CN114014293A - Preparation method of sodium ion battery material - Google Patents
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Abstract
The invention discloses a preparation method of a sodium-ion battery material. Mixing sodium bicarbonate and a titanium organic matter, adding iron phosphate, adding water for slurrying, and stirring and mixing to obtain mixed slurry; adding the mixed slurry into conductive graphite, and then adding the conductive graphite into a sand mill for sanding, wherein the grain diameter of the sand mill is 250-300 nm; spray drying, calcining the obtained dried material at high temperature, keeping the calcining process in a nitrogen atmosphere, and then screening for removing iron to obtain the sodium-ion battery material. The invention combines the advantages of sodium ferric phosphate and sodium titanate to form mutual doping, thereby obtaining the material with high capacity and good cycle performance, and the final material has low cost which is about 50 percent of that of the lithium iron phosphate material, but the capacity is equivalent to that of the lithium iron phosphate, and the competitive advantage is very obvious.
Description
Technical Field
The invention relates to a preparation method of a sodium-ion battery material, belonging to the technical field of new energy materials.
Background
The field of power batteries is increasingly diversified, competition is continuously upgraded, and the power batteries are the leading ones in the future, are liked to be the heart power batteries of new energy automobiles, and are concerned with the temperature rise of the new energy automobile market. At present, due to the continuous change of technology and the factors of raw material price fluctuation and the like, the field of power batteries is undergoing new changes.
In the past, lithium iron phosphate batteries (LFP) and ternary lithium batteries (NCM, the positive electrode material is three materials of nickel, cobalt and manganese) have been very competitive. The yield of the lithium iron phosphate battery is the first anti-super ternary lithium battery in 5 months in 2021. According to the prediction of the industry, the loading amount of the lithium iron phosphate battery is expected to exceed that of the ternary lithium battery in 6 months, and the lithium iron phosphate battery can recapture the champion seat in the power battery market. The lithium iron power battery loading amount is expected to be equal to that of the ternary power battery in autumn all the year in 2021, and the lithium iron power battery loading amount is expected to be more comprehensive than that of the ternary power battery in 2022. At present, the conventional process is that iron phosphate is prepared by a liquid phase, and then is washed, dried and calcined to obtain anhydrous iron phosphate, wastewater containing ammonia nitrogen, sulfate radical and phosphate radical is generated at the same time, wastewater treatment is needed, and the obtained anhydrous iron phosphate is added with a lithium source, a carbon source and the like for grinding, drying and calcining.
However, the cost of lithium iron phosphate is greatly affected by the increase in the price of lithium sources and the like, and in 9 months at 2021, the price of lithium iron phosphate is increased to 9-10 ten thousand per ton, so that a material with lower cost is urgently needed to replace the lithium iron phosphate material.
The sodium battery material does not need lithium salt, so the cost is greatly reduced. However, the common sodium battery materials have a certain problem, namely that the sodium iron phosphate has low capacity, but the cycle life is long, and the layered oxide has high capacity, but the cycle life is short.
Disclosure of Invention
Aiming at the existing problems, the invention provides a preparation method of a sodium ion battery material, which combines the advantages of sodium iron phosphate and sodium titanate to form mutual doping, thereby obtaining a material with high capacity and good cycle performance, and the final material has low cost which is about 50 percent of that of a lithium iron phosphate material, but the capacity is equivalent to that of the lithium iron phosphate, and the competitive advantage is very obvious.
The invention solves the technical problems by the following technical means:
the invention relates to a preparation method of a sodium-ion battery material, which has the following molecular formula: xNaTiO2.yNaFePO4The molar ratio of x to y is 0.7-0.8: 0.2-0.3; the preparation method comprises the following steps:
1) mixing sodium bicarbonate and a titanium organic matter, adding iron phosphate (the preparation of the iron phosphate can be put in the first step), then adding water for slurrying, and then stirring and mixing to obtain mixed slurry; the preparation method of the iron phosphate comprises the following steps: ball-milling furnace slag generated by smelting yellow phosphorus, calcining the furnace slag in a high-temperature air atmosphere at the calcining temperature of 500-700 ℃ for 4-6h, magnetically separating the obtained material, adding a phosphoric acid solution into the residual material for dissolving, filtering, adding ammonia water into the obtained filtrate, adjusting the pH value to 1.8-2.2 to obtain ferric phosphate dihydrate, filtering, drying, crushing and deironing to obtain the ferric phosphate dihydrate, and concentrating and crystallizing the filtered filtrate to obtain the ammonium phosphate compound fertilizer;
2) adding the mixed slurry into conductive graphite, and then adding the conductive graphite into a sand mill for sanding, wherein the grain diameter of the sand mill is 250-300 nm;
3) spray drying, calcining the obtained dried material at high temperature, keeping the calcining process in a nitrogen atmosphere, and then screening for removing iron to obtain the sodium-ion battery material.
In the step (1), the iron-phosphorus ratio of the iron phosphate is 1.0-1.05; 1 and BET of 30 to 50m2(ii)/g, the primary particle diameter is 30-60nm, and D50 is 3-10 μm.
The ball milling process is carried out by adopting a ball mill, wherein the ball mill adopts zirconia balls, the diameter of the zirconia balls is 1-3cm, then the zirconia balls are sieved, undersize products of 200 meshes are calcined, and oversize products are returned for ball milling; calcining by adopting a rotary kiln; the concentration of the phosphoric acid solution is 0.5-1mol/L, and the solid-liquid mass ratio is 1: 3-4.
The organic compound of titanium in the step (1) is a titanium organic compound which is not hydrolyzed and is dissolved in water.
The molar ratio of sodium bicarbonate to organic titanium to iron phosphate in the step (1) is 1: 0.7-0.8:0.2-0.3, and the mass fraction of water in the mixed slurry is 60-70%.
The mass of the conductive graphite added in the step (2) is 0.2-0.5% of the mass of the mixed slurry; before the conductive graphite is added into the mixed slurry, the conductive graphite is firstly added into water, then the conductive graphite is mixed and stirred, and then the conductive graphite is put into a sand mill to be ground until the particle size is 100-150nm, and then the slurry is poured into the mixed slurry to be ground.
In the spray drying process in the step (3), the D50 of the obtained spray-dried material is 3-10 μm.
In the step (3), in the calcination process, the whole calcination period is 25-30h, the heating rate is 80-120 ℃/h, then the temperature of the first heat preservation area is 750 ℃, the heat preservation time is 1h, then the heat preservation temperature is 550-.
And in the screening process, screening by using an 80-150-mesh ultrasonic vibration screen, removing iron by using an electromagnetic iron remover until the content of magnetic substances is less than or equal to 1ppm, discharging, and performing vacuum packaging to obtain the sodium ion battery.
The sodium battery material is a sodium battery material compounded by the layered oxide and the polyanion, not only is the advantage of high energy density of the layered oxide utilized, but also the advantage of stability of the polyanion is utilized, the layered oxide is coated on the polyanion, a small amount of titanium can be doped into NaFePO4 at the same time, the ionic conductivity is improved, and the inorganic carbon source is coated by the conductive graphite.
Meanwhile, the iron phosphate is prepared by smelting yellow phosphorus to produce slag which is an industrial waste and low in price, contains elements such as iron and phosphorus and mainly takes iron-phosphorus alloy as a main material, then is calcined at high temperature to obtain iron phosphate and other iron-phosphorus compounds, then is reacted with phosphoric acid to obtain iron dihydrogen phosphate, and then is adjusted back in pH to obtain the iron phosphate, wherein the obtained filtrate is the ammonium phosphate compound fertilizer. The preparation process of the iron phosphate is low in cost and high in utilization rate of each component.
Chemical reaction equation during calcination:
FeP+2O2----FePO4
in the phosphoric acid dissolving process:
FePO4+2H3PO4---Fe(H2PO4)3
during the process of adjusting the pH value:
Fe(H2PO4)3+4NH3.H2O---FePO4.2H2O+2(NH4)2HPO4+2H2O
the invention has the beneficial effects that: the advantages of sodium ferric phosphate and sodium titanate are combined to form mutual doping, so that the material with high capacity and good cycle performance is obtained, the cost of the final material is very low and is about 50 percent of that of a lithium iron phosphate material, but the capacity is equivalent to that of lithium iron phosphate, and the competitive advantage is very obvious.
Drawings
FIG. 1 is a SEM of example 1 of the invention.
FIG. 2 is a SEM of example 2 of the invention.
FIG. 3 is a SEM of example 3 of the invention.
Detailed Description
The invention will be described in detail below with reference to the accompanying figure 1 and specific examples: in the preparation method of the sodium-ion battery material of the embodiment, the molecular formula of the sodium-ion battery material is as follows: xNaTiO2.yNaFePO4The molar ratio of x to y is 0.7-0.8: 0.2-0.3; the preparation method comprises the following steps:
1) mixing sodium bicarbonate and a titanium organic matter, adding iron phosphate, adding water for slurrying, and stirring and mixing to obtain mixed slurry;
2) adding the mixed slurry into conductive graphite, and then adding the conductive graphite into a sand mill for sanding, wherein the grain diameter of the sand mill is 250-300 nm;
3) spray drying, calcining the obtained dried material at high temperature, keeping the calcining process in a nitrogen atmosphere, and then screening for removing iron to obtain the sodium-ion battery material.
In the step (1), the preparation method of the iron phosphate comprises the following steps: ball-milling furnace slag generated by smelting yellow phosphorus, calcining the furnace slag in a high-temperature air atmosphere at the calcining temperature of 500-700 ℃ for 4-6h, magnetically separating the obtained material, adding a phosphoric acid solution into the residual material for dissolving, filtering, adding ammonia water into the obtained filtrate, adjusting the pH value to 1.8-2.2 to obtain ferric phosphate dihydrate, filtering, drying, crushing and deironing to obtain the ferric phosphate dihydrate, and concentrating and crystallizing the filtered filtrate to obtain the ammonium phosphate compound fertilizer; the iron-phosphorus ratio of the iron phosphate is 1.0-1.05; 1 and BET of 30 to 50m2(ii)/g, the primary particle diameter is 30-60nm, and D50 is 3-10 μm.
The ball milling process is carried out by adopting a ball mill, wherein the ball mill adopts zirconia balls, the diameter of the zirconia balls is 1-3cm, then the zirconia balls are sieved, undersize products of 200 meshes are calcined, and oversize products are returned for ball milling; calcining by adopting a rotary kiln; the concentration of the phosphoric acid solution is 0.5-1mol/L, and the solid-liquid mass ratio is 1: 3-4.
The organic compound of titanium in the step (1) is a titanium organic compound which is not hydrolyzed and is dissolved in water.
The molar ratio of sodium bicarbonate to organic titanium to iron phosphate in the step (1) is 1: 0.7-0.8:0.2-0.3, and the mass fraction of water in the mixed slurry is 60-70%.
The mass of the conductive graphite added in the step (2) is 0.2-0.5% of the mass of the mixed slurry; before the conductive graphite is added into the mixed slurry, the conductive graphite is firstly added into water, then the conductive graphite is mixed and stirred, and then the conductive graphite is put into a sand mill to be ground until the particle size is 100-150nm, and then the slurry is poured into the mixed slurry to be ground.
In the spray drying process in the step (3), the D50 of the obtained spray-dried material is 3-10 μm.
In the step (3), in the calcination process, the whole calcination period is 25-30h, the heating rate is 80-120 ℃/h, then the temperature of the first heat preservation area is 750 ℃, the heat preservation time is 1h, then the heat preservation temperature is 550-.
And in the screening process, screening by using an 80-150-mesh ultrasonic vibration screen, removing iron by using an electromagnetic iron remover until the content of magnetic substances is less than or equal to 1ppm, discharging, and performing vacuum packaging to obtain the sodium ion battery.
Example 1
A preparation method of a sodium-ion battery material is disclosed, wherein the molecular formula of the sodium-ion battery material is as follows: 0.75NaTiO2.0.25NaFePO4. The preparation method comprises the following steps:
1. mixing sodium bicarbonate and a titanium organic matter, adding iron phosphate, adding water for slurrying, and stirring and mixing to obtain mixed slurry;
2. adding conductive graphite into the mixed slurry, and then adding the mixed slurry into a sand mill for sand milling, wherein the grain diameter of the sand mill is 280 nm;
3. and (3) spray drying, calcining the obtained dried material, keeping the calcining process in a nitrogen atmosphere, and then screening for removing iron to obtain the sodium-ion battery material.
The preparation method of the iron phosphate comprises the following steps: the method comprises the steps of ball-milling furnace slag generated by smelting yellow phosphorus, calcining the furnace slag in a high-temperature air atmosphere at the calcining temperature of 600 ℃, magnetically separating the obtained materials, adding phosphoric acid into the residual materials to dissolve the residual materials, filtering, returning the obtained filtrate, adding ammonia water, adjusting the pH value to 2 to obtain ferric phosphate dihydrate, filtering, drying, crushing and removing iron to obtain the ferric phosphate dihydrate, and concentrating and crystallizing the filtered filtrate to obtain the ammonium phosphate compound fertilizer. The iron-phosphorus ratio of the iron phosphate is 1.02; 1 and BET at 42m2/g, a primary particle size of 46nm, and D50 at 7 μm;
the organic compound of titanium is a titanium organic compound which is not hydrolyzed and is soluble in water;
the molar ratio of titanium to iron phosphate in the sodium bicarbonate and titanium organic matter is 1:0.75:0.25, and the mass fraction of water in the mixed slurry is 63%.
The mass of the conductive graphite added in the step (2) is 0.42 percent of the mass of the mixed slurry. Before the conductive graphite is added into the mixed slurry, adding the conductive graphite into water, then mixing and stirring the conductive graphite, putting the conductive graphite into a sand mill, grinding the conductive graphite to reach the particle size of 123nm, then pouring the slurry into the mixed slurry, and then grinding the conductive graphite;
in the spray drying process in step (3), the D50 of the spray-dried material was 4.6. mu.m.
And in the calcining process, the whole calcining period is 28 hours, the heating rate is 135 ℃/h, then the temperature of the first heat preservation area is 750 ℃, the heat preservation time is 1h, then the heat preservation temperature is 650 ℃ for heat preservation for 6h, then the temperature is reduced to the temperature of the material which is less than or equal to 100 ℃, and then the material is discharged.
And in the screening process, a 100-mesh ultrasonic vibration screen is adopted for screening, an electromagnetic iron remover is adopted for iron removal, the materials are discharged after the iron removal is carried out until the magnetic substances are less than or equal to 1ppm, and the sodium ion battery is obtained after vacuum packaging.
The detection data of the finally obtained sodium battery material are as follows:
the compaction density is 2.5T pressure data. The test pressure of the internal resistance of the powder is 10 MPa.
From the detection data, the product has the advantages of higher discharge capacity, high compaction density, low powder internal resistance, low magnetic substance and good product performance;
the invention has moderate BET, high 10C discharge capacity and excellent rate performance. The sodium battery material obtained in the embodiment is used for preparing a 3Ah soft package battery core, the negative electrode adopts hard carbon, and the capacity retention rate is 93% after the circulation is performed for 500 weeks at 25 ℃ according to 0.5C. The cycle performance is excellent.
As shown in FIG. 1, from SEM, the secondary particle size is spherical, and the primary particle size is about 120-150nm, the structure is compact, so that the processing performance is good, and the electrical performance is excellent.
Example 2
The molecular formula of the sodium-ion battery material is as follows: 0.8NaTiO2.0.2NaFePO4The preparation method comprises the following steps:
1) mixing sodium bicarbonate and a titanium organic matter, adding iron phosphate, adding water for slurrying, and stirring and mixing to obtain mixed slurry;
2) adding conductive graphite into the mixed slurry, and then adding the mixed slurry into a sand mill for sand milling, wherein the grain diameter of the sand mill is 280 nm;
3) spray drying, calcining the obtained dried material at high temperature, keeping the calcining process in a nitrogen atmosphere, and then screening for removing iron to obtain the sodium-ion battery material.
In the step (1), the preparation method of the iron phosphate comprises the following steps: ball-milling furnace slag generated by smelting yellow phosphorus, calcining the furnace slag in a high-temperature air atmosphere, magnetically separating the obtained material, adding a phosphoric acid solution into the residual material for dissolving, filtering, adding ammonia water into the obtained filtrate, adjusting the pH value to 1.9 to obtain ferric phosphate dihydrate, filtering, drying, crushing and removing iron to obtain the ferric phosphate dihydrate, and concentrating and crystallizing the filtered filtrate to obtain the ammonium phosphate compound fertilizer; the iron-phosphorus ratio of the iron phosphate is 1.03; 1 and BET of 42m2A primary particle size of 40nm per g, and a D50 particle size of 8.4. mu.m.
The ball milling process is carried out by adopting a ball mill, wherein the grinding ball adopts zirconia balls, the diameter of each zirconia ball is 1cm, then the zirconia balls are sieved, undersize products of 200 meshes are calcined, and oversize products are returned for ball milling; calcining by adopting a rotary kiln; the concentration of the phosphoric acid solution is 0.8mol/L, and the solid-liquid mass ratio is 1: 4.
The organic compound of titanium in the step (1) is triisostearoyl isopropyl titanate.
The molar ratio of sodium bicarbonate to organic titanium to iron phosphate in the step (1) is 1: 0.8:0.2, and the mass fraction of water in the mixed slurry is 60%.
The mass of the conductive graphite added in the step (2) is 0.4% of the mass of the mixed slurry; before the conductive graphite is added into the mixed slurry, the conductive graphite is added into water, then the conductive graphite is mixed and stirred, and then the mixture is put into a sand mill to be ground until the particle size is 130nm, and then the slurry is poured into the mixed slurry and then ground.
In the spray drying process in step (3), the D50 of the spray-dried material was 6.2 μm.
In the calcining process in the step (3), the whole calcining period is 28 hours, the heating rate is 100 ℃/h, the temperature of a first heat preservation area is 750 ℃, the heat preservation time is 1h, the heat preservation temperature is 550 ℃ for 5 hours, the temperature is reduced to the material temperature which is less than or equal to 100 ℃, then the material is discharged, an induced draft fan is adopted to continuously pump the gas in the furnace, meanwhile, nitrogen is continuously supplied in the furnace, the purity of the nitrogen is more than or equal to 99.999 percent, the mass fraction of water of the nitrogen is less than 0.1ppm, the humidity content of a heat preservation section is maintained to be less than 5ppm, and the furnace pressure in the whole sintering furnace is 80 Pa.
And in the screening process, screening by using an 80-mesh ultrasonic vibration screen, removing iron by using an electromagnetic iron remover until the content of magnetic substances is less than or equal to 1ppm, discharging, and performing vacuum packaging to obtain the sodium ion battery.
The detection data of the finally obtained sodium battery material are as follows:
the SEM of the sodium battery material obtained in this example is shown in fig. 2, and the primary particle size is small.
Example 3
The molecular formula of the sodium-ion battery material is as follows: 0.7NaTiO2.0.3NaFePO4(ii) a The preparation method comprises the following steps:
1) mixing sodium bicarbonate and a titanium organic matter, adding iron phosphate, adding water for slurrying, and stirring and mixing to obtain mixed slurry;
2) adding conductive graphite into the mixed slurry, and then adding the mixed slurry into a sand mill for sand milling, wherein the grain diameter of the sand mill is 250 nm;
3) spray drying, calcining the obtained dried material at high temperature, keeping the calcining process in a nitrogen atmosphere, and then screening for removing iron to obtain the sodium-ion battery material.
In the step (1), the preparation method of the iron phosphate comprises the following steps: ball-milling furnace slag generated by smelting yellow phosphorus, calcining the furnace slag in high-temperature air atmosphere at 680 ℃ for 5 hours, magnetically separating the obtained material, adding a phosphoric acid solution to the residual material for dissolving, filtering, adding ammonia water into the obtained filtrate, adjusting the pH value to 1.9 to obtain ferric phosphate dihydrate, filtering, drying, crushing and removing iron to obtain the ferric phosphate dihydrate, and concentrating and crystallizing the filtered filtrate to obtain the ammonium phosphate compound fertilizer; the iron-phosphorus ratio of the iron phosphate is 1.04; 1 and BET of 45m2(ii)/g, primary particle diameter of 30nm, and D50 of 5.8 μm.
The ball milling process is carried out by adopting a ball mill, wherein the grinding ball adopts zirconia balls, the diameter of the zirconia balls is 3cm, then the zirconia balls are sieved, undersize products of 200 meshes are calcined, and oversize products are returned for ball milling; calcining by adopting a rotary kiln; the concentration of the phosphoric acid solution is 0.9mol/L, and the solid-liquid mass ratio is 1: 3.5.
The organic compound of titanium in the step (1) is chelate type titanate.
The molar ratio of sodium bicarbonate to organic titanium to iron phosphate in the step (1) is 1: 0.7:0.3, and the mass fraction of water in the mixed slurry is 70%.
The mass of the conductive graphite added in the step (2) is 0.35% of the mass of the mixed slurry; before the conductive graphite is added into the mixed slurry, the conductive graphite is firstly added into water, then the conductive graphite is mixed and stirred, and then the mixture is put into a sand mill to be ground until the particle size is 120nm, and then the slurry is poured into the mixed slurry to be ground.
In the spray drying process in step (3), the D50 of the spray-dried material obtained was 6.1. mu.m.
In the calcining process in the step (3), the whole calcining period is 30 hours, the heating rate is 85 ℃/h, then the temperature of a first heat preservation area is 750 ℃, the heat preservation time is 1h, then the heat preservation temperature is 600 ℃ for 6 hours, then the temperature is reduced to the material temperature which is less than or equal to 100 ℃, then the material is discharged, an induced draft fan is adopted to continuously pump away the gas in the furnace, meanwhile, nitrogen is continuously supplied in the furnace, the purity of the nitrogen is more than or equal to 99.999%, the mass fraction of water in the nitrogen is less than 0.1ppm, the humidity content of a heat preservation section is maintained to be less than 5ppm, and the furnace pressure in the whole sintering furnace is 70 Pa.
And in the screening process, a 150-mesh ultrasonic vibration screen is adopted for screening, an electromagnetic iron remover is adopted for iron removal, the materials are discharged after the iron removal is carried out until the magnetic substances are less than or equal to 1ppm, and the sodium ion battery is obtained after vacuum packaging.
The detection data of the finally obtained sodium battery material are as follows:
the SEM of the sodium battery material obtained in this example is shown in fig. 2, and the primary particle size is small.
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 (9)
1. A preparation method of a sodium ion battery material is characterized by comprising the following steps: the molecular formula of the sodium-ion battery material is as follows: xNaTiO2.yNaFePO4The molar ratio of x to y is 0.7-0.8: 0.2-0.3; the preparation method comprises the following steps:
1) mixing sodium bicarbonate and a titanium organic matter, adding iron phosphate, adding water for slurrying, and stirring and mixing to obtain mixed slurry; the preparation method of the iron phosphate comprises the following steps: ball-milling furnace slag generated by smelting yellow phosphorus, calcining the furnace slag in a high-temperature air atmosphere at the calcining temperature of 500-700 ℃ for 4-6h, magnetically separating the obtained material, adding a phosphoric acid solution into the residual material for dissolving, filtering, adding ammonia water into the obtained filtrate, adjusting the pH value to 1.8-2.2 to obtain ferric phosphate dihydrate, filtering, drying, crushing and deironing to obtain the ferric phosphate dihydrate, and concentrating and crystallizing the filtered filtrate to obtain the ammonium phosphate compound fertilizer;
2) adding the mixed slurry into conductive graphite, and then adding the conductive graphite into a sand mill for sanding, wherein the grain diameter of the sand mill is 250-300 nm;
3) spray drying, calcining the obtained dried material at high temperature, keeping the calcining process in a nitrogen atmosphere, and then screening for removing iron to obtain the sodium-ion battery material.
2. The method for preparing a sodium-ion battery material according to claim 1, wherein the method comprises the following steps: the iron-phosphorus ratio of the ferric phosphate in the step (1) is 1.0-1.05; 1 and BET of 30 to 50m2(ii)/g, the primary particle diameter is 30-60nm, and D50 is 3-10 μm.
3. The method for preparing a sodium-ion battery material according to claim 2, wherein the method comprises the following steps: the ball milling process is carried out by adopting a ball mill, wherein the ball mill adopts zirconia balls, the diameter of the zirconia balls is 1-3cm, then the zirconia balls are sieved, undersize products of 200 meshes are calcined, and oversize products are returned for ball milling; calcining by adopting a rotary kiln; the concentration of the phosphoric acid solution is 0.5-1mol/L, and the solid-liquid mass ratio is 1: 3-4.
4. The method for preparing a sodium-ion battery material according to claim 1, wherein the method comprises the following steps: the organic compound of titanium in the step (1) is a titanium organic compound which is not hydrolyzed and is dissolved in water.
5. The method for preparing a sodium-ion battery material according to claim 1, wherein the method comprises the following steps: the molar ratio of sodium bicarbonate to organic titanium to iron phosphate in the step (1) is 1: 0.7-0.8:0.2-0.3, and the mass fraction of water in the mixed slurry is 60-70%.
6. The method for preparing a sodium-ion battery material according to claim 1, wherein the method comprises the following steps: the mass of the conductive graphite added in the step (2) is 0.2-0.5% of the mass of the mixed slurry; before the conductive graphite is added into the mixed slurry, the conductive graphite is firstly added into water, then the conductive graphite is mixed and stirred, and then the conductive graphite is put into a sand mill to be ground until the particle size is 100-150nm, and then the slurry is poured into the mixed slurry to be ground.
7. The method for preparing a sodium-ion battery material according to claim 1, wherein the method comprises the following steps: in the spray drying process in the step (3), the D50 of the obtained spray-dried material is 3-10 μm.
8. The method for preparing a sodium-ion battery material according to claim 1, wherein the method comprises the following steps: in the step (3), in the calcination process, the whole calcination period is 25-30h, the heating rate is 80-120 ℃/h, then the temperature of the first heat preservation area is 750 ℃, the heat preservation time is 1h, then the heat preservation temperature is 550-.
9. The method for preparing a sodium-ion battery material according to claim 1, wherein the method comprises the following steps: and in the screening process, screening by using an 80-150-mesh ultrasonic vibration screen, removing iron by using an electromagnetic iron remover until the content of magnetic substances is less than or equal to 1ppm, discharging, and performing vacuum packaging to obtain the sodium ion battery.
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| CN114784270B (en) * | 2022-03-05 | 2023-09-19 | 四川龙蟒磷化工有限公司 | Preparation method of sodium ion battery material |
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