CN108862226A - A kind of preparation method of high-purity battery-grade iron phosphate - Google Patents
A kind of preparation method of high-purity battery-grade iron phosphate Download PDFInfo
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- CN108862226A CN108862226A CN201810928292.3A CN201810928292A CN108862226A CN 108862226 A CN108862226 A CN 108862226A CN 201810928292 A CN201810928292 A CN 201810928292A CN 108862226 A CN108862226 A CN 108862226A
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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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- 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
- C01P2006/80—Compositional purity
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Abstract
The present invention relates to lithium ion battery material technical fields, specifically disclose a kind of preparation method of high-purity battery-grade iron phosphate, include the following steps：Source of iron is dissolved in wiring solution-forming a in distilled water；Phosphorus source is dissolved in wiring solution-forming b in distilled water；Solution a and solution b is sufficiently mixed by iron and phosphorus equimolar proportion, then heats up and is reacted to obtain mixed solution；Alkaline solution is added in mixed solution and adjusts the pH value of reaction solution, and continues to be stirred to react to obtain ferric phosphate crude product；Ferric phosphate crude product is subjected to pickling conversion；By the product filtering after pickling；Product is dried.The synthetic method of battery-grade iron phosphate of the present invention is relatively simple, is easy to operate and control, and can realize industrialized production well；And using by the crude product technical solution that pickling converts in phosphoric acid solution, solves the problems, such as that production process is rambunctious, improve homogeneity of product and lot stability, make the iron phosphorus of product than more stable.
Description
Technical field
The present invention relates to lithium ion battery material technical field, the preparation side of specifically a kind of high-purity battery-grade iron phosphate
Method.
Background technique
Positive electrode of the LiFePO 4 as the automobile-used power-type lithium ion battery of New energy electric has huge application
Prospect, and in numerous techniques for preparing LiFePO 4, using phosphate dihydrate iron (FePO4·2H2O) it is used as Fe source compound
It is one of the important materials of presoma for manufacturing lithium ion battery anode material lithium iron phosphate.
Through consult lot of documents, at present both at home and abroad for ferric phosphate synthesis patent and document it is quite a lot of, by conclude and
The Industrialized synthesis method for summarizing ferric phosphate is broadly divided into following three kinds：
(1) it is reacted and is made under higher temperature in closed container with trivalent iron salt and phosphate；
(2) it uses divalent ferrous salt, phosphoric acid or phosphate for raw material, is made under the conditions of having existing for oxidant；
(3) it uses trivalent iron salt, phosphoric acid or phosphate for raw material, the side of solution acid alkalinity is adjusted by the way that alkaline solution is added
Method is made.
There are pyroreaction the high requirements on the equipment for above-mentioned synthesis technology (1), and energy consumption is high, are not suitable for lacking for industrialized production
It falls into；One step liquid-phase precipitation crystallization processes of synthesis technology (2) (3) there are production process control difficulty is larger and homogeneity of product compared with
The problem of difference.
It is low using price in a kind of China's 201610373707.6 " synthetic methods of low-cost cell-grade ferric phosphate " of application
Honest and clean ferrous sulfate controls pH value when product precipitating by adjusting the concentration of reaction solution as source of iron, and this method exists anti-
Should during need to consume more aqueous solvent to dilute source of iron and phosphorus source so that the production efficiency of this method unit volume compared with
Low, energy consumption is higher；Furthermore China's application 201610374836.7 " a kind of preparation methods of ferric phosphate " and 201610373365.8
Technique in " a method of prepare ferric phosphate " using iron powder or ferriferous oxide as source of iron, phosphoric acid as phosphorus source, these
Though method avoids the generation of a large amount of by-product salt, there is also a large amount of H of by-product2The problem of, bring security risk, production cost
The defects of higher and product is not easy to control.
Currently, different manufacturers are since synthesis technology difference causes commercially available phosphate dihydrate iron material also inconsistent, specific body
Present product colour, iron phosphorus ratio (Fe/P), granularity and tap density etc..Wherein iron phosphorus ratio is to measure ferric phosphate quality most to close
The index of key, and determine the factor of LiFePO4 quality most critical.High-purity phosphate dihydrate iron (Fe/P=0.97~1.02)
Color be near-white or slightly color powder.If iron phosphorus is than relatively low (Fe/P<0.97), product appearance can be white in canescence or dull gray
Color；If iron phosphorus is than higher (Fe/P>1.02), product appearance is then in dark yellow.
Wherein iron phosphorus is measured than measurement by " HGT4701-2014 battery ferric phosphate professional standard ".
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of high-purity battery-grade iron phosphate, and source of iron and phosphorus source are dissolved in steaming
It is mixed after distilled water, then ensures that mixed solution only has positive ferric ion, adding alkaline solution adjusting pH value makes to have precipitated
It is complete to be precipitated, ferric phosphate crude product is obtained by filtration, crude product is finally subjected to pickling conversion again, solves that production process is rambunctious to ask
Topic, improves homogeneity of product and lot stability, makes the iron phosphorus of product than more stable.
In order to solve the above technical problems, the present invention provides a kind of preparation methods of high-purity battery-grade iron phosphate, including
Following steps：
S1, source of iron is dissolved in distilled water, is made into the solution a that concentration is 1.0-2.0mol/L；
S2, phosphorus source is dissolved in distilled water, is made into the solution b that concentration is 1.0-2.0mol/L；
Solution a and solution b is sufficiently mixed by iron and phosphorus equimolar proportion, then rises to the reaction of setting by S3, at room temperature
Temperature is reacted, and mixed solution is obtained；
If having Fe in S4, source of iron2+Form exist, then at the reaction temperatures into mixed solution be added excessive oxidant it is molten
Liquid is aoxidized, and the Fe in mixed solution is made2+It is completely converted into Fe3+；
S5, the PH for adjusting reaction solution for the alkaline solution that mass fraction is 5-25% is added after mixed solution heat preservation 1-3h
It is worth to 1.5-2.5, and continues to be stirred to react 0.5-1h, obtains ferric phosphate crude product；
S6, ferric phosphate crude product is subjected to pickling conversion 2h with phosphoric acid solution；
S7, the product after pickling is filtered, filter cake is washed with distilled water；
S8, S7 resulting product is dried, obtains high-purity battery-grade iron phosphate.
Further, source of iron described in S1 is frerrous chloride, ferric nitrate, ferrous sulfate, iron chloride, ferric sulfate and oxalic acid
One or more of iron.
Further, phosphorus source described in S2 be phosphoric acid, phosphoric acid dihydro amine, diammonium hydrogen phosphate, ammonium phosphate, sodium dihydrogen phosphate,
One or more of disodium hydrogen phosphate and sodium phosphate.
Specifically, reaction temperature described in S3 is 40-70 DEG C, reaction time 0.5-2h.
Specifically, oxidizing reaction temperature is 30-90 DEG C in S4, and the mass concentration of oxidant is 5%-30%, the oxidation
Agent is one or more of sodium hypochlorite, calcium hypochlorite or hydrogenperoxide steam generator.
Further, S5 neutral and alkali solution is in ammonia solution, sodium hydroxide solution, potassium hydroxide solution or urea liquid
One or more.
Specifically, ferric phosphate crude product is added to 5-10 times of phosphoric acid solution in S6, the concentration of phosphoric acid solution is 1%-5%,
It stirs and is warming up to 30-100 DEG C, reaction was completed by heat preservation 1-3h.
Specifically, in S7 in filter process, filter cake is washed for several times with distilled water, until the pH value of the washing lotion after washing
For 6.5-7.5.
Specifically, the temperature dried in S8 is 90-120 DEG C.
The beneficial effects of the invention are as follows：
1, the synthetic method of battery-grade iron phosphate of the present invention is relatively simple, is easy to operate and control, can be well
Realize industrialized production.
2, it is difficult to control to solve production process using by the crude product technical solution that pickling converts in phosphoric acid solution by the present invention
The problem of, homogeneity of product and lot stability are improved, stablizes the iron phosphorus ratio (Fe/P) of product 0.985~0.990.
Specific embodiment
The technical solution in the present invention will be clearly and completely described below, it is clear that described embodiment is only
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
In a specific embodiment of the present invention, a kind of preparation method of high-purity battery-grade iron phosphate is specifically disclosed, is wrapped
Include following steps：
S1, source of iron is dissolved in distilled water, is made into the solution a that concentration is 1.0-2.0mol/L；
S2, phosphorus source is dissolved in distilled water, is made into the solution b that concentration is 1.0-2.0mol/L；
Solution a and solution b is sufficiently mixed by iron and phosphorus equimolar proportion, then is warming up to 40-70 DEG C by S3, at room temperature
After carry out reaction 0.5-2h, obtain mixed solution；
If having Fe in S4, source of iron2+Form exist, then at the reaction temperatures into mixed solution be added excessive oxidant it is molten
Liquid is aoxidized, and oxidizing reaction temperature is 30-90 DEG C, and the mass concentration of oxidant is 5%-30%, makes the Fe in mixed solution2+
It is completely converted into Fe3+；
S5, the PH for adjusting reaction solution for the alkaline solution that mass fraction is 5-25% is added after mixed solution heat preservation 1-3h
It is worth to 1.5-2.5, and continues to be stirred to react 0.5-1h, obtains ferric phosphate crude product；
S6, ferric phosphate crude product is subjected to pickling conversion, ferric phosphate crude product is added to 5-10 times of phosphate aqueous solution, phosphoric acid water
The concentration of solution is 1%-5%, stirs and is warming up to 30-100 DEG C, and reaction was completed by heat preservation 1-3h；
S7, the product after pickling is filtered, in filter process, filter cake is washed for several times with distilled water, until after washing
Washing lotion pH value be 6.5-7.5；
S8, S7 resulting product is dried, the temperature of drying is 90-120 DEG C, obtains high-purity battery-grade iron phosphate.
The ferric phosphate crude product that molysite is directly reacted with microcosmic salt is not a pure ferric phosphate crystalline solid, it be by
Iron hydroxide, ferric phosphate, ferric phosphate the substances such as phosphoric acid complex mixture, the ratio of phosphorus and iron is unstable, due to not being
The crystalline solid of regular shape is so also adsorbed a part of impurity.It is converted in phosphoric acid solution by certain time, mixture and phosphorus
The ferric phosphate crystalline solid of sour reactive crystallization formation rule shape, while the impurity adsorbed is dissolved in phosphoric acid solution.
Embodiment 1：
162.2g iron chloride is dissolved in 500mL distilled water, is added 0.5L phosphoric acid solution (c=2.0mol/L), at room temperature
It is uniformly mixed；Reaction is risen to 60 DEG C and insulated and stirred 1.0h, is adjusted with the sodium hydroxide solution that mass fraction is 20%
The pH value of reaction solution continues to filter to obtain ecru ferric phosphate crude product after being stirred to react 0.5h to 2.5；Above-mentioned ferric phosphate crude product is added
Enter in the phosphate aqueous solution for being 1% to 1860g concentration, 60 DEG C of pickling 2.0h, solid filtering is washed to neutrality, and 110 DEG C are dried to
Constant weight obtains 184.5g rice white high-purity phosphoric acid iron (Fe/P=0.990).
Embodiment 2：
278.0g ferrous sulfate is dissolved in 1000mL distilled water, is added 1L phosphoric acid solution (c=1.0mol/L), at room temperature
It is uniformly mixed；The hydrogenperoxide steam generator of 68.0g30%, insulated and stirred 2.0h are added after reaction is warming up to 50 DEG C；It is added
Mass fraction is that the pH value that 15% ammonium hydroxide adjusts solution is 2.0, continue to be stirred to react filter after 0.5h ecru ferric phosphate is thick
Product；Above-mentioned ferric phosphate crude product is added in the phosphate aqueous solution that 1674g concentration is 1.5%, is filtered after 80 DEG C of pickling 2.0h, filtered
Cake is washed to neutrality, and 90 DEG C drying to constant weight, obtains 182.5g rice white high-purity phosphoric acid iron (Fe/P=0.988).
Embodiment 3：
278.0g ferrous sulfate is dissolved in 1000mL distilled water, is added 1L sodium dihydrogen phosphate (c=1.0mol/L),
It is uniformly mixed at room temperature；The liquor natrii hypochloritis of 74.5g 20%, insulated and stirred are added after reaction is warming up to 70 DEG C
3.0h；It is the pH value of 10% sodium hydroxide solution adjusting solution to 1.5 that mass fraction, which is added, continues to filter after being stirred to react 1.0h
Obtain ecru ferric phosphate crude product；Above-mentioned ferric phosphate crude product is added in the phosphate aqueous solution that 840g concentration is 5%, 90 DEG C of pickling
It is filtered after 2.0h, filter cake is washed to neutrality, and 100 DEG C drying to constant weight, obtains 185.5g rice white high-purity phosphoric acid iron (Fe/P=
0.986)。
Embodiment 4
179.9g ferric nitrate is dissolved in 500mL distilled water, is added 1L phosphoric acid solution (c=1.0mol/L), stirs at room temperature
It mixes uniformly mixed；Reaction is risen to 80 DEG C and insulated and stirred 1.0h, adjusts reaction solution with the sodium hydroxide solution of mass fraction 5%
PH value to 1.8, continue to filter to obtain ecru ferric phosphate crude product after being stirred to react 0.5h；Above-mentioned ferric phosphate crude product is added to
In the phosphate aqueous solution that 1116g concentration is 4.5%, filtered after 90 DEG C of pickling 2.0h, filter cake is washed to neutrality, and 120 DEG C are dried to
Constant weight obtains 183.5g rice white high-purity phosphoric acid iron (Fe/P=0.987).
Embodiment 5
198.8g frerrous chloride is dissolved in 500mL distilled water, 0.5L ammonium dihydrogen phosphate (c=2.0mol/ is added
L), it is uniformly mixed at room temperature；Reaction is warming up to after 60 DEG C and is slowly added to 204g10% hydrogenperoxide steam generator, insulated and stirred
2.0h；It is 2.5 that the pH value that mass fraction is 25% ammonia spirit adjusting solution, which is added, continues to filter to obtain rice after being stirred to react 1.0h
Yellow ferric phosphate crude product；Above-mentioned ferric phosphate crude product is added in the phosphate aqueous solution that 1302g concentration is 4%, 50 DEG C of pickling
It is filtered after 2.0h, filter cake is washed to neutrality, and 110 DEG C drying to constant weight, obtains 185.1g rice white high-purity phosphoric acid iron (Fe/P=
0.990)。
Embodiment 6
By 400.0kg ferric sulfate solution in 1t distilled water, it is added 1t phosphoric acid solution (c=1.0mol/L), stirs at room temperature
It is uniformly mixed；Reaction is risen to 80 DEG C and insulated and stirred 1.0h, the ammonia spirit that mass fraction 25% is added adjusts reaction solution
PH value continues to filter to obtain ecru ferric phosphate crude product after being stirred to react 0.5h to 1.5；It is dense that above-mentioned ferric phosphate crude product is added to 3t
In the phosphate aqueous solution that degree is 3%, filtered after 70 DEG C of pickling 2.0h, filter cake is washed to neutrality, and 100 DEG C drying to constant weight, obtains
182.0kg rice white high-purity phosphoric acid iron (Fe/P=0.986).
The beneficial effects of the invention are as follows：
1, the synthetic method of battery-grade iron phosphate of the present invention is relatively simple, is easy to operate and control, can be well
Realize industrialized production.
2, it is difficult to control to solve production process using by the crude product technical solution that pickling converts in phosphoric acid solution by the present invention
The problem of, homogeneity of product and lot stability are improved, stablizes the iron phosphorus ratio (Fe/P) of product 0.985~0.990.
Above disclosed be only a kind of preferred embodiment of the invention, cannot limit the present invention's certainly with this
Interest field, therefore equivalent changes made in accordance with the claims of the present invention, are still within the scope of the present invention.
Claims (9)
1. a kind of preparation method of high-purity battery-grade iron phosphate, which is characterized in that include the following steps：
S1, source of iron is dissolved in distilled water, is made into the solution a that concentration is 1.0-2.0mol/L；
S2, phosphorus source is dissolved in distilled water, is made into the solution b that concentration is 1.0-2.0mol/L；
Solution a and solution b is sufficiently mixed by iron and phosphorus equimolar proportion, then rises to the reaction temperature of setting by S3, at room temperature
It is reacted, obtains mixed solution；
If having Fe in S4, source of iron2+Form exist, then at the reaction temperatures into mixed solution be added oxidizing agent solution carry out oxygen
Change, makes the Fe in mixed solution2+It is completely converted into Fe3+；
S5, the pH value for adjusting mixed solution for the alkaline solution that mass fraction is 5-25% is added after mixed solution heat preservation 1-3h
To 1.5-2.5, and continue to be stirred to react 0.5-1h, obtains ferric phosphate crude product；
S6, ferric phosphate crude product is subjected to pickling conversion 1-3h with phosphoric acid solution；
S7, the product after pickling is filtered, filter cake is washed with distilled water；
S8, S7 resulting product is dried, obtains high-purity battery-grade iron phosphate.
2. a kind of preparation method of high-purity battery-grade iron phosphate according to claim 1, which is characterized in that described in S1
Source of iron is one or more of frerrous chloride, ferric nitrate, ferrous sulfate, iron chloride, ferric sulfate and ferric oxalate.
3. a kind of preparation method of high-purity battery-grade iron phosphate according to claim 1, which is characterized in that described in S2
Phosphorus source is one in phosphoric acid, phosphoric acid dihydro amine, diammonium hydrogen phosphate, ammonium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate and sodium phosphate
Kind is several.
4. a kind of preparation method of high-purity battery-grade iron phosphate according to claim 1, which is characterized in that described in S3
Reaction temperature is 40-70 DEG C, reaction time 0.5-2h.
5. a kind of preparation method of high-purity battery-grade iron phosphate according to claim 1, which is characterized in that aoxidized in S4
Reaction temperature is 30-90 DEG C, and the mass concentration of oxidant is 5%-30%, the oxidant be sodium hypochlorite, calcium hypochlorite or
One or more of person's hydrogenperoxide steam generator.
6. a kind of preparation method of high-purity battery-grade iron phosphate according to claim 1, which is characterized in that S5 neutral and alkali
Solution is one or more of ammonia solution, sodium hydroxide solution, potassium hydroxide solution or urea liquid.
7. a kind of preparation method of high-purity battery-grade iron phosphate according to claim 1, which is characterized in that by phosphorus in S6
5-10 times of phosphoric acid solution is added in sour iron crude product, and the concentration of phosphoric acid solution is 1%-5%, stirs and is warming up to 30-100 DEG C, guarantor
Reaction was completed by warm 1-3h.
8. a kind of preparation method of high-purity battery-grade iron phosphate according to claim 1, which is characterized in that filtered in S7
In the process, filter cake is washed for several times with distilled water, until the pH value of the washing lotion after washing is 6.5-7.5.
9. a kind of preparation method of high-purity battery-grade iron phosphate according to claim 1, which is characterized in that dried in S8
Temperature be 90-120 DEG C.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110683528A (en) * | 2019-10-17 | 2020-01-14 | 湖南雅城新材料有限公司 | Regeneration method of iron phosphate waste |
| CN111591970A (en) * | 2020-05-30 | 2020-08-28 | 康桓铭 | Battery-grade iron phosphate and preparation method thereof |
| CN111908441A (en) * | 2020-08-24 | 2020-11-10 | 湖北融通高科先进材料有限公司 | Method for preparing titanium doped iron phosphate by wet process |
| CN112357898A (en) * | 2020-11-23 | 2021-02-12 | 湖南金源新材料股份有限公司 | Three-stage reverse impurity washing method for crude ferric phosphate |
| CN114014290A (en) * | 2021-11-30 | 2022-02-08 | 中钢天源股份有限公司 | Method and equipment for preparing stable iron phosphate at low cost |
| CN114988383A (en) * | 2022-07-12 | 2022-09-02 | 国环电池科技(苏州)有限公司 | Efficient preparation method of battery-grade iron phosphate |
| CN115231539A (en) * | 2022-07-12 | 2022-10-25 | 国环电池科技(苏州)有限公司 | Preparation method of high-purity iron phosphate |
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2018
- 2018-08-15 CN CN201810928292.3A patent/CN108862226A/en not_active Withdrawn
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110683528A (en) * | 2019-10-17 | 2020-01-14 | 湖南雅城新材料有限公司 | Regeneration method of iron phosphate waste |
| CN111591970A (en) * | 2020-05-30 | 2020-08-28 | 康桓铭 | Battery-grade iron phosphate and preparation method thereof |
| CN111591970B (en) * | 2020-05-30 | 2022-11-22 | 康桓铭 | Battery-grade iron phosphate and preparation method thereof |
| CN111908441A (en) * | 2020-08-24 | 2020-11-10 | 湖北融通高科先进材料有限公司 | Method for preparing titanium doped iron phosphate by wet process |
| CN111908441B (en) * | 2020-08-24 | 2023-07-04 | 湖北融通高科先进材料集团股份有限公司 | Method for preparing titanium-doped ferric phosphate by wet process |
| CN112357898A (en) * | 2020-11-23 | 2021-02-12 | 湖南金源新材料股份有限公司 | Three-stage reverse impurity washing method for crude ferric phosphate |
| CN114014290A (en) * | 2021-11-30 | 2022-02-08 | 中钢天源股份有限公司 | Method and equipment for preparing stable iron phosphate at low cost |
| CN114014290B (en) * | 2021-11-30 | 2022-11-29 | 中钢天源股份有限公司 | Method and equipment for preparing stable iron phosphate at low cost |
| CN114988383A (en) * | 2022-07-12 | 2022-09-02 | 国环电池科技(苏州)有限公司 | Efficient preparation method of battery-grade iron phosphate |
| CN115231539A (en) * | 2022-07-12 | 2022-10-25 | 国环电池科技(苏州)有限公司 | Preparation method of high-purity iron phosphate |
| CN115231539B (en) * | 2022-07-12 | 2023-10-10 | 国环电池科技(苏州)有限公司 | Preparation method of high-purity ferric phosphate |
| CN114988383B (en) * | 2022-07-12 | 2023-12-15 | 华辰环保能源(广州)有限责任公司 | Efficient preparation method of battery-grade ferric phosphate |
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