CN105977040B - A kind of metal organic framework electrode material of ultracapacitor and the preparation method of the electrode material - Google Patents
A kind of metal organic framework electrode material of ultracapacitor and the preparation method of the electrode material Download PDFInfo
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Abstract
The invention discloses a kind of metal organic framework electrode material of ultracapacitor and the preparation methods of the electrode material, the metal organic framework electrode material of the ultracapacitor is by two kinds of different transition metal ions, organic ligand is configured by certain mole, it is added to anhydrous N, it is mixed in N-dimethylformamide (DMF) organic solvent, bimetallic MOFs is obtained by the reaction through oil bath heating, and its structure is made to disintegrate, the wherein unstable MOFs of removal, to obtain another HP MOFs stablized, the HP MOFs are the organic backbone electrode material that can be used as high-performance super capacitor；Its advantage is that the material is high and with being layered porous, large specific surface area advantage with stability, and this method has technical process simple, is not necessarily to high temperature and pressure, and operability is strong, and material consumption is few, and yield is high, advantage at low cost.
Description
Technical field
The present invention relates to electrochemical technology fields, particularly with regard to the electrode material applied to ultracapacitor, tool
It is a kind of metal organic framework electrode material of ultracapacitor and the preparation method of the electrode material that body, which is said,.
Background technology
Ultracapacitor, also referred to as electrochemical capacitor are a kind of electrifications between traditional capacitor and secondary cell
Energy storage device is learned, capacity is up to hundreds of or even thousands of farads.Compared to current rechargeable battery, ultracapacitor have than
The outstanding advantages such as energy is high, specific power is high, operating temperature range is wide, service life length.Currently, ultracapacitor has been used as storage
Energy component is applied in hybrid-power bus, extended-range electric bus, fuel cell car, urban track traffic, pure electric vehicle
On automobile, mainly with other energy members parallel operations, the high power of vehicle launch demand is provided.For ultracapacitor, electricity
The effect of pole can not be substituted, and electrode material is the side such as specific surface area, conductivity and chemical stability at present
It is very urgent to improve electrode material in order to enhance the practicability of ultracapacitor for face.
Metal organic frame（MOFs）It is the material of the porous structure and function cut of novel nano occurred recently.
Under normal conditions, the aperture of MOFs materials is respectively less than 2 nm, is limiting their practical application down to a certain degree.Although
There are certain methods that can prepare the MOFs of larger hole, but it is porous to synthesize the layering with height structural controllability and stability
MOFs（HP-MOFs）It is still highly difficult.
Currently, not only limitation is single metal MOFs to metal organic frame, many bimetallic MOFs are successfully closed
At.For example, manganese (Mn)-cobalt (Co) bimetallic MOFs [New Journal of Chemistry, 2016,40 (6): 5531-
5536.] and nickel (Ni)-cobalt (Co) bimetallic MOFs [Advanced Functional Materials, 2016,26 (7):
1098-1103.] all it is successfully synthesized, and applied to absorption and lithium battery energy storage battery field.The bimetallic MOFs that the present invention synthesizes,
One of which MOFs relatively stablizes, and another MOFs is under certain condition（Acid, alkali or aqueous solution）Structure can disintegrate.Such as：
Although MOF-5 is stable in some solvents, water and acid can but lead to collapsing and decomposing for its structure, this is to be demonstrate,proved
Real [Physical Chemistry Chemical Physics, 2008,10 (32): 4732-4739].On the contrary, one
A little MOFs but have chemistry, heat and mechanical stability, as UiO-66 (Zr), even it can keep its structural stability to exist
In acid solution.It can synthesize bimetallic MOFs using these difference in stability, one of which made by certain condition
MOFs structures are disintegrated, to realize the purpose for increasing the apertures MOFs and surface area.
Invention content
One of the technical problem to be solved in the present invention is to provide a kind of organic backbone electrode material of ultracapacitor, should
Electrode material is a kind of transition metal organic backbone electrode material, with stability it is good and be layered porous, large specific surface area
Advantage.
The second technical problem to be solved by the present invention is to provide a kind of organic backbone electrode material of above-mentioned ultracapacitor
Preparation method.This method has technical process simple, is not necessarily to high temperature and pressure, and operability is strong, and material consumption is few, and yield is high, at
This low advantage.
One of technical solution of the invention：
A kind of organic backbone electrode material of ultracapacitor, which is characterized in that by two kinds of transition metal ions, You Jipei
Body is added to anhydrous n,N dimethylformamide (DMF) organic solvent by being that 1 ︰, 0.1 ~ 5 ︰ 0.5 ~ 10 are configured in molar ratio
Middle mixing, is added in anhydrous n,N dimethylformamide organic solvent and mixes, and above two mistake is obtained by the reaction through oil bath heating
The bimetallic MOFs of metal is crossed, and its structure is made to disintegrate, the wherein unstable MOFs of removal, to obtain another stabilization
HP-MOFs, which is that can be used for the organic backbone electrode material of high-performance super capacitor.
As a preferred embodiment of the above technical solution,
Two kinds of transition metal ions are preferable over Zn-Zr, Fe-Zr, Ni-Zr, Mn-Zr, Zn-Co, Fe-Co, Mn-Co
One group in each combination.
The organic ligand is terephthalic acid (TPA), phthalic acid, benzoic acid, trimesic acid and its derivative or two
Methylimidazole and its derivative.
The two of technical solution of the invention：
The preparation method of the organic backbone electrode material of above-mentioned ultracapacitor, specifically includes following steps：
1. be 1 ︰, 0.1 ~ 5 ︰ 0.5 ~ 10 according to molar ratio, weigh respectively two kinds of different transition metal ions metal salt and
Two kinds of transition metal salts and organic ligand are added to anhydrous n,N dimethylformamide by organic ligand（DMF）In and through ultrasound
Wave processing, flask is transferred to by solution after supersound process, in 80 DEG C ~ 200 DEG C 12 ~ 48h of constant temperature oil bath heating reaction；
2. being cooled to room temperature, acquired solution is centrifuged, anhydrous n,N dimethylformamide is used in combination（DMF）It is clear with acetone
It washes several times, obtains bimetallic mixing MOFs；
3. above-mentioned bimetallic mixing MOFs is placed in the strong acid of pH=1,30 ~ 60min of stirring makes it through centrifuging, washing
Structure is disintegrated, vacuum dried to obtain HP-MOFs after the wherein unstable MOFs of removal, which is that can be used as
The organic backbone electrode material of high-performance super capacitor.
Compared with prior art, the present invention has the following advantages：
1. layering Porous transition metal organic backbone electrode material of the present invention, which has, is layered porous, specific surface area
Big advantage, specific surface area is up to 874 m2/g。
2. bath oiling of the present invention is simple and practical, it is not necessarily to high temperature and pressure.
3. the transition metal organic framework material prepared by the present invention is used as electrode material for super capacitor with excellent
High rate performance, cyclical stability and higher energy density.The layering Porous transition metal organic backbone prepared through the invention
Material and conductive black and polytetrafluoroethylene (PTFE)（PVDF）With mass ratio 7:2:After 1 mixing, it is slurred with two pyrrolidones of N- first class
Expect and be uniformly coated onto foam nickel surface, is used as to electrode, mercury-mercury oxide as working electrode, platinized platinum after 80 DEG C of dry 12h
For reference electrode, electrolyte is 6M potassium hydroxide solutions, using three-electrode system, test voltage 0.1 ~ 0.6V of window, tester
Device is Shanghai Chen Hua CHI 660C electrochemical workstations.It is 0.1A/g in current density, specific capacitance is up to 1114F/g.Pass through this
The HP-MOFs prepared is invented as positive electrode, commercialization graphene is negative material, assembles Asymmetric Supercapacitor, electricity
Pressure window is 0 ~ 1.6V, and test equipment is Shanghai Chen Hua CHI 660C electrochemical workstations, and discharge ratio under 0.3A/g constant currents
Capacitance is more than 100F/g, energy density 32W/Kg, power density 240Wh/Kg.
Specific implementation mode
Embodiment 1：
Zn-Zr bimetallics MOFs prepares HP-MOFs, is as follows：
1. according to 1 ︰ of molar ratio, 0.1 ︰ 0.5, accurately weigh 2.33 g zirconium chlorides, 0.29 g zinc nitrate hexahydrates and
0.83 g terephthalic acid (TPA)s, after being added in the beaker for filling 400 mL anhydrous DMFs, ultrasonic 30min turns the solution in beaker
Flask is moved to, magnetic agitation is heated in 180 DEG C of oil bath pans and reacts 12h；
2. being cooled to room temperature, acquired solution is centrifuged, is used in combination anhydrous DMF and acetone to clean several times, obtains Zn-Zr
Bimetallic MOFs；
3. in the strength hydrochloric acid that gained Zn-Zr bimetallics MOFs is placed to 100 pH=1 mL, magnetic agitation 30min, centrifugation
Afterwards, obtained solid is washed with DMF and acetone respectively.Last products therefrom is dried in 60 DEG C of baking ovens to get HP-MOFs.
In the case where current density is 0.1A/g, which is 960 F/g.
Embodiment 2：
Fe-Zr bimetallics MOFs prepares HP-MOFs, is as follows：
1. according to 1 ︰ of molar ratio, 0.5 ︰ 1.5, accurately weigh 2.33 g zirconium chlorides, 1.35 g ferric chloride hexahydrates and
2.49g phthalic acids, after being added in the beaker for filling 400 mL anhydrous DMFs, ultrasonic 30min shifts the solution in beaker
To flask, magnetic agitation reaction is heated in 180 DEG C of oil bath pans for 24 hours；
2. being cooled to room temperature, acquired solution is centrifuged, is used in combination anhydrous DMF and acetone to clean several times, obtains Fe-Zr
Bimetallic MOFs；
3. gained Fe-Zr bimetallics MOFs is placed the strong nitric acid of 100 mL（pH=1）In, magnetic agitation 30min, centrifugation
Afterwards, obtained solid is washed with DMF and acetone respectively.Last products therefrom is dried in 60 DEG C of baking ovens to get HP-MOFs.
In the case where current density is 0.1A/g, which is 888F/g.
Embodiment 3：
Ni-Zr bimetallics MOFs prepares HP-MOFs, is as follows：
1. according to 1 ︰ of molar ratio, 1 ︰ 5,2.33g zirconium chlorides, 2.37g Nickel dichloride hexahydrates and 8.3 g benzene first are accurately weighed
Acid is added in the beaker for filling 400 mL anhydrous DMFs, and the solution in beaker is transferred to flask, in 180 by 30 min of ultrasound
Heating magnetic agitation reacts 36h in DEG C oil bath pan；
2. being cooled to room temperature, acquired solution is centrifuged, DMF and acetone is used in combination to clean several times, obtains the bis- gold of Ni-Zr
Belong to MOFs；
3. gained Ni-Zr bimetallics MOFs is placed 100 mL HCl（pH=1）In, magnetic agitation 30min, after centrifugation,
Obtained solid is washed with anhydrous DMF and acetone respectively.Last products therefrom is dried in 60 DEG C of baking ovens to get HP-MOFs.
In the case where current density is 0.1A/g, which is 823 F/g.
Embodiment 4：
Co-Zr bimetallics MOFs prepares HP-MOFs, is as follows：
1. according to 1 ︰ of molar ratio, 2 ︰ 3,2.33g zirconium chlorides, 2.37g cobalt chloride hexahydrates and the equal benzene of 6.3 g are accurately weighed
Tricarboxylic acid is added in the beaker for filling 400 mL anhydrous DMFs, and the solution in beaker is transferred to flask by 30 min of ultrasound, in
Magnetic agitation is heated in 180 DEG C of oil bath pans reacts 48h；
2. being cooled to room temperature, acquired solution is centrifuged, DMF and acetone is used in combination to clean several times, obtains the bis- gold of Co-Zr
Belong to MOFs；
3. gained Co-Zr bimetallics MOFs is placed 100 mL HCl（pH=1）In, magnetic agitation 30min, after centrifugation,
Obtained solid is washed with anhydrous DMF and acetone respectively.Last products therefrom is dried in 60 DEG C of baking ovens to get HP-MOFs.
In the case where current density is 0.1A/g, which is 657 F/g.
Embodiment 5：
Mn-Zr bimetallics MOFs prepares HP-MOFs, is as follows：
1. according to 1 ︰ of molar ratio, 3 ︰ 8,2.33g zirconium chlorides, 5.97 g, tetra- chloride hydrate manganese and 13.3 g pairs are accurately weighed
Phthalic acid is added in the beaker for filling 400 mL anhydrous DMFs, and the solution in beaker is transferred to flask by 30 min of ultrasound,
Magnetic agitation reaction is heated in 180 DEG C of oil bath pans for 24 hours；
2. being cooled to room temperature, acquired solution is centrifuged, is used in combination anhydrous DMF and acetone to clean several times, obtains Mn-Zr
Bimetallic MOFs；
3. gained Mn-Zr bimetallics MOFs is placed 100 mL HCl（pH=1）In, magnetic agitation 30min, after centrifugation,
Obtained solid is washed with DMF and acetone respectively.Last products therefrom is dried in 60 DEG C of baking ovens to get HP-MOFs.
In the case where current density is 0.1A/g, which is 646 F/g.
Embodiment 6：
Mn-Co bimetallics MOFs prepares HP-MOFs, is as follows：
1. according to 1 ︰ of molar ratio, 2 ︰ 3, accurately weigh 2.91 g cabaltous nitrate hexahydrates, 1.97 g, tetra- chloride hydrate manganese and
2.46 g methylimidazoles are added in the beaker for filling 400 mL anhydrous DMFs, ultrasonic 30min, and the solution in beaker is shifted
To flask, magnetic agitation reaction 48h is heated in 180 DEG C of oil bath pans；
2. being cooled to room temperature, acquired solution is centrifuged, is used in combination anhydrous DMF and acetone to clean several times, obtains Mn-Co
Bimetallic MOFs；
3. gained Mn-Co bimetallics MOFs is transferred to 100 mL HCl（pH=1）In, magnetic agitation 30min, centrifugation
Afterwards, obtained solid is washed with DMF and acetone respectively.Last products therefrom is dried in 60 DEG C of baking ovens to get HP-MOFs.
In the case where current density is 0.1A/g, which is 726F/g.
Embodiment 7：
Zn-Co bimetallics MOFs prepares HP-MOFs, is as follows：
1. according to 1 ︰ of molar ratio, 1 ︰ 2,2.37g cabaltous nitrate hexahydrates, 2.97 g zinc nitrate hexahydrates and 1.64 are accurately weighed
G methylimidazoles, are added in the beaker for filling 400 mL anhydrous DMFs, ultrasonic 30min, and the solution in beaker is transferred to burning
Bottle heats magnetic agitation reaction 12h in 180 DEG C of oil bath pans；
2. being cooled to room temperature, acquired solution is centrifuged, n,N-Dimethylformamide and acetone is used in combination to clean several times,
Obtain Zn-Co bimetallic mixing MOFs；
3. gained Zn-Co bimetallics MOFs is transferred to 100 mL HCl（pH=1）In, magnetic agitation 30min, centrifugation
Afterwards, obtained solid is washed with DMF and acetone respectively.Last products therefrom is dried in 60 DEG C of baking ovens to get HP-MOFs.
In the case where current density is 0.1A/g, which is 1031F/g.
Embodiment 8：
Fe-Co bimetallic mixing MOFs prepares HP-MOFs, is as follows：
1. according to 1 ︰ of molar ratio, 5 ︰ 10, accurately weigh 2.37 g cabaltous nitrate hexahydrates, 13.5 g ferric chloride hexahydrates and
8.2 g methylimidazoles are added in the beaker for filling 400 mL anhydrous DMFs, ultrasonic 30min, and the solution in beaker is shifted
To flask, magnetic agitation reaction 36h is heated in 180 DEG C of oil bath pans；
2. being cooled to room temperature, acquired solution is centrifuged, is used in combination anhydrous DMF and acetone to clean several times, obtains Fe-Co
Bimetallic MOFs；
3. gained Fe-Co bimetallic mixing MOFs is transferred to 100 mL HCl（pH=1）In, magnetic agitation 30min, from
After the heart, obtained solid is washed with DMF and acetone respectively.Last products therefrom is dried in 60 DEG C of baking ovens to get HP-MOFs.
In the case where current density is 0.1A/g, which is 768F/g.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
The specific implementation of the present invention is confined to these explanations.For those of ordinary skill in the art to which the present invention belongs, exist
Several equivalent substitute or obvious modifications are made under the premise of not departing from present inventive concept, and performance or use is identical, then should
It is considered as belonging to the protection domain that claims that the present invention is submitted determine.
Claims (5)
1. a kind of organic backbone electrode material of ultracapacitor, which is characterized in that be by two kinds of transition metal ions with it is organic
Ligand is that 1 ︰, 0.1~5 ︰ 0.5~10 are configured in molar ratio, is added in anhydrous n,N dimethylformamide organic solvent and mixes
It closes, the bimetallic MOFs of above two transition metal ions is obtained by the reaction through oil bath heating, gained bimetallic MOFs is transferred to
In the strong acid solution of pH=1,30~60min is stirred, through centrifuging, washing, so that its structure is disintegrated, removal is wherein unstable
MOFs, to obtain another HP-MOFs stablized, which is the organic bone that can be used for high-performance super capacitor
Frame electrode material.
2. a kind of organic backbone electrode material of ultracapacitor as described in claim 1, which is characterized in that described two kinds
Transition metal ions is in one group, every group during Zn-Zr, Fe-Zr, Ni-Zr, Mn-Zr, Zn-Co, Fe-Co, Mn-Co are respectively combined
Two kinds of transition metal ions and organic ligand molar ratio configure, the tandem of two kinds of transition metal ions can not front and rear
It changes.
3. a kind of organic backbone electrode material of ultracapacitor as described in claim 1, which is characterized in that described is organic
Ligand is terephthalic acid (TPA), phthalic acid, benzoic acid, trimesic acid and its derivative or methylimidazole and its derivative
Object.
4. a kind of preparation method of the organic backbone electrode material of ultracapacitor described in claim 1, specifically includes following
Step：
(1) it is 1 ︰, 0.1~5 ︰ 0.5~10 according to molar ratio, weighs the metal salt of two kinds of different transition metal ions respectively and have
Two kinds of transition metal salts and organic ligand are added in anhydrous n,N dimethylformamide organic solvent and mix and surpass by machine ligand
Solution after supersound process is transferred to flask by sonication, in 80 DEG C~200 DEG C 12~48h of constant temperature oil bath heating reaction；
(2) it is cooled to room temperature, acquired solution is centrifuged, is used in combination anhydrous n,N dimethylformamide and acetone to clean several times, obtains
To bimetallic MOFs；
(3) gained bimetallic MOFs is transferred in the strong acid solution of pH=1,30~60min of stirring makes it through centrifuging, washing
Structure is disintegrated, vacuum dried to obtain HP-MOFs after the wherein unstable MOFs of removal.
5. the preparation method of organic backbone electrode material as claimed in claim 4, which is characterized in that the pH=1's is strong
Acid, the strong acid are any one in hydrochloric acid, nitric acid, sulfuric acid, perchloric acid, hydrofluoric acid or hydroiodic acid.
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