CN114084879B - Lithium iron phosphate and production method and application thereof - Google Patents
Lithium iron phosphate and production method and application thereof Download PDFInfo
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- CN114084879B CN114084879B CN202111385552.5A CN202111385552A CN114084879B CN 114084879 B CN114084879 B CN 114084879B CN 202111385552 A CN202111385552 A CN 202111385552A CN 114084879 B CN114084879 B CN 114084879B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/40—Electric properties
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- 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
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Abstract
The invention discloses lithium iron phosphate and a production method and application thereof; the production method of the lithium iron phosphate comprises the following steps: (1) Ferric salt, phytic acid and phosphate are mixed and reacted in water to obtain ferric phosphate precursor liquid; (2) Mixing the ferric phosphate precursor liquid with lithium salt and a carbon source, and then drying and calcining to obtain the lithium iron phosphate. According to the invention, the low-temperature performance of the prepared lithium iron phosphate is obviously improved through the matched use of the phytic acid and the phosphate. Meanwhile, the method directly uses the ferric phosphate precursor liquid for producing the lithium iron phosphate, and compared with the traditional method using the ferric phosphate powder raw material, the method saves the steps of drying and calcining the ferric phosphate, and greatly saves the production cost.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to lithium iron phosphate and a production method and application thereof.
Background
With the continuous decrease of petroleum resources and the increasing pollution of automobile exhaust to the environment worldwide, hybrid Electric Vehicles (HEV) and Electric Vehicles (EV) have become attractive as alternatives to fuel-driven automobiles in the future, and mobile power systems are one of the key components of electric automobiles. Therefore, high performance (i.e., high specific energy, long life, safety), low cost, and environmentally friendly batteries will be an important and hot spot for the development of the mobile power industry. Lithium ion batteries are a new generation of green high-energy rechargeable batteries developed to meet this demand. It has the outstanding advantages of high voltage, small volume, light weight, high specific energy, no memory effect, no pollution, small self-discharge, long service life, etc.
The Padhi et al report that the lithium iron phosphate material with the olivine structure can be used as the positive electrode material of the lithium ion battery in 1997, and the lithium iron phosphate material is one of the positive electrode materials with the highest potential at present because of the advantages of low price, environmental protection, no pollution, no moisture absorption, good thermal stability and the like, and is concerned by vast scientific research institutions and commercial institutions. In recent years, a lot of research, development and improvement are carried out on the material by many scientific researchers, and the material is gradually commercialized and applied to the markets of high-capacity, high-power and long-service-life lithium ion batteries. Lithium iron phosphate represents a future development of positive electrode materials for power cells.
At present, a solid-phase synthesis method is a main method for preparing commercial lithium iron phosphate, but the defects of high cost of ferrous iron source, difficult preservation, large particle size of synthesized lithium iron phosphate, poor uniformity and the like are difficult to meet the requirements of a power type lithium ion battery. Therefore, ferric iron with low cost and stable performance is adopted to replace ferrous iron as an iron source, and synthetic ferric phosphate is adopted as a precursor to prepare the lithium iron phosphate. The synthesis method of the synthesized ferric phosphate generally comprises the steps of reacting ferric trichloride or ferric nitrate solution with phosphoric acid, and then decomposing and volatilizing hydrogen chloride or nitric acid at high temperature to obtain the ferric phosphate.
However, lithium iron phosphate has low electron conductivity and ion diffusion rate at room temperature of 10 due to its inherent characteristics (respectively -8 -10 -10 S/cm and 10 -12 -10 -14 cm 2 S) results in a significant degradation of the charge and discharge properties of the lithium iron phosphate as a positive electrode material at low temperatures.
Disclosure of Invention
The invention aims to provide lithium iron phosphate, a production method and application thereof, which can obviously improve the low-temperature performance of the lithium iron phosphate.
In order to achieve the above purpose, the present invention adopts the technical scheme that:
the invention discloses a production method of lithium iron phosphate, which comprises the following steps:
(1) Ferric salt, phytic acid and phosphate are mixed and reacted in water to obtain ferric phosphate precursor liquid;
(2) Mixing the ferric phosphate precursor liquid obtained in the step (1) with lithium salt and a carbon source, and then drying and calcining to obtain lithium iron phosphate.
As a preferred technical scheme, in the step (1), the ferric salt includes, but is not limited to, one or a mixture of ferric chloride, ferric nitrate and ferric sulfate.
As a preferred embodiment, in the step (1), the phosphate includes, but is not limited to, H 3 PO 4 、(NH 4 ) 3 PO 4 、(NH 4 ) 2 HPO 4 、(NH 4 )H 2 PO 4 One or more of the following.
As a preferable technical scheme, in the step (1), the molar ratio of the phytic acid to the phosphate is 1:999-999:1.
In the step (1), alkali liquor is added into the reaction system to control the pH value to be less than 7.
As a preferred technical scheme, the alkali liquor comprises one or a mixture of more than one of ammonia water, sodium hydroxide solution, sodium acetate solution and ammonium acetate solution.
In a preferred embodiment, in the step (1), the reaction is a normal temperature reaction.
As a preferred technical scheme, in the step (2), the lithium salt includes, but is not limited to, one or more of lithium carbonate, lithium hydroxide, lithium nitrate and lithium oxalate.
As a preferred technical scheme, in the step (2), the carbon source includes, but is not limited to, one or a mixture of several of glucose, sucrose, carbon nanotubes and graphene.
The invention also discloses application of the lithium iron phosphate produced by the production method in a positive electrode material of a lithium ion battery.
The invention has the beneficial effects that:
the invention utilizes phytic acid and phosphate to form phosphate groups as a phosphorus source, synthesizes ferric phosphate with ferric salt, and then directly mixes ferric phosphate precursor liquid with lithium salt and a carbon source to prepare lithium iron phosphate. According to the invention, the low-temperature performance of the prepared lithium iron phosphate is obviously improved through the matched use of the phytic acid and the phosphate. Meanwhile, the method directly uses the ferric phosphate precursor liquid for producing the lithium iron phosphate, and compared with the traditional method using the ferric phosphate powder raw material, the method saves the steps of drying and calcining the ferric phosphate, and greatly saves the production cost.
Drawings
FIG. 1 is a process flow diagram for preparing lithium iron phosphate from ferric salts;
FIG. 2 is a block diagram of an apparatus for preparing lithium iron phosphate from a ferric salt;
FIG. 3 is an SEM image of lithium iron phosphate of example 1;
FIG. 4 is a graph showing the 0.2C discharge capacity at-20℃of the soft-pack battery made of lithium iron phosphate of example 1;
FIG. 5 is a graph showing the 0.2C discharge capacity at-20℃of the soft-pack battery made of lithium iron phosphate of example 2;
fig. 6 is a graph showing the 0.2C discharge capacity at-20C of the soft pack battery fabricated from the lithium iron phosphate of comparative example 1.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent.
Example 1
As shown in fig. 1 to 2, lithium iron phosphate was prepared by the following steps:
(1) Ferric chloride solution, phytic acid, (NH) 4 )H 2 PO 4 Adding ammonia water into the reaction kettle, and controlling phytic acid and (NH) 4 )H 2 PO 4 The molar ratio of (2) is 1:99, controlling the addition amount of ammonia water to adjust the pH value of the system to about 2, and then mixing and stirring the mixture in a reaction kettle at normal temperature for reaction for 1 hour; and pumping the reaction slurry into an aging kettle for aging for 1 hour to obtain ferric phosphate precursor liquid.
(2) Adding lithium carbonate and glucose into an aging kettle, fully mixing and dispersing the lithium carbonate and the glucose with ferric phosphate precursor liquid, and pumping the obtained mixed slurry into a finished product tank for temporary storage; and pumping the mixed slurry into a plate-and-frame filter for filtering, adding the wet material into a flash evaporation dryer for flash evaporation drying, and adding the wet material into a rotary kiln for calcination to obtain the lithium iron phosphate.
Example 2
As shown in fig. 1 to 2, lithium iron phosphate was prepared by the following steps:
(1) Ferric chloride solution, phytic acid and H 3 PO 4 Adding ammonia water into the reaction kettle, and controlling phytic acid and H 3 PO 4 The molar ratio of (2) is 1:99, controlling the addition amount of ammonia water to adjust the pH value of the system to about 2, and then mixing and stirring the mixture in a reaction kettle at normal temperature for reaction for 1 hour; and pumping the reaction slurry into an aging kettle for aging for 1 hour to obtain ferric phosphate precursor liquid.
(2) Adding lithium carbonate and glucose into an aging kettle, fully mixing and dispersing the lithium carbonate and the glucose with ferric phosphate precursor liquid, and pumping the obtained mixed slurry into a finished product tank for temporary storage; and pumping the mixed slurry into a plate-and-frame filter for filtering, adding the wet material into a flash evaporation dryer for flash evaporation drying, and adding the wet material into a rotary kiln for calcination to obtain the lithium iron phosphate.
Comparative example 1
The lithium iron phosphate is prepared by the following steps:
(1) Ferric chloride solution, H 3 PO 4 Adding ammonia water into a reaction kettle, controlling the adding amount of the ammonia water to adjust the pH value of the system to about 2, and then mixing and stirring the ammonia water in the reaction kettle at normal temperature for reaction for 1 hour; and pumping the reaction slurry into an aging kettle for aging for 1 hour to obtain ferric phosphate precursor liquid.
(2) Adding lithium carbonate and glucose into an aging kettle, fully mixing and dispersing the lithium carbonate and the glucose with ferric phosphate precursor liquid, and pumping the obtained mixed slurry into a finished product tank for temporary storage; and pumping the mixed slurry into a plate-and-frame filter for filtering, adding the wet material into a flash evaporation dryer for flash evaporation drying, and adding the wet material into a rotary kiln for calcination to obtain the lithium iron phosphate.
Fig. 3 is an SEM image of the lithium iron phosphate prepared in example 1, and it can be seen from the figure that the lithium iron phosphate prepared in example 1 has a uniform particle size.
The lithium iron phosphate prepared in example 1, example 2 and comparative example 1 were used as positive electrode materials, respectively, and positive electrode sheets were prepared first: and (3) carrying out positive electrode material proportioning on the positive electrode material, the binder and the conductive agent to obtain uniform positive electrode slurry, and uniformly coating the prepared positive electrode slurry on a positive electrode current collector aluminum foil to obtain a positive electrode plate. And winding the positive plate, the negative plate and the diaphragm to prepare a lithium ion battery core, and injecting electrolyte to prepare the soft-package battery.
FIG. 4 is a graph showing that the discharge capacity of the soft-pack battery prepared from the lithium iron phosphate of example 1 at-20 ℃ reaches 688mAh at-20 ℃.
FIG. 5 is a graph showing that the discharge capacity of the soft-pack battery prepared from the lithium iron phosphate of example 2 at-20 ℃ reaches 596mAh at-20 ℃.
FIG. 6 is a graph showing that the discharge capacity of the soft pack battery prepared from the lithium iron phosphate of comparative example 1 at-20 ℃ is 0.2C, and the discharge capacity of the soft pack battery at-20 ℃ can reach 455mAh.
As can be seen from the comparison, compared with the comparison example using only phosphoric acid, the low-temperature performance of the prepared lithium iron phosphate is obviously improved through the matched use of the phytic acid and the phosphate.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A production method of lithium iron phosphate is characterized in that: the method comprises the following steps:
(1) Ferric salt, phytic acid and phosphate are mixed and reacted in water to obtain ferric phosphate precursor liquid;
(2) Mixing the ferric phosphate precursor liquid obtained in the step (1) with lithium salt and a carbon source, and then drying and calcining to obtain lithium iron phosphate;
in the step (1), the molar ratio of the phytic acid to the phosphate is 1:999-1:99.
2. The method for producing lithium iron phosphate according to claim 1, characterized in that: in the step (1), the ferric salt comprises one or a mixture of several of ferric chloride, ferric nitrate and ferric sulfate.
3. The method for producing lithium iron phosphate according to claim 1, characterized in that: in step (1), the phosphate includes, but is not limited to, H 3 PO 4 、(NH 4 ) 3 PO 4 、(NH 4 ) 2 HPO 4 、(NH 4 )H 2 PO 4 One or more of the following.
4. The method for producing lithium iron phosphate according to claim 1, characterized in that: in the step (1), alkali liquor is added into the reaction system, and the pH value is controlled to be less than 7.
5. The method for producing lithium iron phosphate according to claim 4, wherein: the alkali liquor comprises one or a mixture of several of ammonia water, sodium hydroxide solution, sodium acetate solution and ammonium acetate solution.
6. The method for producing lithium iron phosphate according to claim 1, characterized in that: in the step (1), the reaction is a normal temperature reaction.
7. The method for producing lithium iron phosphate according to claim 1, characterized in that: in the step (2), the lithium salt comprises one or a mixture of several of lithium carbonate, lithium hydroxide, lithium nitrate and lithium oxalate.
8. The method for producing lithium iron phosphate according to claim 1, characterized in that: in the step (2), the carbon source includes, but is not limited to, one or a mixture of several of glucose, sucrose, carbon nanotubes and graphene.
9. Use of lithium iron phosphate produced by the production method of any one of claims 1 to 8 in a positive electrode material of a lithium ion battery.
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