water-based batteries, super capacitors or energy storage devices.
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| US20160055984A1 (en) * | 2014-08-21 | 2016-02-25 | Council Of Scientific & Industrial Research | P-toluenesulfonate doped polypyrrole/carbon composite electrode and a process for the preparation thereof |
| CN108172412A (en) * | 2017-12-24 | 2018-06-15 | 桂林理工大学 | The preparation method of polypyrrole/nickel hydroxide composite electrode material for super capacitor |
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| US20160055984A1 (en) * | 2014-08-21 | 2016-02-25 | Council Of Scientific & Industrial Research | P-toluenesulfonate doped polypyrrole/carbon composite electrode and a process for the preparation thereof |
| CN108172412A (en) * | 2017-12-24 | 2018-06-15 | 桂林理工大学 | The preparation method of polypyrrole/nickel hydroxide composite electrode material for super capacitor |
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| 潘慧玲;吕梦婕;戴秋维;郭燕妮;刘刚;高林枫;章霞飞;戴国梁;: "一种新型三氮唑及其铜配合物的合成与表征", 广州化工, no. 08 * |
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