CN110540185A - synthesis process of battery-grade iron phosphate - Google Patents
synthesis process of battery-grade iron phosphate Download PDFInfo
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- CN110540185A CN110540185A CN201910875696.5A CN201910875696A CN110540185A CN 110540185 A CN110540185 A CN 110540185A CN 201910875696 A CN201910875696 A CN 201910875696A CN 110540185 A CN110540185 A CN 110540185A
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
the invention discloses a synthesis process of battery-grade iron phosphate, which comprises impurity removal and purification of ferrous sulfate and synthesis of iron phosphate. The method solves at least one of the following problems 1, and solves the problem of high production cost of the iron phosphate of the current battery by adopting ferrous sulfate as a byproduct of titanium dioxide as a raw material; 2. the full-parameter control of the production process is realized, so that the defects of non-uniform reaction time, change of PH value of reaction liquid and the like in the traditional process route are overcome, the sizes and the shapes of the obtained iron phosphate crystals are consistent, the stability and the consistency of the product are fully ensured, and the product difference among batches is small; 3. the impurities are few, and the high quality of the product is realized.
Description
Technical Field
The invention relates to the field of inorganic materials, in particular to a synthesis process of battery-grade iron phosphate.
background
With the vigorous development of the lithium ion battery industry, the research on the lithium ion battery anode material is more and more deep. Lithium iron phosphate is one of the most important members of the positive electrode materials of lithium ion batteries, and is widely applied to the fields of automobiles, electric tools, energy storage equipment, emergency power supply equipment, mobile power supplies and the like at present. The synthesis process of the lithium iron phosphate mostly uses the iron phosphate as a raw material, and the internal structure of the iron phosphate is similar to that of the lithium iron phosphate, so that the lithium iron phosphate can obtain better electrochemical performance. The high-quality ferric phosphate is a key material for producing high-quality lithium iron phosphate, and the ferric phosphate is mostly prepared by taking ferrous sulfate (or ferric sulfate) and phosphate (monoammonium phosphate, diammonium phosphate and phosphoric acid) as raw materials. Ferrous sulfate is mostly adopted in production, the common ferrous sulfate cannot meet the preparation requirement due to low purity, and the ferrous sulfate with high purity is unsustainable in view of development due to high cost and large consumption of steel.
China is a large country for producing titanium dioxide, and 3.5-4 tons of ferrous sulfate heptahydrate can be produced as a byproduct when one ton of titanium dioxide is produced. Because the quality of the ferrous sulfate byproduct is poor, the ferrous sulfate byproduct cannot meet the use standard and is discarded in large quantity, thereby causing serious resource waste and environmental pollution. Therefore, the purification of the ferrous sulfate byproduct of the titanium dioxide can greatly reduce the production cost of the battery, fully recycle the iron resource in the titanium dioxide byproduct and eliminate the adverse effect on the environment.
At present, most of domestic iron phosphate production processes are as follows: firstly, oxidizing a food-grade ferrous sulfate solution by using hydrogen peroxide, adding phosphate or phosphoric acid for synthesis and conversion, and then washing, removing impurities and calcining. The process has complex synthesis process and can not be accurately controlled, the whole synthesis conversion reaction is not carried out in the same stable state from excessive ferric sulfate to excessive phosphate when the synthesis reaction is started, so that the product quality is unstable, the impurity content is high, the crystal size is different, the shape is different, and the final performance of the product is influenced.
Disclosure of Invention
The invention provides a synthesis process of battery-grade iron phosphate, which at least solves the following problems: 1. the production cost is high; 2. the stability and consistency of the product are poor; 3. the product purity is not high.
In order to achieve the purpose, the invention provides a synthesis process of battery-grade iron phosphate, which comprises the following steps:
a. preparing a ferrous sulfate solution containing 0.5-1mol/L of iron from the by-product ferrous sulfate of the titanium dioxide, adding an adsorbent and a regulator, regulating the pH of the solution to 1-2.5, adding a flocculating agent, and filtering to obtain a solution A;
b. Adjusting the pH value of the solution A to 0.5-2 by using the regulator, preparing a phosphate solution containing 1-2mol/L phosphorus, dripping the adjusted solution A, the prepared phosphate and a prepared oxidant into a reaction kettle at the same time, performing a synthetic reaction, adjusting the pH value to be stable at 0.5-2.5 by adding ammonia water or phosphoric acid, and filtering after the reaction is finished to obtain a filter cake;
c. Adding deionized water into the filter cake, washing, removing impurities, and pulping to obtain a solution B;
d. Adding phosphoric acid into the solution B, controlling the concentration of the phosphoric acid in the solution B to be 0.3-0.8mol/L, and carrying out conversion reaction to obtain a solution C;
e. And filtering, washing, drying and calcining the solution C to obtain the iron phosphate.
Compared with the prior art, the synthesis process of the battery-grade iron phosphate solves at least one of the following problems 1, and solves the problem of high production cost of the battery iron phosphate by adopting ferrous sulfate as a byproduct of titanium dioxide as a raw material; 2. the full-parameter control of the production process is realized, so that the defects of non-uniform reaction time, change of PH value of reaction liquid and the like in the traditional process route are overcome, the sizes and the shapes of the obtained iron phosphate crystals are consistent, the stability and the consistency of the product are fully ensured, and the product difference among batches is small; 3. the impurities are few, and the high quality of the product is realized.
Drawings
fig. 1 is a process flow diagram of a process for synthesizing battery grade iron phosphate according to an embodiment of the present invention.
Detailed Description
the present invention aims to solve one of the following problems: 1. the production cost is high; 2. the stability and consistency of the product are poor; 3. the product purity is not high.
In an embodiment of the present invention, a process for synthesizing battery grade iron phosphate comprises the following steps:
a. preparing a ferrous sulfate solution containing 0.5-1mol/L of iron from the by-product ferrous sulfate of the titanium dioxide, adding an adsorbent and a regulator, regulating the pH of the solution to 1-2.5, adding a flocculating agent, and filtering to obtain a solution A;
b. Adjusting the pH value of the solution A to 0.5-2 by using the regulator, preparing a phosphate solution containing 1-2mol/L phosphorus, dripping the adjusted solution A, the prepared phosphate and a prepared oxidant into a reaction kettle at the same time, performing a synthetic reaction, adjusting the pH value to be stable at 0.5-2.5 by adding ammonia water or phosphoric acid, and filtering after the reaction is finished to obtain a filter cake;
c. adding deionized water into the filter cake, washing, removing impurities, and pulping to obtain a solution B;
d. Adding phosphoric acid into the solution B, controlling the concentration of the phosphoric acid in the solution B to be 0.3-0.8mol/L, and carrying out conversion reaction to obtain a solution C;
e. And filtering, washing, drying and calcining the solution C to obtain the iron phosphate.
The adsorbent in the step a is one of polymerized phosphate, and the mass ratio of the adsorbent to ferrous sulfate is 0.04-0.06: 1. The regulator in the step a and the step b is sulfuric acid or phosphoric acid. The flocculant in the step a is one of polyacrylamide, poly dimethyl diallyl ammonium chloride and polyethyleneimine, and the mass ratio of the flocculant to ferrous sulfate is 0.02-0.04: 1. The phosphate in the step b is a mixture of monoammonium phosphate, diammonium phosphate and phosphoric acid, and the ratio of the amount of the added phosphorus ion substances to the amount of ferrous substances of ferrous sulfate in the phosphate is 1-1.3: 1. The oxidant in the step b is hydrogen peroxide with the concentration of 27.5-30%, and the addition amount of the oxidant is 1.2-2.4 times of the theoretical amount of the ferrous ions after the ferrous ions are completely oxidized into the ferric ions. And c, dropwise adding the three synthetic reactions in the step b into the reaction kettle for 30-90min, and simultaneously finishing the dropwise adding at the constant temperature of 40-88 ℃ for 3-5 h. The reaction temperature of the conversion reaction in the step d is constant at 90-98 ℃, and the reaction time is 2-3 h. The calcination temperature in the step e is 550-650 ℃, and the reaction time is 4-6 h.
When preparing ferrous sulfate solution containing 0.5-1mol/L of iron, the titanium dioxide byproduct solid ferrous sulfate is dissolved by water to prepare the titanium dioxide solution.
The impurity removal principle of ferrous sulfate in the step a is as follows: the method mainly comprises the steps that the polyphosphate has a specific adsorption effect on impurities such as Ti, Mn, Mg and the like in a ferrous sulfate solution at a proper temperature and pH, a flocculating agent is added to flocculate the adsorbed impurities together, so that the impurities are conveniently filtered and removed, the use requirement is met, and after the impurities are removed, the contents of Ti, Mn and Mg in the ferrous sulfate are below 100 PPm.
In the step b, the oxidation of ferrous sulfate and the synthesis of phosphate are synchronously carried out, the process is short, the whole synthesis reaction process can be ensured, the process is carried out in the same stable state, the crystal size and the shape of the obtained product are consistent, the stability and the consistency of the product are fully ensured, and the product difference among batches is small. The synthesis reaction process and the conversion reaction process are separated, so that the impurity removal effect of the product is ensured (impurities such as Mn, Mg, S and the like must be removed after synthesis, and the impurities can be fused with the product after conversion, so that the product purity is higher.
In actual operation:
example 1:
Dissolving 500g of titanium dioxide byproduct ferrous sulfate, preparing into ferrous sulfate solution with iron concentration of 0.5mol/L, adjusting pH to 1-1.2 (which can be adjusted by phosphoric acid or sulfuric acid), adding 20g of adsorbent, controlling stirring speed at 100r/min, stirring at normal temperature for 30min, adding 10g of flocculant, stirring for 5min, stopping stirring, and standing for 10 min. Then filtering to remove impurities until the solution is completely clear, and obtaining a ferrous solution for later use.
500mL of the purified ferrous sulfate solution is taken, and concentrated sulfuric acid (or phosphoric acid) is added to adjust the pH value of the solution to 0.5. And (3) dropwise adding the acidified ferrous sulfate solution, 250ml of phosphate solution with the phosphorus content of 1mol/L and 15.45ml of 30% hydrogen peroxide into a reaction system at the same time, wherein the pH of the system is stabilized at 0.5 (regulated by ammonia water or phosphoric acid), and the dropwise adding is completed within 30min synchronously. The temperature of the solution is raised to 40 ℃, stirred at the speed of 200r/min and reacted for 3 hours at constant temperature. And (3) filtering and washing the reacted yellow slurry (basic iron phosphate), adding 350ml of deionized water into a filter cake for pulping, adding 7.18ml of 85% concentrated phosphoric acid to ensure that the concentration of the phosphoric acid in the solution is 0.3mol/L, raising the temperature of a reaction system to 90 ℃, and carrying out heat preservation reaction for 2 hours at the stirring speed of 200 r/min. And after the reaction is finished, filtering and washing the slurry to obtain a white filter cake, drying the filter cake, and calcining at 550 ℃ for 4 hours to obtain the anhydrous iron phosphate.
Example 2:
dissolving 500g of titanium dioxide byproduct ferrous sulfate to prepare a ferrous sulfate solution with the iron concentration of 0.75mol/L, adjusting the pH value to 1.2-1.8, then adding 25g of adsorbent, controlling the stirring speed to be 150r/min, stirring at normal temperature for 30min, adding 15g of flocculant, stirring for 5min, stopping stirring the materials, and standing for 10 min. And (3) filtering and removing impurities from the materials for many times until the solution is completely clear, and obtaining a ferrous solution for later use.
500mL of the purified ferrous sulfate solution is taken, and concentrated sulfuric acid or ammonia water is added to adjust the pH value of the solution to 1.25. The acidified ferrous sulfate solution, 288ml of phosphate solution with the phosphorus content of 1.5mol/L and 34.77ml of 30% hydrogen peroxide are simultaneously dripped into a reaction system, the pH of the system is stabilized at 1.5 (adjusted by ammonia water or phosphoric acid), and the dripping is completed in 60 min. After the completion of the dropwise addition, the temperature of the solution was raised to 65 ℃ and the reaction was carried out at a constant temperature for 4 hours with stirring at a rate of 250 r/min. And filtering and washing the reacted yellow slurry, adding 350ml of deionized water into a filter cake for pulping, adding 13.16ml of 85% concentrated phosphoric acid to ensure that the concentration of the phosphoric acid in the solution is 0.55mol/L, raising the temperature of a reaction system to 94 ℃, and carrying out heat preservation reaction for 2.5 hours at the stirring speed of 250 r/min. And after the reaction is finished, filtering and washing the slurry to obtain a white filter cake, drying the filter cake, and calcining at 600 ℃ for 5 hours to obtain the anhydrous iron phosphate.
example 3:
Dissolving 500g of titanium dioxide byproduct ferrous sulfate to prepare a ferrous sulfate solution with iron concentration of 1mol/L, adjusting pH to 1.8-2.5, adding 30g of adsorbent, controlling stirring speed at 200r/min, stirring at normal temperature for 30min, adding 20g of flocculant, stirring for 5min, stopping stirring, and standing for 10 min. And (3) filtering and removing impurities from the materials for many times until the solution is completely clear, and obtaining a ferrous solution for later use.
and (3) taking 500mL of the purified ferrous sulfate solution, and adding concentrated sulfuric acid or ammonia water to adjust the pH value of the solution to 2. And simultaneously dropwise adding the acidified ferrous sulfate solution, 325ml of phosphate solution with the phosphorus content of 2mol/L and 61.82ml of 30% hydrogen peroxide into a reaction system, wherein the pH of the system is stabilized at 2.5 (regulated by ammonia water or phosphoric acid), and synchronously dropwise adding the acidified ferrous sulfate solution, the phosphate solution with the phosphorus content of 2mol/L and the 30% hydrogen peroxide for 90 min. After the completion of the dropwise addition, the temperature of the solution was raised to 88 ℃ and stirred at a rate of 300r/min, followed by isothermal reaction for 5 hours. And filtering and washing the reacted yellow slurry, adding 350ml of deionized water into a filter cake for pulping, adding 19.14ml of 85% concentrated phosphoric acid to ensure that the concentration of the phosphoric acid in the solution is 0.8mol/L, raising the temperature of a reaction system to 98 ℃, and carrying out heat preservation reaction for 3 hours at the stirring speed of 300 r/min. And after the reaction is finished, filtering and washing the slurry to obtain a white filter cake, drying the filter cake, and calcining at 650 ℃ for 6 hours to obtain the anhydrous iron phosphate.
table 1 test results:
it can be seen that the iron phosphate prepared by the invention has low impurity content below 50PPm, and part of the iron phosphate is below 10PPm, and the impurity content of iron phosphate S, Mg, Mn and the like produced by the common process is generally about 150 PPm. The tap density is above 0.85g/cm3, and the tap density of the iron phosphate produced by the common process is generally between 0.6 and 0.7. The iron phosphate produced by the process has stable quality and good product consistency, the quality indexes can be regularly adjusted, and each index can be accurately adjusted according to the needs of users, so that the requirements of different users are met. The iron phosphate crystal of the invention has high purity, low impurity content, good product purity and uniform crystal size which is about 100nm, is a product which does not need to be dispersed and ground by a plagiarism sand mill, and is a high-efficiency raw material for the prepared battery lithium iron phosphate. The content of S in the dihydrate iron phosphate prepared by the method is below 200PPm, and the dihydrate iron phosphate can be directly used for preparing lithium iron phosphate, so that the dihydrate iron phosphate has high economic efficiency.
And c, adding a step of recycling waste liquid, wherein the waste liquid recycling treatment comprises the steps of collecting filtrate ammonium sulfate filtered by the synthesis reaction in the step b, collecting filtrate phosphoric acid generated by filtering the solution c in the step e, adding ammonia water into phosphoric acid filtrate to obtain monoammonium phosphate, and separating concentrated water and fresh water by passing the filtrate ammonium sulfate and the filtrate monoammonium phosphate through a reverse osmosis concentration membrane, wherein the fresh water can be reused for washing water washed in the step c and the step e, the washed washing water can also be reused for preparing ferrous sulfate in the step a and phosphate in the step b, and the concentrated water can be subjected to vacuum concentration crystallization to prepare ammonium sulfate and monoammonium phosphate.
And (c) filtering the filter cake generated in the step (b) to obtain a yellow filter cake (basic ferric phosphate), wherein the main component of the generated filtrate is low-concentration 4% ammonium sulfate waste liquid. White materials generated in the conversion process are filtered to obtain a white filter cake (ferric phosphate dihydrate), and the generated filtrate mainly contains low-concentration phosphoric acid and can be added with ammonia water to obtain monoammonium phosphate waste liquid with the concentration of about 4%. The two waste liquids are deeply concentrated by a membrane method (reverse osmosis concentration membrane), the initial concentration of the waste liquid is about 4 percent and is concentrated to about 15 percent, and concentrated water is separated from fresh water. The fresh water can reach the standard of deionized water, the conductivity is below 20us/cm, and the fresh water can be reused as washing water in a process system. Concentrated water is subjected to vacuum concentration and crystallization at different temperatures and concentrations to respectively produce ammonium sulfate and monoammonium phosphate products.
the washing water generated in the washing process from the yellow filter cake (basic ferric phosphate) to the white filter cake (ferric phosphate dihydrate) can be used for dissolving ferrous sulfate and phosphate to realize the reutilization of waste liquid, the waste liquid is concentrated by an osmotic membrane and then is subjected to vacuum concentration and crystallization, the produced ammonium sulfate and monoammonium phosphate have certain economic value, the cost of waste liquid treatment can be completely compensated, the zero discharge of sewage is realized, and the environmental protection and economic benefit are good.
various modifications and variations of the embodiments of the present invention may be made by those skilled in the art, and they are also within the scope of the present invention, provided they are within the scope of the claims of the present invention and their equivalents. What is not described in detail in the specification is prior art that is well known to those skilled in the art.
Claims (10)
1. A synthesis process of battery-grade iron phosphate is characterized by comprising the following steps:
a. Preparing a ferrous sulfate solution containing 0.5-1mol/L of iron from the by-product ferrous sulfate of the titanium dioxide, adding an adsorbent and a regulator, regulating the pH of the solution to 1-2.5, adding a flocculating agent, and filtering to obtain a solution A;
b. adjusting the pH value of the solution A to 0.5-2 by using the regulator, preparing a phosphate solution containing 1-2mol/L phosphorus, dripping the adjusted solution A, the prepared phosphate and a prepared oxidant into a reaction kettle at the same time, performing a synthetic reaction, adjusting the pH value to be stable at 0.5-2.5 by adding ammonia water or phosphoric acid, and filtering after the reaction is finished to obtain a filter cake;
c. Adding deionized water into the filter cake, washing, removing impurities, and pulping to obtain a solution B;
d. Adding phosphoric acid into the solution B, controlling the concentration of the phosphoric acid in the solution B to be 0.3-0.8mol/L, and carrying out conversion reaction to obtain a solution C;
e. And filtering, washing, drying and calcining the solution C to obtain the iron phosphate.
2. The process for synthesizing battery grade iron phosphate according to claim 1, further comprising a waste liquid recycling treatment, wherein the waste liquid recycling treatment comprises collecting filtrate ammonium sulfate filtered by the synthesis reaction in the step b, collecting filtrate phosphoric acid generated by filtering the solution c in the step e, adding ammonia water into phosphoric acid filtrate to obtain monoammonium phosphate, and then passing the filtrate ammonium sulfate and the filtrate monoammonium phosphate through a reverse osmosis concentration membrane to separate concentrated water and fresh water, wherein the fresh water can be reused for the washing water washed in the step c and the step e, the washed washing water can be reused for the configuration of ferrous sulfate in the step a and phosphate in the step b, and the concentrated water can be subjected to vacuum concentration and crystallization to prepare ammonium sulfate and monoammonium phosphate.
3. The process for synthesizing battery grade iron phosphate according to claim 1, wherein the adsorbent in the step a is one of polymeric phosphates, and the mass ratio of the adsorbent to ferrous sulfate is 0.04-0.06: 1.
4. The process for synthesizing battery grade iron phosphate according to claim 3, wherein the regulator in step a and step b is sulfuric acid or phosphoric acid.
5. The process for synthesizing battery grade iron phosphate according to claim 4, wherein the flocculant in the step a is one of polyacrylamide, polydimethyldiallylammonium chloride and polyethyleneimine, and the mass ratio of the flocculant to ferrous sulfate is 0.02-0.04: 1.
6. the process for synthesizing battery grade iron phosphate according to claim 5, wherein the phosphate in step b is a mixture of monoammonium phosphate, diammonium phosphate and phosphoric acid, and the ratio of the amount of the added substance of phosphorus ions to the amount of the ferrous substance of ferrous sulfate in the phosphate is 1-1.3: 1.
7. The synthesis process of battery-grade iron phosphate according to claim 6, wherein the oxidant in step b is 27.5% -30% hydrogen peroxide, and the addition amount of the oxidant is 1.2-2.4 times of the theoretical amount of the ferrous ions after all ferrous ions are oxidized into the ferric ions.
8. The synthesis process of battery grade iron phosphate according to claim 7, characterized in that the three dropwise addition reactions of step b are completed simultaneously within 30-90min at a constant temperature of 40-88 ℃ for 3-5 h.
9. The process for synthesizing battery grade iron phosphate according to claim 8, wherein the reaction temperature of the conversion reaction in the step d is constant at 90-98 ℃ and the reaction time is 2-3 h.
10. The process for synthesizing battery grade iron phosphate according to claim 9, wherein the calcination temperature in step e is 550-650 ℃ and the reaction time is 4-6 h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110980678A (en) * | 2019-12-26 | 2020-04-10 | 湖南雅城新材料有限公司 | Preparation method of iron phosphate with low cost and low impurities |
| CN111333047A (en) * | 2020-01-09 | 2020-06-26 | 瓮福（集团）有限责任公司 | Method for synthesizing high-purity iron phosphate by using ferrous sulfate as byproduct of titanium dioxide |
| CN114506831A (en) * | 2022-02-22 | 2022-05-17 | 四川大学 | Method for preparing battery-grade anhydrous iron phosphate by using liquid crude monoammonium phosphate |
| CN114516625A (en) * | 2022-03-23 | 2022-05-20 | 华东理工大学 | Iron phosphate and preparation method and application thereof |
| CN114644325A (en) * | 2021-12-07 | 2022-06-21 | 上海安赐环保科技股份有限公司 | Device and method for preparing battery-grade iron phosphate by using by-product ferrous sulfate |
| CN114772571A (en) * | 2022-04-26 | 2022-07-22 | 万向一二三股份公司 | Preparation method of anhydrous iron phosphate and preparation method of lithium iron phosphate carbon composite material |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1219002A (en) * | 1967-04-07 | 1971-01-13 | Sincat Spa | The production of ammonium phosphates |
| CN103145193A (en) * | 2011-12-06 | 2013-06-12 | 北京三聚环保新材料股份有限公司 | Method of preparing iron oxide yellow by using titanium dioxide by-product |
| CN106044735A (en) * | 2016-05-31 | 2016-10-26 | 百川化工(如皋)有限公司 | Synthesizing method for low-cost battery-grade iron phosphate |
| CN109250856A (en) * | 2018-10-19 | 2019-01-22 | 湖南雅城新材料有限公司 | It is a kind of low cost ferric phosphate nitrogen-containing wastewater processing and recovery method as resource |
| CN109368612A (en) * | 2018-11-30 | 2019-02-22 | 乳源东阳光磁性材料有限公司 | Method for preparing battery-grade iron phosphate by using iron phosphate production wastewater and iron phosphate prepared by method |
| CN109809382A (en) * | 2019-03-28 | 2019-05-28 | 衢州华友钴新材料有限公司 | A method of ferric phosphate is synthesized using the waste phosphoric acid salt that precipitating micro heavy generates |
| CN110002415A (en) * | 2019-04-01 | 2019-07-12 | 湖南中金岭南康盟环保科技有限公司 | A method of phosphate radical and sulfate radical are recycled from ferric phosphate production waste water |
-
2019
- 2019-09-17 CN CN201910875696.5A patent/CN110540185A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1219002A (en) * | 1967-04-07 | 1971-01-13 | Sincat Spa | The production of ammonium phosphates |
| CN103145193A (en) * | 2011-12-06 | 2013-06-12 | 北京三聚环保新材料股份有限公司 | Method of preparing iron oxide yellow by using titanium dioxide by-product |
| CN106044735A (en) * | 2016-05-31 | 2016-10-26 | 百川化工(如皋)有限公司 | Synthesizing method for low-cost battery-grade iron phosphate |
| CN109250856A (en) * | 2018-10-19 | 2019-01-22 | 湖南雅城新材料有限公司 | It is a kind of low cost ferric phosphate nitrogen-containing wastewater processing and recovery method as resource |
| CN109368612A (en) * | 2018-11-30 | 2019-02-22 | 乳源东阳光磁性材料有限公司 | Method for preparing battery-grade iron phosphate by using iron phosphate production wastewater and iron phosphate prepared by method |
| CN109809382A (en) * | 2019-03-28 | 2019-05-28 | 衢州华友钴新材料有限公司 | A method of ferric phosphate is synthesized using the waste phosphoric acid salt that precipitating micro heavy generates |
| CN110002415A (en) * | 2019-04-01 | 2019-07-12 | 湖南中金岭南康盟环保科技有限公司 | A method of phosphate radical and sulfate radical are recycled from ferric phosphate production waste water |
Non-Patent Citations (2)
| Title |
|---|
| 徐寿昌: "《工业冷却水处理技术》", 31 August 1984, 化学工业出版社 * |
| 曾华梁等: "《电镀工艺手册》", 30 April 1989, 机械工业出版社 * |
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