CN107195473A - A kind of preparation method of two-dimentional club shaped structure vanadium metal organic backbone electrode material - Google Patents
A kind of preparation method of two-dimentional club shaped structure vanadium metal organic backbone electrode material Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 18
- 239000002184 metal Substances 0.000 title claims abstract description 18
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 18
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical class CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 22
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 20
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 20
- 239000011734 sodium Substances 0.000 claims abstract description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 claims abstract description 17
- 239000007790 solid phase Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- 125000005287 vanadyl group Chemical group 0.000 claims description 2
- 235000021050 feed intake Nutrition 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 239000003990 capacitor Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000010992 reflux Methods 0.000 abstract description 2
- 239000012621 metal-organic framework Substances 0.000 description 14
- 239000003921 oil Substances 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 230000005518 electrochemistry Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 230000006399 behavior Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- BMOFLINJXRPQCY-UHFFFAOYSA-N gold vanadium Chemical compound [V].[Au] BMOFLINJXRPQCY-UHFFFAOYSA-N 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical class CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- KZNFRTXTQCISLO-UHFFFAOYSA-N oxovanadium;sulfuric acid Chemical compound [V]=O.OS(O)(=O)=O KZNFRTXTQCISLO-UHFFFAOYSA-N 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/84—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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
A kind of preparation method of two-dimentional club shaped structure vanadium metal organic backbone electrode material, belongs to the production technical field of electrode material for super capacitor.The para-phthalic sodium of the vanadic sulfate of preheating and preheating is dissolved in N, N dimethylformamides, then mixture is heated into backflow to be reacted, the solid phase that negating to generate is dried in vacuo after being washed with methanol, obtains two-dimentional club shaped structure vanadium metal organic backbone electrode material.The present invention is using the method for being easily heated to reflux synthesis, and raw material is easy to get, equipment cost is cheap, simple to operate, time-consuming short.Compared with prior art, preparation method is simple, it is adaptable to mass produce, while prepared material possesses good cyclical stability.
Description
Technical field
The invention belongs to the production technical field of electrode material for super capacitor.
Background technology
The energy be the mankind depend on for existence, society and sustainable economic development material base.In recent years, with society and warp
The high speed development of Ji, people increasingly increase the demand of the energy, consume and largely can not in the production, life process in the mankind
The fossil energy of regeneration, such as：Coal, oil, natural gas etc., while generating some poisonous, pernicious gases and greenhouse gases, are caused
Serious energy crisis and environmental problem so that the living environment of the mankind receive serious threat, society and it is economical can
Sustainable development is faced with formidable challenges.In face of the crisis that fossil energy is exhausted, find new alternative energy source and improve depositing for the energy
Storage and utilization ratio are as very urgent problem.
Ultracapacitor is a kind of novel energy memory device between battery and traditional capacitor, and traditional quiet
Electric capacitor is compared with battery, and ultracapacitor has fast power density height, charge-discharge velocity, good cycling stability, using temperature
Spend that scope is wide, safe, environment-friendly and the low feature of maintenance cost.Ultracapacitor is once appearance just by the wide of people
General concern, the application succeeded in numerous areas, such as：Serve as the electronic products such as memory stick, notebook computer, timer
Back-up source, the accessory power supply of main power source, solar cell as electronic toy.With electric automobile and oil electricity or pneumoelectric
The rise and development of hybrid vehicle research, ultracapacitor, with the use of composition composite power source, are answered with all kinds of electrokinetic cells
Used for the activation system of automobile, or directly as the electrical source of power of automobile.Total rule of ultracapacitor industry in 2009
About 27.5 hundred million dollars of mould, stopped according to estimation by 2014, and the every annual of market value of ultracapacitor is with 21.4% increasing rate.With
Continuing to develop for supercapacitor technologies, the market share of ultracapacitor also will constantly expand.
Metal organic framework represents a major class quantity, the multifarious material of the Nomenclature Composition and Structure of Complexes.Metal organic framework can be with
Compared with by cheap, prepared by the synthetic method of high yield under low temperature.Hydro-thermal solvent-thermal method is most common method, may be used also in addition
Synthesized by microwave, ultrasonic wave, electrochemistry and the method for diffusion.Metal organic framework can pass through relatively relatively inexpensive forerunner
It is prepared by body.The inorganic salts such as nitrate, sulfate and chlorate are used as typical metal ion presoma.Organic linker is typically adopted
With multiple tooth organic ligand, such as carboxylate, azole and nitrile.Among many synthesis, structure directing agent is often used in side
Construction unit is helped to assemble to form metal organic framework without participating among the structural formula of final compound.
Compared with the high-specific surface area of inorganic porous material, some metal organic frameworks show a kind of flexible structure, it
Can behave as dynamic behaviour, with external factor such as guest molecule, temperature, pressure etc. and change.Metal organic framework it is whole
Individual framework is that have coordinate bond or other weak mutual synergisms（Hydrogen bond, pi-pi bond, Van der Waals for）To support.Therefore,
Configuration flexibility is typically that in a mild condition, this condition can allow those metal organic frameworks to be adjusted according to external factor is reversible
The size of knothole gap.This flexibility separates for exploration catalysis, gas, medicament storage and transport, imaging are with sensing.Photoelectricity and energy
The performances such as source storage provide new possibility.Although the structure of metal organic framework, synthesis, property and the application in various fields
It was discussed in detail in many literature reviews, but their applications in electrochemical field are not also by play-by-play
Cross.The research of metal organic framework in this respect is just gradually spread out recently, the important application in electrochemistry be energy stores and
Conversion（Ultracapacitor, battery, fuel cell）, the reduction of high oxidation thing and toxic compounds.According to definition, electrochemistry is related to
And electronics is in the transfer and storage of electrode and electrolyte interface.Most of metal-organic framework materials are due to its weaker electric conductivity
Them can be made to exclude outside preferentially as electrode material and catalysis material.But metal organic framework is by successful conduct
The electrode material of rechargeable battery, also contemplates the method for overcoming their insulating property (properties)s.Metal organic framework internal metal ion
Redox behavior a kind of approach of electro transfer can be provided, the adjustment of polymeric inner bridge conjoined structure in addition may be led
Cause more preferable electro transfer.
So far, application of the metal organic framework in electrochemistry is main：1st, as the electrode material of battery, including
Do the positive pole of lithium ion battery, negative pole, the positive pole of lithium-sulfur cell；2nd, occur in fuel cell or electrolyzer certain is important
The elctro-catalyst of reaction；3rd, as electrode material for super capacitor etc..Above by metal-organic framework materials for super
Capacitor electrode material, but its high rate performance and cyclical stability need to be improved, therefore it is organic to prepare high performance metal
Skeleton electrode material has very big application value.
The content of the invention
It is an object of the invention to provide a kind of two-dimentional club shaped structure vanadium metal organic backbone electrode material for ultracapacitor
The preparation method of material.
The technical scheme is that：The para-phthalic sodium of the vanadic sulfate of preheating and preheating is dissolved in N, N- dimethyl methyls
Acid amides, is then heated to backflow by mixture and is reacted, the solid phase that negating to generate is dried in vacuo after being washed with methanol,
Obtain two-dimentional club shaped structure vanadium metal organic backbone electrode material.
The present invention is using the method for being easily heated to reflux synthesis, and raw material is easy to get, equipment cost is cheap, simple to operate, consumption
When it is short.Compared with prior art, preparation method is simple, it is adaptable to mass produce, while prepared material possesses good
Cyclical stability.The present invention is on the basis of using vanadium metal organic backbone high capacitance activity and high conductivity, by being formed
Two-dimentional club shaped structure carrys out increasing specific surface area, makes the product of acquisition and has outstanding super capacitor performance.In 0.5 A/g electric current
Under density, specific capacitance can reach 513 F/g；Under 10 A/g high current density, specific capacitance still can reach 425 F/g；1
Under A/g current density, by 10000 charge and discharge cycles, its capacity is original 92.8%.
Further, the temperature of the vanadic sulfate of preheating of the present invention is 80 DEG C.The para-phthalic sodium of the preheating
Temperature be 80 DEG C.At such a temperature, it can both ensure that vanadic sulfate and para-phthalic sodium were fully dried, sulphur can be ensured again
The chemical property of sour vanadyl and para-phthalic sodium does not change.And use the vanadic sulfate and para-phthalic sodium of drying can
To reduce the generation of the side reaction in follow-up anhydrous DMF system in heating response, reaction production is improved
Rate.
The molar ratio of the vanadic sulfate and para-phthalic sodium is 1: 1.Under conditions of the rate of charge, sulfuric acid oxygen
Vanadium and para-phthalic sodium meet atom economy, and abundant progress beneficial to reaction and two kinds of raw materials make full use of.
The total amount of the vanadic sulfate and para-phthalic sodium and the rate of charge of N,N-dimethylformamide be 1mmol: 5~
10 mL.Under conditions of the rate of charge, vanadic sulfate, para-phthalic sodium can be completely dissolved in DMF
In.
The mixing temperature of the reaction is 160 DEG C.Under the temperature conditionss, most useful for being formed, two-dimentional club shaped structure vanadium is golden
Belong to organic backbone.
Brief description of the drawings
Fig. 1 is the scanning electron microscope diagram of the two-dimentional club shaped structure vanadium metal organic backbone electrode material prepared.
Fig. 2 is the constant current charge-discharge diagram of the two-dimentional club shaped structure vanadium metal organic backbone electrode material prepared.
Fig. 3 is the stable circulation performance figure of the two-dimentional club shaped structure vanadium metal organic backbone electrode material prepared.
Embodiment
2nd, two-dimentional club shaped structure vanadium metal organic backbone electrode material is prepared：
Explanation：Medicine used in the present invention is commercially available prod or laboratory conventional medication.
Embodiment 1：Vanadic sulfate and para-phthalic sodium are heated 12 hours using preceding under conditions of 80 DEG C, will
2.0 mmol vanadic sulfate and 2.0 mmol para-phthalic sodium are added in round-bottomed flask, are subsequently added 20 mL N, N-
Dimethylformamide, oil bath heats the mixture to 160 DEG C, and back flow reaction 72 hours yellow solid phase occurs, by solid phase in solution
Repeatedly washed with methanol, then dried 12 hours under vacuum under conditions of 80 DEG C, obtain two-dimentional club shaped structure vanadium metal organic
Skeleton electrode material.
Embodiment 2：Vanadic sulfate and para-phthalic sodium are heated 12 hours using preceding under conditions of 80 DEG C, will
2.0 mmol vanadic sulfate and 2.0 mmol para-phthalic sodium are added in round-bottomed flask, are subsequently added 30 mL N, N-
Dimethylformamide, oil bath heats the mixture to 160 DEG C, and back flow reaction 72 hours yellow solid phase occurs, by solid phase in solution
Repeatedly washed with methanol, take solid phase to wash, dried under vacuum under conditions of 80 DEG C and obtain within 12 hours two-dimentional club shaped structure vanadium gold
Belong to organic backbone electrode material.
Embodiment 3：Vanadic sulfate and para-phthalic sodium are heated 12 hours using preceding under conditions of 80 DEG C, will
2.0 mmol vanadic sulfate and 2.0 mmol para-phthalic sodium are added in round-bottomed flask, are subsequently added 40 mL N, N-
Dimethylformamide, oil bath heats the mixture to 160 DEG C, and back flow reaction 72 hours yellow solid phase occurs, by solid phase in solution
Repeatedly washed with methanol, take solid phase to wash, dried under vacuum under conditions of 80 DEG C and obtain within 12 hours two-dimentional club shaped structure vanadium gold
Belong to organic backbone electrode material.
2nd, ultracapacitor is prepared：
Take two-dimentional club shaped structure vanadium metal organic backbone electrode material 80mg that each example of the above is made respectively with acetylene black 15mg, poly-
Tetrafluoroethene 5mg is mixed, and is carried out with mortar being fully ground mixing respectively, then dropwise addition 3~5mL isopropanols, by mixed solution
Carry out ultrasonically treated 10~15min.
Then mixed solution is uniformly added dropwise in three pieces of nickel foams respectively, tabletting after spontaneously drying 1~2 day obtains electricity
Pole piece sample.
Again respectively using three pieces of electrode samples as working electrode, using saturated calomel electrode as reference electrode, using platinum plate electrode as
To electrode, using 1mol/L metabisulfite solutions as electrolyte, assembling experiment ultracapacitor carries out constant current charge-discharge test.
The constant current charge-discharge of the two-dimentional club shaped structure vanadium metal organic backbone electrode material of preparation is as shown in Fig. 2 can by Fig. 2
See：The electrode material tests charge-discharge performance under 0.5,1,2,5 and 10 A/g current density, calculates obtained specific capacitance
The F/g of respectively 572,520,516,505 and 495.
The stable circulation performance of the two-dimentional club shaped structure vanadium metal organic backbone electrode material of preparation is as shown in figure 3, by Fig. 3
It can be seen that：Specific capacitance residue 92.8% after being circulated 10000 times under 1 A/g current density.
Claims (6)
1. a kind of preparation method of two-dimentional club shaped structure vanadium metal organic backbone electrode material, it is characterised in that：By the sulphur of preheating
Sour vanadyl and the para-phthalic sodium of preheating are dissolved in DMF, and mixture then is heated into backflow is carried out instead
Should, the solid phase that negating to generate is dried in vacuo after being washed with methanol, obtains two-dimentional club shaped structure vanadium metal organic backbone electrode
Material.
2. preparation method according to claim 1, it is characterised in that：The temperature of the vanadic sulfate of the preheating is 80 DEG C.
3. preparation method according to claim 1, it is characterised in that：The temperature of the para-phthalic sodium of the preheating is 80
℃。
4. preparation method according to claim 1, it is characterised in that：The vanadic sulfate and para-phthalic sodium feed intake
Mol ratio is 1: 1.
5. preparation method according to claim 4, it is characterised in that：The total amount of the vanadic sulfate and para-phthalic sodium
Rate of charge with N,N-dimethylformamide is 1mmol: 5~10 mL.
6. preparation method according to claim 1, it is characterised in that：The mixing temperature of the reaction is 160 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710627766.6A CN107195473B (en) | 2017-07-28 | 2017-07-28 | A kind of preparation method of two dimension club shaped structure vanadium metal organic backbone electrode material |
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| CN201710627766.6A CN107195473B (en) | 2017-07-28 | 2017-07-28 | A kind of preparation method of two dimension club shaped structure vanadium metal organic backbone electrode material |
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| CN107195473A true CN107195473A (en) | 2017-09-22 |
| CN107195473B CN107195473B (en) | 2018-12-11 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525121A (en) * | 2014-12-03 | 2015-04-22 | 浙江大学 | Adsorbent for olefin/alkane mixed gas separation and preparation method and application thereof |
-
2017
- 2017-07-28 CN CN201710627766.6A patent/CN107195473B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525121A (en) * | 2014-12-03 | 2015-04-22 | 浙江大学 | Adsorbent for olefin/alkane mixed gas separation and preparation method and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| FABIAN CARSON等: "Framework Isomerism in Vanadium Metal−Organic Frameworks:MIL-88B(V) and MIL-101(V)", 《CRYSTAL GROWTH & DESIGN》 * |
| KAREN LEUS等: "The coordinatively saturated vanadium MIL-47 as a low leaching heterogeneous catalyst in the oxidation of cyclohexene", 《JOURNAL OF CATALYSIS》 * |
| PASCAL VAN DER VOORT等: "Vanadium metal–organic frameworks: structures and applications", 《NEW JOURNAL OF CHEMISTRY》 * |
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