CN105895914A - Preparation method of iron phosphate dihydrate - Google Patents
Preparation method of iron phosphate dihydrate Download PDFInfo
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- CN105895914A CN105895914A CN201610307885.9A CN201610307885A CN105895914A CN 105895914 A CN105895914 A CN 105895914A CN 201610307885 A CN201610307885 A CN 201610307885A CN 105895914 A CN105895914 A CN 105895914A
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- iron phosphate
- phosphate dihydrate
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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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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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- 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 provides a preparation method of iron phosphate dihydrate. The method comprises the following steps: adding 115-126 parts by weight of phosphoric acid to 400 parts by weight of deionized water to prepare a phosphoric acid solution and keeping the temperature of the solution at 50-65 DEG C; adding 56 parts by weight of reduced iron powder in a stirring state, reacting for 1-3 hours, adding the obtained product to a ball mill for ball-milling to obtain a ball-milled material; putting the taken ball-milled material into a container, adding 56-68 parts of hydrogen peroxide, stirring the hydrogen peroxide evenly and then putting the hydrogen peroxide into a reaction kettle for treatment at 60-140 DEG C for 6-12 hours to obtain a reaction product; and stirring and dispersing the reaction product evenly and then carrying out spray drying at 150-180 DEG C to obtain the iron phosphate dihydrate. The iron phosphate dihydrate synthesized by the method has the characteristics of being high in purity, simple in preparation technology, low in cost and free of pollution in treatment, and can be used as a raw material of producing lithium iron phosphate.
Description
Technical field
The invention belongs to chemical field, relate to a kind of lithium ion battery material, a kind of iron phosphate two is hydrated specifically
The preparation method of thing.
Background technology
As the upstream of new-energy automobile industrial chain, lithium battery industry starts gradually to step into Rapid development stage.But, dynamic
The proportion that power lithium battery cost accounts for entire new energy automobile cost is higher, close to 40%.Therefore, control the lithium battery cost of raw material,
Exploitation lithium battery new material, is current many lithium battery manufacturing enterprises and emphasis that research and development institution carries out the work.Domestic power current
Pond is used mostly ferric phosphate lithium cell and ternary battery, is applied to new forms of energy car and big bus.Ferric phosphate lithium cell safety is relatively
Good, cost also has bigger decline in recent years, it is contemplated that the Maturity of battery technology, economy, current Prospect of EVS Powered with Batteries
Main still based on ferric phosphate lithium cell.
LiFePO4 is as the new-energy automobile pole material of power-type lithium ion battery ferric phosphate lithium cell, and it synthesizes bar
Part and electrochemical characteristic depend primarily on presoma, and good presoma can provide more excellent electricity for LiFePO 4 material
Chemical property.Iron phosphate has the plurality of advantages such as stable structure, cost is relatively low, security performance is high, environmental friendliness, topmost
It is that iron phosphate is similar with the crystal structure of LiFePO4, cell parameter is the most close, selects iron phosphate as presoma, prepare phosphoric acid
Ferrum lithium electrode material, can effectively control the factors such as LiFePO4 size, and therefore iron phosphate is lithium ion cell electrode material
The preferable presoma of material LiFePO4.
At present, iron salt is made hydrated ferric oxide. by the preparation of iron phosphate after being mostly metallic iron is made iron salt, then by hydroxide
Ferrum and phosphatase reaction prepare iron phosphate；Or iron salt and phosphate generation metathesis reaction are prepared iron phosphate.Wherein use ammonia more
Water regulates the pH value of reaction system, uses the ferric phosphate powder body prepared by said method, it may be possible to hydroxyl and water of crystallization quantity
Uncertain alkali formula hypophosphite monohydrate Fe (OH)x(PO4)yNH2O, it is also possible to hydroxyl, ammonium root and the uncertain alkali of water of crystallization quantity
Formula hypophosphite monohydrate ammonium ferrum Fe (NH4)x(OH) y(PO4)zNH2O.If directly utilizing this crystal structure, ferrum phosphorus ratio, hydroxyl, ammonium root
Iron phosphate uncertain with water of crystallization particular number prepares LiFePO 4 as raw material, can make in final raw mixture
Lithium ferrum phosphorus ratio is difficult to control the 1:1:1 to LiFePO 4 requirement, and complex technical process.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides the preparation side of a kind of iron phosphate dihydrate
Method, the preparation method of described this iron phosphate dihydrate to solve the structure of the iron phosphate that method of the prior art obtains
Formula is uncertain, thus affects its technical problem used in LiFePO 4.
The invention provides the preparation method of a kind of iron phosphate dihydrate, comprise the steps:
1) phosphoric acid of 115 ~ 126 weight portions is joined in the deionized water of 400 weight portions, be configured to phosphoric acid solution, keep molten
Liquid temp 50 ~ 65 DEG C, adds the reduced iron powder of 56 weight portions under stirring, and after reaction 1 ~ 3h, the product of gained adds
In ball mill, ball milling, obtain ball milling material；
2) taking-up of above-mentioned ball milling material being positioned in a container, be added thereto to the hydrogen peroxide of 56 ~ 68 weight portions, stirring is all
Putting into after even in reactor and process, treatment temperature is 60 ~ 140 DEG C, and the process time is 6 ~ 12h, obtains product；
3) it is spray-dried at 150 ~ 180 DEG C after uniform for above-mentioned product dispersed with stirring, i.e. obtains iron phosphate two hydration
Thing.
Further, the raw material used by preparation process, to calculate according to the mass fraction, its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 15 parts,
Hydrogen peroxide 56 parts,
Processing procedure in described reactor, treatment temperature is 60 DEG C, processes time 12h.
Further, the raw material used by preparation process, to calculate according to the mass fraction, its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 21 parts,
Hydrogen peroxide 62 parts,
Processing procedure in described reactor, treatment temperature is 100 DEG C, processes time 9h.
Further, the raw material used by preparation process, to calculate according to the mass fraction, its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 26 parts,
Hydrogen peroxide 68 parts,
Processing procedure in described reactor, treatment temperature is 140 DEG C, processes time 6h.
Further, the raw material used by preparation process, to calculate according to the mass fraction, its composition and content are as follows:
Reduced iron powder 56 parts
Phosphatase 11 21 parts,
Hydrogen peroxide 56 parts,
Processing procedure in described reactor, treatment temperature is 100 DEG C, processes time 12h.
Further, the raw material used by preparation process, to calculate according to the mass fraction, its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 26 parts,
Hydrogen peroxide 62 parts,
Processing procedure in described reactor, treatment temperature is 140 DEG C, processes time 9h.
Further, the raw material used by preparation process, to calculate according to the mass fraction, its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 15 parts,
Hydrogen peroxide 68 parts,
Processing procedure in described reactor, treatment temperature is 60 DEG C, processes time 6h.
Further, the raw material used by preparation process, to calculate according to the mass fraction, its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 26 parts,
Hydrogen peroxide 56 parts,
Processing procedure in described reactor, treatment temperature is 140 DEG C, processes time 12h.
Further, the raw material used by preparation process, to calculate according to the mass fraction, its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 15 parts,
Hydrogen peroxide 62 parts,
Processing procedure in described reactor, treatment temperature is 60 DEG C, processes time 9h.
Further, the raw material used by preparation process, to calculate according to the mass fraction, its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 21 parts,
Hydrogen peroxide 68 parts,
Processing procedure in described reactor, treatment temperature is 100 DEG C, processes time 6h.
The present invention is in the selection of raw material, relative to using ferrous salt/iron salt and phosphoric acid/phosphate as Material synthesis phosphorus
The method of acid ferrum, the preparation method of the iron phosphate dihydrate of the present invention uses reduced iron powder and phosphoric acid as raw material, hydrogen peroxide
As oxidant.In building-up process, ferrum, P elements nearly 100% is obtained by, and reaction occurs without soluble-salt impurity after terminating,
The discharge of non-environmental-pollution the GN 2 oxide, sulfide, carbon monoxide, carbon dioxide etc., has extraordinary environmental protection special
Property；And the cost of raw material is low.
The preparation method of the iron phosphate dihydrate of the present invention uses ball grinding technique refinement intermediate product (reduced iron powder and phosphorus
The insoluble matter ferrous phosphate of acid reaction gained) granule, it is simple to the grain refine of next step reactor processing procedure；Because of product
Middle without soluble impurity, it is not necessary to carry out separating-purifying and sewage disposal, it is not required to through filtration repeatedly, washing process, can be straight
Connect and use spray drying technology by dry materials, obtain the iron phosphate dihydrate with spherical morphology feature simultaneously.Therefore, should
Technical process has the advantages such as granule fine uniform in the synthesis of conventional solution method, good dispersion, grain morphology be easily controllable, simultaneously
Without having to worry about because filtering, washing process produce the process of a large amount of waste water, thus reduce the production cost of iron phosphate dihydrate.
The present invention compares with prior art, and its technological progress is significant.The present invention solves prior art and prepares phosphoric acid
The complex process of iron material, the shortcomings such as production cost is high, Composition Control difficulty.The side preparing iron phosphate dihydrate of the present invention
Method is that a kind of production technology is simple, low cost, and raw material nearly 100% utilizes, the iron phosphate dihydrate synthesis work of pollution-free process
Skill.Use the iron phosphate dihydrate granule fine uniform of method synthesis of the present invention, good dispersion, there is spherical morphology special
Levying, purity is high, can be as the desirable feedstock producing LiFePO 4 material.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of embodiment 1 gained iron phosphate dihydrate.
Fig. 2 is the SEM collection of illustrative plates of embodiment 1 gained iron phosphate dihydrate.
Detailed description of the invention
Below by embodiment and combine accompanying drawing the present invention is described in detail, but it is not limiting as the present invention.
Embodiment 1
A kind of iron phosphate dihydrate (FePO42H2O) preparation method, comprises the steps:
(1) by 115 parts of phosphoric acid 400 parts of deionized waters of addition are configured to phosphoric acid solution, solution temperature 60 is controlledoC.At stirring shape
After being slowly added to 56 parts of reduced iron powder reaction 2h under state, the product of gained adds in ball mill, and ball milling 2h obtains ball milling material
A；
(2) step (1) gained ball milling material A is taken out, be added thereto to 56 parts of hydrogen peroxide, put in reactor after stirring
Processing, temperature is 60 DEG C, and the time is 12h, obtains product B；
(3) it is spray-dried at 170 DEG C after uniform for step (2) gained product B dispersed with stirring, i.e. obtains iron phosphate two water
Compound powder body.
Use the X-ray diffractometer (XRD, Rigaku Rigaku) the iron phosphate dihydrate powder body to embodiment 1 gained
Detecting, gained XRD testing result is as shown in Figure 1.From figure 1 it appears that all of diffraction maximum all can be marked in this collection of illustrative plates
It is set to iron phosphate dihydrate (FePO42H2O) diffraction maximum of standard card PDF#01-072-0464, does not has the peak of other materials
Position occurs, the iron phosphate dihydrate that iron phosphate dihydrate powder body is pure phase using said method to prepare is described
(FePO42H2O)。
Use scanning electron microscope (SEM, NEC 6700F) that the iron phosphate dihydrate powder body of embodiment 1 gained is carried out
Morphology observation, the SEM observed result of gained is as shown in Figure 2.From figure 2 it can be seen that the iron phosphate that said method prepares
Dihydrate presents spherical morphology, and median is at 5 microns, granule fine uniform, good dispersion.The upper right corner in Fig. 2
Illustration is the amplification of single spherical granule, shows that these spheroidal particle are to be reunited by the most tiny micro-nano granules with forming.
Embodiment 2
A kind of iron phosphate dihydrate (FePO42H2O) preparation method, comprises the steps:
(1) by 121 parts of phosphoric acid 400 parts of deionized waters of addition are configured to phosphoric acid solution, solution temperature 60 is controlledoC.At stirring shape
After being slowly added to 56 parts of reduced iron powder reaction 2h under state, the product of gained adds in ball mill, and ball milling 2h obtains ball milling material
A；
(2) step (1) gained ball milling material A is taken out, be added thereto to 62 parts of hydrogen peroxide, put in reactor after stirring
Processing, temperature is 100 DEG C, and the time is 9h, obtains product B；
(3) it is spray-dried at 170 DEG C after uniform for step (2) gained product B dispersed with stirring, i.e. obtains iron phosphate two water
Compound powder body.
Use the X-ray diffractometer (XRD, Rigaku Rigaku) the iron phosphate dihydrate powder body to embodiment 2 gained
Detecting, gained XRD testing result is similar with Fig. 1, and all of diffraction maximum all can be demarcated as iron phosphate dihydrate (FePO4?
2H2O) diffraction maximum of standard card, illustrates to obtain in embodiment 2 the iron phosphate dihydrate (FePO of pure phase42H2O).Use is swept
Retouch Electronic Speculum (SEM, NEC 6700F) and the iron phosphate dihydrate powder body of embodiment 2 gained is carried out morphology observation, gained
SEM observed result is similar with Fig. 2, it is thus achieved that ball shape ferric phosphate dihydrate be similarly more tiny micro-nano granules reunite and
Become.
Embodiment 3
A kind of iron phosphate dihydrate (FePO42H2O) preparation method, comprises the steps:
(1) by 126 parts of phosphoric acid 400 parts of deionized waters of addition are configured to phosphoric acid solution, solution temperature 60 is controlledoC.At stirring shape
After being slowly added to 56 parts of reduced iron powder reaction 2h under state, the product of gained adds in ball mill, and ball milling 2h obtains ball milling material
A；
(2) step (1) gained ball milling material A is taken out, be added thereto to 68 parts of hydrogen peroxide, put in reactor after stirring
Processing, temperature is 140 DEG C, and the time is 6h, obtains product B；
(3) it is spray-dried at 170 DEG C after uniform for step (2) gained product B dispersed with stirring, i.e. obtains iron phosphate two water
Compound powder body.
Use the X-ray diffractometer (XRD, Rigaku Rigaku) the iron phosphate dihydrate powder body to embodiment 3 gained
Detecting, gained XRD testing result is similar with Fig. 1, and all of diffraction maximum all can be demarcated as iron phosphate dihydrate (FePO4?
2H2O) diffraction maximum of standard card, illustrates to obtain in embodiment 3 the iron phosphate dihydrate (FePO of pure phase42H2O).Use is swept
Retouch Electronic Speculum (SEM, NEC 6700F) and the iron phosphate dihydrate powder body of embodiment 3 gained is carried out morphology observation, gained
SEM observed result is similar with Fig. 2, it is thus achieved that ball shape ferric phosphate dihydrate be similarly more tiny micro-nano granules reunite and
Become.
Embodiment 4
A kind of iron phosphate dihydrate (FePO42H2O) preparation method, comprises the steps:
(1) by 121 parts of phosphoric acid 400 parts of deionized waters of addition are configured to phosphoric acid solution, solution temperature 60 is controlledoC.At stirring shape
After being slowly added to 56 parts of reduced iron powder reaction 2h under state, the product of gained adds in ball mill, and ball milling 2h obtains ball milling material
A；
(2) step (1) gained ball milling material A is taken out, be added thereto to 56 parts of hydrogen peroxide, put in reactor after stirring
Processing, temperature is 100 DEG C, and the time is 12h, obtains product B；
(3) it is spray-dried at 170 DEG C after uniform for step (2) gained product B dispersed with stirring, i.e. obtains iron phosphate two water
Compound powder body.
Use the X-ray diffractometer (XRD, Rigaku Rigaku) the iron phosphate dihydrate powder body to embodiment 4 gained
Detecting, gained XRD testing result is similar with Fig. 1, and all of diffraction maximum all can be demarcated as iron phosphate dihydrate (FePO4?
2H2O) diffraction maximum of standard card, illustrates to obtain in embodiment 4 the iron phosphate dihydrate (FePO of pure phase42H2O).Use is swept
Retouch Electronic Speculum (SEM, NEC 6700F) and the iron phosphate dihydrate powder body of embodiment 4 gained is carried out morphology observation, gained
SEM observed result is similar with Fig. 2, it is thus achieved that ball shape ferric phosphate dihydrate be similarly more tiny micro-nano granules reunite and
Become.
Embodiment 5
A kind of iron phosphate dihydrate (FePO42H2O) preparation method, comprises the steps:
(1) by 126 parts of phosphoric acid 400 parts of deionized waters of addition are configured to phosphoric acid solution, solution temperature 60 is controlledoC.At stirring shape
After being slowly added to 56 parts of reduced iron powder reaction 2h under state, the product of gained adds in ball mill, and ball milling 2h obtains ball milling material
A；
(2) step (1) gained ball milling material A is taken out, be added thereto to 62 parts of hydrogen peroxide, put in reactor after stirring
Processing, temperature is 140 DEG C, and the time is 9h, obtains product B；
(3) it is spray-dried at 170 DEG C after uniform for step (2) gained product B dispersed with stirring, i.e. obtains iron phosphate two water
Compound powder body.
Use the X-ray diffractometer (XRD, Rigaku Rigaku) the iron phosphate dihydrate powder body to embodiment 5 gained
Detecting, gained XRD testing result is similar with Fig. 1, and all of diffraction maximum all can be demarcated as iron phosphate dihydrate (FePO4?
2H2O) diffraction maximum of standard card, illustrates to obtain in embodiment 5 the iron phosphate dihydrate (FePO of pure phase42H2O).Use is swept
Retouch Electronic Speculum (SEM, NEC 6700F) and the iron phosphate dihydrate powder body of embodiment 5 gained is carried out morphology observation, gained
SEM observed result is similar with Fig. 2, it is thus achieved that ball shape ferric phosphate dihydrate be similarly more tiny micro-nano granules reunite and
Become.
Embodiment 6
A kind of iron phosphate dihydrate (FePO42H2O) preparation method, comprises the steps:
(1) by 115 parts of phosphoric acid 400 parts of deionized waters of addition are configured to phosphoric acid solution, solution temperature 60 is controlledoC.At stirring shape
After being slowly added to 56 parts of reduced iron powder reaction 2h under state, the product of gained adds in ball mill, and ball milling 2h obtains ball milling material
A；
(2) step (1) gained ball milling material A is taken out, be added thereto to 68 parts of hydrogen peroxide, put in reactor after stirring
Processing, temperature is 60 DEG C, and the time is 6h, obtains product B；
(3) it is spray-dried at 170 DEG C after uniform for step (2) gained product B dispersed with stirring, i.e. obtains iron phosphate two water
Compound powder body.
Use the X-ray diffractometer (XRD, Rigaku Rigaku) the iron phosphate dihydrate powder body to embodiment 6 gained
Detecting, gained XRD testing result is similar with Fig. 1, and all of diffraction maximum all can be demarcated as iron phosphate dihydrate (FePO4?
2H2O) diffraction maximum of standard card, illustrates to obtain in embodiment 6 the iron phosphate dihydrate (FePO of pure phase42H2O).Use is swept
Retouch Electronic Speculum (SEM, NEC 6700F) and the iron phosphate dihydrate powder body of embodiment 6 gained is carried out morphology observation, gained
SEM observed result is similar with Fig. 2, it is thus achieved that ball shape ferric phosphate dihydrate be similarly more tiny micro-nano granules reunite and
Become.
Embodiment 7
A kind of iron phosphate dihydrate (FePO42H2O) preparation method, comprises the steps:
(1) by 126 parts of phosphoric acid 400 parts of deionized waters of addition are configured to phosphoric acid solution, under stirring, 56 parts it are slowly added to
After reduced iron powder reaction 2h, the product of gained adds in ball mill, and ball milling 2h obtains ball milling material A；
(2) step (1) gained ball milling material A is taken out, be added thereto to 56 parts of hydrogen peroxide, put in reactor after stirring
Processing, temperature is 140 DEG C, and the time is 12h, obtains product B；
(3) it is spray-dried at 170 DEG C after uniform for step (2) gained product B dispersed with stirring, i.e. obtains iron phosphate two water
Compound powder body.
Use the X-ray diffractometer (XRD, Rigaku Rigaku) the iron phosphate dihydrate powder body to embodiment 7 gained
Detecting, gained XRD testing result is similar with Fig. 1, and all of diffraction maximum all can be demarcated as iron phosphate dihydrate (FePO4?
2H2O) diffraction maximum of standard card, illustrates to obtain in embodiment 7 the iron phosphate dihydrate (FePO of pure phase42H2O).Use is swept
Retouch Electronic Speculum (SEM, NEC 6700F) and the iron phosphate dihydrate powder body of embodiment 7 gained is carried out morphology observation, gained
SEM observed result is similar with Fig. 2, it is thus achieved that ball shape ferric phosphate dihydrate be similarly more tiny micro-nano granules reunite and
Become.
Embodiment 8
A kind of iron phosphate dihydrate (FePO42H2O) preparation method, comprises the steps:
(1) by 115 parts of phosphoric acid 400 parts of deionized waters of addition are configured to phosphoric acid solution, solution temperature 60 is controlledoC.At stirring shape
After being slowly added to 56 parts of reduced iron powder reaction 2h under state, the product of gained adds in ball mill, and ball milling 2h obtains ball milling material
A；
(2) step (1) gained ball milling material A is taken out, be added thereto to 62 parts of hydrogen peroxide, put in reactor after stirring
Processing, temperature is 60 DEG C, and the time is 9h, obtains product B；
(3) it is spray-dried at 170 DEG C after uniform for step (2) gained product B dispersed with stirring, i.e. obtains iron phosphate two water
Compound powder body.
Use the X-ray diffractometer (XRD, Rigaku Rigaku) the iron phosphate dihydrate powder body to embodiment 8 gained
Detecting, gained XRD testing result is similar with Fig. 1, and all of diffraction maximum all can be demarcated as iron phosphate dihydrate (FePO4?
2H2O) diffraction maximum of standard card, illustrates to obtain in embodiment 8 the iron phosphate dihydrate (FePO of pure phase42H2O).Use is swept
Retouch Electronic Speculum (SEM, NEC 6700F) and the iron phosphate dihydrate powder body of embodiment 8 gained is carried out morphology observation, gained
SEM observed result is similar with Fig. 2, it is thus achieved that ball shape ferric phosphate dihydrate be similarly more tiny micro-nano granules reunite and
Become.
Embodiment 9
A kind of iron phosphate dihydrate (FePO42H2O) preparation method, comprises the steps:
(1) by 121 parts of phosphoric acid 400 parts of deionized waters of addition are configured to phosphoric acid solution, solution temperature 60 is controlledoC.At stirring shape
After being slowly added to 56 parts of reduced iron powder reaction 2h under state, the product of gained adds in ball mill, and ball milling 2h obtains ball milling material
A；
(2) step (1) gained ball milling material A is taken out, be added thereto to 68 parts of hydrogen peroxide, put in reactor after stirring
Processing, temperature is 100 DEG C, and the time is 6h, obtains product B；
(3) it is spray-dried at 170 DEG C after uniform for step (2) gained product B dispersed with stirring, i.e. obtains iron phosphate two water
Compound powder body.
Use the X-ray diffractometer (XRD, Rigaku Rigaku) the iron phosphate dihydrate powder body to embodiment 9 gained
Detecting, gained XRD testing result is similar with Fig. 1, and all of diffraction maximum all can be demarcated as iron phosphate dihydrate (FePO4?
2H2O) diffraction maximum of standard card, illustrates to obtain in embodiment 9 the iron phosphate dihydrate (FePO of pure phase42H2O).Use is swept
Retouch Electronic Speculum (SEM, NEC 6700F) and the iron phosphate dihydrate powder body of embodiment 9 gained is carried out morphology observation, gained
SEM observed result is similar with Fig. 2, it is thus achieved that ball shape ferric phosphate dihydrate be similarly more tiny micro-nano granules reunite and
Become.
In sum, the preparation method of a kind of iron phosphate dihydrate of the present invention, use cheap reduced iron powder and phosphorus
Acid is as raw material, by technical processs such as ball milling, Hydrothermal Synthesis and spray drying, it is thus achieved that the iron phosphate dihydrate material of pure phase
Material.This preparation method production technology is simple, low cost.The iron phosphate dihydrate material purity obtained is high, ferrum, P elements nearly hundred
/ hundred are obtained by, and without waste water and discarded discharge in whole production process.Therefore the iron phosphate dihydrate of the present invention
Preparation method has the advantage of high-purity, low cost and environmental protection.By the pure phase obtained by preparation method of the present invention
Iron phosphate dihydrate presents spherical morphology feature, granule fine uniform.Can be as the ideal producing LiFePO 4 material
Raw material.
Foregoing is only the basic explanation under present inventive concept, and according to technical scheme made any etc.
Effect conversion, all should belong to protection scope of the present invention.
Claims (10)
1. the preparation method of an iron phosphate dihydrate, it is characterised in that comprise the steps:
1) phosphoric acid of 115 ~ 126 weight portions is joined in the deionized water of 400 weight portions, be configured to phosphoric acid solution, keep molten
Liquid temp 50 ~ 65 DEG C, adds the reduced iron powder of 56 weight portions under stirring, and after reaction 1 ~ 3h, the product of gained adds
In ball mill, ball milling, obtain ball milling material；
2) taking-up of above-mentioned ball milling material being positioned in a container, be added thereto to the hydrogen peroxide of 56 ~ 68 weight portions, stirring is all
Putting into after even in reactor and process, treatment temperature is 60 ~ 140 DEG C, and the process time is 6 ~ 12h, obtains product；
3) it is spray-dried at 150 ~ 180 DEG C after uniform for above-mentioned product dispersed with stirring, i.e. obtains iron phosphate two hydration
Thing.
The preparation method of a kind of iron phosphate dihydrate the most as claimed in claim 1, it is characterised in that: used by preparation process
Raw material, calculates according to the mass fraction, and its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 15 parts,
Hydrogen peroxide 56 parts,
Processing procedure in described reactor, treatment temperature is 60 DEG C, processes time 12h.
The preparation method of a kind of iron phosphate dihydrate the most as claimed in claim 1, it is characterised in that: used by preparation process
Raw material, calculates according to the mass fraction, and its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 21 parts,
Hydrogen peroxide 62 parts,
Processing procedure in described reactor, treatment temperature is 100 DEG C, processes time 9h.
The preparation method of a kind of iron phosphate dihydrate the most as claimed in claim 1, it is characterised in that: used by preparation process
Raw material, calculates according to the mass fraction, and its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 26 parts,
Hydrogen peroxide 68 parts,
Processing procedure in described reactor, treatment temperature is 140 DEG C, processes time 6h.
The preparation method of a kind of iron phosphate dihydrate the most as claimed in claim 1, it is characterised in that: used by preparation process
Raw material, calculates according to the mass fraction, and its composition and content are as follows:
Reduced iron powder 56 parts
Phosphatase 11 21 parts,
Hydrogen peroxide 56 parts,
Processing procedure in described reactor, treatment temperature is 100 DEG C, processes time 12h.
The preparation method of a kind of iron phosphate dihydrate the most as claimed in claim 1, it is characterised in that: used by preparation process
Raw material, calculates according to the mass fraction, and its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 26 parts,
Hydrogen peroxide 62 parts,
Processing procedure in described reactor, treatment temperature is 140 DEG C, processes time 9h.
The preparation method of a kind of iron phosphate dihydrate the most as claimed in claim 1, it is characterised in that: used by preparation process
Raw material, calculates according to the mass fraction, and its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 15 parts,
Hydrogen peroxide 68 parts,
Processing procedure in described reactor, treatment temperature is 60 DEG C, processes time 6h.
The preparation method of a kind of iron phosphate dihydrate the most as claimed in claim 1, it is characterised in that: used by preparation process
Raw material, calculates according to the mass fraction, and its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 26 parts,
Hydrogen peroxide 56 parts,
Processing procedure in described reactor, treatment temperature is 140 DEG C, processes time 12h.
The preparation method of a kind of iron phosphate dihydrate the most as claimed in claim 1, it is characterised in that: used by preparation process
Raw material, calculates according to the mass fraction, and its composition and content are as follows:
Reduced iron powder 56 parts,
Phosphatase 11 15 parts,
Hydrogen peroxide 62 parts,
Processing procedure in described reactor, treatment temperature is 60 DEG C, processes time 9h.
The preparation method of a kind of iron phosphate dihydrate the most as claimed in claim 1, it is characterised in that: used by preparation process
Raw material, calculate according to the mass fraction, its composition and content as follows:
Reduced iron powder 56 parts,
Phosphatase 11 21 parts,
Hydrogen peroxide 68 parts,
Processing procedure in described reactor, treatment temperature is 100 DEG C, processes time 6h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106586996A (en) * | 2017-01-25 | 2017-04-26 | 上海应用技术大学 | Preparation method of anhydrous iron phosphate |
| CN106809810A (en) * | 2017-01-25 | 2017-06-09 | 上海应用技术大学 | A kind of preparation method of anhydrous ferric orthophosphate |
| CN106876705A (en) * | 2017-03-31 | 2017-06-20 | 合肥国轩电池材料有限公司 | A kind of preparation method of fabricated in situ carbon/CNT coated lithium iron phosphate composite |
| CN110482512A (en) * | 2019-07-12 | 2019-11-22 | 乳源东阳光磁性材料有限公司 | A kind of preparation method of battery-grade iron phosphate |
| CN111924818A (en) * | 2020-08-21 | 2020-11-13 | 辽宁科技大学 | Preparation method of nanoscale iron phosphate powder |
| CN113526484A (en) * | 2021-08-06 | 2021-10-22 | 唐山亨坤新能源材料有限公司 | Preparation method of lithium iron phosphate, product and application thereof |
| CN114180547A (en) * | 2021-12-31 | 2022-03-15 | 常州锂源新能源科技有限公司 | Preparation method of low-cost high-power lithium iron phosphate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101640268A (en) * | 2009-09-09 | 2010-02-03 | 中南大学 | Preparation method of precursor iron phosphate of cathode material lithium iron phosphate of lithium ion battery |
| CN101913586A (en) * | 2010-08-09 | 2010-12-15 | 中钢集团安徽天源科技股份有限公司 | Preparation method of ferric phosphate and product thereof |
| US20110068295A1 (en) * | 2009-09-18 | 2011-03-24 | A123 Systems, Inc. | Ferric phosphate and methods of preparation thereof |
| CN102544447A (en) * | 2010-12-30 | 2012-07-04 | 北京当升材料科技股份有限公司 | Method for preparing positive electrode material of lithium ion battery |
| CN103208614A (en) * | 2013-04-15 | 2013-07-17 | 上海应用技术学院 | Synthesis method of lithium iron phosphate positive material for lithium ion battery |
-
2016
- 2016-05-11 CN CN201610307885.9A patent/CN105895914A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101640268A (en) * | 2009-09-09 | 2010-02-03 | 中南大学 | Preparation method of precursor iron phosphate of cathode material lithium iron phosphate of lithium ion battery |
| US20110068295A1 (en) * | 2009-09-18 | 2011-03-24 | A123 Systems, Inc. | Ferric phosphate and methods of preparation thereof |
| CN101913586A (en) * | 2010-08-09 | 2010-12-15 | 中钢集团安徽天源科技股份有限公司 | Preparation method of ferric phosphate and product thereof |
| CN102544447A (en) * | 2010-12-30 | 2012-07-04 | 北京当升材料科技股份有限公司 | Method for preparing positive electrode material of lithium ion battery |
| CN103208614A (en) * | 2013-04-15 | 2013-07-17 | 上海应用技术学院 | Synthesis method of lithium iron phosphate positive material for lithium ion battery |
Non-Patent Citations (1)
| Title |
|---|
| 叶焕英: "纳米片磷酸铁和磷酸铁锂的制备与表征", 《中国优秀硕士学位论文全文数据库工程科技Ⅱ辑》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106586996A (en) * | 2017-01-25 | 2017-04-26 | 上海应用技术大学 | Preparation method of anhydrous iron phosphate |
| CN106809810A (en) * | 2017-01-25 | 2017-06-09 | 上海应用技术大学 | A kind of preparation method of anhydrous ferric orthophosphate |
| CN106586996B (en) * | 2017-01-25 | 2019-05-24 | 上海应用技术大学 | A kind of preparation method of anhydrous iron phosphate |
| CN106876705A (en) * | 2017-03-31 | 2017-06-20 | 合肥国轩电池材料有限公司 | A kind of preparation method of fabricated in situ carbon/CNT coated lithium iron phosphate composite |
| CN106876705B (en) * | 2017-03-31 | 2020-06-26 | 合肥国轩电池材料有限公司 | Preparation method of in-situ synthesized carbon/carbon nanotube coated lithium iron phosphate composite material |
| CN110482512A (en) * | 2019-07-12 | 2019-11-22 | 乳源东阳光磁性材料有限公司 | A kind of preparation method of battery-grade iron phosphate |
| CN111924818A (en) * | 2020-08-21 | 2020-11-13 | 辽宁科技大学 | Preparation method of nanoscale iron phosphate powder |
| CN113526484A (en) * | 2021-08-06 | 2021-10-22 | 唐山亨坤新能源材料有限公司 | Preparation method of lithium iron phosphate, product and application thereof |
| CN114180547A (en) * | 2021-12-31 | 2022-03-15 | 常州锂源新能源科技有限公司 | Preparation method of low-cost high-power lithium iron phosphate |
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