CN109437240A - A kind of preparation method of kalium ion battery high potential positive electrode - Google Patents
A kind of preparation method of kalium ion battery high potential positive electrode Download PDFInfo
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- CN109437240A CN109437240A CN201811228311.8A CN201811228311A CN109437240A CN 109437240 A CN109437240 A CN 109437240A CN 201811228311 A CN201811228311 A CN 201811228311A CN 109437240 A CN109437240 A CN 109437240A
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- positive electrode
- ion battery
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- high potential
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/08—Simple or complex cyanides of metals
- C01C3/12—Simple or complex iron cyanides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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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
- 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
- Y02E60/10—Energy storage using batteries
Abstract
A kind of preparation method of kalium ion battery high potential positive electrode includes the following steps: S1, potassium ferrocyanide is added to deionized water dissolving, forms solution A；S2, deionized water will be added as the molysite of source of iron, potassium citrate, citric acid and iron powder, forms mixed liquid B；S3, solution A is instilled in mixed liquid B, and be stirred continuously；S4, to after reaction, stand；S5, it collects and precipitates and dry.Preparation method of the invention operates conveniently, low in cost, favorable reproducibility, and the Prussian blue of synthesis is nano-scale, can be improved the cycle performance of battery using the kalium ion battery that the positive electrode makes.
Description
Technical field
The present invention relates to kalium ion battery material, especially a kind of preparation side of kalium ion battery high potential positive electrode
Method.
Background technique
With the sharply promotion of the continuous consumption and price of lithium and cobalt ore resource, cause to rely on the product of lithium ion battery at
This is constantly increased, this problem seriously limits application of the lithium ion battery in large-scale energy storage field.Find resourceful, energy
The novel ion battery of metric density height, high circulation service life and safety is a current research hotspot.
Recently, kalium ion battery due to can with the advantages such as commercial graphite matched well and potassium element be resourceful,
Receive the extensive concern of educational circles and industry.Finding at present and can matching potassium ion positive electrode is a hot and difficult issue.It is general
Shandong scholar's indigo plant analog K2M[Fe(CN)6] (PBs) due to having spacious gap site, long circulation life, high working voltage, high ratio
The advantages that energy and low preparation cost, shows one's talent in potassium electricity positive electrode.The white analog in Prussia has stable crystal frame
Frame structure, cyanide ligands alternately connect MN6And FeC6Octahedron constructs three-dimensional (3D) stable frame, has opening
Ion channel, in charge and discharge process, M (Mn, Fe, Co, Ni) and Fe are electro-chemical activities, and theoretical capacity is in 140mA
H/g or so.If considering the quality and volume of full battery, the specific energy and energy density of KIBs is suitable with NIBs.
PBs common preparation method has simple precipitation method, hydro-thermal method, single source of iron method, cyantype etc. at present, using difference
The obtained PBs of method component, partial size and in terms of have nothing in common with each other, it is also different in terms of chemical property.
Simple precipitation method compared to other methods have simple process, low in cost, applicability it is wide, can mass production etc. it is excellent
Point.But also there is some problems, Prussian blue during synthesis, Fe simultaneously2+It is easily oxidized, leads to the PB of synthesis
Potassium content is lower, and theoretical capacity also decreases.Precipitation method reaction speed is fast simultaneously, reunion easy to form, and contains in lattice
There is constitution water.The above problem can reduce Prussian blue initial capacity, and the presence of constitution water can produce in charge and discharge process
Raw side reaction, and make lattice damage, deteriorate cycle performance.Presently mainly passing through reduces the concentration of reaction solution and is passed through inertia
Atmosphere protection improves this problem.But inert atmosphere protection can be such that whole cost significantly increases.
Summary of the invention
It is a primary object of the present invention to overcome the deficiencies of the prior art and provide a kind of kalium ion battery high potential anode material
The preparation method of material is oxidized in the synthesis process with solving Prussian blue positive electrode, and potassium content is low, and poor circulation etc. is asked
Topic.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of kalium ion battery high potential positive electrode, includes the following steps:
S1, potassium ferrocyanide is added to deionized water dissolving, forms solution A；
S2, deionized water will be added as the molysite of source of iron, potassium citrate, citric acid and iron powder, forms mixed liquid B；
S3, solution A is instilled in mixed liquid B, and be stirred continuously；
S4, to after reaction, stand；
S5, it collects and precipitates and dry.
Further:
The source of iron is ferrous ion metal salt.
The ferrous ion metal salt is ferrous sulfate or frerrous chloride.
The molar ratio of the potassium ferrocyanide and the source of iron is 2:3.
The mass ratio of the potassium citrate and the citric acid is 4:1.
The mass ratio of the iron powder and the citric acid is 1:20.
The molar concentration of potassium citrate is in 1.6~1.7mol/L in mixed liquid B.
In step S3, it is 0.7~0.9ml/min, preferably 0.8ml/min that the solution A, which instills rate,.
In step S4, to which after reaction, static 12~14h is collected by centrifugation the precipitating, and is cleaned with deionized water.
In step S4, centrifuge speed 8000r/min.
In step S5, the step S4 precipitating obtained is put into 80 DEG C of vacuum drying oven drying for 24 hours.
The invention has the following beneficial effects:
In the preparation method of kalium ion battery high potential positive electrode of the invention, citric acid is reacted with iron powder generates hydrogen
Gas, make device spontaneously form positive atmosphere protection, avoid air in positive electrode synthesis process enter oxidation it is Prussian blue, mention
High Prussian blue potassium content and initial capacity, the powder generated in reaction process is white, the potassium content in PBs compared with
It is more.The addition of potassium citrate reduces reaction rate, effectively reduces the reunion degree of PBs nano particle, reduces lattice and contain
Water facilitates the cyclical stability for promoting the later period.Kalium ion battery high potential method for preparing anode material operation of the invention
Convenient, low in cost, favorable reproducibility, the Prussian blue of synthesis is nano-scale, the potassium ion electricity made using the positive electrode
Pond can be improved the cycle performance of battery.
Detailed description of the invention
Fig. 1 is electricity of the kalium ion battery high potential positive electrode of the embodiment of the present invention production under two kinds of dimension scales
Mirror figure.
Fig. 2 is that the charge and discharge of the battery of the kalium ion battery high potential positive electrode made using the embodiment of the present invention are followed
Ring performance schematic diagram.
Specific embodiment
It elaborates below to embodiments of the present invention.It is emphasized that following the description is only exemplary,
The range and its application being not intended to be limiting of the invention.In the absence of conflict, the embodiment and embodiment in the present invention
In feature can be combined with each other.
In one embodiment, a kind of preparation method of kalium ion battery high potential positive electrode, includes the following steps:
Step S1, deionized water dissolving is added in potassium ferrocyanide, forms solution A；
Step S2, deionized water will be added as the molysite of source of iron, potassium citrate, citric acid and iron powder, forms mixed liquor
B；
Step S3, solution A is instilled in mixed liquid B, and be stirred continuously；
Step S4, to after reaction, stand；
Step S5, it collects and precipitates and dry.
Since citric acid and iron powder reaction generate hydrogen in the synthesis process, positive atmosphere protection is spontaneously formed to device,
The entrance oxidation sample for avoiding the oxygen in synthesis, improves Prussian blue potassium content and initial capacity.Lemon is added simultaneously
The reducing agents such as acid and complexing agent reduce reaction speed, reduce the reunion of nano particle, reduce lattice water content, facilitate
The cyclical stability in later period.
In some preferred embodiments, the source of iron is ferrous ion metal salt.
It is highly preferred that the source of iron is ferrous sulfate or frerrous chloride.
In some preferred embodiments, the molar ratio of the potassium ferrocyanide and the source of iron is 2:3.
In some preferred embodiments, the mass ratio of the potassium citrate and the citric acid is 4:1.
In some preferred embodiments, the mass ratio of the iron powder and the citric acid is 1:20.
In some preferred embodiments, the molar concentration of potassium citrate is in 1.6~1.7mol/L in mixed liquid B.
In some preferred embodiments, in step S3, it is 0.7~0.9ml/min that the solution A, which instills rate, preferably
0.8ml/min。
In some preferred embodiments, in step S4, to which after reaction, static 12~14h, it is described heavy to be collected by centrifugation
It forms sediment, and is cleaned with deionized water.
In some preferred embodiments, in step S4, centrifuge speed 8000r/min.
In some preferred embodiments, in step S5, the step S4 precipitating obtained is put into 80 DEG C of vacuum drying oven drying
24h。
According to a typical embodiment, a kind of preparation method of kalium ion battery high potential positive electrode, including it is following
Step: weighing a certain amount of potassium ferrocyanide and be dissolved in deionized water, wiring solution-forming A, weigh source of iron (preferably frerrous chloride, or
Ferrous sulfate), citric acid, potassium citrate wiring solution-forming B in ionized water is added simultaneously, and a certain amount of iron is added into B solution
Powder.Potassium ferrocyanide and frerrous chloride molar ratio are 2:3, and the mass ratio of potassium citrate and citric acid is 4:1, and iron powder is citric acid
The 1/20 of quality.The molar concentration of potassium citrate is in 1.6~1.7mol/L in mixed liquid B.After mixed liquid B is sufficiently stirred evenly, with
Solution A is added dropwise in the rate of about 0.8ml/min, quickly forms the white precipitating in white Prussia.Left undisturbed overnight after reaction.Precipitating is old
After changing an evening, precipitating is collected by centrifugation, and be washed with deionized water three times.Solid is then put into 80 DEG C of vacuum drying oven drying for 24 hours.
Specific explaination is done to the embodiment of the present invention below with reference to attached drawing.
A kind of preparation method of kalium ion battery high potential positive electrode of the embodiment of the present invention, specific steps include:
Step 1, the potassium ferrocyanide for weighing 2.5mmol is dissolved in the deionization solution of 60ml；
Step 2, frerrous chloride, 4g potassium citrate, 1g citric acid and the 50mg iron powder for weighing 3mmol, are dissolved in 80ml's
In deionized water, mixed liquid B is formed；
Step 3, then potassium ferrocyanide solution is instilled in mixed liquid B with the rate of 0.8ml/min, is quickly generated white
Precipitating, and be stirred continuously；
Step 4, to after reaction, static 12~14h.Centrifuge is adjusted to 8000r/min and collects powder, and washes three
It is secondary.
Obtained sample is put into 80 DEG C of vacuum drying ovens by step 5, and drying is about for 24 hours.
Battery, electrochemical property test are made using kalium ion battery high potential positive electrode prepared by the embodiment of the present invention
Process is as follows: by Prussian blue material, conductive agent and binder according to the ratio mixed slurry of 7:2:1, then control is certain thick
Degree is coated in the aluminum foil current collector of spray carbon.With 0.5mol/L KPF6/EC+DEC (volume ratio 1:1) for electrolyte, K piece is negative
Pole, diaphragm are layer of glass fiber and one layer of Cellgard-2400 type polypropylene screen.Button is assembled into the glove box full of argon gas
Battery.Then charge/discharge capacity is carried out in the LandCT2001A type battery test system of Wuhan Jin Nuo Electronics Co., Ltd. production
And cycle life test.
As shown in fig. 1, the kalium ion battery high potential positive electrode of the embodiment of the present invention preparation, has nanometer ruler
Very little, granular size is about 30~40nm, and crystal form is relatively complete, and agglomeration is substantially reduced.As shown in Fig. 2, with 45mA/g size
Testing current its cycle performance, it can be seen that this method is capable of providing high initial discharge capacity, and cycle performance is more steady
Fixed, 100 circle of circulation still has the discharge capacity of 80mA h/g.
The above content is combine it is specific/further detailed description of the invention for preferred embodiment, cannot recognize
Fixed specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs,
Without departing from the inventive concept of the premise, some replacements or modifications can also be made to the embodiment that these have been described,
And these substitutions or variant all shall be regarded as belonging to protection scope of the present invention.
Claims (10)
1. a kind of preparation method of kalium ion battery high potential positive electrode, which comprises the steps of:
S1, potassium ferrocyanide is added to deionized water dissolving, forms solution A；
S2, deionized water will be added as the molysite of source of iron, potassium citrate, citric acid and iron powder, forms mixed liquid B；
S3, solution A is instilled in mixed liquid B, and be stirred continuously；
S4, to after reaction, stand；
S5, it collects and precipitates and dry.
2. the preparation method of kalium ion battery high potential positive electrode according to claim 1, which is characterized in that the iron
Source is ferrous ion metal salt, preferably ferrous sulfate or frerrous chloride.
3. the preparation method of kalium ion battery high potential positive electrode according to claim 1 or 2, which is characterized in that institute
The molar ratio for stating potassium ferrocyanide and the source of iron is 2:3.
4. the preparation method of kalium ion battery high potential positive electrode according to any one of claims 1 to 3, feature exist
In the mass ratio of the potassium citrate and the citric acid is 4:1.
5. the preparation method of kalium ion battery high potential positive electrode according to any one of claims 1 to 4, feature exist
In the mass ratio of the iron powder and the citric acid is 1:20.
6. the preparation method of kalium ion battery high potential positive electrode according to any one of claims 1 to 5, feature exist
In the molar concentration of potassium citrate is in 1.6~1.7mol/L in mixed liquid B.
7. the preparation method of kalium ion battery high potential positive electrode according to any one of claims 1 to 6, feature exist
In in step S3, it is 0.7~0.9ml/min, preferably 0.8ml/min that the solution A, which instills rate,.
8. the preparation method of kalium ion battery high potential positive electrode according to any one of claims 1 to 7, feature exist
In in step S4, to which after reaction, static 12~14h is collected by centrifugation the precipitating, and is cleaned with deionized water.
9. the preparation method of kalium ion battery high potential positive electrode according to claim 8, which is characterized in that step S4
In, centrifuge speed 8000r/min.
10. the preparation method of kalium ion battery high potential positive electrode according to any one of claims 1 to 9, feature exist
In in step S5, the step S4 precipitating obtained is put into the drying of 80 DEG C of vacuum drying ovens for 24 hours.
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Cited By (5)
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| CN110002466A (en) * | 2019-04-28 | 2019-07-12 | 电子科技大学 | Ferrous cyanogen manganese potassium prussian blue cubic crystal of low water low defect and preparation method thereof |
| CN110010892A (en) * | 2019-03-29 | 2019-07-12 | 华中科技大学 | A kind of aluminium ion cell positive material, preparation method and application |
| CN111943225A (en) * | 2020-08-24 | 2020-11-17 | 全球能源互联网研究院有限公司 | Prussian blue type sodium ion battery positive electrode material and preparation method thereof |
| CN112209409A (en) * | 2020-09-28 | 2021-01-12 | 浙江凯恩电池有限公司 | Method for rapidly preparing Prussian white serving as positive electrode material of sodium-ion battery |
| CN114497495A (en) * | 2022-01-24 | 2022-05-13 | 辽宁大学 | Prussian blue electrode material with high potassium storage capacity and preparation method and application thereof |
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Cited By (6)
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| CN110010892A (en) * | 2019-03-29 | 2019-07-12 | 华中科技大学 | A kind of aluminium ion cell positive material, preparation method and application |
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| CN110002466B (en) * | 2019-04-28 | 2022-05-03 | 电子科技大学 | Low-water low-defect ferrous cyanide manganese potassium prussian blue cubic crystal and preparation method thereof |
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| CN112209409A (en) * | 2020-09-28 | 2021-01-12 | 浙江凯恩电池有限公司 | Method for rapidly preparing Prussian white serving as positive electrode material of sodium-ion battery |
| CN114497495A (en) * | 2022-01-24 | 2022-05-13 | 辽宁大学 | Prussian blue electrode material with high potassium storage capacity and preparation method and application thereof |
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