CN115231539B - Preparation method of high-purity ferric phosphate - Google Patents
Preparation method of high-purity ferric phosphate Download PDFInfo
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- CN115231539B CN115231539B CN202210820483.4A CN202210820483A CN115231539B CN 115231539 B CN115231539 B CN 115231539B CN 202210820483 A CN202210820483 A CN 202210820483A CN 115231539 B CN115231539 B CN 115231539B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
A preparation method of high-purity ferric phosphate relates to the technical field of ferric phosphate preparation. The invention aims to solve the problems that the reaction process of the traditional wet method for preparing the ferric phosphate needs to adjust the PH and control the reaction speed, the subsequent washing and impurity removal requirements are high due to the fact that the ions involved in the reaction are more numerous, and the purity and the yield of the prepared ferric phosphate material are low. The method comprises the following steps: step S1: preparing ferric chloride solution; step S2: preparing monoammonium phosphate solution; step S3: adding a polyaluminum chloride solution into an ammonium dihydrogen phosphate solution, and uniformly stirring to obtain a solution a; step S4: adding the solution a into ferric chloride solution, and stirring for reaction to obtain solution b; step S5: filtering, washing and drying the solution b to obtain ferric phosphate solid; step S6: and calcining the ferric phosphate solid at high temperature to obtain the high-purity ferric phosphate. The invention can obtain the preparation method of the high-purity ferric phosphate.
Description
Technical Field
The invention relates to the technical field of iron phosphate preparation, in particular to a preparation method of high-purity iron phosphate.
Background
The ferric phosphate has wide application, is mainly used for manufacturing lithium iron phosphate battery materials, is one of a few molluscicides approved for use in organic agriculture, and is nontoxic to pets and wild animals. Meanwhile, the iron phosphate is adhered to the surfaces of the steel and the metal, so that the metal can be prevented from being further oxidized, and the iron phosphate has innocuity and stability. The technology for preparing the ferric phosphate at home and abroad is relatively pure, and the traditional preparation method comprises a dry method and a wet method. The wet method mainly uses ferrous sulfate and phosphoric acid as main raw materials, but the reaction process needsThe pH is regulated, the reaction speed is controlled, and the requirement of subsequent washing and impurity removal is relatively high due to more participation of reaction ions, so that the whole experiment is complicated in steps and harsh in conditions, the cost is increased, and the method is not in line with the low-carbon environment-friendly new energy battery industry advocated by the current market in China. Therefore, in order to meet the development of the trend, the preparation steps of the iron phosphate material are simplified from the source to the precursor, the quality is strictly implemented according to the battery-grade iron phosphate industry standard HG/T4701-2014, and the tap density is required to be more than or equal to 0.7g/cm 3 The granularity is 2-6 μm.
Disclosure of Invention
The invention aims to solve the problems that the reaction process of the traditional wet method for preparing the ferric phosphate needs to adjust the PH and control the reaction speed, the subsequent washing and impurity removal requirements are high due to the fact that the ions involved in the reaction are more numerous, and the purity and the yield of the prepared ferric phosphate material are low, and provides a preparation method of high-purity ferric phosphate.
The preparation method of the high-purity ferric phosphate comprises the following steps:
step S1: preparing ferric chloride solution;
step S2: preparing monoammonium phosphate solution;
step S3: adding a polyaluminum chloride solution into an ammonium dihydrogen phosphate solution, and uniformly stirring to obtain a solution a; the volume ratio of the ferric chloride solution, the ammonium dihydrogen phosphate solution and the polyaluminum chloride solution is 100mL:100mL: (10-300) mu L;
step S4: adding the solution a into ferric chloride solution, and stirring and reacting for 60-300 min to obtain solution b;
step S5: filtering, washing and drying the solution b to obtain ferric phosphate solid;
step S6: calcining the ferric phosphate solid at 400-700 ℃ for 300-900 min to obtain the high-purity ferric phosphate.
The invention has the beneficial effects that:
(1) According to the preparation method of the high-purity ferric phosphate, ammonium dihydrogen phosphate and ferric chloride are used as raw materials, and the polyaluminium chloride net capturing agent is innovatively added, so that the ferric phosphate can be quickly settled in the reaction process, and the generation of large loss in filtering and washing is avoided, so that the yield is improved. More importantly, trace amounts of the net capturing agent play a role in providing crystal nuclei, but do not affect the quality and performance of the iron phosphate. Therefore, the addition of the aluminum chloride net capturing agent can increase the yield, optimize the process of preparing the ferric phosphate in the aqueous solution by a homogeneous precipitation method, improve the quality of the ferric phosphate and be more beneficial to preparing the high-performance lithium iron phosphate material.
The invention takes ferric chloride and ammonium dihydrogen phosphate as an iron source and a phosphorus source, does not need to adjust PH, does not need to react with an oxidant, and is simple and quick; the optimal preparation method of the ferric phosphate is explored by controlling a certain material ratio, a certain dispersion mode and adding the polyaluminium chloride net capturing agent. The invention has the biggest innovation point that high-quality ferric phosphate can be produced rapidly by adding trace polyaluminium chloride net capturing agent, because the polyaluminium chloride can gather particles rapidly, the filtering period is shortened, the particle size of the particles can not be increased, and the standard requirement of raw materials for battery level production is met. In addition, the raw materials of ferric chloride and monoammonium phosphate are simple and convenient in the filtering and washing steps, the trouble of sulfate radical or ferrous ion which is difficult to remove is avoided, and the quality of the product is improved. Since high-quality ferric phosphate is a key factor for preparing lithium iron phosphate as a positive electrode material of a lithium ion battery, the preparation of low-cost, high-efficiency and high-quality ferric phosphate is particularly important.
(2) The preparation method has the greatest advantages of simple preparation steps, high yield and good quality of the ferric phosphate. The raw materials adopt ferric chloride to replace ferrous sulfate, so that the reaction step of hydrogen peroxide and ferrous is skipped, the efficiency is improved, the reaction ratio is more accurate, and the reaction is more thorough. The invention does not need to add ammonia water or phosphoric acid to regulate and control pH, so that the reaction is easier to control, more importantly, the invention adds the polyaluminium chloride net catcher in the reaction process, because ferric phosphate can be rapidly precipitated at a specific pH, ferric chloride solution is biased to acid (pH is less than 2), so that ferric phosphate is difficult to generate precipitation in the system, but polyaluminium chloride provides crystal nucleus in the reaction process, so that ferric phosphate is rapidly precipitated, the particle size is uniform, and the yield is improved. Finally, the iron phosphate prepared by the homogeneous precipitation method reduces the interference of impurities, and is suitable for preparing the iron phosphate material with high compaction density and high purity.
The invention can obtain the preparation method of the high-purity ferric phosphate.
Drawings
FIG. 1 is a flow chart showing a process for producing iron phosphate in comparative example 1.
Fig. 2 is an XRD pattern of the iron phosphate material prepared in comparative example 1.
Fig. 3 is an SEM image of the iron phosphate material prepared in comparative example 1.
Fig. 4 is an XRD pattern of the high purity iron phosphate material prepared in example 3.
Fig. 5 is an SEM image of the high purity iron phosphate material prepared in example 3.
Detailed Description
The first embodiment is as follows: the preparation method of the high-purity ferric phosphate comprises the following steps:
step S1: preparing ferric chloride solution;
step S2: preparing monoammonium phosphate solution;
step S3: adding a polyaluminum chloride solution into an ammonium dihydrogen phosphate solution, and uniformly stirring to obtain a solution a; the volume ratio of the ferric chloride solution, the ammonium dihydrogen phosphate solution and the polyaluminum chloride solution is 100mL:100mL: (10-300) mu L;
step S4: adding the solution a into ferric chloride solution, and stirring and reacting for 60-300 min to obtain solution b;
step S5: filtering, washing and drying the solution b to obtain ferric phosphate solid;
step S6: calcining the ferric phosphate solid at 400-700 ℃ for 300-900 min to obtain the high-purity ferric phosphate.
The second embodiment is as follows: the present embodiment differs from the specific embodiment in that: the concentration of the ferric chloride solution in the step S1 is 0.8-5 mol/L.
The other steps are the same as in the first embodiment.
And a third specific embodiment: the present embodiment differs from the first or second embodiment in that: the concentration of the monoammonium phosphate solution in the step S2 is 1.2-5 mol/L.
Other steps are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: one difference between this embodiment and the first to third embodiments is that: the volume ratio of the ferric chloride solution, the ammonium dihydrogen phosphate solution and the polyaluminum chloride solution is 100mL:100mL:10 mu L.
Other steps are the same as those of the first to third embodiments.
Fifth embodiment: one to four differences between the present embodiment and the specific embodiment are: in the step S3, the mass fraction of the polyaluminum chloride in the polyaluminum chloride solution is 3-5 mg/L.
Other steps are the same as those of the first to fourth embodiments.
Specific embodiment six: the present embodiment differs from the first to fifth embodiments in that: the stirring speed in the step S3 is 80-100 r/min.
Other steps are the same as those of the first to fifth embodiments.
Seventh embodiment: one difference between the present embodiment and the first to sixth embodiments is that: in the step S4, the dropping speed of the solution a is 10-60 mL/min.
Other steps are the same as those of embodiments one to six.
Eighth embodiment: one difference between the present embodiment and the first to seventh embodiments is that: the drying temperature in the step S5 is 100-200 ℃, and the drying time is 300-900 min.
Other steps are the same as those of embodiments one to seven.
Detailed description nine: one of the differences between this embodiment and the first to eighth embodiments is: and in the step S6, the solid ferric phosphate is calcined for 300-900 min at the temperature of 400-650 ℃.
Other steps are the same as those of embodiments one to eight.
The following examples are used to verify the benefits of the present invention:
comparative example 1: as shown in fig. 1, the preparation method of the ferric phosphate comprises the following steps:
step S1: preparing 100mL of 0.8mol/L ferric chloride solution;
step S2: preparing 100mL of 1.3mol/L monoammonium phosphate solution;
step S3: slowly dripping the ammonium dihydrogen phosphate solution into the ferric chloride solution at the speed of 20mL/min, stirring and reacting for 180min, and gradually generating white precipitate (namely ferric phosphate dihydrate) from the reddish brown solution to obtain the ferric phosphate dihydrate solution;
step S4: filtering and washing the ferric phosphate dihydrate solution, and drying for 480 minutes at the temperature of 100 ℃ to obtain ferric phosphate solid;
step S5: the iron phosphate solid was placed in a muffle furnace and calcined at 500 ℃ for 600min to remove the crystal water, thereby obtaining high-purity iron phosphate with a yield of about 4g and a yield of 80%.
The anhydrous iron phosphate powder prepared in this example was tested using an X-ray diffractometer (XRD) and the results obtained are shown in fig. 2, where the main peak in XRD is in line with the standard card for iron phosphate, indicating that the material prepared was iron phosphate, but some impurity peaks were present.
As shown in FIG. 3, the iron phosphate was subjected to a Scanning Electron Microscope (SEM), and the obtained material had a size of about 4. Mu.m, and the surface was not smooth enough but had a good crystallinity.
Comparative example 2: the preparation method of the ferric phosphate comprises the following steps:
step S1: preparing 100mL of 0.8mol/L ferric chloride solution;
step S2: preparing 100mL of 1.3mol/L monoammonium phosphate solution;
step S3: the ammonium dihydrogen phosphate solution is slowly dripped into the ferric chloride solution at the speed of 20mL/min, ultrasonic dispersion is carried out for 30min, and the reddish brown solution gradually generates white precipitate (namely ferric phosphate dihydrate), but the reaction is incomplete and full, and the white precipitate (ferric phosphate) and the reddish brown precipitate (ferric hydroxide) coexist, so that the yield is reduced, and the purity of the product is greatly reduced.
Example 3: the preparation method of the high-purity ferric phosphate comprises the following steps:
step S1: preparing 100mL of 0.8mol/L ferric chloride solution;
step S2: preparing 100mL of 1.3mol/L monoammonium phosphate solution;
step S3: adding 10 mu L of a 10g/L polyaluminum chloride solution into an ammonium dihydrogen phosphate solution, and stirring at a speed of 80r/min for 5min to obtain a solution a;
step S4: slowly dripping the solution a into ferric chloride solution at the speed of 20mL/min, stirring and reacting for 180min, and gradually generating white precipitate (namely ferric phosphate dihydrate) from the reddish brown solution to obtain ferric phosphate dihydrate solution;
step S5: filtering and washing the ferric phosphate dihydrate solution, and drying for 480 minutes at the temperature of 100 ℃ to obtain ferric phosphate solid;
step S6: the iron phosphate solid was placed in a muffle furnace and calcined at 500 ℃ for 600min to remove the crystal water, thereby obtaining high-purity iron phosphate with a yield of about 6g and a yield of 80%.
The anhydrous iron phosphate powder of this example was tested using an X-ray diffractometer (XRD) and the results obtained are shown in fig. 4, and the main peak of the iron phosphate is the same as in comparative example 1, demonstrating that the material is iron phosphate. However, the present example is superior to comparative example 1 in that it has fewer impurity peaks and higher crystallinity (peak intensity is about 3000), indicating that the addition of the polyaluminum chloride solution can effectively reduce impurities and is advantageous in improving crystallinity.
The result of Scanning Electron Microscope (SEM) of the ferric phosphate is shown in figure 5, the size is about 2 mu m, the crystal surface is smooth, the crystallinity is very high, and the standard requirement of ferric phosphate used for preparing high-performance lithium iron phosphate material is met.
As can be seen, comparative example 1 is a blank group, and iron chloride and ammonium dihydrogen phosphate are used as raw materials to produce iron phosphate, and the yield is not ideal. Comparative example 2 to investigate the effect of different dispersion modes, comparative example 1 was magnetic stirring and comparative example 2 was ultrasonic dispersion. In comparative example 2, not only iron phosphate but also a large amount of iron hydroxide was produced, and it is apparent that the yield and purity of comparative example 2 were lower than those of comparative example 1. The last example 3 is to explore the effect of adding trace amounts of polyaluminium chloride during the reaction. The yield was first increased by 50% over comparative example 1, because the net-capturing agent polyaluminum chloride contributes to the formation of iron phosphate precipitate, the amount of loss during the filtration washing is low, and trace amounts of net-capturing agent do not affect the quality and performance of iron phosphate, example 3 illustrates that polyaluminum chloride exists as a catalyst, promoting the formation of reaction.
In summary, example 3 discloses a rapid preparation process of battery grade ferric phosphate, which uses ammonium dihydrogen phosphate and ferric chloride as raw materials, and innovatively adds a polyaluminium chloride net capturing agent, so that ferric phosphate can be rapidly settled in the reaction process, and larger loss in filtration and washing is avoided, thereby improving the yield. More importantly, trace amounts of the net capturing agent play a role in providing crystal nuclei, but do not affect the quality and performance of the iron phosphate. Therefore, the addition of the aluminum chloride net capturing agent can increase the yield, optimize the process of preparing the ferric phosphate in the aqueous solution by a homogeneous precipitation method, improve the quality of the ferric phosphate and be more beneficial to preparing the high-performance lithium iron phosphate material.
Claims (7)
1. The preparation method of the high-purity ferric phosphate is characterized by comprising the following steps of:
step S1: preparing ferric chloride solution;
step S2: preparing monoammonium phosphate solution;
step S3: adding a polyaluminum chloride solution into an ammonium dihydrogen phosphate solution, and uniformly stirring to obtain a solution a; the volume ratio of the ferric chloride solution, the ammonium dihydrogen phosphate solution and the polyaluminum chloride solution is 100mL:100mL:10 mu L of polyaluminum chloride solution, wherein the mass fraction of polyaluminum chloride in the polyaluminum chloride solution is 3-5 mg/L;
step S4: adding the solution a into ferric chloride solution, and stirring and reacting for 60-300 min to obtain solution b;
step S5: filtering, washing and drying the solution b to obtain ferric phosphate solid;
step S6: calcining the ferric phosphate solid at 400-700 ℃ for 300-900 min to obtain the high-purity ferric phosphate.
2. The method for producing high-purity iron phosphate according to claim 1, wherein the concentration of the ferric chloride solution in step S1 is 0.8 to 5mol/L.
3. The method for producing high-purity iron phosphate according to claim 1 or 2, wherein the concentration of the monoammonium phosphate solution in step S2 is 1.2 to 5mol/L.
4. The method for producing high-purity iron phosphate according to claim 1, wherein the stirring speed in step S3 is 80 to 100r/min.
5. The method for producing high-purity iron phosphate according to claim 1 or 4, wherein the dropping speed of the solution a in step S4 is 10 to 60mL/min.
6. The method for preparing high-purity iron phosphate according to claim 1, wherein the drying temperature in step S5 is 100-200 ℃ and the drying time is 300-900 min.
7. The method for producing high-purity iron phosphate according to claim 1 or 6, wherein in step S6, the iron phosphate solid is calcined at a temperature of 400 to 650 ℃ for 300 to 900 minutes.
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| CN108584900A (en) * | 2018-05-23 | 2018-09-28 | 福建荣华科技有限公司 | A kind of battery-grade iron phosphate and its collection, preparation method |
| CN108862226A (en) * | 2018-08-15 | 2018-11-23 | 南通百川新材料有限公司 | A kind of preparation method of high-purity battery-grade iron phosphate |
| CN112645299A (en) * | 2020-12-03 | 2021-04-13 | 广东邦普循环科技有限公司 | Preparation method and application of iron phosphate |
| CN113603071A (en) * | 2021-07-23 | 2021-11-05 | 广东邦普循环科技有限公司 | Nano flaky iron phosphate and preparation method and application thereof |
| CN114644327A (en) * | 2022-04-22 | 2022-06-21 | 上海鑫忆丹新材料有限公司 | Preparation method of iron phosphate and application of iron phosphate |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108584900A (en) * | 2018-05-23 | 2018-09-28 | 福建荣华科技有限公司 | A kind of battery-grade iron phosphate and its collection, preparation method |
| CN108862226A (en) * | 2018-08-15 | 2018-11-23 | 南通百川新材料有限公司 | A kind of preparation method of high-purity battery-grade iron phosphate |
| CN112645299A (en) * | 2020-12-03 | 2021-04-13 | 广东邦普循环科技有限公司 | Preparation method and application of iron phosphate |
| WO2022116702A1 (en) * | 2020-12-03 | 2022-06-09 | 广东邦普循环科技有限公司 | Method for preparing iron phosphate and use thereof |
| CN113603071A (en) * | 2021-07-23 | 2021-11-05 | 广东邦普循环科技有限公司 | Nano flaky iron phosphate and preparation method and application thereof |
| CN114644327A (en) * | 2022-04-22 | 2022-06-21 | 上海鑫忆丹新材料有限公司 | Preparation method of iron phosphate and application of iron phosphate |
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