CN109004190A - A kind of ferrous sulfide anode material and preparation method - Google Patents
A kind of ferrous sulfide anode material and preparation method Download PDFInfo
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- CN109004190A CN109004190A CN201810756332.0A CN201810756332A CN109004190A CN 109004190 A CN109004190 A CN 109004190A CN 201810756332 A CN201810756332 A CN 201810756332A CN 109004190 A CN109004190 A CN 109004190A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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
The invention discloses a kind of ferrous sulfide anode material and preparation methods, anode material therein includes the raw material of following parts by weight: 20-30 parts of vulcanized sodium, 20-30 parts of ferrous sulfate, N, 5-10 parts of dinethylformamide, 3-9 parts of terephthalic acid (TPA), 10-15 parts of organic siliconresin, preparation method includes the following steps: S1: vulcanized sodium is put into Agitation Tank, water is added to be stirred, then N is added, dinethylformamide and organic siliconresin stirring, mixing time is 10-15min, and the first mixed solution is made after mixing evenly；S2: ferrous sulfate is put into mixing plant, is added water and stirred, mixing time 10-15min, after mixing evenly, the second mixed solution is made.Preparation method of the present invention is simple, shortens manufacturing cycle, has saved production cost.
Description
Technical field
The present invention relates to ferrous sulfide preparation field more particularly to a kind of ferrous sulfide anode material and preparation sides
Method.
Background technique
Ferrous sulfide is blue-green monoclinic crystal or particle, odorlessness.The weathering in dry air, the table in humid air
Face is oxidized to the ferric subsulfate of brown.Become tetrahydrate at 56.6 DEG C, becomes monohydrate at 65 DEG C.It is dissolved in water, it is several
Ethyl alcohol is not dissolved in.It slowly aoxidizes when its water-soluble liquid cooling, is comparatively fast aoxidized in heat in air.Alkali or exposure, which is added, can accelerate it
Oxidation.Relative density (d15) 1.897, it is irritant.Anhydrous slufuric acid ferrous iron is white powder, and what it is containing the crystallization water is light green color crystalline substance
Body, crystal are commonly called as " green vitriol ", and being dissolved in water aqueous solution is light green color.Ferrous sulfate can be used for chromatography reagent, spot analysis is surveyed
Determine platinum, selenium, nitrite and nitrate, ferrous sulfate be also used as reducing agent, manufacture ferrite, water purification, polymerization catalyst,
Photomechanical production etc., through retrieving, the patent document of application number 201510014150.2 discloses a kind of lithium ion battery negative material
The preparation method and applications of selenium ferrous sulfide, comprising: iron powder, selenium powder and sulphur powder mixing pressure target；Under argon atmosphere, use
Tube furnace is sintered selenium ferrous sulfide；Ball milling.Selenium iron sulfide prepared by the present invention is used as lithium ion battery negative material.Of the invention
Preparation method is easy to operate, simple process, is suitble to large-scale production；Selenium iron sulfide negative electrode material ratio with higher of the invention
Capacity, high circulation performance and high rate capability are a kind of lithium ion battery negative materials of good performance, but its lithium for mentioning
The preparation method of ion battery cathode material selenium ferrous sulfide, relatively complicated, production cost is higher, long preparation period, therefore I
Propose a kind of ferrous sulfide anode material and preparation method, for solving the above problems.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of ferrous sulfide anode material and preparations
Method.
A kind of ferrous sulfide anode material proposed by the present invention, the raw material including following parts by weight: vulcanized sodium 20-30
Part, 20-30 parts of ferrous sulfate, 5-10 parts of N,N-dimethylformamide, 3-9 parts of terephthalic acid (TPA), 10-15 parts of organic siliconresin.
Preferably, the raw material including following parts by weight: 21-29 parts of vulcanized sodium, 21-29 parts of ferrous sulfate, N, N- dimethyl
6-9 parts of formamide, 4-8 parts of terephthalic acid (TPA), 11-14 parts of organic siliconresin.
Preferably, the weight of the vulcanized sodium, ferrous sulfate, n,N-Dimethylformamide, terephthalic acid (TPA), organic siliconresin
Amount is than being 21-29:21-29:6-9:4-8:11-14.
The invention also provides a kind of preparation methods of ferrous sulfide anode material, comprising the following steps:
S1: vulcanized sodium is put into Agitation Tank, and water is added and is stirred, n,N-Dimethylformamide and organosilicon tree is then added
The first mixed solution is made in rouge stirring, mixing time 10-15min after mixing evenly；
S2: ferrous sulfate is put into mixing plant, is added water and stirred, mixing time 10-15min, after mixing evenly, is made the
Two mixed solutions；
S3: the first mixed solution described in S1 and S2 and the second mixed solution being put into consersion unit, are uniformly mixed,
Mixing time is 20-30min, and reaction temperature is 30-40 DEG C, and third mixed solution is made；
S4: being filtered precipitating to mixed liquor described in S3, and washed with deionized water to sediment, vacuum drying,
Ferrous sulfide anode material is made.
Preferably, in the S2, when configuring the second mixed solution, purification processes first are carried out to ferrous sulfate, then will
Ferrous sulfate after purification is put into mixing plant, and distilled water is added, stirs evenly.
Preferably, in the S1, vulcanized sodium is crushed, vulcanized sodium powder is put into Agitation Tank, added by milling processing
Enter distilled water to stir evenly.
Preferably, it in the S3, the first mixed solution described in S1 and S2 is put into react with the second mixed solution sets
It is standby interior, it is uniformly mixed, mixing time 21-29min, reaction temperature is 31-39 DEG C, and third mixed solution is made.
Preferably, in the S4, the sediment after washing to be put into vacuum oven, drying temperature is 50-100 DEG C,
Drying time is 30-60min.
Preferably, in the S1, vulcanized sodium will be put into Agitation Tank, water is added and is stirred, will be mixed after the completion of stirring
Close object put into blender, then be added n,N-Dimethylformamide and organic siliconresin stirring, blender revolving speed be 300 turns/
min。
Preferably, in the S2, ferrous sulfate will be put into blender, be added water and stirred, blender revolving speed be 400 turns/
min。
The beneficial effects of the present invention are: manufacturing cycle can be shortened by the preparation process for simplifying anode material, save
About production cost, preparation method of the present invention is simple, shortens manufacturing cycle, saved production cost.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
Embodiment one
The invention proposes a kind of ferrous sulfide anode material, the raw material including following parts by weight: 20 parts of vulcanized sodium, sulfuric acid
Ferrous 20 parts, 5 parts of N,N-dimethylformamide, 3 parts of terephthalic acid (TPA), 10 parts of organic siliconresin；
Preparation method includes the following steps:
S1: vulcanized sodium is put into Agitation Tank, and water is added and is stirred, n,N-Dimethylformamide and organosilicon tree is then added
The first mixed solution is made in rouge stirring, mixing time 10min after mixing evenly；
S2: ferrous sulfate is put into mixing plant, is added water and stirred, mixing time 10min, after mixing evenly, is made second
Mixed solution；
S3: the first mixed solution described in S1 and S2 and the second mixed solution being put into consersion unit, are uniformly mixed,
Mixing time is 20min, and reaction temperature is 30 DEG C, and third mixed solution is made；
S4: being filtered precipitating to mixed liquor described in S3, and washed with deionized water to sediment, vacuum drying,
Ferrous sulfide anode material is made.
Embodiment two
The invention proposes a kind of ferrous sulfide anode material, the raw material including following parts by weight: 22 parts of vulcanized sodium, sulfuric acid
Ferrous 22 parts, 6 parts of N,N-dimethylformamide, 4 parts of terephthalic acid (TPA), 11 parts of organic siliconresin；
Preparation method includes the following steps:
S1: vulcanized sodium is put into Agitation Tank, and water is added and is stirred, n,N-Dimethylformamide and organosilicon tree is then added
The first mixed solution is made in rouge stirring, mixing time 11min after mixing evenly；
S2: ferrous sulfate is put into mixing plant, is added water and stirred, mixing time 11min, after mixing evenly, is made second
Mixed solution；
S3: the first mixed solution described in S1 and S2 and the second mixed solution being put into consersion unit, are uniformly mixed,
Mixing time is 22min, and reaction temperature is 32 DEG C, and third mixed solution is made；
S4: being filtered precipitating to mixed liquor described in S3, and washed with deionized water to sediment, vacuum drying,
Ferrous sulfide anode material is made.
Embodiment three
The invention proposes a kind of ferrous sulfide anode material, the raw material including following parts by weight: 28 parts of vulcanized sodium, sulfuric acid
Ferrous 28 parts, 8 parts of N,N-dimethylformamide, 7 parts of terephthalic acid (TPA), 13 parts of organic siliconresin；
Preparation method includes the following steps:
S1: vulcanized sodium is put into Agitation Tank, and water is added and is stirred, n,N-Dimethylformamide and organosilicon tree is then added
The first mixed solution is made in rouge stirring, mixing time 13min after mixing evenly；
S2: ferrous sulfate is put into mixing plant, is added water and stirred, mixing time 13min, after mixing evenly, is made second
Mixed solution；
S3: the first mixed solution described in S1 and S2 and the second mixed solution being put into consersion unit, are uniformly mixed,
Mixing time is 28min, and reaction temperature is 37 DEG C, and third mixed solution is made；
S4: being filtered precipitating to mixed liquor described in S3, and washed with deionized water to sediment, vacuum drying,
Ferrous sulfide anode material is made.
Example IV
The invention proposes a kind of ferrous sulfide anode material, the raw material including following parts by weight: 30 parts of vulcanized sodium, sulfuric acid
Ferrous 30 parts, 10 parts of N,N-dimethylformamide, 9 parts of terephthalic acid (TPA), 15 parts of organic siliconresin；
Preparation method includes the following steps:
S1: vulcanized sodium is put into Agitation Tank, and water is added and is stirred, n,N-Dimethylformamide and organosilicon tree is then added
The first mixed solution is made in rouge stirring, mixing time 15min after mixing evenly；
S2: ferrous sulfate is put into mixing plant, is added water and stirred, mixing time 15min, after mixing evenly, is made second
Mixed solution；
S3: the first mixed solution described in S1 and S2 and the second mixed solution being put into consersion unit, are uniformly mixed,
Mixing time is 30min, and reaction temperature is 40 DEG C, and third mixed solution is made；
S4: being filtered precipitating to mixed liquor described in S3, and washed with deionized water to sediment, vacuum drying,
Ferrous sulfide anode material is made.
The ferrous sulfide anode material as made from embodiment one, two, three, four can effectively shorten preparation week
Phase saves production cost.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of ferrous sulfide anode material, which is characterized in that the raw material including following parts by weight: 20-30 parts of vulcanized sodium,
20-30 parts of ferrous sulfate, 5-10 parts of N,N-dimethylformamide, 3-9 parts of terephthalic acid (TPA), 10-15 parts of organic siliconresin.
2. a kind of ferrous sulfide anode material according to claim 1, which is characterized in that including following parts by weight
Raw material: 21-29 parts of vulcanized sodium, 21-29 parts of ferrous sulfate, 6-9 parts of N,N-dimethylformamide, 4-8 parts of terephthalic acid (TPA), organic
11-14 parts of silicone resin.
3. a kind of ferrous sulfide anode material according to claim 1, which is characterized in that the vulcanized sodium, sulfuric acid
Ferrous iron, N,N-dimethylformamide, terephthalic acid (TPA), organic siliconresin weight ratio be 21-29:21-29:6-9:4-8:11-
14。
4. a kind of preparation method of ferrous sulfide anode material, which comprises the following steps:
S1: vulcanized sodium is put into Agitation Tank, and water is added and is stirred, n,N-Dimethylformamide and organosilicon tree is then added
The first mixed solution is made in rouge stirring, mixing time 10-15min after mixing evenly；
S2: ferrous sulfate is put into mixing plant, is added water and stirred, mixing time 10-15min, after mixing evenly, is made the
Two mixed solutions；
S3: the first mixed solution described in S1 and S2 and the second mixed solution being put into consersion unit, are uniformly mixed,
Mixing time is 20-30min, and reaction temperature is 30-40 DEG C, and third mixed solution is made；
S4: being filtered precipitating to mixed liquor described in S3, and washed with deionized water to sediment, vacuum drying,
Ferrous sulfide anode material is made.
5. a kind of preparation method of ferrous sulfide anode material according to claim 4, which is characterized in that the S2
In, when configuring the second mixed solution, purification processes first are carried out to ferrous sulfate, then the ferrous sulfate after purification is put into and is stirred
In mixing equipment, distilled water is added, stirs evenly.
6. a kind of preparation method of ferrous sulfide anode material according to claim 4, which is characterized in that the S1
In, vulcanized sodium is crushed, milling processing puts vulcanized sodium powder in Agitation Tank into, and distilled water is added and stirs evenly.
7. a kind of preparation method of ferrous sulfide anode material according to claim 4, which is characterized in that the S3
In, the first mixed solution described in S1 and S2 and the second mixed solution are put into consersion unit, are uniformly mixed, is stirred
Time is 21-29min, and reaction temperature is 31-39 DEG C, and third mixed solution is made.
8. a kind of preparation method of ferrous sulfide anode material according to claim 4, which is characterized in that the S4
In, the sediment after washing is put into vacuum oven, drying temperature is 50-100 DEG C, drying time 30-60min.
9. a kind of preparation method of ferrous sulfide anode material according to claim 4, which is characterized in that the S1
In, vulcanized sodium will be put into Agitation Tank, water is added and is stirred, puts mixture in blender into after the completion of stirring, then
N,N-Dimethylformamide and organic siliconresin stirring is added, blender revolving speed is 300 turns/min.
10. a kind of preparation method of ferrous sulfide anode material according to claim 4, which is characterized in that described
In S2, ferrous sulfate will be put into blender, be added water and stirred, blender revolving speed is 400 turns/min.
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Application publication date: 20181214 |