CN111232945A - Preparation method of battery-grade iron phosphate - Google Patents
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Abstract
The invention discloses a preparation method of battery-grade iron phosphate. Adding pure water into phosphorous acid powder to dissolve the phosphorous acid powder to a phosphorous acid solution with the mass fraction of 20-30%, then mixing and reacting iron powder or waste iron material and the phosphorous acid solution until the molar ratio of iron to phosphorus in the solution is 0.985-0.995, stopping the reaction, and then filtering to obtain a first filtrate and a first filter residue; spray drying the first filtrate, wherein the air inlet temperature in the spray drying process is 200-; and (3) placing the dried material into a rotary kiln, blowing air, and calcining at the temperature of 600-650 ℃ for 2-4h to obtain the battery-grade iron phosphate. The method has the advantages of no wastewater generation, simple process, short flow, high recovery rate of iron and phosphorus and low cost.
Description
Technical Field
The invention relates to a preparation method of battery-grade iron phosphate, belonging to the field of new energy materials of lithium batteries.
Background
Iron phosphate, also known as ferric phosphate,Ferric orthophosphateMolecular formula of FePO4It is white and off-white monoclinic crystal powder. The material containing crystal water is white and slightly powdery, and the anhydrous ferric phosphate is white and slightly yellow. The method is mainly used for manufacturing lithium iron phosphate battery materials, catalysts, ceramics and the like.
The olivine structure (LiMPO) is published in the United states in irreconcilable fashion with Japan4) This material has received great attention and has led to extensive research and rapid development. Compared with the conventional lithium ion secondary battery cathode material, the spinel-structured LiMn2O4And laminated LiCoO2In contrast, LiMPO4The raw materials have wider sources, lower price and no environmental pollution.
The conventional preparation process of the conventional lithium iron phosphate is a solid-phase method, the iron phosphate is the most mainstream precursor of the lithium iron phosphate, and the iron phosphate synthesized by the conventional liquid phase contains two crystal waters, so that the iron phosphate dihydrate is generally obtained by drying the iron phosphate, and then the battery-grade anhydrous iron phosphate is obtained by high-temperature dehydration.
However, the process has the disadvantages of large wastewater treatment capacity, complex process, long flow, low recovery rate of iron and phosphorus, large equipment investment and high energy consumption.
Disclosure of Invention
In view of the above, the invention provides a preparation method of battery-grade iron phosphate, which has the advantages of no wastewater generation, simple process, short flow, high recovery rate of iron and phosphorus and low cost.
The invention solves the technical problems by the following technical means:
a preparation method of battery-grade iron phosphate comprises the following steps: adding pure water into phosphorous acid powder to dissolve the phosphorous acid powder to a phosphorous acid solution with the mass fraction of 20-30%, then mixing and reacting iron powder or waste iron material and the phosphorous acid solution until the molar ratio of iron to phosphorus in the solution is 0.985-0.995, stopping the reaction, and then filtering to obtain a first filtrate and a first filter residue;
spray drying the first filtrate, wherein the air inlet temperature in the spray drying process is 200-;
and (3) placing the dried material into a rotary kiln, blowing air, and calcining at the temperature of 600-650 ℃ for 2-4h to obtain the battery-grade iron phosphate.
The phosphorous acid powder is of industrial purity, the phosphorous acid solution is used after being filtered by a ceramic membrane, and the aperture of the ceramic membrane is 20-50 nm.
When the iron powder or the waste iron material is mixed with the phosphorous acid solution for reaction, the reaction temperature is 60-80 ℃, and the obtained first filter residue is returned to be mixed with the iron powder or the waste iron material for use.
The molar ratio of iron to calcium and magnesium in the iron powder or the waste iron material is more than 1 ten thousand times, and the molar ratio of iron to nickel, chromium, copper and zinc is more than 2 ten thousand times.
The spray drying adopts a centrifugal spray dryer, the rotating speed of an atomizing wheel is more than 15000r/min, the mass fraction of free water in the drying material is less than or equal to 0.5 percent, the particle size of the drying material is 1-20 mu m, and the measurement method of the particle size of the drying material is that a laser particle sizer is adopted for measurement, and a dispersion medium is an organic solvent which does not dissolve the drying material.
In the calcining process, the volume of air blown in per hour is 50-200 times of the volume of the rotary kiln, the volume of drying material in the rotary kiln is not more than 0.2 time of the volume of the rotary kiln, and the material is discharged, cooled to the temperature of lower than 80 ℃, screened, deironized and vacuum-packaged.
Sieving with 60-100 mesh ultrasonic vibration sieve, and electromagnetically removing iron with an electromagnetic iron remover.
And the first filtrate is subjected to iron removal through a 10-20 grade permanent magnet iron remover before being subjected to spray drying.
The process comprises the steps of reacting iron powder with a phosphorous acid solution, determining a reaction end point by controlling the iron-phosphorus ratio in the solution, filtering, removing magnetic substances from obtained filtrate through a multi-stage iron remover, carrying out spray drying to obtain a dried material, and calcining the dried material in an air atmosphere to obtain the battery-grade iron phosphate.
By adopting the process, the generation of waste water can be avoided, and meanwhile, in the whole production process, no other impurity ions such as sulfate radicals, chloride ions, nitrate radicals, ammonium radicals and the like exist, so that the purity of the obtained iron phosphate is very high, meanwhile, the reaction end point is controlled by controlling the iron-phosphorus ratio, the iron-phosphorus ratio of a final product can be freely adjusted, and the utilization rate of iron and phosphorus is high.
In the calcining process, air is introduced to completely convert phosphite into phosphate radical, and the iron phosphate is calcined at high temperature, so that the crystallinity of the iron phosphate is improved. Because phosphite has strong reducibility and is easily oxidized by oxygen in the air, the reaction is more easily generated at high temperature, and simultaneously, the ferrous ions of the invention are also oxidized into ferric iron at high temperature in the air atmosphere.
The phosphorous acid is solid, compared with the phosphoric acid which is liquid, the phosphorous acid is convenient to transport, and the price of the phosphorous acid is about 10 percent lower than that of the phosphoric acid (the content is 100 percent, the concentration of a phosphoric acid solution is generally 80 percent), so the process cost of the invention is lower.
Meanwhile, the acidity of the product is stronger than that of phosphoric acid, and the reaction speed is higher.
The invention has the beneficial effects that: no waste water, simple process, short flow, high recovery rate of iron and phosphorus and low cost.
Drawings
FIG. 1 is an SEM of a dried material obtained in example 1 of the present invention.
Fig. 2 is an SEM of the iron phosphate obtained in example 1 of the present invention.
Figure 3 is an XRD of the iron phosphate obtained in example 1 of the present invention.
FIG. 4 is an SEM of iron phosphate obtained in example 2 of the present invention.
Figure 5 is an SEM of the iron phosphate obtained in example 3 of the present invention.
Figure 6 is a graph of the particle size distribution of the iron phosphate obtained in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific examples, wherein the method for preparing battery grade iron phosphate of the present embodiment comprises the following steps: adding pure water into phosphorous acid powder to dissolve the phosphorous acid powder to a phosphorous acid solution with the mass fraction of 20-30%, then mixing and reacting iron powder or waste iron material and the phosphorous acid solution until the molar ratio of iron to phosphorus in the solution is 0.985-0.995, stopping the reaction, and then filtering to obtain a first filtrate and a first filter residue;
spray drying the first filtrate, wherein the air inlet temperature in the spray drying process is 200-;
and (3) placing the dried material into a rotary kiln, blowing air, and calcining at the temperature of 600-650 ℃ for 2-4h to obtain the battery-grade iron phosphate.
The phosphorous acid powder is of industrial purity, the phosphorous acid solution is used after being filtered by a ceramic membrane, and the aperture of the ceramic membrane is 20-50 nm.
When the iron powder or the waste iron material is mixed with the phosphorous acid solution for reaction, the reaction temperature is 60-80 ℃, and the obtained first filter residue is returned to be mixed with the iron powder or the waste iron material for use.
The molar ratio of iron to calcium and magnesium in the iron powder or the waste iron material is more than 1 ten thousand times, and the molar ratio of iron to nickel, chromium, copper and zinc is more than 2 ten thousand times.
The spray drying adopts a centrifugal spray dryer, the rotating speed of an atomizing wheel is more than 15000r/min, the mass fraction of free water in the drying material is less than or equal to 0.5 percent, the particle size of the drying material is 1-20 mu m, and the measurement method of the particle size of the drying material is that a laser particle sizer is adopted for measurement, and a dispersion medium is an organic solvent which does not dissolve the drying material.
In the calcining process, the volume of air blown in per hour is 50-200 times of the volume of the rotary kiln, the volume of drying material in the rotary kiln is not more than 0.2 time of the volume of the rotary kiln, and the material is discharged, cooled to the temperature of lower than 80 ℃, screened, deironized and vacuum-packaged.
Sieving with 60-100 mesh ultrasonic vibration sieve, and electromagnetically removing iron with an electromagnetic iron remover.
And the first filtrate is subjected to iron removal through a 10-20 grade permanent magnet iron remover before being subjected to spray drying.
Example 1
A preparation method of battery-grade iron phosphate comprises the following steps: adding pure water into phosphorous acid powder to dissolve the phosphorous acid powder into a phosphorous acid solution with the mass fraction of 25%, then mixing and reacting iron powder and the phosphorous acid solution until the molar ratio of iron to phosphorus in the solution is 0.989, stopping the reaction, and then filtering to obtain a first filtrate and a first filter residue;
spray drying the first filtrate, wherein the air inlet temperature in the spray drying process is 250 ℃, the discharging temperature is less than or equal to 100 ℃, so as to obtain a dried material, and the dried material is sampled and detected, and the result is as follows:
as shown in fig. 1, the desiccant material is in the form of granules.
And (3) placing the dried material into a rotary kiln, blowing air, and calcining at 630 ℃ for 3h to obtain the battery-grade iron phosphate.
The phosphorous acid powder is of industrial purity, the phosphorous acid solution is used after being filtered by a ceramic membrane, and the aperture of the ceramic membrane is 30 nm.
When the iron powder and the phosphorous acid solution are mixed and reacted, the reaction temperature is 70 ℃, and the obtained first filter residue is returned to be mixed with the iron powder for use.
The molar ratio of iron to calcium and magnesium in the iron powder is more than 1 ten thousand times, and the molar ratio of iron to nickel, chromium, copper and zinc is more than 2 ten thousand times.
The spray drying adopts a centrifugal spray dryer, the rotating speed of an atomizing wheel is more than 15000r/min, the mass fraction of free water in the drying material is less than or equal to 0.5 percent, the particle size of the drying material is 8.5 mu m, and the measurement method of the particle size of the drying material is that a laser particle sizer is adopted for measurement, and a dispersion medium is an organic solvent which does not dissolve the drying material.
In the calcining process, the volume of air blown in per hour is 100 times of the volume of the rotary kiln, the volume of drying material in the rotary kiln is not more than 0.2 time of the volume of the rotary kiln, and the material is discharged, cooled to the temperature of lower than 80 ℃, screened, deironized and vacuum-packaged.
Screening by an 80-mesh ultrasonic vibration screen, and performing electromagnetic iron removal by an electromagnetic iron remover.
The first filtrate is subjected to iron removal through a 15-stage permanent magnet iron remover before being subjected to spray drying.
The detection result of the finally obtained anhydrous iron phosphate product is as follows:
| index (I) | Iron to phosphorus ratio | Fe | D10 | D50 | D90 |
| Numerical value | 0.991 | 36.86％ | 2.5μm | 3.7μm | 8.8μm |
| D100 | Cd | Co | Pb | Ca | Na |
| 12.5μm | 6.1ppm | 12.1ppm | 1.2ppm | 25.5ppm | 24.1ppm |
| Ni | Mn | Zn | Cr | Al | Ti |
| 11.6ppm | 24.8ppm | 11.1ppm | 5.1ppm | 12.2ppm | 1.0ppm |
| Tap density | Sulfur | Chloride ion | BET | Magnetic foreign matter | |
| 1.17g/mL | 28.6ppm | 12.7ppm | 10.5m2/g | 0.22ppm |
Example 2
A preparation method of battery-grade iron phosphate comprises the following steps: adding pure water into phosphorous acid powder to dissolve the phosphorous acid powder into a phosphorous acid solution with the mass fraction of 25%, then mixing and reacting iron powder and the phosphorous acid solution until the molar ratio of iron to phosphorus in the solution is 0.991, stopping the reaction, and then filtering to obtain a first filtrate and a first filter residue;
spray drying the first filtrate, wherein the air inlet temperature in the spray drying process is 280 ℃, the discharging temperature is less than or equal to 100 ℃, and a dried material is obtained;
and (3) placing the dried material into a rotary kiln, blowing air, and calcining for 3h at 640 ℃ to obtain the battery-grade iron phosphate.
The phosphorous acid powder is of industrial purity, the phosphorous acid solution is used after being filtered by a ceramic membrane, and the aperture of the ceramic membrane is 25 nm.
When the iron powder and the phosphorous acid solution are mixed and reacted, the reaction temperature is 75 ℃, and the obtained first filter residue is returned to be mixed with the iron powder for use.
The molar ratio of iron to calcium and magnesium in the iron powder is more than 1 ten thousand times, and the molar ratio of iron to nickel, chromium, copper and zinc is more than 2 ten thousand times.
The spray drying adopts a centrifugal spray dryer, the rotating speed of an atomizing wheel is more than 15000r/min, the mass fraction of free water in the drying material is less than or equal to 0.5 percent, the particle size of the drying material is 14.5 mu m, and the measurement method of the particle size of the drying material is that a laser particle sizer is adopted for measurement, and a dispersion medium is an organic solvent which does not dissolve the drying material.
In the calcining process, the volume of air blown in per hour is 150 times of the volume of the rotary kiln, the volume of drying material in the rotary kiln is not more than 0.2 time of the volume of the rotary kiln, and the material is discharged, cooled to the temperature of lower than 80 ℃, screened, deironized and vacuum-packaged.
Screening by adopting a 60-mesh ultrasonic vibration screen, and performing electromagnetic iron removal by adopting an electromagnetic iron remover.
The first filtrate is subjected to iron removal through a 20-grade permanent magnet iron remover before being subjected to spray drying.
The detection result of the finally obtained anhydrous iron phosphate product is as follows:
| index (I) | Iron to phosphorus ratio | Fe | D10 | D50 | D90 |
| Numerical value | 0.994 | 36.82％ | 3.5μm | 5.3μm | 9.8μm |
| D100 | Cd | Co | Pb | Ca | Na |
| 19.5μm | 6.5ppm | 11.4ppm | 1.1ppm | 29.5ppm | 21.5ppm |
| Ni | Mn | Zn | Cr | Al | Ti |
| 11.1ppm | 22.1ppm | 11.5ppm | 5.3ppm | 12.9ppm | 1.0ppm |
| Tap density | Sulfur | Chloride ion | BET | Magnetic foreign matter | |
| 1.11g/mL | 28.9ppm | 12.3ppm | 10.2m2/g | 0.12ppm |
Example 3
A preparation method of battery-grade iron phosphate comprises the following steps: adding pure water into phosphorous acid powder to dissolve the phosphorous acid powder into a phosphorous acid solution with the mass fraction of 25%, then mixing and reacting the waste iron material and the phosphorous acid solution until the molar ratio of iron to phosphorus in the solution is 0.991, stopping the reaction, and then filtering to obtain a first filtrate and a first filter residue;
spray drying the first filtrate, wherein the air inlet temperature in the spray drying process is 280 ℃, the discharging temperature is less than or equal to 100 ℃, and a dried material is obtained;
and (3) placing the dried material into a rotary kiln, blowing air, and calcining for 3h at 640 ℃ to obtain the battery-grade iron phosphate.
The phosphorous acid powder is of industrial purity, the phosphorous acid solution is used after being filtered by a ceramic membrane, and the aperture of the ceramic membrane is 30 nm.
When the waste iron material and the phosphorous acid solution are mixed and reacted, the reaction temperature is 70 ℃, and the obtained first filter residue is returned to be mixed with the waste iron material for use.
The mole ratio of iron to calcium and magnesium in the waste iron material is more than 1 ten thousand times, and the mole ratio of iron to nickel, chromium, copper and zinc is more than 2 ten thousand times.
The spray drying adopts a centrifugal spray dryer, the rotating speed of an atomizing wheel is more than 15000r/min, the mass fraction of free water in the drying material is less than or equal to 0.5 percent, the particle size of the drying material is 11.8 mu m, and the measurement method of the particle size of the drying material is that a laser particle sizer is adopted for measurement, and a dispersion medium is an organic solvent which does not dissolve the drying material.
In the calcining process, the volume of air blown in per hour is 180 times of the volume of the rotary kiln, the volume of drying materials in the rotary kiln is not more than 0.2 time of the volume of the rotary kiln, and the materials are discharged, cooled to the temperature of lower than 80 ℃, screened, deironized and vacuum-packed.
Screening by using a 100-mesh ultrasonic vibration screen, and performing electromagnetic iron removal by using an electromagnetic iron remover.
The first filtrate is subjected to iron removal through a 20-grade permanent magnet iron remover before being subjected to spray drying.
The detection result of the finally obtained anhydrous iron phosphate product is as follows:
| index (I) | Iron to phosphorus ratio | Fe | D10 | D50 | D90 |
| Numerical value | 0.994 | 36.86％ | 3.6μm | 6.3μm | 11.2μm |
| D100 | Cd | Co | Pb | Ca | Na |
| 18.6μm | 4.5ppm | 16.4ppm | 1.8ppm | 35.5ppm | 28.5ppm |
| Ni | Mn | Zn | Cr | Al | Ti |
| 13.7ppm | 26.7ppm | 15.3ppm | 5.1ppm | 17.5ppm | 1.0ppm |
| Tap density | Sulfur | Chloride ion | BET | Magnetic foreign matter | |
| 1.18g/mL | 32.5ppm | 16.6ppm | 11.5m2/g | 0.19ppm |
As shown in fig. 2, the SEM of the iron phosphate obtained in example 1 shows that the obtained iron phosphate has a granular morphology in which the iron phosphate is adhered to each other, fig. 3 shows the XRD of the iron phosphate obtained in example 1, shows the iron phosphate with high crystallinity and no impurity phase, and fig. 6 shows the particle size distribution diagram of the iron phosphate obtained in example 1 of the present invention.
Fig. 4 is an SEM of the iron phosphate obtained in example 2, and fig. 5 is an SEM of the iron phosphate obtained in example 3. Similar to the SEM of iron phosphate obtained in example 1, all were in the form of particles, with the size of the individual particles being around 500 nm.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (8)
1. A preparation method of battery-grade iron phosphate is characterized by comprising the following steps: adding pure water into phosphorous acid powder to dissolve the phosphorous acid powder to a phosphorous acid solution with the mass fraction of 20-30%, then mixing and reacting iron powder or waste iron material and the phosphorous acid solution until the molar ratio of iron to phosphorus in the solution is 0.985-0.995, stopping the reaction, and then filtering to obtain a first filtrate and a first filter residue;
spray drying the first filtrate, wherein the air inlet temperature in the spray drying process is 200-;
and (3) placing the dried material into a rotary kiln, blowing air, and calcining at the temperature of 600-650 ℃ for 2-4h to obtain the battery-grade iron phosphate.
2. The method of preparing battery grade iron phosphate according to claim 1, characterized in that: the phosphorous acid powder is of industrial purity, the phosphorous acid solution is used after being filtered by a ceramic membrane, and the aperture of the ceramic membrane is 20-50 nm.
3. The method of preparing battery grade iron phosphate according to claim 1, characterized in that: when the iron powder or the waste iron material is mixed with the phosphorous acid solution for reaction, the reaction temperature is 60-80 ℃, and the obtained first filter residue is returned to be mixed with the iron powder or the waste iron material for use.
4. The method of preparing battery grade iron phosphate according to claim 1, characterized in that: the molar ratio of iron to calcium and magnesium in the iron powder or the waste iron material is more than 1 ten thousand times, and the molar ratio of iron to nickel, chromium, copper and zinc is more than 2 ten thousand times.
5. The method of preparing battery grade iron phosphate according to claim 1, characterized in that: the spray drying adopts a centrifugal spray dryer, the rotating speed of an atomizing wheel is more than 15000r/min, the mass fraction of free water in the drying material is less than or equal to 0.5 percent, the particle size of the drying material is 1-20 mu m, and the measurement method of the particle size of the drying material is that a laser particle sizer is adopted for measurement, and a dispersion medium is an organic solvent which does not dissolve the drying material.
6. The method of preparing battery grade iron phosphate according to claim 1, characterized in that: in the calcining process, the volume of air blown in per hour is 50-200 times of the volume of the rotary kiln, the volume of drying material in the rotary kiln is not more than 0.2 time of the volume of the rotary kiln, and the material is discharged, cooled to the temperature of lower than 80 ℃, screened, deironized and vacuum-packaged.
7. The method of preparing battery grade iron phosphate according to claim 6, characterized in that: sieving with 60-100 mesh ultrasonic vibration sieve, and electromagnetically removing iron with an electromagnetic iron remover.
8. The method of preparing battery grade iron phosphate according to claim 1, characterized in that: and the first filtrate is subjected to iron removal through a 10-20 grade permanent magnet iron remover before being subjected to spray drying.
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| CN101244813A (en) * | 2007-02-15 | 2008-08-20 | 比亚迪股份有限公司 | Alkali type iron ammonium phosphate and production method, production method of iron phosphate and production method of ferrous lithium phosphate |
| CN101290988A (en) * | 2008-06-16 | 2008-10-22 | 中南大学 | Preparation of positive electrode material of lithium ion cell namely lithium iron phosphate |
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