CN108183234B - Preparation method of lithium iron phosphate/carbon composite material - Google Patents
Preparation method of lithium iron phosphate/carbon composite material Download PDFInfo
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- CN108183234B CN108183234B CN201810010936.0A CN201810010936A CN108183234B CN 108183234 B CN108183234 B CN 108183234B CN 201810010936 A CN201810010936 A CN 201810010936A CN 108183234 B CN108183234 B CN 108183234B
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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
- 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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
Abstract
The invention relates to a preparation method of a lithium iron phosphate/carbon composite material, which comprises the following steps: (1) preparing a ferrous iron source solution from a ferrous iron source and water, and preparing a phosphorus source solution from a phosphorus source and water; (2) dropwise adding the prepared ferrous iron source solution, phosphorus source solution, oxidant and precipitator into a reaction kettle, and fully reacting to obtain ferric phosphate dihydrate slurry; (3) filtering the ferric phosphate dihydrate slurry obtained by the reaction into a ferric phosphate dihydrate filter cake by using a filter press; (4) adding the obtained ferric phosphate dihydrate filter cake, a lithium source and a carbon source into water, stirring and dispersing, transferring the dispersed slurry into a sanding device for grinding, spray-drying the ground slurry, feeding the dried material into an inert atmosphere furnace for calcining, and calcining to obtain the lithium iron phosphate/carbon composite material. The preparation method has the advantages of short process flow, low equipment investment cost, low energy consumption and capability of ensuring the electrical property of the product.
Description
Technical Field
The invention relates to the technical field of preparation of lithium battery anode materials, in particular to a preparation method of a lithium iron phosphate/carbon composite material.
Background
Lithium iron phosphate/carbon (LiFePO)4the/C) composite material is a lithium battery anode material, and is widely applied to power supplies of equipment such as electric tools, miner lamps, electric bicycles, electric automobiles, hybrid electric vehicles, satellites, weaponry and the like because the composite material has the advantages of no toxicity, environmental friendliness, high specific capacity, good cycling stability and the like.
At present, iron phosphate is mostly adopted as a precursor for preparing the lithium iron phosphate/carbon composite material, and because the iron and phosphorus contents of iron phosphate purchased from the market after being placed for a period of time are difficult to determine and are inconvenient to prepare, the iron phosphate generally needs to be dried or directly prepared on site for use. The mainstream preparation process of the lithium iron phosphate/carbon composite material comprises the following steps: preparing iron phosphate dihydrate slurry, filtering, washing and drying the iron phosphate dihydrate slurry, removing crystal water at high temperature to obtain precursor anhydrous iron phosphate, mixing the anhydrous iron phosphate, a lithium source, a carbon source and a solvent, grinding the mixed slurry, spray drying and sintering at high temperature to obtain the lithium iron phosphate/carbon composite material.
However, the above preparation process has the following drawbacks: firstly, the process flow is long, the equipment investment is high, and the energy consumption is high, mainly because the dihydrate ferric phosphate slurry needs to be dried by using a flash dryer, after drying, the crystal water needs to be removed by using a high-temperature dehydration furnace to prepare the anhydrous ferric phosphate, the equipment investment of the flash dryer and the high-temperature dehydration furnace is high, and a large amount of electric energy and natural gas need to be consumed; and secondly, the particle size of the material is not controlled, and the prepared lithium iron phosphate/carbon composite material has poor performance, because the dihydrate ferric phosphate particles can generate grain boundary fusion during drying, particularly high-temperature dehydration, so that the dehydrated anhydrous ferric phosphate primary particles are enlarged, the finally obtained lithium iron phosphate/carbon composite material has overlarge particles to reduce the rate performance and low-temperature performance, the time required by grinding is prolonged due to the overlarge anhydrous ferric phosphate particles, the energy consumption is increased, and the productivity is reduced.
Therefore, it is very important to develop a preparation process which has short process flow, low equipment investment and low energy consumption and can improve the performance of the lithium iron phosphate/carbon composite material.
Disclosure of Invention
Based on the above, the invention aims to provide a preparation method of a lithium iron phosphate/carbon composite material, which has the advantages of short process flow, low equipment investment cost, low energy consumption and capability of ensuring the electrical performance of a product.
The technical scheme adopted by the invention is as follows:
a preparation method of a lithium iron phosphate/carbon composite material comprises the following steps:
(1) preparing a ferrous iron source solution from a ferrous iron source and water, and preparing a phosphorus source solution from a phosphorus source and water;
(2) dropwise adding the prepared ferrous iron source solution, phosphorus source solution, oxidant and precipitator into a reaction kettle, and fully reacting to obtain ferric phosphate dihydrate slurry;
(3) filtering the ferric phosphate dihydrate slurry obtained by the reaction into a ferric phosphate dihydrate filter cake by using a filter press;
(4) adding the obtained ferric phosphate dihydrate filter cake, a lithium source and a carbon source into water, stirring and dispersing, transferring the dispersed slurry into a sanding device for grinding, spray-drying the ground slurry, feeding the dried material into an inert atmosphere furnace for calcining, and calcining to obtain the lithium iron phosphate/carbon composite material.
Compared with the method adopting anhydrous ferric phosphate as a precursor, the method adopts the dihydrate ferric phosphate filter cake which is not dried and dehydrated as the precursor, and the dihydrate ferric phosphate filter cake does not need to be dried by a flash dryer and crystal water is removed by a high-temperature dehydration furnace, so that the process flow is greatly shortened, and the equipment investment and the production energy consumption are reduced. And secondly, the ferric phosphate dihydrate is not subjected to flash drying, so that the damage of the flash drying process to the appearance of the ferric phosphate dihydrate particles is avoided, the crystal water of the ferric phosphate dihydrate is not removed at high temperature, and the growth of primary particles due to crystal boundary fusion caused by high-temperature dehydration is avoided, so that the appearance of the primary particles of the ferric phosphate dihydrate is fine, the integrity of secondary particles formed by agglomeration of the primary particles is ensured, and the rate capability and the low-temperature performance of the final lithium iron phosphate/carbon composite material product are improved. Moreover, because the primary particles of the ferric phosphate dihydrate filter cake are fine, the time required by the subsequent grinding procedure to reach the particle size standard is shorter, the grinding efficiency is further improved, and the energy consumption of the sanding equipment is saved.
Under the same carbon content, the lithium iron phosphate/carbon composite material product prepared by the preparation method disclosed by the invention has the advantages that the charge and discharge capacity, the multiplying power, the powder resistance and other properties are better than those of a product prepared by taking anhydrous iron phosphate as a precursor, and the product has better conductivity, multiplying power performance and low-temperature performance.
Compared with the method of directly adopting the ferric phosphate dihydrate as the precursor, the method adopts the ferric phosphate dihydrate filter cake which is not dried and has certain water content as the precursor, avoids the severe damage to the shape of the ferric phosphate dihydrate particles in the flash drying process, is favorable for improving the electrical property of the lithium iron phosphate/carbon composite material product, and simultaneously reduces the treatment cost of the ferric phosphate dihydrate.
The invention breaks through the design idea of the conventional process route which uses the iron phosphate which is completely dried or dehydrated at high temperature as the precursor, changes the design idea into the design idea that uses the filter cake of the ferric phosphate dihydrate which is not dried or dehydrated at high temperature as the precursor, and realizes the technical effects of reducing the production cost and improving the product performance.
Further, in the step (1), the ferrous iron source is ferrous sulfate, and the iron content of the prepared ferrous iron source solution is 5-7% by mass percent.
Further, in the step (1), the phosphorus source is one or more of ammonium dihydrogen phosphate, diammonium hydrogen phosphate and phosphoric acid, and the phosphorus content of the prepared phosphorus source solution is 4-6% by mass percent.
Further, in the step (2), the oxidant is one or two of hydrogen peroxide and peroxyacetic acid, and the precipitant is one or more of ammonia water, sodium hydroxide and urea.
Further, in the step (2), the ratio of iron (Fe) in the ferrous iron source solution is determined according to the ratio of iron (Fe): phosphorus (P) in the phosphorus source solution: the molar ratio of the oxidant is 0.97-1: 1-1.05: 0.5-0.7, and simultaneously dropwise adding the ferrous iron source solution, the phosphorus source solution, the oxidant and the precipitator into the reaction kettle.
Further, in the step (2), the stirring speed of the reaction kettle is 200-600 rpm, the pH value of the reaction slurry is controlled within 1.8-2.2, the reaction temperature is controlled within 90-100 ℃, and the reaction time is 2-6 hours.
Further, the step (3) is as follows: filtering the ferric phosphate dihydrate slurry obtained by the reaction by using a filter press to obtain a ferric phosphate dihydrate filter cake, washing the ferric phosphate dihydrate filter cake by using pure water, and pressing the ferric phosphate dihydrate filter cake to a water content of 30-40%, preferably, pressing the ferric phosphate dihydrate filter cake to a water content of 35 +/-2%.
And (3) limiting the water content of the ferric phosphate dihydrate filter cake within a proper range, on one hand, ensuring that the filter press is easy to realize, and on the other hand, controlling the iron and phosphorus contents in the ferric phosphate dihydrate filter cake, and reducing the dosage in the subsequent step (4), thereby reducing the material handling capacity and reducing the production energy consumption.
Further, in the step (4), the lithium source is one or two of lithium carbonate and lithium hydroxide, and the carbon source is one or more of glucose, sucrose and starch.
Furthermore, in the step (4), the grinding medium filled in the sanding equipment is zirconia with the granularity of 0.2-0.5 mm, the grinding time is 1-4 hours, and the granularity of ground slurry is 0.2-0.4 μm.
Further, in the step (4), the calcining temperature is 600-800 ℃, and the calcining time is 4-6 hours.
For a better understanding and practice, the invention is described in detail below with reference to the accompanying drawings.
Drawings
FIG. 1 is an SEM electron micrograph of an iron phosphate dihydrate filter cake obtained in step (3) of example 1;
FIG. 2 is an SEM electron micrograph of dried ferric phosphate dihydrate;
FIG. 3 is an SEM electron micrograph of the anhydrous iron phosphate obtained in step (3) of the comparative example.
Detailed Description
Example 1
The preparation method of the lithium iron phosphate/carbon composite material comprises the following steps:
(1) ferrous sulfate is put into a dissolving tank filled with water to prepare a ferrous sulfate solution with the iron content of 5.8 percent (by mass percentage). Ammonium dihydrogen phosphate is put into a dissolving tank filled with water to prepare an ammonium dihydrogen phosphate solution with the phosphorus content of 4.6 percent (by mass percentage).
(2) Dropwise adding 2320kg of prepared ferrous sulfate solution, 1700kg of ammonium dihydrogen phosphate solution, 160kg of hydrogen peroxide with the mass concentration of 30% and 7kg of ammonia water with the mass concentration of 25% into a reaction kettle with the stirring speed of 600rpm simultaneously for reaction, controlling the pH value of the reaction slurry to be 2.1, controlling the reaction temperature to be 90 ℃, and reacting for 4 hours to obtain the ferric phosphate dihydrate slurry.
(3) Filtering the ferric phosphate dihydrate slurry obtained by the reaction by using a vertical filter press to obtain a ferric phosphate dihydrate filter cake, washing the ferric phosphate dihydrate filter cake by using pure water until the conductivity of washing liquor is 400 mu S/cm, and pressing the ferric phosphate dihydrate filter cake to the water content of 35% (by mass percentage) by using the water pressure of 0.7 Mpa.
(4) 800kg of ferric phosphate dihydrate filter cake with 35% of water content, 99kg of lithium carbonate and 40kg of glucose are added into a 700kg stirring kettle filled with water, after stirring and dispersing for 1 hour, the dispersed slurry is transferred into a sanding device filled with zirconia grinding media with the granularity of 0.2mm for grinding for 4 hours, so that the granularity D of the slurry is ensured50And (3) spray-drying the ground slurry to 0.25 mu m, feeding the dried material into a nitrogen atmosphere furnace, calcining at the constant temperature of 780 ℃ for 6 hours, and cooling to room temperature in the nitrogen atmosphere furnace to obtain the lithium iron phosphate/carbon composite material.
Example 2
The preparation method of the lithium iron phosphate/carbon composite material comprises the following steps:
(1) ferrous sulfate is put into a dissolving tank filled with water to prepare a ferrous sulfate solution with the iron content of 6 percent (by mass percentage). The phosphoric acid is put into a dissolving tank filled with water to prepare a phosphoric acid solution with 5 percent of phosphorus content (by mass percent).
(2) And simultaneously dropwise adding 2240kg of prepared ferrous sulfate solution, 1500kg of phosphoric acid solution, 160kg of hydrogen peroxide with the mass concentration of 30% and 10kg of ammonia water with the mass concentration of 25% into a reaction kettle with the stirring speed of 500rpm for reaction, controlling the pH value of the reaction slurry to be 2.2, controlling the reaction temperature to be 95 ℃, and reacting for 3.5 hours to obtain the ferric phosphate dihydrate slurry.
(3) Filtering the ferric phosphate dihydrate slurry obtained by the reaction by using a vertical filter press to obtain a ferric phosphate dihydrate filter cake, washing the ferric phosphate dihydrate filter cake by using pure water until the conductivity of washing liquor is 400 mu S/cm, and pressing the ferric phosphate dihydrate filter cake to the water content of 40% (by mass percent) by using the water pressure of 0.7 Mpa.
(4) 840kg of ferric phosphate dihydrate filter cake with the water content of 40 percent, 100kg of lithium carbonate and 40kg of glucose are added into a 600kg stirring kettle filled with water, after stirring and dispersing for 1.5 hours, the dispersed slurry is transferred into a sanding device filled with zirconia grinding media with the granularity of 0.3mm for grinding for 3.5 hours, so that the granularity D of the slurry is ensured50And (3) spray-drying the ground slurry to 0.25 mu m, feeding the dried material into a nitrogen atmosphere furnace, calcining at the constant temperature of 780 ℃ for 6 hours, and cooling to room temperature in the nitrogen atmosphere furnace to obtain the lithium iron phosphate/carbon composite material.
Example 3
The preparation method of the lithium iron phosphate/carbon composite material comprises the following steps:
(1) ferrous sulfate is put into a dissolving tank filled with water to prepare a ferrous sulfate solution with the iron content of 6.5 percent (by mass percentage). Adding diammonium phosphate into a dissolving tank filled with water to prepare a diammonium phosphate solution with the phosphorus content of 5.5 percent (by mass percentage).
(2) Dropwise adding 2070kg of prepared ferrous sulfate solution, 1350kg of diammonium phosphate solution, 160kg of hydrogen peroxide with the mass concentration of 30% and 5kg of ammonia water with the mass concentration of 25% into a reaction kettle with the stirring speed of 600rpm simultaneously for reaction, controlling the pH value of the reaction slurry to be 1.8, controlling the reaction temperature to be 95 ℃, and reacting for 4 hours to obtain the ferric phosphate dihydrate slurry.
(3) Filtering the ferric phosphate dihydrate slurry obtained by the reaction by using a vertical filter press to obtain a ferric phosphate dihydrate filter cake, washing the ferric phosphate dihydrate filter cake by using pure water until the conductivity of washing liquor is 400 mu S/cm, and pressing the ferric phosphate dihydrate filter cake to the water content of 30% (by mass percentage) by using the water pressure of 0.7 Mpa.
(4) 720kg of ferric phosphate dihydrate filter cake with the water content of 30 percent, 100kg of lithium carbonate and 40kg of glucose are added into a 780kg stirring kettle filled with water, after stirring and dispersing for 1 hour, the dispersed slurry is transferred into a sanding device filled with zirconia grinding media with the granularity of 0.5mm for grinding for 3.5 hours, so that the granularity D of the slurry is ensured500.25 μm, followed by spray drying the ground slurry,and then feeding the dried material into a nitrogen atmosphere furnace, calcining for 6 hours at the constant temperature of 780 ℃, and cooling the nitrogen atmosphere furnace to room temperature to obtain the lithium iron phosphate/carbon composite material.
Comparative example
The steps for preparing the lithium iron phosphate/carbon composite material in the comparative example are as follows:
(1) ferrous sulfate is put into a dissolving tank filled with water to prepare a ferrous sulfate solution with the iron content of 6.5 percent (by mass percentage). Adding diammonium phosphate into a dissolving tank filled with water to prepare a diammonium phosphate solution with the phosphorus content of 6 percent (by mass percentage).
(2) Dropwise adding 2070kg of prepared ferrous sulfate solution, 1240kg of diammonium phosphate solution, 160kg of hydrogen peroxide with the mass concentration of 30% and 5.5kg of ammonia water with the mass concentration of 25% into a reaction kettle with the stirring speed of 600rpm simultaneously for reaction, controlling the pH value of the reaction slurry to be 2.0, controlling the reaction temperature to be 100 ℃, and reacting for 4 hours to obtain the ferric phosphate dihydrate slurry.
(3) Filtering the ferric phosphate dihydrate slurry obtained by the reaction by using a vertical filter press to obtain a ferric phosphate dihydrate filter cake, washing the ferric phosphate dihydrate filter cake by using pure water until the conductivity of washing liquor is 400 mu S/cm, and pressing the ferric phosphate dihydrate filter cake to the water content of 32% (by mass percentage) by using the water pressure of 0.7 Mpa. And then, drying the filter cake of the ferric phosphate dihydrate by using a flash evaporation dryer until the water content is lower than 1%, and then conveying the filter cake of the ferric phosphate dihydrate into a muffle furnace to keep the temperature at 550 ℃ for 4 hours so as to fully remove crystal water and obtain the anhydrous ferric phosphate.
(4) Adding 400kg of anhydrous ferric phosphate filter cake, 100kg of lithium carbonate and 40kg of glucose into a 1100kg stirring kettle filled with water, stirring and dispersing for 2 hours, transferring the dispersed slurry into a sanding device filled with zirconia grinding media with the granularity of 0.5mm, and grinding for 10 hours to ensure that the slurry granularity D is D50And (3) spray-drying the ground slurry to 0.25 mu m, feeding the dried material into a nitrogen atmosphere furnace, calcining at the constant temperature of 780 ℃ for 6 hours, and cooling to room temperature in the nitrogen atmosphere furnace to obtain the lithium iron phosphate/carbon composite material.
The lithium iron phosphate/carbon composite material samples prepared in examples 1 to 3 and the comparative example were subjected to performance tests, and the test results are shown in the following table.
From the above table, under different discharge rates, the specific discharge capacities of the samples of examples 1 to 3 are all larger than those of the samples of the comparative example, and the low-temperature retention rates of the samples of examples 1 to 3 at-20 ℃ are also obviously higher than those of the samples of the comparative example, which indicates that the lithium iron phosphate/carbon composite material product prepared by the preparation method of the present invention has more excellent conductivity, rate capability and low-temperature performance.
Examples 1-3 omit the procedure of flash dryer drying and high temperature dehydration furnace to remove the crystal water, so the total energy consumption of flash drying and high temperature dehydration is 0, while the energy consumption of flash drying and high temperature dehydration treatment for each ton of dihydrate ferric phosphate filter cake is as high as 1800kWh, which shows that the preparation method of the invention can significantly reduce the energy consumption of production. While the grinding time required for examples 1-3 to achieve the same ground particle size of 0.25 μm was less than half that of the comparative example, indicating that the preparation process of the present invention has a higher grinding efficiency and lower energy consumption of the sanding equipment.
In addition, as can be seen from comparing fig. 1 and fig. 2, the primary particles in the filter cake of ferric phosphate dihydrate obtained in step (3) in example 1 are fine, the size is below 50nm, the specific surface area is large, and the grain boundary and the morphology are complete, while the particles of ferric phosphate dihydrate subjected to drying treatment are significantly larger, the size is above several hundred nanometers, the specific surface area is small, and the grain boundary and the morphology are incomplete, which indicates that drying damages the particle morphology of ferric phosphate dihydrate.
As can be seen from comparison of fig. 1 and fig. 3, the primary particles in the iron phosphate dihydrate filter cake obtained in step (3) in example 1 are fine, the size is below 50nm, the specific surface area is large, the grain boundary is complete, and the morphology is complete, whereas the primary particles of the anhydrous iron phosphate obtained in step (3) in the comparative example grow up due to grain boundary fusion caused by high-temperature dehydration, so the particles are significantly larger, the size is more than several hundred nanometers, and the specific surface area is small, which indicates that the preparation method of the present invention can ensure that the iron phosphate dihydrate primary particles are fine and complete in morphology, and is more favorable for improving the electrical properties of the final lithium iron phosphate/carbon composite material product.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (9)
1. A preparation method of a lithium iron phosphate/carbon composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a ferrous iron source solution from a ferrous iron source and water, and preparing a phosphorus source solution from a phosphorus source and water;
(2) dropwise adding the prepared ferrous iron source solution, phosphorus source solution, oxidant and precipitator into a reaction kettle, and fully reacting to obtain ferric phosphate dihydrate slurry;
(3) filtering the ferric phosphate dihydrate slurry obtained by the reaction into a ferric phosphate dihydrate filter cake by using a filter press; filtering the ferric phosphate dihydrate slurry obtained by reaction by using a filter press to obtain a ferric phosphate dihydrate filter cake, washing the ferric phosphate dihydrate filter cake by using pure water, and pressing the ferric phosphate dihydrate filter cake until the water content is 30-40%;
(4) adding the obtained ferric phosphate dihydrate filter cake, a lithium source and a carbon source into water, stirring and dispersing, transferring the dispersed slurry into a sanding device for grinding, spray-drying the ground slurry, feeding the dried material into an inert atmosphere furnace for calcining, and calcining to obtain the lithium iron phosphate/carbon composite material.
2. The method for preparing a lithium iron phosphate/carbon composite material according to claim 1, characterized in that: in the step (1), the ferrous iron source is ferrous sulfate, and the iron content of the prepared ferrous iron source solution is 5-7% by mass percent.
3. The method for preparing a lithium iron phosphate/carbon composite material according to claim 1, characterized in that: in the step (1), the phosphorus source is one or more of ammonium dihydrogen phosphate, diammonium hydrogen phosphate and phosphoric acid, and the phosphorus content of the prepared phosphorus source solution is 4-6% by mass percent.
4. The method for preparing a lithium iron phosphate/carbon composite material according to claim 1, characterized in that: in the step (2), the oxidant is one or two of hydrogen peroxide and peroxyacetic acid, and the precipitator is one or more of ammonia water, sodium hydroxide and urea.
5. The method for preparing a lithium iron phosphate/carbon composite material according to claim 4, characterized in that: in the step (2), according to the iron in the ferrous iron source solution: phosphorus in the phosphorus source solution: the molar ratio of the oxidant is 0.97-1: 1-1.05: 0.5-0.7, and simultaneously dropwise adding the ferrous iron source solution, the phosphorus source solution, the oxidant and the precipitator into the reaction kettle.
6. The method for preparing a lithium iron phosphate/carbon composite material according to claim 5, characterized in that: in the step (2), the stirring speed of the reaction kettle is 200-600 rpm, the pH value of the reaction slurry is controlled within 1.8-2.2, the reaction temperature is controlled within 90-100 ℃, and the reaction time is 2-6 hours.
7. The method for preparing a lithium iron phosphate/carbon composite material according to claim 1, characterized in that: in the step (4), the lithium source is one or two of lithium carbonate and lithium hydroxide, and the carbon source is one or more of glucose, sucrose and starch.
8. The method for preparing a lithium iron phosphate/carbon composite material according to claim 7, characterized in that: in the step (4), the grinding medium filled in the sanding equipment is zirconia with the granularity of 0.2-0.5 mm, the grinding time is 1-4 hours, and the granularity of ground slurry is 0.2-0.4 μm.
9. The method for preparing a lithium iron phosphate/carbon composite material according to claim 7, characterized in that: in the step (4), the calcining temperature is 600-800 ℃, and the calcining time is 4-6 hours.
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| 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 |
| CN101807692A (en) * | 2010-04-30 | 2010-08-18 | 湖南格林新能源有限公司 | Preparation method of lithium ion battery positive material of ferric metasilicate lithium |
| CN102311109A (en) * | 2011-09-07 | 2012-01-11 | 河南帝隆科技研发有限公司 | Method for preparing LiFePO4/C composite cathode material by continuous reaction |
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2018
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Patent Citations (3)
| 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 |
| CN101807692A (en) * | 2010-04-30 | 2010-08-18 | 湖南格林新能源有限公司 | Preparation method of lithium ion battery positive material of ferric metasilicate lithium |
| CN102311109A (en) * | 2011-09-07 | 2012-01-11 | 河南帝隆科技研发有限公司 | Method for preparing LiFePO4/C composite cathode material by continuous reaction |
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