CN110491686A - A kind of preparation method and application of bimetallic organic coordination compounds electrode material - Google Patents
A kind of preparation method and application of bimetallic organic coordination compounds electrode material Download PDFInfo
- Publication number
- CN110491686A CN110491686A CN201910801878.8A CN201910801878A CN110491686A CN 110491686 A CN110491686 A CN 110491686A CN 201910801878 A CN201910801878 A CN 201910801878A CN 110491686 A CN110491686 A CN 110491686A
- Authority
- CN
- China
- Prior art keywords
- electrode material
- coordination compounds
- organic coordination
- bimetallic organic
- stainless
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic System
- C07F15/04—Nickel compounds
- C07F15/045—Nickel compounds without a metal-carbon linkage
-
- 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
-
- 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
-
- 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 present invention relates to a kind of preparation method and application of bimetallic organic coordination compounds electrode material.Its preparation step is as follows: stainless (steel) wire being cut into the square of the cm size of 1cm × 1 first, the stainless (steel) wire cut out is placed in dehydrated alcohol and is impregnated.Weigh a certain amount of Co (CH3COO)2·4H2O and NiCl2·6H2O is dissolved into 30.0 mL toluene, stirs to get the mixed solution of the two；A certain amount of terephthalic acid (TPA) is added to mixed solution, stirring is transferred in 50 mL stainless steel cauldrons, the stainless (steel) wire that it is obtained with processing 120 to being completely dissolvedo15 h are reacted under conditions of C, and obtained product is filtered, it is multiple using ethyl alcohol centrifuge washing, oven drying is put into get bimetallic organic coordination compounds electrode material is arrived.Preparation process of the present invention is simple, and yield is higher, and the bimetallic organic coordination compounds electrode material being prepared has many advantages, such as stable structure, electrochemical performance, is highly suitable as electrode material applied to supercapacitor field.
Description
Technical field
The invention belongs to new energy technical field of electronic materials, are related to a kind of bimetallic organic coordination compounds electrode material
Preparation method and application.
Background technique
In recent years, the design of organometallic complex (MOF), synthesize and apply current chemical field research in
It receives significant attention.They not only have rich and varied topological structure, but also often show peculiar optically nonlinearity,
Fluorescence, magnetism and electrochemical energy storage etc..The emphasis of many work be by control ligand and metal ion come design with
Complex is synthesized, as Liao et al. utilizes isonicotinic acid and Ni (NO3)2A series of Ni-MOF materials are prepared, are swept in 5 mV/s
It retouches under rate, maximum specific capacitance is 634 F/g(Electrochemical Performance of Metal Organic
Framework Synthesized by a Solvothermal Method for Supercapacitors [J].
Microporousand Mesoporous Materials, 2013,171:53-57.)；Lee et al. utilizes Co (NO3)2With
Terephthalic acid (TPA) is 100o50 h are reacted in the n,N-Dimethylformamide of C, another Co-MOF is prepared, in 1 mol/L
In LiOH electrolyte, the specific capacity under 0.6 A/g current density can reach 206.76 F/g, and the good (Unusual of cyclicity
energy storage and charge retention in Co-based metal-organic-frameworks [J].
Microporous and Mesoporous Materials, 2012,153:163-165.).But the big portion reported at present
The active site for dividing MOF based super capacitor electrode material to have the disadvantage in that (1) single metal-coordinating atoms provide has
Limit, causes the specific capacitance value of material smaller；(2) load capacity of active material is lower on electrode slice, limits it in supercapacitor
The practical application in field.For these problems, it is believed that it is more to provide to need to prepare bimetallic organic coordination compounds
Active site, so that the specific capacitance of electrode material is improved, but up to the present, such research is rarely reported.
Summary of the invention
In view of the deficiencies of the prior art, the bimetallic high the present invention provides a kind of specific capacitance height, active material load capacity
The preparation method of organic coordination compounds electrode material.
Technical scheme is as follows:
A kind of preparation method of bimetallic organic coordination compounds electrode material, the specific steps are as follows:
(1) stainless (steel) wire is cut into the square of the cm size of 1 cm × 1 first, the stainless (steel) wire cut out is placed in nothing
It is impregnated in water-ethanol；
(2) 0.1 ~ 1.5 g Co (CH is weighed3COO)2·4H2O and 0.1 ~ 1.5 g NiCl2·6H2O is dissolved into 30.0 mL first
In benzene, uniform solution is stirred to get；
(3) 0.1 ~ 1.0 g terephthalic acid (TPA) is added in mixed solution in step (2), and stirring is to being completely dissolved；
(4) mixed solution and step (1) that step (3) obtains are handled into obtained stainless (steel) wire, is transferred to 50 mL stainless steels
In reaction kettle, 80 ~ 120o15 ~ 48 h are reacted under conditions of C；
(5) product that step (4) obtains is filtered, it is multiple using ethyl alcohol centrifuge washing, it is put into 8 h of oven drying and obtains
A kind of bimetallic organic coordination compounds electrode material.
, according to the invention it is preferred to, Co (CH described in step (2)3COO)2·4H2The dosage of O is 0.76 g.
, according to the invention it is preferred to, NiCl described in step (2)2·6H2The dosage of O is 0.38 g.
, according to the invention it is preferred to, the dosage of terephthalic acid (TPA) described in step (3) is 0.43 g.
, according to the invention it is preferred to, the reaction time described in step (4) is 15 h.
, according to the invention it is preferred to, reaction temperature described in step (4) is 120oC。
A kind of bimetallic organic coordination compounds electrode material, the electrode material for supercapacitor.
Technical advantage of the invention is as follows:
(1) preparation process of the present invention is simple, and yield is higher, load capacity height (15 mg/cm of active material on electrode slice2), it can be with
By controlling the ratio of ligand and metal ion, the preferable electrode material of chemical property is prepared.
(2) a kind of bimetallic organic coordination compounds electrode material is prepared in the present invention, and bimetallic ion can provide
More active sites are highly suitable as electrode material so that material has many advantages, such as that electrochemical performance, specific capacitance are high
Material is applied to supercapacitor field.
Detailed description of the invention
Fig. 1 is the constant current charge-discharge figure of bimetallic organic coordination compounds electrode material made from the embodiment of the present invention 1.
Fig. 2 is the cyclic voltammogram of bimetallic organic coordination compounds electrode material made from the embodiment of the present invention 1.
Fig. 3 is the constant current charge-discharge figure of bimetallic organic coordination compounds electrode material made from comparative example of the present invention.
Specific embodiment
The present invention is described further with attached drawing combined with specific embodiments below, but not limited to this.
Experimental method described in following embodiments is unless otherwise specified conventional method simultaneously；The reagent and material
Material, unless otherwise specified, commercially obtains.
Embodiment 1:
Stainless (steel) wire is cut into the square of the cm size of 1 cm × 1 first, the stainless (steel) wire cut out is placed in anhydrous second
It is impregnated in alcohol, weighs 0.76 g Co (CH3COO)2·4H2O and 0.38 g NiCl2·6H2O is dissolved into 30.0 mL toluene, is stirred
It mixes to obtain uniform solution；0.43 g terephthalic acid (TPA) is added to mixed solution, stirs to being completely dissolved, it is obtained with processing
Stainless (steel) wire, be transferred in 50 mL stainless steel cauldrons, 120o15 h are reacted under conditions of C, by obtained product into
Row filters, multiple using ethyl alcohol centrifuge washing, is put into 8 h of oven drying to get electric to a kind of bimetallic organic coordination compounds
Pole material.
A kind of constant current charge-discharge figure of bimetallic organic coordination compounds electrode material is made in the present embodiment, such as Fig. 1 institute
Show.
A kind of bimetallic organic coordination compounds electrode material is made in the present embodiment, using three-electrode system, with 3.0
Mol/L KOH solution is electrolyte, and measuring specific capacitance value in 0.5 A/g is 3165 F/g, and specific capacitance value when 1 A/g is 2914
It is 1852 F/g that F/g, 10 A/g, which measure specific capacitance,.
Embodiment 2:
Stainless (steel) wire is cut into the square of the cm size of 1cm × 1 first, the stainless (steel) wire cut out is placed in anhydrous second
It is impregnated in alcohol, weighs 0.76 g Co (CH3COO)2·4H2O and 0.76 g NiCl2·6H2O is dissolved into 30.0 mL toluene, is stirred
It mixes to obtain uniform mixed solution；0.43 g terephthalic acid (TPA) is added to mixed solution, stirs to being completely dissolved, by itself and processing
Obtained stainless (steel) wire is transferred in 50 mL stainless steel cauldrons, 105o20 h are reacted under conditions of C, the production that will be obtained
Object is filtered, multiple using ethyl alcohol centrifuge washing, is put into 8 h of oven drying to get a kind of bimetallic organic coordination chemical combination is arrived
Object electrode material.
Using three-electrode system, using 3.0 mol/L KOH solutions as electrolyte, measuring specific capacitance value in 0.5 A/g is
Specific capacitance value when 3135 F/g, 1 A/g is 2971 F/g, and it is 1140 F/g that 10 A/g, which measure specific capacitance,.
Embodiment 3:
Stainless (steel) wire is cut into the square of the cm size of 1 cm × 1 first, the stainless (steel) wire cut out is placed in anhydrous second
It is impregnated in alcohol, weighs 0.38 g Co (CH3COO)2·4H2O and 0.76 g NiCl2·6H2O is dissolved into 30.0 mL toluene, is stirred
It mixes to obtain uniform mixed solution；0.43 g terephthalic acid (TPA) is added to mixed solution, stirs to being completely dissolved, by itself and processing
Obtained stainless (steel) wire is transferred in 50 mL stainless steel cauldrons, 105o24 h are reacted under conditions of C, the production that will be obtained
Object is filtered, multiple using ethyl alcohol centrifuge washing, is put into 8 h of oven drying to get a kind of bimetallic organic coordination chemical combination is arrived
Object electrode material.
Using three-electrode system, using 3.0 mol/L KOH solutions as electrolyte, measuring specific capacitance value in 0.5 A/g is
Specific capacitance value when 2930 F/g, 1 A/g is 2840 F/g, and it is 1320 F/g that 10 A/g, which measure specific capacitance,.
Embodiment 4:
Stainless (steel) wire is cut into the square of the cm size of 1 cm × 1 first, the stainless (steel) wire cut out is placed in anhydrous second
It is impregnated in alcohol, weighs 0.76 g Co (CH3COO)2·4H2O and 0.38 g NiCl2·6H2O is dissolved into 30.0 mL toluene, is stirred
It mixes to obtain uniform mixed solution；0.43 g terephthalic acid (TPA) is added to mixed solution, stirs to being completely dissolved, by itself and processing
Obtained stainless (steel) wire is transferred in 50 mL stainless steel cauldrons, 120o24 h are reacted under conditions of C, the production that will be obtained
Object is filtered, multiple using ethyl alcohol centrifuge washing, is put into 8 h of oven drying to get a kind of bimetallic organic coordination chemical combination is arrived
Object electrode material.
Using three-electrode system, using 3.0 mol/L KOH solutions as electrolyte, measuring specific capacitance value in 0.5 A/g is
Specific capacitance value when 2435 F/g, 1 A/g is 2285 F/g, and it is 1140 F/g that 10 A/g, which measure specific capacitance,.
Comparative example
This comparative example is in solvent thermal reaction, and reaction temperature is 130 DEG C, and for remaining step with embodiment 1, what is obtained is bimetallic
Organic coordination compounds electrode material.
As seen from Figure 3, the bimetallic organic coordination compounds electrode material of this comparative example preparation carries out constant current charge-discharge
Test.Its specific capacitance value in 1 A/g is 1655 F/g, has lower specific capacitance value, and the disadvantage that high rate performance is poor.
Embodiment the result shows that, preparation method of the present invention is simple, bimetallic organic coordination compounds electrode material obtained
Material has many advantages, such as that specific capacitance value is high, load capacity is big, high rate performance is preferable.
Claims (7)
1. a kind of bimetallic organic coordination compounds electrode material, comprises the following steps that
(1) stainless (steel) wire is cut into the square of the cm size of 1 cm × 1 first, the stainless (steel) wire cut out is placed in nothing
It is impregnated in water-ethanol；
(2) 0.1 ~ 1.5 g Co (CH is weighed3COO)2·4H2O and 0.1 ~ 1.5 g NiCl2·6H2O is dissolved into 30.0 mL toluene
In, stir to get uniform mixed solution；
(3) 0.1 ~ 1.0 g terephthalic acid (TPA) is added in mixed solution in step (2), and stirring is to being completely dissolved；
(4) mixed solution and step (1) that step (3) obtains are handled into obtained stainless (steel) wire, is transferred to 50 mL polytetrafluoros
In the stainless steel cauldron of vinyl liner, 80 ~ 120o15 ~ 48 h are reacted under conditions of C；
(5) product that step (4) obtains is filtered, it is multiple using ethyl alcohol centrifuge washing, it is put into 8 h of oven drying and obtains
A kind of bimetallic organic coordination compounds electrode material.
2. bimetallic organic coordination compounds electrode material according to claim 1, which is characterized in that in step (2)
Co(CH3COO)2·4H2The dosage of O is 0.76 g.
3. bimetallic organic coordination compounds electrode material according to claim 1, which is characterized in that in step (2)
NiCl2·6H2The dosage of O is 0.38 g.
4. bimetallic organic coordination compounds electrode material according to claim 1, which is characterized in that in step (3)
The dosage of terephthalic acid (TPA) is 0.43 g.
5. bimetallic organic coordination compounds electrode material according to claim 1, which is characterized in that institute in step (4)
The reaction time stated is 15 h.
6. bimetallic organic coordination compounds electrode material according to claim 1, which is characterized in that institute in step (4)
The reaction temperature stated is 120oC。
7. a kind of bimetallic organic coordination compounds electrode material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910801878.8A CN110491686A (en) | 2019-08-28 | 2019-08-28 | A kind of preparation method and application of bimetallic organic coordination compounds electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910801878.8A CN110491686A (en) | 2019-08-28 | 2019-08-28 | A kind of preparation method and application of bimetallic organic coordination compounds electrode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110491686A true CN110491686A (en) | 2019-11-22 |
Family
ID=68554769
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910801878.8A Pending CN110491686A (en) | 2019-08-28 | 2019-08-28 | A kind of preparation method and application of bimetallic organic coordination compounds electrode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110491686A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011132147A1 (en) * | 2010-04-21 | 2011-10-27 | Basf Se | Novel metal-organic frameworks as electrode material for lithium ion accumulators |
| CN104992848A (en) * | 2015-06-30 | 2015-10-21 | 中国地质大学（武汉） | Binary metal organic framework material applied to super capacitor and preparation method for binary metal organic framework material |
| CN109166733A (en) * | 2018-09-30 | 2019-01-08 | 北京印刷学院 | A kind of method that hydro-thermal method prepares Ni/Co base MOF material |
| CN109553779A (en) * | 2018-11-20 | 2019-04-02 | 三峡大学 | A kind of preparation method and application of three-dimensional manometer flower metal-organic framework material |
| CN109867780A (en) * | 2019-03-05 | 2019-06-11 | 北京化工大学 | It is a kind of to keep the organic polymer of MOFs pattern, preparation method and application |
-
2019
- 2019-08-28 CN CN201910801878.8A patent/CN110491686A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011132147A1 (en) * | 2010-04-21 | 2011-10-27 | Basf Se | Novel metal-organic frameworks as electrode material for lithium ion accumulators |
| CN104992848A (en) * | 2015-06-30 | 2015-10-21 | 中国地质大学（武汉） | Binary metal organic framework material applied to super capacitor and preparation method for binary metal organic framework material |
| CN109166733A (en) * | 2018-09-30 | 2019-01-08 | 北京印刷学院 | A kind of method that hydro-thermal method prepares Ni/Co base MOF material |
| CN109553779A (en) * | 2018-11-20 | 2019-04-02 | 三峡大学 | A kind of preparation method and application of three-dimensional manometer flower metal-organic framework material |
| CN109867780A (en) * | 2019-03-05 | 2019-06-11 | 北京化工大学 | It is a kind of to keep the organic polymer of MOFs pattern, preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| FEIFEI CAO等: "Hierarchical sheet-like Ni–Co layered double hydroxide derived from a MOF template for high-performance supercapacitors", 《SYNTHETIC METALS》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101913655B (en) | Method for preparing lithium manganate cathode material by microwave sintering | |
| CN104979104A (en) | Preparation method of Ni-MOF electrode material | |
| CN103825022B (en) | A kind of preparation method and its usage of lithium phosphate vanadium/carbon composite | |
| CN106904653B (en) | It the preparation method of vanadium dioxide nano material and is applied in magnesium chargeable battery | |
| CN103601756B (en) | Bismuth metal-organic framework material, preparation method and positive electode of lead battery additive thereof | |
| CN109256567A (en) | A kind of preparation method of transition metal/nitrogen doped corrugated carbon nanotube | |
| CN107739023A (en) | A kind of polyhedron bimetallic oxide and its production and use | |
| CN104064739A (en) | Tin cobalt alloy/ graphene composite material and preparation method thereof | |
| CN104998673A (en) | Nitrogen and sulfur co-doped carbon-loaded non-noble metal type oxygen reduction catalyst and preparation method thereof | |
| CN105931855B (en) | The synthesis of nitrogen sulphur codope carbon-polyaniline composite material and be applied to supercapacitor | |
| CN109256546A (en) | A kind of molybdenum disulfide/graphene composite material and its preparation method and application | |
| CN111342019B (en) | Tin-based metal-organic framework, preparation method thereof and application of tin-based metal-organic framework as negative electrode material of lithium ion battery | |
| CN106025178B (en) | It is a kind of to prepare the method for metal oxide and its application in lithium cell cathode material by template of MOF | |
| CN108199041A (en) | A kind of modified phosphate iron lithium material, preparation method and application | |
| CN105977486A (en) | Preparation method and application of sodium-rich transition metal silicate as sodium ion battery cathode material | |
| CN109449415A (en) | A kind of preparation method of manganese dioxide/mangano-manganic oxide laminar composite derived from MOF | |
| CN110980673A (en) | Metal phosphide, preparation method thereof and application thereof in super capacitor | |
| CN114438516B (en) | Preparation method of porous nickel-iron-based bimetallic organic framework electrocatalyst and application of porous nickel-iron-based bimetallic organic framework electrocatalyst in water oxidation reaction | |
| CN104361999A (en) | Carbon nano-tube @ nickel manganese core-shell heterostructure material, and preparation method and application thereof | |
| CN108948100A (en) | The preparation and application of two kinds of three-dimensional pseudorotaxane type polyacid Base Metal organic framework materials | |
| CN106340400B (en) | A kind of carbon coating rhombic system nano bar-shape Nb2O5Material and preparation method thereof | |
| CN104538633B (en) | Lithium ion battery electrode material and preparation method thereof | |
| CN109741959A (en) | A kind of graphene/iron-based MOF super capacitor material and preparation method thereof | |
| CN108598471A (en) | A kind of sodium-ion battery positive electrode containing cobalt and preparation method thereof | |
| CN108511741A (en) | A kind of preparation method of lithium rechargeable battery zinc oxide negative material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191122 |
|
| RJ01 | Rejection of invention patent application after publication |