CN114906830B - Method for controllably preparing battery-grade iron phosphate from pyrite cinder - Google Patents
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Abstract
A method for controllably preparing battery-grade iron phosphate from pyrite cinder comprises the steps of crushing the pyrite cinder, adding the crushed pyrite cinder into acid, stirring, adding water, keeping the temperature, adding water for dilution, and filtering to obtain a reaction solution; adding iron powder into the reaction solution, stirring, and adding water to dilute to obtain a raw material slurry; adding alkali liquor into the reducing slurry to adjust the pH value, and filtering to obtain refined reducing liquid; then adding an oxidant to react to obtain oxidized slurry; adding alkali liquor into the oxidized slurry to adjust the pH, filtering and collecting a filter cake to obtain ferric hydroxide, and washing the ferric hydroxide with water to obtain high-purity ferric hydroxide; adding water into high-purity ferric hydroxide to prepare slurry, mixing the slurry with phosphoric acid, reacting, filtering and collecting a filter cake to obtain a ferric phosphate wet base, washing to obtain the high-purity ferric phosphate wet base, drying to obtain ferric phosphate dihydrate, and calcining to obtain the battery-grade anhydrous ferric phosphate. The method not only effectively utilizes pyrite cinder resources and reduces discharge and pollution, but also provides a cheap and high-quality iron source for iron phosphate production, and prepares the battery-grade high-quality iron phosphate.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to a method for preparing battery-grade iron phosphate by using pyrite cinder.
Background
At present, iron sources of iron phosphate are mainly ferrous sulfate and reduced iron powder which are titanium white byproducts, along with the rapid development of new energy, the price of the iron sources is increased, and the supply and demand relationship becomes tense, so that the search for a cheap and easily available iron source is imperative.
The pyrite cinder is a by-product of sulfuric acid production from pyrite, and the iron content can reach about 60%, but due to the limitation of the prior art, the pyrite cinder is basically sold to a smelting plant at a low price to be used as a blending material for pyrometallurgical iron, so that not only is high energy consumption caused in smelting production, but also the cost for producing acid from pyrite is relatively increased.
Chinese patent publication No. CN109368610A provides a method for preparing iron phosphate from pyrite cinder, which requires pretreatment and increased carbon emission, and the used alkali liquor causes a large amount of wastewater in the production process and acid waste; the added non-ionic flocculant and PEG also increase the production cost; the pickle liquor is not purified, so that the iron phosphate impurity content of the product is higher.
Chinese patent publication No. CN108706561A provides a method for preparing iron phosphate from pyrite cinder, which requires washing and drying of pyrite cinder, resulting in a large amount of wastewater and increased energy consumption. Because the hydrothermal time is long, the ferric hydroxide colloid generated in the process is difficult to filter; in addition, the pH is low, the iron is difficult to control and completely sinks out, a large amount of iron source waste can be caused in large-scale device production, and meanwhile, the hydrothermal reaction liquid is not subjected to impurity removal, so that the product quality is difficult to ensure.
Chinese patent publication No. CN113184820A provides a method for preparing iron phosphate by using ferrous sulfate as a titanium white byproduct, which relates to a purification process of ferrous sulfate heptahydrate, but requires heating in both pH adjustment and oxidation processes, and increases energy consumption. The hydrogen peroxide and the alkali liquor are used as mixed oxidants, so that the oxidation efficiency of the hydrogen peroxide is reduced; the mixed acid is used when the iron phosphate is synthesized, so that the cost is increased, the waste is caused, and meanwhile, the impurity sulfate radicals are introduced, so that the treatment difficulty is increased, and the product purity is not high.
Disclosure of Invention
The invention aims to provide a method for controllably preparing battery-grade iron phosphate from pyrite cinder, which solves the problems of difficulty in impurity removal, high impurity removal cost, more byproducts and difficulty in treatment during utilization of pyrite cinder, effectively utilizes pyrite cinder resources, and provides a cheap and high-quality iron source for production of iron phosphate so as to reduce production cost and emission and pollution and provide battery-grade high-quality iron phosphate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for controllably preparing battery-grade iron phosphate from pyrite cinder comprises the following steps:
s1, crushing pyrite cinder to obtain pyrite cinder powder with uniform particle size, and then adding the pyrite cinder powder into an acid solution to obtain mixed slurry;
s2, stirring the mixed slurry at the normal pressure and at the temperature of 85-116 ℃ for reaction for 2.5-5 hours, adding water, keeping the temperature for 0.5-2 hours, filtering and collecting reaction liquid;
s3, adding iron powder into the reaction liquid, stirring and reacting for 0.5 to 3.0 hours at the temperature of 50 to 95 ℃ under normal pressure, and adding water again to dilute to obtain a raw material slurry;
s4, adding an alkali liquor into the reducing slurry, adjusting the pH value to 5.2 to 7.4, filtering and collecting filtrate to obtain refined reducing liquid;
s5, adding an oxidant into the refined reducing solution, and reacting at 15 to 75 ℃ for 0.5 to 24 hours to obtain an oxide slurry;
s6, adding an alkali liquor into the oxide slurry, adjusting the pH to 2.8 to 4.8, filtering and collecting a filter cake to obtain iron hydroxide;
s7, washing the ferric hydroxide by using water to obtain high-purity ferric hydroxide;
s8, adding water into high-purity iron hydroxide to prepare slurry containing 2-12% of iron, mixing the slurry with phosphoric acid, reacting at the temperature of 60-97 ℃ for 1.8-5.5 hours under normal pressure, filtering, and collecting a filter cake to obtain an iron phosphate wet base;
s9, washing the iron phosphate wet base for 1 to 3 times to obtain a high-purity iron phosphate wet base;
s10, drying the high-purity iron phosphate wet base at 105-500 ℃ to obtain ferric phosphate dihydrate;
s11, calcining the dihydrate ferric phosphate at 680-950 ℃ for 1-2 hours to obtain the battery-grade anhydrous ferric phosphate.
Preferably, in step S1, the pyrite cinder contains Fe 2 O 3 、Fe 3 O 4 And FeO, the mass content of the single iron is 45-60%, and the pyrite cinder contains impurities of Si, al, ca, zn and Mg.
Preferably, in the step S1, the particle size of the crushed pyrite cinder powder is 80 to 600 meshes; the acid solution is sulfuric acid with the mass concentration of 38-65%, and the use amount of the sulfuric acid is 1.5-3 times of the mass of the pyrite cinder.
Preferably, in the step S2, the stirring reaction temperature is 93 to 115 ℃, and the reaction time is 2.5 to 3.5 hours.
Preferably, in the step S3, the iron powder is recovered scrap iron foundry iron powder and/or primary reduced iron powder, and the using amount of the iron powder is 0.5 to 0.8 times of that of ferric iron measured by sampling in the reaction liquid in the step S2; adding water to ensure that the iron content is 3-9%; the reaction temperature is 65 to 85 ℃ under stirring, and the reaction time is 0.5 to 2.0 hours.
Preferably, in the steps S4 and S6, the alkali liquor is one of 10-38% of sodium hydroxide, 10-35% of sodium carbonate, 10-30% of ammonia water and 10-30% of urea by mass concentration.
Preferably, in step S4, the pH is adjusted to 5.5 to 6.5.
Preferably, in the step S5, the oxidant is hydrogen peroxide or air, and the molar ratio of hydrogen peroxide to iron is 0.5; the reaction temperature after the addition of the oxidant is 25 to 55 ℃, the reaction time is 0.5 to 2 hours, and the oxidation time after the addition of air is 3 to 24 hours.
Preferably, in step S6, the pH is adjusted to be 3.2 to 4.2.
Preferably, in step S8, water is added to high-purity iron hydroxide to prepare a slurry containing 2% to 12% of iron, and the molar ratio of phosphorus in the charged phosphoric acid to phosphorus in the iron-containing iron hydroxide is 0.95 to 1.2:1; the reaction temperature of the slurry and phosphoric acid after mixing is 60 to 80 ℃, and the reaction time is 2.2 to 3.5 hours.
Preferably, in the step S10, the drying temperature is 180 to 300 ℃.
Preferably, in step S11, the calcination temperature is 650 to 750 ℃.
According to the technical scheme, pyrite cinder is crushed and then added into an acid solution, the temperature is raised, the reaction is carried out under the condition of heat preservation, then water is added for dilution, the filtrate is filtered and collected after the reaction, the filtrate is reduced by using simple substance iron to obtain a ferrous solution, the reduced solution is added with alkali to adjust the pH value to 5.2 to 7.4, then filtration and impurity removal are carried out, then an oxidant, namely divalent iron oxide, is added into the filtrate, then the alkali is added again to adjust the pH value to 2.8 to 4.8, iron is precipitated in the form of iron hydroxide, iron hydroxide is obtained by filtering slurry, the iron hydroxide is washed again and then prepared into slurry, the slurry is reacted with phosphoric acid at the temperature of 60 to 97 ℃ for 1.8 to 5.5 hours, iron phosphate is obtained by filtration, the iron phosphate is washed, dried and calcined, and the high-purity battery-grade iron phosphate is obtained. The method only needs to crush the pyrite cinder in the pretreatment, does not need to input other raw materials, is simple and easy to implement, does not generate three wastes, and has low cost. The method has the advantages of mild reaction conditions, short reaction time, modularized working procedures, high controllability of products and high purity of the products, the iron hydroxide can be used as a raw material of products and downstream iron-based products, the generated waste residues are recycled, the waste liquid is mainly sulfate, the shunting is simple, the iron phosphate washing water can be used for washing the iron hydroxide, and the water discharge is small.
Drawings
Fig. 1 is an SEM image of iron phosphate prepared in example 1 of the present invention;
figure 2 is an XRD primary iron phosphate peak finding pattern for iron phosphate prepared in example 1 of the present invention.
Detailed Description
The contents and effects of the present invention will be further described and illustrated by examples. The examples listed are only some of the examples of the present invention and not all of them.
The contents of the components in the pyrite cinder raw materials selected in the examples and comparative examples of the present invention are shown in table 1.
TABLE 1 ingredient content table of pyrite cinder raw material used in examples
Example 1
A method for controllably preparing battery-grade iron phosphate from pyrite cinder comprises the following steps:
s1, crushing pyrite cinder of a raw material 1 in the table 1 to 350 meshes, and then slowly adding the crushed pyrite cinder into a sulfuric acid solution with the mass concentration of 50% while stirring to obtain mixed slurry; the mass of the pure sulfuric acid is 2 times of that of the pyrite cinder;
s2, stirring the mixed slurry at the normal pressure and the temperature of 100 ℃ for reaction for 3 hours, then adding water, preserving heat for 0.5 hour, filtering and collecting reaction liquid;
s3, adding iron powder with the mass 0.6 time that of ferric iron contained in the reaction liquid into the reaction liquid, and then stirring and reacting for 1 hour under the conditions of normal pressure and 80 ℃ to obtain raw material slurry;
s4, adding a sodium hydroxide solution with the mass concentration of 15% into the reduced slurry, adjusting the pH to 5.8, filtering and collecting filtrate to obtain a refined ferrous sulfate solution;
s5, adding hydrogen peroxide into the refined ferrous sulfate solution, and reacting for 1 hour at 30 ℃ to obtain oxidized slurry; the molar ratio of hydrogen peroxide to iron is 0.65;
s6, adding a sodium hydroxide solution with the mass concentration of 15% into the oxidized slurry, adjusting the pH to 4.2, filtering and collecting a filter cake to obtain ferric hydroxide;
s7, washing the ferric hydroxide for 2 times by using water to obtain high-purity ferric hydroxide;
s8, adding water into high-purity ferric hydroxide to prepare ferric hydroxide slurry containing 8% of iron, mixing the ferric hydroxide slurry with phosphoric acid, reacting at the normal pressure and the temperature of 80 ℃ for 3 hours in a heat preservation manner, filtering and collecting a filter cake to obtain a ferric phosphate wet base; the molar ratio of phosphorus to iron of phosphorus and iron hydroxide of the fed phosphoric acid is 1.01;
s9, washing the iron phosphate wet base for 2 times to obtain a high-purity iron phosphate wet base;
s10, drying the high-purity iron phosphate wet base at 300 ℃ to obtain ferric phosphate dihydrate;
s11, calcining the dihydrate ferric phosphate at 750 ℃ for 1.5 hours to obtain the battery-grade anhydrous ferric phosphate.
Example 2
A method for controllably preparing battery-grade iron phosphate from pyrite cinder comprises the following steps:
s1, crushing pyrite cinder of a raw material 2 in the table 1 to 80 meshes, and then slowly adding the crushed pyrite cinder into a sulfuric acid solution with the mass concentration of 38% under stirring to obtain mixed slurry; the mass of the pure sulfuric acid is 3 times of that of the pyrite cinder;
s2, stirring the mixed slurry at the normal pressure and 85 ℃ for reaction for 2.5 hours, then adding water for dilution until the iron content is 9%, preserving heat for 1 hour, filtering and collecting reaction liquid;
s3, adding iron powder with the mass 0.8 time that of ferric iron contained in the reaction liquid into the reaction liquid, and then stirring and reacting for 2 hours under the conditions of normal pressure and 85 ℃ to obtain raw material slurry;
s4, adding a sodium carbonate solution with the mass concentration of 20% into the reduced slurry, adjusting the pH value to 6.5, filtering and collecting filtrate to obtain a refined ferrous sulfate solution;
s5, adding hydrogen peroxide into the refined ferrous sulfate solution, and reacting for 1.5 hours at 15 ℃ to obtain oxidized slurry; the molar ratio of hydrogen peroxide to iron is 0.7;
s6, adding a sodium carbonate solution with the mass concentration of 35% into the oxidized slurry, adjusting the pH to 4.8, filtering and collecting a filter cake to obtain ferric hydroxide;
s7, washing the ferric hydroxide for 2 times by using water to obtain high-purity ferric hydroxide;
s8, adding water into high-purity ferric hydroxide to prepare ferric hydroxide slurry containing 12% of iron, mixing the ferric hydroxide slurry with phosphoric acid, reacting at the normal pressure and the temperature of 97 ℃ for 1.8 hours in a heat preservation manner, filtering and collecting a filter cake to obtain a ferric phosphate wet base; the molar ratio of phosphorus to iron is 0.95;
s9, washing the iron phosphate wet base for 2 times to obtain a high-purity iron phosphate wet base;
s10, drying the high-purity iron phosphate wet base at 105 ℃ to obtain ferric phosphate dihydrate;
s11, calcining the dihydrate ferric phosphate at 680 ℃ for 2 hours to obtain the battery-grade anhydrous ferric phosphate.
Example 3
A method for controllably preparing battery-grade iron phosphate from pyrite cinder comprises the following steps:
s1, crushing pyrite cinder of a raw material 2 in the table 1 to 600 meshes, and then slowly adding the crushed pyrite cinder into a sulfuric acid solution with the mass concentration of 65% while stirring to obtain mixed slurry; the mass of the pure sulfuric acid is 1.5 times of that of the pyrite cinder;
s2, stirring the mixed slurry at the normal pressure and 85 ℃ for reaction for 3.5 hours, then adding water for dilution until the iron content is 3%, preserving heat for 2 hours, filtering and collecting reaction liquid;
s3, adding iron powder which is 0.5 time of the weight of ferric iron contained in the reaction solution into the reaction solution, and then stirring and reacting for 0.5 hour under the conditions of normal pressure and 50 ℃ to obtain returned raw material slurry;
s4, adding ammonia water with the mass concentration of 15% into the reduced slurry, adjusting the pH value to 6.5, filtering and collecting filtrate to obtain a refined ferrous sulfate solution;
s5, adding hydrogen peroxide into the refined ferrous sulfate solution, and reacting for 2 hours at 75 ℃ to obtain oxidized slurry; the molar ratio of hydrogen peroxide to iron is 0.5;
s6, adding a urea solution with the mass concentration of 10% into the oxidized slurry, adjusting the pH to 2.8, filtering and collecting a filter cake to obtain ferric hydroxide;
s7, washing the ferric hydroxide for 2 times by using water to obtain high-purity ferric hydroxide;
s8, adding water into high-purity ferric hydroxide to prepare ferric hydroxide slurry containing 2% of iron, mixing the ferric hydroxide slurry with phosphoric acid, reacting at the normal pressure and 60 ℃ for 5.5 hours in a heat preservation manner, filtering and collecting a filter cake to obtain a ferric phosphate wet base; the molar ratio of phosphorus to iron is 1.2;
s9, washing the iron phosphate wet base for 2 times to obtain a high-purity iron phosphate wet base;
s10, drying the high-purity iron phosphate wet base at 500 ℃ to obtain ferric phosphate dihydrate;
s11, calcining the dihydrate ferric phosphate at 950 ℃ for 1 hour to obtain the battery-grade anhydrous ferric phosphate.
Example 4
A method for controllably preparing battery-grade iron phosphate from pyrite cinder comprises the following steps:
s1, crushing pyrite cinder of a raw material 2 in the table 1 to 400 meshes, and then slowly adding the crushed pyrite cinder into a sulfuric acid solution with the mass concentration of 38% while stirring to obtain mixed slurry; the mass of the pure sulfuric acid is 1.5 times of that of the pyrite cinder;
s2, stirring the mixed slurry at the normal pressure and at the temperature of 85 ℃ for reaction for 3.5 hours, adding water for dilution until the iron content is 8%, preserving heat for 0.5 hour, filtering and collecting to obtain a reaction solution;
s3, adding recovered waste iron which is 0.7 time of the mass of ferric iron contained in the reaction liquid into the reaction liquid to prepare iron powder, and then stirring and reacting for 1.5 hours under the conditions of normal pressure and 50 ℃ to obtain a raw material slurry;
s4, adding a urea solution with the mass concentration of 30% into the reduced slurry, adjusting the pH value to 6.5, filtering and collecting filtrate to obtain a refined ferrous sulfate solution;
s5, introducing air into the refined ferrous sulfate solution, and reacting for 24 hours at 35 ℃ to obtain oxidized slurry;
s6, adding a urea solution with the mass concentration of 30% into the oxidized slurry, adjusting the pH to 2.8, filtering and collecting a filter cake to obtain ferric hydroxide;
s7, washing the ferric hydroxide for 2 times by using water to obtain high-purity ferric hydroxide;
s8, adding water into high-purity ferric hydroxide to prepare ferric hydroxide slurry containing 2% of iron, mixing the ferric hydroxide slurry with phosphoric acid, reacting at the normal pressure and 60 ℃ for 5.5 hours in a heat preservation manner, filtering and collecting a filter cake to obtain a ferric phosphate wet base; the molar ratio of phosphorus to iron is 1.06;
s9, washing the iron phosphate wet base for 2 times to obtain a high-purity iron phosphate wet base;
s10, drying the high-purity iron phosphate wet base at 300 ℃ to obtain ferric phosphate dihydrate;
s11, calcining the dihydrate ferric phosphate at 700 ℃ for 1.5 hours to obtain the battery-grade anhydrous ferric phosphate.
In the above examples, the recovery rate of iron in the pyrite cinder, and the quality of the obtained intermediate iron hydroxide and the final iron phosphate are shown in tables 2, 3, and 4.
TABLE 2 example iron recovery of pyrite cinder
Iron hydroxide product index in Table 3 example
Table 4 index of iron phosphate product obtained in example
It can be seen from tables 2, 3 and 4 that the recovery rate of iron in pyrite cinder is very high by the method of the present invention, which is much higher than the recovery rate of the prior art. The purity of the ferric hydroxide and the ferric phosphate prepared by the method is very high, and each index of the ferric phosphate is higher than the industrial standard.
Taking the above example 1 as an example, the microstructure of the iron phosphate product prepared by the method is tested, and fig. 1 and fig. 2 show an SEM image (surface microstructure photographed by a scanning electron microscope) and an XRD image (X-ray diffraction pattern) of the iron phosphate product prepared by the example 1, respectively.
According to the figure 1, the iron phosphate product is a nano-scale spherical aggregate, has loose and porous appearance and relatively uniform particle size, has a higher specific surface area, and is favorable for improving the reactivity of the iron phosphate serving as the next step.
The XRD peak spectrum of the iron phosphate and the iron phosphate are subjected to peak fitting and peak searching to obtain a graph 2, and all peak spectrums of the product are completely coincided with the iron phosphate in the example 1, so that the product is the high-purity iron phosphate.
The embodiment of the invention is not limited to the above embodiment, and in the method of the invention, each technical parameter can be adjusted within a certain range, such as the used pyrite cinder raw material containing Fe 2 O 3 、Fe 3 O 4 FeO, raw materials with the iron mass content of 45-60% can be used, and the raw materials inevitably contain impurity SiO 2 、Al 2 O 3 CaO, znO, mgO, and the like. In the step S1, the particle size of the crushed pyrite cinder powder can be 80-600 meshes, the used acid solution can be sulfuric acid with the mass concentration of 38-65%, and the use amount of the sulfuric acid is 1.5-3 times of the mass of the pyrite cinder powder; in the step S2, the mixed slurry can be stirred and reacted for 2.5 to 5 hours at the temperature of 85 to 116 ℃, then water is added, the temperature is kept for 0.5 to 2 hours, and the reaction solution is obtained after filtration and collection; in the step S3, adding iron powder into the reaction liquid, and then stirring and reacting at 50 to 95 ℃ for 0.5 to 3.0 hours to obtain a raw material slurry; adding alkali liquor into the reducing slurry in the step S4, adjusting the pH to 5.2 to 7.4, filtering and collecting filtrate to obtain refined reducing liquid; in step S5, adding an oxidant into the refined reducing solution, and reacting at 15 to 75 ℃ for 0.5 to 24 hours to obtain an oxidation slurry; adding an alkali liquor into the oxide slurry in the step S6, adjusting the pH to 2.8 to 4.8, filtering and collecting a filter cake to obtain ferric hydroxide; step S8, adding water into high-purity iron hydroxide to prepare slurry containing 2-12% of iron, mixing the slurry with phosphoric acid, reacting at normal pressure and 60-97 ℃ for 1.8-5.5 hours in a heat preservation manner, and filtering and collecting a filter cake to obtain an iron phosphate wet base; in the step S10, the high-purity iron phosphate wet base can be dried at the temperature of 105 to 500 ℃; in the step S11, the ferric phosphate dihydrate can be calcined at 680 to 950 ℃ for 1 to 2 hours to obtain the battery grade anhydrous ferric phosphate. The alkali liquor can be one of 10-38% of sodium hydroxide, 10-35% of sodium carbonate, 10-30% of ammonia water and 10-30% of urea by mass concentration. The oxidant can be hydrogen peroxide or air, and the molar ratio of hydrogen peroxide to iron is (0.5) - (1 to 0.7); the reaction temperature after the addition of the oxidant is 25 to 55 ℃, the reaction time is 0.5 to 2 hours, and the oxidation time after the addition of air is 3 to 24 hours.
All percentages stated in the present invention are percentages by mass, unless otherwise stated.
Claims (9)
1. The method for controllably preparing battery-grade iron phosphate from pyrite cinder is characterized by comprising the following steps of:
s1, crushing pyrite cinder to obtain pyrite cinder powder with uniform particle size, and then adding the pyrite cinder powder into an acid solution to obtain mixed slurry;
s2, stirring the mixed slurry at normal pressure and 85-116 ℃ for reaction for 2.5-5 hours, adding water, preserving heat for 0.5-2 hours, adding water for dilution, filtering and collecting reaction liquid;
s3, adding iron powder into the reaction liquid, stirring and reacting for 0.5-3.0 hours at the normal pressure and the temperature of 50-95 ℃, and adding water again to dilute to obtain a raw material slurry;
s4, adding alkali liquor into the reducing slurry, adjusting the pH value to 5.2-7.4, filtering and collecting filtrate to obtain refined reducing liquid;
s5, adding an oxidant into the refined reducing solution, and reacting at 15-75 ℃ for 0.5-24 hours to obtain oxidized slurry;
s6, adding alkali liquor into the oxidized slurry, adjusting the pH to 2.8-4.8, filtering and collecting a filter cake to obtain ferric hydroxide;
s7, washing the ferric hydroxide by using water to obtain high-purity ferric hydroxide;
s8, adding water into high-purity ferric hydroxide to prepare slurry containing 2-12% of iron, mixing the slurry with phosphoric acid, reacting at the normal pressure and the temperature of 60-97 ℃ for 1.8-5.5 hours in a heat preservation manner, filtering, and collecting a filter cake to obtain a ferric phosphate wet base;
s9, washing the iron phosphate wet base for 1-3 times to obtain a high-purity iron phosphate wet base;
s10, drying the high-purity ferric phosphate wet base at 105-500 ℃ to obtain ferric phosphate dihydrate;
s11, calcining the dihydrate ferric phosphate at 680-950 ℃ for 1-2 hours to obtain the battery-grade anhydrous ferric phosphate.
2. The method for controllably preparing battery-grade iron phosphate from pyrite cinder according to claim 1, wherein in step S1, the pyrite cinder contains Fe 2 O 3 、Fe 3 O 4 Of FeO, ironThe weight content is 45-60%, and the pyrite cinder contains impurities of Si, al, ca, zn and Mg.
3. The method for controllably preparing the battery-grade iron phosphate from the pyrite cinder according to claim 1, wherein in the step S1, the particle size of the crushed pyrite cinder powder is 80-600 meshes; the acid solution is sulfuric acid with the mass concentration of 38-65%, and the use amount of the sulfuric acid is 1.5-3 times of the mass of the pyrite cinder.
4. The method for controllably preparing the battery-grade iron phosphate from the pyrite cinder according to claim 1, wherein in the step S2, the stirring reaction temperature is 93-115 ℃ and the reaction time is 2.5-3.5 hours.
5. The method for controllably preparing battery-grade iron phosphate from pyrite cinder according to claim 1, wherein in step S3, the iron powder is recycled scrap iron-making iron powder and/or primary reduced iron powder, and the amount of the iron powder is 0.5-0.8 times of the amount of ferric iron measured by sampling in the reaction solution of step S2; after water is added, the iron content is 3-9%; the stirring reaction temperature is 65-85 ℃, and the reaction time is 0.5-2.0 hours.
6. The method for controllably preparing battery-grade iron phosphate from pyrite cinder according to claim 1, wherein in steps S4 and S6, the alkali liquor is one of sodium hydroxide with a mass concentration of 10% -38%, sodium carbonate with a mass concentration of 10% -35%, ammonia water with a mass concentration of 10% -30%, and urea with a mass concentration of 10% -30%.
7. The method for controllably preparing battery-grade iron phosphate from pyrite cinder according to claim 1, wherein in step S5, the oxidant is hydrogen peroxide or air, and the molar ratio of hydrogen peroxide to iron is from 0.5 to 1.7; the reaction temperature after adding the oxidant is 25-55 ℃, the reaction time after adding the hydrogen peroxide is 1-2 hours, and the oxidation time after adding the air is 3-24 hours.
8. The method for controllably preparing the battery-grade iron phosphate from the pyrite cinder according to claim 1, wherein in the step S6, the pH is adjusted to 3.2-4.2.
9. The method for controllably preparing battery-grade iron phosphate from pyrite cinder, according to claim 1, is characterized in that in step S8, high-purity ferric hydroxide is added with water to prepare slurry containing 2% -12% of iron, and the molar ratio of phosphorus content of the fed phosphoric acid to iron content of ferric hydroxide is 0.95-1.2: 1; the reaction temperature of the slurry and the phosphoric acid after mixing is 60 to 80 ℃, and the reaction time is 2.2 to 3.5 hours.
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