CN112573497A - Method for preparing iron phosphate by using ferric oxide - Google Patents
Method for preparing iron phosphate by using ferric oxide Download PDFInfo
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- CN112573497A CN112573497A CN202011318876.2A CN202011318876A CN112573497A CN 112573497 A CN112573497 A CN 112573497A CN 202011318876 A CN202011318876 A CN 202011318876A CN 112573497 A CN112573497 A CN 112573497A
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- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a method for preparing iron phosphate by using ferric oxide, which comprises the following steps: s1, adding the elementary iron into the mixed acid solution to obtain a raw material solution; s2, adding ferric oxide into the raw material liquid under the heating condition to obtain a crude ferric phosphate solution; s3, adding an oxidant into the rough ferric phosphate solution, and preserving heat to obtain ferric phosphate slurry; and S4, performing solid-liquid separation on the iron phosphate slurry, collecting a solid phase, washing, and calcining to obtain the anhydrous iron phosphate. The iron phosphate prepared by the method has two crystal forms, the ratio of the two crystal forms is controlled by the combination of simple substance iron and ferric oxide, and the iron-phosphorus ratio of the finally prepared iron phosphate is controlled; the method realizes the control of the thickness of the iron phosphate crystal by regulating and controlling the concentration of phosphate radical; according to the scheme, the iron phosphate is obtained by reaction in a sulfur-free environment, so that the sulfur content in the finished iron phosphate product is greatly reduced.
Description
Technical Field
The invention relates to the technical field of lithium ion battery materials, in particular to a method for preparing iron phosphate by using ferric oxide.
Background
The lithium iron phosphate is one kind of positive pole material for lithium ion cell and features great discharge capacity, high safety, long service life, low cost, no toxicity, no pollution and wide material source. Lithium iron phosphate batteries are widely used in electric tools, UPS's, emergency lights, warning lights and mining lights; the lithium iron phosphate battery is also an important development direction of a power battery for a new energy automobile and is used for an electric bus; in addition, the method also has application in the field of energy storage. The P-O bond in the lithium iron phosphate crystal is stable and difficult to decompose, and the structure of the lithium iron phosphate crystal does not collapse and generate heat or form a strong oxidizing substance like lithium cobaltate even at high temperature or during overcharge, so that the lithium iron phosphate battery has good safety and cycle performance.
The iron phosphate is an important raw material for producing the lithium iron phosphate, and battery material manufacturers generally adopt a high-temperature solid-phase method of the iron phosphate and lithium salt to produce the lithium iron phosphate. Along with the popularization and application of new energy automobiles and the development of energy storage batteries in China, the demand of lithium iron phosphate will increase rapidly, and the demand of corresponding raw material iron phosphate also increases explosively. The requirement on the indexes of battery-grade iron phosphate is more and more strict, and the iron-phosphorus ratio is required to be more than 0.97 by the existing enterprises; the content of impurity elements such as Ti, Mn, Mg, Zn, Cu and S is less than 0.005%.
The iron phosphate raw material enterprises have the technical current situation that: the iron-phosphorus ratio of products of most enterprises is 0.96-0.97, and the iron-phosphorus ratio of products of few enterprises can reach more than 0.97, but the S content obviously exceeds the standard and reaches more than 0.01 percent; in order to prepare iron phosphate with low impurity content, the related art uses refined ferrous sulfate, ferric chloride, ferric nitrate, ferric chloride or high-purity iron powder and sulfuric acid as raw materials, and although the obtained iron phosphate has low impurity content, the raw material cost is high. The iron phosphate is synthesized by adopting cheap ferrous sulfate as a byproduct of titanium dioxide, and the production cost is low, but the impurity content of the final iron phosphate product is high due to the high impurity content of Mn, Mg, Ti, Ca and the like in the ferrous sulfate raw material. Researchers also study the impurity removal of ferrous sulfate, and the impurities are difficult to be removed completely, especially Mn and Mg, no matter the impurities are removed by adopting iron powder purification or by adopting phosphate and sulfide precipitation. Attempts have also been made to remove impurities by adsorption on resins, since the solution contains a large amount of Fe2+Will be coated with resinAdsorption is performed first, thereby hindering the removal of impurity metal ions.
Meanwhile, the control of iron-phosphorus ratio, impurity elements, specific surface area and moisture, which are key indexes, is rarely mentioned in the related art. The obtained iron phosphate is unstable in component, and acid salt is easily formed under improper condition control, so that the iron-phosphorus ratio is lower and is only about 0.96; although the iron-phosphorus ratio reaches 0.97-1.00, the iron phosphate generally contains a small amount of ferric hydroxide, and a large amount of impurity ions are adsorbed, so that the impurity ions of S, Mn and Mg are higher, and the requirement of battery-grade iron phosphate is difficult to meet.
In addition, the iron phosphate crystal form has a great influence on the performance (such as compaction density, specific capacity and the like) of the prepared lithium iron phosphate.
Based on this, there is still a need to develop further processes for producing iron phosphate with high iron to phosphorus ratio.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the ferric phosphate obtained by the method has higher olivine crystal form (rodoliote) ferric phosphate crystal form content.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a method for preparing iron phosphate by using ferric oxide, comprising the following steps:
s1, adding the elementary iron into the acid solution to obtain a raw material solution;
s2, adding ferric oxide into the raw material liquid under the heating condition to obtain a crude ferric phosphate solution;
s3, adding an oxidant into the rough ferric phosphate solution, and preserving heat to obtain ferric phosphate slurry;
s4, performing solid-liquid separation on the iron phosphate slurry, collecting a solid phase, washing, and calcining to obtain anhydrous iron phosphate;
wherein the acid solution contains phosphoric acid.
According to some embodiments of the invention, the acid solution consists of a phosphoric acid solution and a strong acid solution; wherein, the ratio of the amount of the strong acid to the phosphoric acid in the acid solution is (0-1) to (4-5).
According to some embodiments of the invention, the strong acid solution is at least one of a hydrochloric acid or nitric acid solution.
According to some embodiments of the invention, the iron trioxide is recovered from a waste residue of a steel mill.
The waste slag of steel plants is utilized, and the production cost is greatly reduced.
According to some embodiments of the invention, the heating temperature is 90 to 95 ℃.
According to some embodiments of the invention, the elemental iron is more than 0.5 times the amount of ferric oxide species.
Controlling the ratio of the simple substance iron to the ferric oxide, and adjusting the ratio of different crystal forms of the ferric phosphate in the final finished product.
According to some embodiments of the invention, the amount of elemental phosphorus in the crude ferric phosphate solution is greater than 1.3 times the amount of elemental iron species.
The concentration change of the phosphate radical realizes the control of the thickness of the ferric phosphate crystal.
According to some embodiments of the invention, the oxidizing agent is at least one of hydrogen peroxide or nitric acid.
According to some embodiments of the invention, the holding temperature is 90-95 ℃ and the holding time is 0.5-4 h.
According to some embodiments of the invention, the conductivity of the filtrate in said washing operation is below 500 μ S/cm.
According to some embodiments of the invention, the calcination temperature is 500 to 600 ℃ and the calcination time is 4 to 6 hours.
The method for preparing iron phosphate by using ferric oxide according to the embodiment of the invention has at least the following beneficial effects: according to the invention, the content of olivine crystal form iron phosphate in the prepared high-iron-phosphorus-ratio iron phosphate is higher by using the elementary substance iron and the ferric oxide in a combined manner, and the lithium iron phosphate prepared by using the iron phosphate has higher compaction density and higher specific charge capacity; the iron phosphate is obtained by reaction in a sulfur-free environment, so that the sulfur content in the finished iron phosphate product is greatly reduced (the sulfur content of the iron phosphate prepared by the scheme of the invention is usually 15-30 ppm, and the sulfur content of the iron phosphate prepared by the related technology is usually 80-150 ppm).
Drawings
FIG. 1 is a SEM image of iron phosphate prepared in the first example;
FIG. 2 is an SEM image of ferric phosphate prepared in example II;
FIG. 3 is an SEM image (high magnification) of iron phosphate prepared in example III;
FIG. 4 is an SEM image (low magnification) of iron phosphate prepared in example III;
FIG. 5 is an XRD pattern of iron phosphate prepared in the first example;
FIG. 6 is an XRD pattern of iron phosphate prepared in comparative example.
Detailed Description
In order to explain technical contents, achieved objects, and effects of the present invention in detail, the following description is made with reference to the accompanying drawings in combination with the embodiments. The test methods used in the examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are commercially available reagents and materials unless otherwise specified.
The first embodiment of the invention is as follows: a method for preparing iron phosphate by using ferric oxide comprises the following steps:
s1, adding 576.47g of 85% (w.t.) phosphoric acid into 112g of iron powder, stirring, adding water to dilute to 1.8L, and collecting a liquid phase after complete dissolution to obtain a raw material solution;
s2, adding 213g of ferric oxide into the raw material liquid, stirring and heating to 92 ℃, and setting the heat preservation temperature to 92 ℃ to obtain a crude ferric phosphate solution;
s3, after the crude iron phosphate solution turns white, adding an oxidant into the crude iron phosphate, and then keeping the temperature for 3 hours to obtain iron phosphate slurry;
and S4, filtering the iron phosphate slurry, washing the iron phosphate filter cake until the conductivity of the filtrate is below 500 mu S/cm, and calcining the washed iron phosphate filter cake at 550 ℃ for 240min to obtain the anhydrous iron phosphate.
The iron-phosphorus ratio of the anhydrous ferric phosphate material prepared by the embodiment is 0.985.
The second embodiment of the invention is as follows: a method for preparing iron phosphate from ferric oxide, which adopts the steps similar to the method of the first embodiment, and only differs from the first embodiment in that: when the crude iron phosphate solution is prepared, the concentration of phosphate radical is 3.13mol/L, and the quantity ratio of total iron element to phosphorus element is 1: 1.5.
The iron-phosphorus ratio of the anhydrous ferric phosphate material prepared by the embodiment is 0.979.
The third embodiment of the invention is as follows: a method for preparing iron phosphate by using ferric oxide comprises the following steps:
s1, adding 461.17g of 85% (mass fraction) phosphoric acid into 112g of iron powder, stirring, adding water to dilute to 1.8L, and collecting a liquid phase after complete dissolution to obtain a raw material liquid;
s2, adding 213g of ferric oxide and 94.45g of concentrated nitric acid (mass fraction is about 66%) into the raw material liquid, stirring and heating to 92 ℃, and setting the heat preservation temperature to 92 ℃ to obtain a crude ferric phosphate solution;
s3, after the crude iron phosphate solution turns white, adding an oxidant into the crude iron phosphate, and then keeping the temperature for 3 hours to obtain iron phosphate slurry;
and S4, filtering the iron phosphate slurry, washing the iron phosphate filter cake until the conductivity of the filtrate is below 500 mu S/cm, and calcining the washed iron phosphate filter cake at 550 ℃ for 240min to obtain the anhydrous iron phosphate.
The iron-phosphorus ratio of the anhydrous ferric phosphate material prepared by the embodiment is 0.975.
The fourth embodiment of the invention is as follows: a method for preparing iron phosphate by using ferric oxide, which adopts the steps similar to the method of the first embodiment, and the only difference from the first embodiment is that: in the preparation of the crude iron phosphate solution, the ratio of the total iron to phosphorus species was 1: 1.3.
The iron-phosphorus ratio of the anhydrous ferric phosphate material prepared in this example was 1.012.
The fifth embodiment of the invention is as follows: a method for preparing iron phosphate by using ferric oxide, which adopts the steps similar to the method of the first embodiment, and the only difference from the first embodiment is that: in the preparation of the crude iron phosphate solution, the ratio of the total iron to phosphorus species was 1: 1.7.
The iron-phosphorus ratio of the anhydrous ferric phosphate material prepared by the embodiment is 0.980.
The first comparative example of the present invention is: a method for preparing iron phosphate by using ferric oxide, which adopts the steps similar to the method of the first embodiment, and the only difference from the first embodiment is that: 112g of iron powder was replaced with 160g of iron trioxide.
The comparative example produced an iron phosphate material having a sulfur content of 238 ppm.
The iron phosphate prepared in the first to fifth examples was used to determine the iron-phosphorus ratio and the sulfur content, and the results are shown in table 1 below:
table 1 examples one-five iron phosphate products obtained have the iron to phosphorus ratio and the sulphur content
| The quantitative ratio of phosphate radical to total iron species | Iron to phosphorus ratio | Sulfur content (ppm) | |
| Example one | 1.5∶1 | 0.985 | 21.3 |
| Example two | 1.5∶1 | 0.979 | 15 |
| EXAMPLE III | 1.2：1 | 0.975 | 29.3 |
| Example four | 1.3∶1 | 1.012 | 10.6 |
| EXAMPLE five | 1.7∶1 | 0.980 | 15.2 |
As can be seen from the data in Table 1, the iron-phosphorus ratio in the iron phosphate material produced continuously decreases as the concentration of phosphate radical increases.
Example one SEM image of the prepared iron phosphate material is shown in fig. 1, and it is known from fig. 1 that the prepared iron phosphate is flaky; SEM image of the iron phosphate prepared in example II is shown in FIG. 2, and it is known from FIG. 2 that the iron phosphate prepared is in block form; as can be seen from the comparison between fig. 1 and fig. 2, the increased concentration of phosphate radical causes the iron phosphate product to be transformed from a sheet shape to a block shape, and the prepared iron phosphate material becomes thicker obviously.
SEM images of different magnifications of the iron phosphate material prepared in example III are shown in FIGS. 3 and 4, and it can be seen from FIGS. 3 and 4 that the iron phosphate material is in a block shape.
An XRD (X-ray diffraction) pattern of the iron phosphate material prepared in the first embodiment is shown in figure 5, and it is known from figure 5 that the different crystal forms of the prepared iron phosphate comprise 13.5% of other iron phosphates (PDF #04-011-0358) and 86.5% of olivine crystal form iron phosphate (PDF # 00-050-1635); the XRD pattern of the iron phosphate material prepared by the reaction of pure iron red and phosphoric acid is shown in figure 6, and it is known from figure 6 that the different crystal forms of the prepared iron phosphate comprise 40.6 percent of other iron phosphate (PDF # 04-011-.
The iron phosphates prepared in the above examples one and comparative examples one were measured for their compacted density and specific charge capacity (0.1C), and the results are shown in the following table 2:
table 2 compacted density and specific charge capacity of iron phosphate prepared in example one and comparative example one
It can be known from the data in table 2 that the specific charge capacity of the iron phosphate material prepared in the first example is much higher than that of the iron phosphate prepared by reacting pure iron oxide red with phosphoric acid, which indicates that the higher the content of the olivine crystal form iron phosphate is, the larger the specific capacity of the iron phosphate is.
In the embodiment of the invention, the iron oxide red can be prepared into the iron phosphate without dissolving, grinding and high temperature and high pressure, the generated iron phosphate has two crystal forms, and the proportion of the two crystal forms is changed by adjusting the proportion of ferrous iron, the iron oxide red and phosphate ions in the solution.
In summary, according to the method for preparing iron phosphate provided by the invention, the prepared iron phosphate has two crystal forms, and the ratio of the two crystal forms and the iron-phosphorus ratio of the finally prepared iron phosphate are controlled by regulating the ratio of the raw material iron powder to the ferric oxide; the scheme realizes the control of the thickness of the iron phosphate crystal by regulating and controlling the concentration of phosphate radical; according to the scheme, the iron phosphate is obtained by reaction in a sulfur-free environment, so that the sulfur content in the finished iron phosphate product is greatly reduced.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to the related technical fields, are included in the scope of the present invention.
Claims (10)
1. A method for preparing iron phosphate by using ferric oxide is characterized by comprising the following steps: comprises the following steps:
s1, adding the elementary iron into the acid solution to obtain a raw material solution;
s2, adding ferric oxide into the raw material liquid under the heating condition to obtain a crude ferric phosphate solution;
s3, adding an oxidant into the rough ferric phosphate solution, and preserving heat to obtain ferric phosphate slurry;
s4, performing solid-liquid separation on the iron phosphate slurry, collecting a solid phase, washing, and calcining to obtain anhydrous iron phosphate;
wherein the acid solution contains phosphoric acid.
2. The method for preparing iron phosphate by using ferric oxide according to claim 1, wherein the method comprises the following steps: the acid solution consists of a phosphoric acid solution and a strong acid solution; wherein, the ratio of the amount of the strong acid to the phosphoric acid in the acid solution is (0-1) to (4-5).
3. The method for preparing iron phosphate by using ferric oxide according to claim 2, wherein the method comprises the following steps: the strong acid solution is at least one of hydrochloric acid and nitric acid solution.
4. The method for preparing iron phosphate by using ferric oxide according to claim 1, wherein the method comprises the following steps: the heating temperature is 88-100 ℃.
5. The method for preparing iron phosphate by using ferric oxide according to claim 1, wherein the method comprises the following steps: the amount of the simple substance iron is more than 0.5 times of the amount of the ferric oxide substance.
6. The method for preparing iron phosphate by using ferric oxide according to claim 1, wherein the method comprises the following steps: the phosphorus element in the crude ferric phosphate solution is more than 1.3 times of the amount of the iron element substance.
7. The method for preparing iron phosphate by using ferric oxide according to claim 1, wherein the method comprises the following steps: the oxidant is at least one of hydrogen peroxide or nitric acid.
8. The method for preparing iron phosphate by using ferric oxide according to claim 1, wherein the method comprises the following steps: the heat preservation temperature is 88-100 ℃, and the heat preservation time is 0.5-4 h.
9. The method for preparing iron phosphate by using ferric oxide according to claim 1, wherein the method comprises the following steps: in the washing operation, the electric conductivity of the filtrate is below 500 mu S/cm.
10. The method for preparing iron phosphate by using ferric oxide according to claim 1, wherein the method comprises the following steps: the calcination temperature is 500-600 ℃, and the calcination time is 2-6 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115340075A (en) * | 2022-05-18 | 2022-11-15 | 四川大学 | Method for preparing battery-grade iron phosphate by adopting iron oxide and dilute phosphoric acid |
| CN115432683A (en) * | 2022-10-09 | 2022-12-06 | 铜陵安伟宁新能源科技有限公司 | Method for preparing high-compaction battery-grade iron phosphate under low-temperature condition |
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| US20120039783A1 (en) * | 2009-02-26 | 2012-02-16 | Chemische Fabrik Budenheim Kg | Production of iron orthophosphate |
| CN107032316A (en) * | 2017-06-12 | 2017-08-11 | 百川化工(如皋)有限公司 | A kind of preparation method of ferric phosphate |
| CN108609595A (en) * | 2018-05-10 | 2018-10-02 | 湖南雅城新材料有限公司 | Ferric phosphate and its preparation method and application |
| CN111056543A (en) * | 2019-12-26 | 2020-04-24 | 湖南雅城新材料有限公司 | Preparation method of low-specific-surface high-compaction iron phosphate |
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2020
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Patent Citations (4)
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| US20120039783A1 (en) * | 2009-02-26 | 2012-02-16 | Chemische Fabrik Budenheim Kg | Production of iron orthophosphate |
| CN107032316A (en) * | 2017-06-12 | 2017-08-11 | 百川化工(如皋)有限公司 | A kind of preparation method of ferric phosphate |
| CN108609595A (en) * | 2018-05-10 | 2018-10-02 | 湖南雅城新材料有限公司 | Ferric phosphate and its preparation method and application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115340075A (en) * | 2022-05-18 | 2022-11-15 | 四川大学 | Method for preparing battery-grade iron phosphate by adopting iron oxide and dilute phosphoric acid |
| CN115432683A (en) * | 2022-10-09 | 2022-12-06 | 铜陵安伟宁新能源科技有限公司 | Method for preparing high-compaction battery-grade iron phosphate under low-temperature condition |
| CN115432683B (en) * | 2022-10-09 | 2024-04-26 | 铜陵安伟宁新能源科技有限公司 | Method for preparing high-compaction battery-level ferric phosphate under low-temperature condition |
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Application publication date: 20210330 |