CN109775679B - Preparation method of iron phosphate for high-purity high-compaction lithium iron phosphate - Google Patents
Preparation method of iron phosphate for high-purity high-compaction lithium iron phosphate Download PDFInfo
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Abstract
The invention relates to the technical field of lithium battery raw material preparation, in particular to a preparation method of iron phosphate for high-purity high-compaction lithium iron phosphate, which comprises the following steps: the method comprises the steps of using ferrous sulfate as a titanium dioxide byproduct as a raw material, basically removing impurity elements in the ferrous sulfate through the reverse precipitation of sulfide and ferric hydroxide, preparing ferric phosphate from a ferric hydroxide filter cake to obtain superfine ferric phosphate slurry, mixing the superfine ferric phosphate slurry and the ferric phosphate with the slurry particle size distribution of 3.0-16 mu m in a pressure container according to a certain proportion, stirring, aging, performing suction filtration and washing to obtain ferric phosphate dihydrate, and performing spray granulation and dehydration to obtain anhydrous ferric phosphate; the method utilizes industrial semi-solid waste ferrous sulfate to prepare anhydrous iron phosphate with high purity and simple process, and utilizes two types of iron phosphate with particle size distribution to prepare raw materials for high-compaction lithium iron in a mixing manner at a slurry process, the mixing is more uniform, and the compaction density of the lithium iron phosphate prepared from the raw materials exceeds 2.4g/cm3。
Description
Technical Field
The invention relates to the technical field of lithium battery raw material preparation, in particular to a preparation method of iron phosphate for high-purity high-compaction lithium iron phosphate.
Background
In recent years, with the strong support of national policies, lithium ion battery materials, in particular lithium iron phosphate and ternary materials, have developed rapidly. Policy adjustment puts higher requirements on the energy density of the lithium iron phosphate battery, so that the compacted density of the lithium iron phosphate needs to be improved, and most of the compacted density of the lithium iron phosphate in the current market is 2.2-2.4 g/cm3. The iron phosphate serving as a raw material for preparing the lithium iron phosphate has direct influence on the compacted density of the lithium iron phosphate, and the invention aims to prepare the high-purity high-compaction iron phosphateThe energy density of the lithium iron phosphate battery pack is finally improved by using the raw material iron phosphate for the lithium iron phosphate.
The chinese patent application CN109192948A provides a high-compaction-density lithium iron phosphate and a preparation method thereof, wherein spherical small-particle lithium iron is filled into large-particle lithium iron phosphate, and the lithium iron phosphate anode material is obtained through three-stage sintering and cooling. The method adopts a physical mechanical method to mix solid lithium iron phosphate, which causes uneven mixing, small particles can not be effectively filled, and the obtained product may have different batches with larger difference of compaction density. The Chinese patent application CN108840317A provides a preparation method of high-purity high-compaction battery-grade iron phosphate, which comprises the steps of firstly reacting a certain amount of iron with 15-25% of phosphoric acid at 40-100 ℃ to generate a ferrous-containing phosphoric acid solution, then introducing ozone for oxidation to obtain iron phosphate slurry, filtering and washing, and then dehydrating to obtain anhydrous iron phosphate. The invention uses pure iron and ozone as raw materials, has higher cost and is difficult to realize industrialization at present. The invention utilizes ferric hydroxide to prepare ferric phosphate when precipitating at lower pH, the particle size distribution of the ferric phosphate is mainly 0.2-4.0 μm, the particle size distribution of the ferric phosphate prepared by ferric iron source and calcium phosphate is mainly 3.0-16 μm, the ferric phosphate slurry of the two particle sizes is stirred and mixed under certain pressure, the large and small particles are fully mixed, atomized, granulated and dehydrated to obtain the high-compaction ferric phosphate.
Disclosure of Invention
The invention provides a preparation method of iron phosphate for high-purity high-compaction lithium iron phosphate, which is characterized by comprising the following steps of:
(1) removing impurities and purifying ferrous sulfate: dissolving ferrous sulfate serving as a titanium dioxide byproduct in deionized water at the concentration of 0.6-1.6 mol/L and the water bath temperature of 10-60 ℃, adding a small amount of reduced iron powder and sulfide, stirring, standing and filtering;
(2) preparing ferric hydroxide precipitate: adding an oxidant into the filtrate obtained in the step (1) for oxidation, adjusting the water bath temperature to 40-90 ℃, then adjusting the pH to 3.0-6.0 by using an adjusting agent, adding a flocculating agent, performing suction filtration, and washing to obtain an iron hydroxide filter cake;
(3) synthesis of slurry A: dissolving the filter cake prepared in the step (2) in deionized water, heating to 60-95 ℃, adding phosphate and a dispersing agent, adding dilute acid to adjust the pH value to 0.6-1.8, and stirring to obtain slurry A;
(4) synthesizing slurry B: with a source of trivalent iron and Ca3(PO4)2Stirring ferric iron source iron with the concentration of 0.5-1.8 mol/L in a water bath at the temperature of 60-95 ℃, adding phosphoric acid to adjust the pH value to 1.0-1.6, and reacting to obtain slurry B;
(5) mixing: and stirring and mixing the slurry A and the slurry B in a pressure container according to a certain proportion to obtain slurry C, aging, carrying out suction filtration and washing to obtain ferric phosphate dihydrate, atomizing, granulating and dehydrating to obtain the high-purity high-compaction anhydrous ferric phosphate.
Preferably, in step (1):
the sulfide is one or two of sodium sulfide and ferrous sulfide;
the addition amount of the sulfide is 1-1.5 times of the molar amount of heavy metal in ferrous sulfate, and preferably 1.1-1.2;
the adding amount of the iron powder is 0.5-1.5% of the ferrous sulfate;
preferably, the stirring time in the step (1) is 30 min-1 h.
Preferably, in step (2):
the oxidant is selected from hydrogen peroxide and sodium peroxide;
the adding amount of the oxidant is 1-1.5 times, preferably 1-1.2 times of the mole number of the iron in the ferrous sulfate;
the regulator is selected from one or more of sodium hydroxide, ammonia water, potassium hydroxide or sodium carbonate;
the flocculating agent in the step (2) is polyacrylamide;
the addition amount of the flocculating agent is 0.1-1% of the volume of the ferrous sulfate solution, and preferably 0.5-1%;
the reaction time in the step (2) is 1-5 h, preferably 2-4 h.
Preferably, in step (3):
the phosphate is selected from one or more of sodium phosphate, sodium dihydrogen phosphate, sodium monohydrogen phosphate or ammonium dihydrogen phosphate;
the dispersing agent is selected from one or more of ethylene glycol, polyethylene glycol or SIMULSOL 265;
the dilute acid is selected from dilute sulfuric acid, dilute hydrochloric acid and dilute phosphoric acid; the concentration is preferably 0.5-2 mol/L;
the molar ratio of phosphorus to an iron source of the phosphate is 1.0-1.5: 1, preferably 1.0 to 1.2: 1;
the reaction time in the step (3) is 2-10 h, preferably 4-6 h.
Preferably, in step (4):
the ferric iron source is selected from ferric chloride or ferric nitrate;
the Ca3(PO4)2The molar ratio of the reaction with the ferric iron source is as follows: 0.4-0.8: 1;
the concentration of the phosphoric acid is 0.5-2.0 mol/L;
the reaction time in the step (4) is 2-8 h, preferably 4-6 h.
Preferably, in step (5):
the mol ratio of the slurry A to the slurry B is 1: 2-10, preferably 1: 4-6;
the pressure of the pressure container is 0.5-20.0 Mpa; the aging time is 2-48 h, preferably 4-24 h, and more preferably 8-12 h.
Furthermore, the atomization granulation temperature is 90-120 ℃, and the drying temperature is 500-700 ℃.
The invention also relates to high-purity high-compaction lithium iron phosphate which is prepared by taking the iron phosphate prepared by any one of the methods as a raw material, wherein the compaction density of the lithium iron phosphate can reach 2.4g/cm3The above.
The method solves the technical problem that the electric performance of the lithium iron phosphate battery is influenced due to lower compactness and purity of the iron phosphate in the current industrial production.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention prepares two kinds of iron phosphate with different particle size distributions by using different methods, wherein the particle size distribution of slurry A is mainly 0.2-4.0 mu m, and the particle size distribution of slurry B is 3.0-16 mu m; then the two kinds of slurry with the particle size distribution are fully stirred and mixed according to a certain proportion, high-density ferric phosphate is obtained under the action of certain pressure in a pressure container,the high-compaction lithium iron phosphate can be prepared by using the material as a raw material, and the compaction density of the high-compaction lithium iron phosphate is detected to be 2.4-2.53 g/cm3；
(2) The raw material for preparing the superfine ferric phosphate is ferrous sulfate as a byproduct of titanium dioxide, most impurities are removed through the reverse precipitation of sulfide and ferric hydroxide in the preparation process, the electrochemical performance of the final product lithium ferric phosphate can be effectively improved, the industrial semi-solid waste is fully utilized, and the resources are saved;
(3) the method can control and obtain iron phosphate with different particle sizes by adjusting the pH value of the prepared ferric hydroxide precipitate;
(4) the preparation process of the invention has simple flow and low cost, and can be used for industrial mass production.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a schematic flow chart of the method of the present invention
Detailed Description
The present invention will be further described with reference to the following examples. The described embodiments and their results are only intended to illustrate the invention and should not be taken as limiting the invention described in detail in the claims.
Example 1
(1) Removing impurities and purifying ferrous sulfate: dissolving 500g of titanium dioxide byproduct ferrous sulfate in 1.2L of deionized water, adding 5g of iron powder and 10g of sodium sulfide nonahydrate at the water bath temperature of 30 ℃, stirring for 30min, and filtering;
(2) preparing ferric hydroxide precipitate: adding 250 ml of 30% hydrogen peroxide into the filtrate obtained in the step (1) for oxidation, then placing the filtrate into a water bath at 60 ℃, adjusting the pH to 3.0 by using a 30% sodium hydroxide solution, adding polyacrylamide (0.5% of the volume of a ferrous sulfate solution), reacting for 5 hours, carrying out suction filtration, and washing to obtain an iron hydroxide filter cake;
(3) synthesis of slurry A: dissolving the ferric hydroxide filter cake prepared in the step (2) in deionized water, heating to 95 ℃, adding 200 ml of 9mol/L sodium monohydrogen phosphate solution and 6ml of polyethylene glycol, adding 0.5mol/L dilute sulfuric acid to adjust the pH value to 1.5, and stirring for 10 hours to obtain slurry A;
(4) synthesizing slurry B: adding 8.5L of 1.8mol/L ferric nitrate, slowly adding 5kg of calcium phosphate powder, adding phosphoric acid to adjust the pH to 1.6, reacting in a water bath at 95 ℃, stirring for 8h to obtain slurry B,
(5) slurry A, B mixing: mixing the slurry A and the slurry B according to a molar ratio of 1: stirring and mixing the mixture for 48 hours at the temperature of 60 ℃ in a pressure container according to the proportion of 10, obtaining slurry C with the pressure value of 20Mpa, aging, carrying out suction filtration and washing to obtain ferric phosphate dihydrate, and carrying out atomization granulation and dehydration to obtain the high-purity high-compaction anhydrous ferric phosphate.
(6) The iron phosphate, lithium carbonate and glucose prepared by the method are calcined at 600 ℃ to obtain the lithium iron phosphate.
Example 2
(1) Removing impurities and purifying ferrous sulfate: dissolving 500g of titanium dioxide byproduct ferrous sulfate in 1.6L of deionized water, adding 10g of iron powder and 15g of sodium sulfide nonahydrate at the water bath temperature of 60 ℃, stirring for 30min, and filtering;
(2) preparing ferric hydroxide precipitate: adding 250 ml of 30% hydrogen peroxide into the filtrate obtained in the step (1) for oxidation, then placing the filtrate into a water bath at 90 ℃, adjusting the pH to 4.5 by using a 30% sodium hydroxide solution, adding polyacrylamide (1% of the volume of a ferrous sulfate solution), reacting for 2 hours, performing suction filtration, and washing to obtain an iron hydroxide filter cake;
(3) synthesis of slurry A: dissolving the ferric hydroxide filter cake prepared in the step (2) in deionized water, heating to 80 ℃, adding 200 ml of 9mol/L ammonium dihydrogen phosphate solution and 10ml of polyethylene glycol, adding 1.5mol/L dilute sulfuric acid to adjust the pH value to 1.2, and stirring for 6 hours to obtain slurry A;
(4) synthesizing slurry B: adding 7.5L of 1.1mol/L ferric nitrate, slowly adding 2.5kg of calcium phosphate powder, adding phosphoric acid to adjust the pH to 1.0, reacting in a water bath at 90 ℃, stirring for 5h to obtain slurry B,
(5) slurry A, B mixing: mixing the slurry A and the slurry B according to a molar ratio of 1: 5, stirring and mixing the mixture for 24 hours at the temperature of 60 ℃ in a pressure container with the pressure value of 0.5Mpa to obtain slurry C, aging, carrying out suction filtration and washing to obtain ferric phosphate dihydrate, and then carrying out atomization granulation and dehydration to obtain the high-purity high-compaction anhydrous ferric phosphate.
(6) The iron phosphate, lithium carbonate and glucose prepared by the method are calcined at 600 ℃ to obtain the lithium iron phosphate.
Example 3
(1) Removing impurities and purifying ferrous sulfate: dissolving 500g of titanium dioxide byproduct ferrous sulfate in 2.0L of deionized water, adding 5g of iron powder and 7g of sodium sulfide nonahydrate at the water bath temperature of 40 ℃, stirring for 30min, and filtering;
(2) preparing ferric hydroxide precipitate: adding 250 ml of 30% hydrogen peroxide into the filtrate obtained in the step (1) for oxidation, then placing the filtrate into a water bath at 40 ℃, adjusting the pH to 6.0 by using a 30% sodium hydroxide solution, adding polyacrylamide (0.2% of the volume of a ferrous sulfate solution), reacting for 4 hours, carrying out suction filtration, and washing to obtain an iron hydroxide filter cake;
(3) synthesis of slurry A: dissolving the ferric hydroxide filter cake prepared in the step (2) in deionized water, heating to 60 ℃, adding 200 ml of 9mol/L ammonium dihydrogen phosphate solution and 15ml of SIMULSOL 265, adding 2.0mol/L dilute sulfuric acid to adjust the pH value to 0.6, and stirring for 2 hours to obtain slurry A;
(4) synthesizing slurry B: adding 2.0L of 1.5mol/L ferric chloride, slowly adding 1.0kg of calcium phosphate powder, adding phosphoric acid to adjust pH to 1.3, reacting in water bath at 60 deg.C, stirring for 2 hr to obtain slurry B,
(5) slurry A, B mixing: mixing the slurry A and the slurry B according to a molar ratio of 1: stirring and mixing the mixture for 2 hours at the temperature of 60 ℃ in a pressure container according to the proportion of 2, obtaining slurry C with the pressure value of 10Mpa, aging, carrying out suction filtration and washing to obtain ferric phosphate dihydrate, and carrying out atomization granulation and dehydration to obtain the high-purity high-compaction anhydrous ferric phosphate.
(6) The iron phosphate, lithium carbonate and glucose prepared by the method are calcined at 600 ℃ to obtain the lithium iron phosphate.
Example 4
(1) Removing impurities and purifying ferrous sulfate: dissolving 500g of titanium dioxide byproduct ferrous sulfate in 1.5L of deionized water, adding 10g of iron powder and 3g of ferrous sulfide at the water bath temperature of 50 ℃, stirring for 30min, and filtering;
(2) preparing ferric hydroxide precipitate: adding 250 ml of 30% hydrogen peroxide into the filtrate obtained in the step (1) for oxidation, then placing the filtrate into a water bath at 60 ℃, adjusting the pH to 4.5 by using a 30% sodium hydroxide solution, adding polyacrylamide (0.5% of the volume of a ferrous sulfate solution), reacting for 2 hours, carrying out suction filtration, and washing to obtain an iron hydroxide filter cake;
(3) synthesis of slurry A: dissolving the ferric hydroxide filter cake prepared in the step (2) in deionized water, heating to 80 ℃, adding 200 ml of 9mol/L ammonium phosphate solution and 10ml of ethylene glycol, adding 1.0mol/L dilute sulfuric acid to adjust the pH value to 1.2, and stirring for 10 hours to obtain slurry A;
(4) synthesizing slurry B: adding 5.0L of 1.5mol/L ferric chloride, slowly adding 2.5kg of calcium phosphate powder, adding phosphoric acid to adjust pH to 1.3, reacting in water bath at 80 deg.C, stirring for 10 hr to obtain slurry B,
(5) slurry A, B mixing: mixing the slurry A and the slurry B according to a molar ratio of 1: 5, stirring and mixing the mixture for 8 hours at the temperature of 60 ℃ in a pressure container with the pressure value of 20Mpa to obtain slurry C, aging, performing suction filtration and washing to obtain ferric phosphate dihydrate, and performing atomization granulation and dehydration to obtain the high-purity high-compaction anhydrous ferric phosphate.
(6) The iron phosphate, lithium carbonate and glucose prepared by the method are calcined at 600 ℃ to obtain the lithium iron phosphate.
Comparative example 1
The concrete implementation method refers to example 1 except that the step (5) is reacted in a general vessel at a pressure value of 1 atm.
Comparative example 2
(1) Synthesizing slurry: adding 2.0L of 1.5mol/L ferric chloride, slowly adding 1.0kg of calcium phosphate powder, adding phosphoric acid to adjust pH to 1.3, reacting in water bath at 60 deg.C, stirring for 2 hr to obtain slurry B,
(2) drying and dehydrating: and aging the obtained slurry B for 2h, performing suction filtration and washing to obtain ferric phosphate dihydrate, and performing atomization granulation and dehydration to obtain anhydrous ferric phosphate.
(3) The iron phosphate, lithium carbonate and glucose prepared by the method are calcined at 600 ℃ to obtain the lithium iron phosphate.
The parameters of the compacted density of the lithium iron phosphate obtained by the test are shown in the table 1.
TABLE 1
According to the embodiment and the comparative example, the compacted density of the prepared lithium iron phosphate can reach 2.4g/cm3Above, comparative example 1 without mixing in a pressurized vessel, the compacted density was less than 2.4g/cm3Comparative example 2 did not adopt the method of the present invention, and thus the result was poor.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation.
Claims (19)
1. A preparation method of iron phosphate for lithium iron phosphate is characterized by comprising the following steps:
(1) removing impurities and purifying ferrous sulfate: dissolving ferrous sulfate serving as a titanium dioxide byproduct in deionized water at the concentration of 0.6-1.6 mol/L and the water bath temperature of 10-60 ℃, adding a small amount of reduced iron powder and sulfide, stirring, standing and filtering;
(2) preparing ferric hydroxide precipitate: adding an oxidant into the filtrate obtained in the step (1) for oxidation, adjusting the water bath temperature to 40-90 ℃, then adjusting the pH to 3.0-6.0 by using an adjusting agent, adding a flocculating agent, performing suction filtration, and washing to obtain an iron hydroxide filter cake;
(3) synthesis of slurry A: dissolving the filter cake prepared in the step (2) in deionized water, heating to 60-95 ℃, adding phosphate and a dispersing agent, adding dilute acid to adjust the pH value to 0.6-1.8, and stirring to obtain slurry A;
(4) synthesizing slurry B: with a source of trivalent iron and Ca3(PO4)2Stirring ferric iron source iron with the concentration of 0.5-1.8 mol/L in a water bath at the temperature of 60-95 ℃, adding phosphoric acid to adjust the pH value to 1.0-1.6, and reacting to obtain slurry B;
(5) mixing: and stirring and mixing the slurry A and the slurry B in a pressure container according to a certain proportion to obtain slurry C, aging, carrying out suction filtration and washing to obtain ferric phosphate dihydrate, atomizing, granulating and dehydrating to obtain the anhydrous ferric phosphate.
2. The production method according to claim 1, wherein in step (1):
the sulfide is one or two of sodium sulfide and ferrous sulfide;
the addition amount of the sulfide is 1-1.5 times of the molar amount of heavy metal in the ferrous sulfate;
the adding amount of the iron powder is 0.5 to 1.5 percent of the weight of the ferrous sulfate.
3. The production method according to claim 2, wherein in step (1): the addition amount of the sulfide is 1.1-1.2 times of the molar amount of heavy metal in the ferrous sulfate.
4. The production method according to claim 1, step (2):
the oxidant is selected from hydrogen peroxide, ozone and sodium peroxide;
the addition amount of the oxidant is 1-1.5 times of the mole number of the iron in the ferrous sulfate;
the regulator is selected from one or more of sodium hydroxide, ammonia water, potassium hydroxide or sodium carbonate;
the flocculating agent in the step (2) is polyacrylamide;
the addition amount of the flocculating agent is 0.1 to 1 percent of the volume of the ferrous sulfate solution;
the reaction time in the step (2) is 1-5 h.
5. The preparation method according to claim 4, wherein the amount of the oxidant added in the step (2) is 1 to 1.2 times of the mole number of the iron in the ferrous sulfate.
6. The preparation method according to claim 4, wherein the flocculant is added in the step (2) in an amount of 0.5-1% by volume of the ferrous sulfate solution.
7. The preparation method according to claim 4, wherein the reaction time in the step (2) is 2-4 h.
8. The production method according to claim 1, step (3):
the phosphate is selected from one or more of sodium phosphate, sodium dihydrogen phosphate, sodium monohydrogen phosphate or ammonium dihydrogen phosphate;
the dispersing agent is selected from one or more of ethylene glycol, polyethylene glycol or SIMULSOL 265;
the dilute acid is selected from dilute sulfuric acid, dilute hydrochloric acid and dilute phosphoric acid;
the molar ratio of phosphorus to iron source of the phosphate is 1: 1-1.5: 1;
the reaction time in the step (3) is 2-10 h.
9. The preparation method according to claim 8, wherein the dilute acid concentration in the step (3) is 0.5-2 mol/L.
10. The method according to claim 8, wherein the phosphate of step (3) has a phosphorus to iron source molar ratio of 1.0: 1-1.2: 1.
11. the preparation method according to claim 8, wherein the reaction time in step (3) is 4-6 h.
12. The production method according to claim 1, step (4):
the ferric iron source is selected from ferric chloride or ferric nitrate;
the Ca3(PO4)2The molar ratio of the reaction with the ferric iron source is as follows: 0.4: 1-0.8: 1;
the concentration of the phosphoric acid is 0.5-2.0 mol/L;
the reaction time in the step (4) is 2-8 h.
13. The preparation method according to claim 12, wherein the reaction time in step (4) is 4-6 h.
14. The production method according to claim 1, step (5):
the mol ratio of the slurry A to the slurry B is 1: 2-1: 10;
the pressure of the pressure container is 0.5-20.0 Mpa; the aging time is 2-48 h.
15. The method of claim 14, wherein the molar ratio of slurry a to slurry B in step (5) is 1: 4-1: 6.
16. the preparation method according to claim 14, wherein the aging time in step (5) is 4-24 h.
17. The preparation method according to claim 14, wherein the aging time in step (5) is 8-12 h.
18. The method according to claim 14, wherein the atomizing and granulating temperature is 90 to 120 ℃ and the drying temperature is 500 to 700 ℃.
19. Lithium iron phosphate prepared by using the iron phosphate prepared by the method of any one of claims 1 to 18 as a raw material, wherein the compacted density of the lithium iron phosphate can reach 2.4g/cm3The above.
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| CN110690429B (en) * | 2019-10-14 | 2021-07-06 | 王敏 | Treatment method of waste lithium iron phosphate |
| CN111268663A (en) * | 2020-01-19 | 2020-06-12 | 江苏乐能电池股份有限公司 | Preparation method of high-compaction iron phosphate particles |
| CN111533104B (en) * | 2020-06-23 | 2022-11-01 | 王家祥 | Method for preparing battery-grade iron phosphate |
| CN111777049A (en) * | 2020-07-31 | 2020-10-16 | 湖北融通高科先进材料有限公司 | Method for preparing iron phosphate by using mixed iron source |
| CN115650188A (en) * | 2022-09-08 | 2023-01-31 | 广西金茂钛业有限公司 | Method for preparing iron phosphate by using titanium dioxide byproduct ferrous sulfate |
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