CN113184822B - Method for synthesizing battery-grade iron phosphate by using ilmenite - Google Patents
Method for synthesizing battery-grade iron phosphate by using ilmenite Download PDFInfo
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- CN113184822B CN113184822B CN202110515085.7A CN202110515085A CN113184822B CN 113184822 B CN113184822 B CN 113184822B CN 202110515085 A CN202110515085 A CN 202110515085A CN 113184822 B CN113184822 B CN 113184822B
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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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- C01B25/00—Phosphorus; Compounds thereof
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses a method for synthesizing battery-grade iron phosphate by utilizing ilmenite, and belongs to the technical field of chemical materials. The method comprises the following steps: reacting ilmenite with hydrochloric acid, and performing iron extraction on liquid obtained by solid-liquid separation to obtain an organic phase containing ferric trichloride. Reacting the initiator with a precipitator and an organic phase containing ferric trichloride, separating out a precipitate obtained by the reaction, and then calcining. According to the method, the iron phosphate with high purity can be obtained through ilmenite, an oxidation step is not needed in the synthesis process, the working procedures are simplified, the production cost is reduced, and the method is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of chemical materials, in particular to a method for synthesizing battery-grade iron phosphate by utilizing ilmenite.
Background
Ferric phosphate, also known as ferric phosphate, ferric orthophosphate, of the molecular formula FePO 4 It is white and off-white monoclinic crystal powder.
At present, the production process of the iron phosphate has long production time and high energy consumption, and other byproducts which are difficult to follow-up treatment are easy to generate.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a method for synthesizing battery-grade iron phosphate by utilizing ilmenite, which can obtain iron phosphate with higher purity, does not need an oxidation step in the synthesis process, simplifies the working procedures, reduces the production cost and is suitable for industrial production.
The application can be realized as follows:
the application provides a method for synthesizing battery-grade iron phosphate by utilizing ilmenite, which comprises the following steps of: reacting ilmenite with hydrochloric acid, and performing iron extraction on liquid obtained by solid-liquid separation to obtain an organic phase containing ferric trichloride.
Reacting the initiator with a precipitant and an organic phase containing ferric trichloride, separating out the precipitate obtained by the reaction, and then calcining.
In an alternative embodiment, the concentration of hydrochloric acid is from 10 to 15vt%, the mass ratio of hydrochloric acid to ilmenite is from 1 to 10: 1.
in an alternative embodiment, the reaction of ilmenite with hydrochloric acid is carried out at 10-35 ℃ for 10-24 h.
In an alternative embodiment, the volume ratio of extraction reagent to liquid used for iron extraction is 3-5: 1.
in an alternative embodiment, the extraction reagent comprises an iron extractant.
In an alternative embodiment, the iron extractant includes at least one of trioctylamine, a secondary primary amine, tributylphosphate, bis (1-methylheptyl) methylphosphonate.
In an alternative embodiment, the extraction reagent further comprises an oil phase solvent.
In an alternative embodiment, the oil phase solvent comprises at least one of toluene, isoamyl alcohol, and sulfonated kerosene.
In an alternative embodiment, the extraction reagent consists of trioctylamine and sulfonated kerosene.
In an alternative embodiment, the volume ratio of trioctylamine to sulfonated kerosene is 1-3: 1.
in an alternative embodiment, the initiator is reacted with the precipitating agent and the organic phase containing ferric chloride at a pH of 1.5 to 2.0 and a temperature of 60 to 70 ℃.
In an alternative embodiment, the precipitant and the organic phase comprising ferric chloride are added dropwise to the mixture of initiator and water after mixing.
In an alternative embodiment, the initiator is iron phosphate crystals.
In an alternative embodiment, the precipitation agent comprises at least one of phosphoric acid and a phosphate salt.
In an alternative embodiment, the phosphate salt comprises at least one of sodium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, potassium phosphate, dipotassium hydrogen phosphate, and potassium dihydrogen phosphate.
In an alternative embodiment, the calcination is carried out at 500-600 ℃ for 20-40 min.
The beneficial effect of this application includes:
according to the method, after ilmenite and hydrochloric acid react, liquid obtained through solid-liquid separation is subjected to iron extraction to obtain an organic phase containing ferric trichloride. And then reacting the initiator, the precipitator and the organic phase containing ferric trichloride to obtain a ferric phosphate precursor, and calcining to obtain the high-purity ferric phosphate. The method can directly obtain the iron phosphate with higher purity from the ilmenite, does not need an oxidation step in the synthesis process, simplifies the working procedures compared with the prior art, reduces the production cost, and is suitable for industrial production.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is an SEM image of the iron phosphate product prepared in example 1 of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The method for synthesizing battery grade iron phosphate by using ilmenite provided by the application is specifically explained below.
The inventor researches and discovers that the iron phosphate prepared in the prior art is prepared by using ferrous sulfate as an iron source, and the prepared iron phosphate has low purity and can influence the electrochemical performance of a battery when used as a battery material.
In view of this, the inventors have creatively proposed a new method for synthesizing battery grade iron phosphate using ilmenite, which comprises the following steps: reacting ilmenite with hydrochloric acid, and performing iron extraction on liquid obtained by solid-liquid separation to obtain an organic phase containing ferric trichloride. Then the initiator is reacted with a precipitant and an organic phase containing ferric trichloride, and the precipitate obtained by the reaction is separated and then calcined.
After the ilmenite is reacted with hydrochloric acid, solid-liquid separation (e.g., filtration) is performed to obtain a clear liquid and a solid. The solid is high-content titanium slag solid (the titanium content is not less than 30 percent), and the titanium content in the clear liquid is not more than 0.1 percent.
According to the method provided by the application, the ilmenite directly reacts with the hydrochloric acid, and then the ferric trichloride component is extracted into the organic phase, so that high-purity ferric trichloride can be obtained compared with the prior art that Fe is directly dissolved in the water phase without adopting an extraction technology. In addition, the method can directly obtain the ferric trichloride from the ilmenite without adding an additional iron source, and the obtained ferric trichloride has stable property and does not need to be oxidized by adding an oxidant in the subsequent iron phosphate preparation process. In the prior art, ferrous sulfate contains ferrous iron which is ferrous iron, and an oxidant is required to be added for oxidation in the process of preparing iron phosphate.
In alternative embodiments, the concentration of hydrochloric acid in the present application may be 10-15vt%, such as 10 vt%, 11 vt%, 12 vt%, 13 vt%, 14 vt% or 15vt%, but may also be 10.5 vt%, 11.5 vt%, 12.5 vt%, 13.5 vt% or 14.5 vt%, and may also be other concentration values in the range of 10-15 vt%.
The mass ratio of the hydrochloric acid to the ilmenite can be 1-10: 1, as 1: 1. 2: 1. 3: 1. 4: 1. 5: 1. 6: 1. 7: 1. 8: 1. 9: 1 or 10: 1, etc., and may be 1 to 10: other mass ratios within 1.
It is worth to say that the concentration of hydrochloric acid and the mass ratio of the hydrochloric acid to the ilmenite in the application are set so that high-purity ferric trichloride can be obtained at lower cost. If the hydrochloric acid concentration is higher than 15vt% or the mass ratio of hydrochloric acid to ilmenite is higher than 10: after 1, the iron in the ilmenite is dissolved and simultaneously the titanium is dissolved, and the subsequent operation is influenced. If the concentration of the hydrochloric acid is lower than 10vt percent or the mass ratio of the hydrochloric acid to the ilmenite is lower than 1: 1, in turn, may result in insufficient dissolution of iron from the ilmenite.
In an alternative embodiment, the reaction of ilmenite with hydrochloric acid may be carried out at 10-35 ℃ (e.g. 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃ or 35 ℃) for 10-24h (e.g. 10h, 15h, 20h or 24h, etc.). The reaction temperature mentioned above is also understood to be room temperature. After the ilmenite reacts with the hydrochloric acid, the iron in the ilmenite can be fully dissolved and leached.
After the ilmenite and the hydrochloric acid react, the reaction product is separated, and the clear liquid obtained after separation is extracted so as to extract all iron in the clear liquid into an organic phase, while the rest substances in the clear liquid can not be extracted into the organic phase, thereby further improving the purity of the ferric trichloride.
In an alternative embodiment, the volume ratio of extraction reagent to liquid to be extracted for iron extraction may be 3-5: 1, as in 3: 1. 3.5: 1. 4: 1. 4.5: 1 or 5: 1, etc.
In an alternative embodiment, the extraction reagent comprises an iron extractant. By reference, the iron extractant may comprise, for example, at least one of trioctylamine, a secondary primary amine, tributylphosphate, bis (1-methylheptyl) methylphosphonate.
In addition, the extraction reagent may also include an oil phase solvent. By reference, the oil phase solvent may include at least one of toluene, isoamyl alcohol, and sulfonated kerosene.
In some preferred embodiments, the extraction reagent consists of trioctylamine and sulfonated kerosene. The volume ratio of the trioctylamine to the sulfonated kerosene can be 1-3: 1, as 1: 1. 1.5: 1. 2: 1. 2.5: 1 or 3: 1, etc.
In the extraction process, the iron extractant directionally transfers the ferric trichloride in the liquid to be extracted into the extraction reagent to obtain an organic phase containing the ferric trichloride, so that the iron is completely separated from the rest components in the liquid to be extracted.
Further, reacting the organic phase containing ferric trichloride with an initiator and a precipitator to obtain the iron phosphate precursor.
In an alternative embodiment, the initiator and precipitant, as well as the organic phase comprising ferric chloride, can be reacted at a pH of 1.5 to 2.0 (e.g., 1.5, 1.6, 1.7, 1.8, 1.9, or 2.0) and a temperature of 60 to 70 deg.C (e.g., 60 deg.C, 62 deg.C, 65 deg.C, 68 deg.C, or 70 deg.C, etc.).
In an alternative embodiment, the precipitant and the organic phase comprising ferric chloride are added dropwise to the mixture of initiator and water after mixing. The method specifically comprises the following steps: mixing an initiator and water, heating to 60-70 ℃, adjusting the pH value to 1.5-2.0, simultaneously dropwise adding a precipitator and an organic phase containing ferric trichloride, and keeping the pH value at 1.5-2.0 till the target amount is finished.
The above process can be carried out in a reaction kettle. The above process mainly uses alkali to adjust pH, and the alkali can be sodium hydroxide or potassium hydroxide, etc.
In an alternative embodiment, the initiator is iron phosphate crystals. Specifically, the initiator can be directly purchased nano-scale iron phosphate substances, or iron phosphate substances prepared by water, ferric trichloride and phosphoric acid.
In an alternative embodiment, the precipitation agent may include at least one of phosphoric acid and phosphate. The phosphate may, by reference, include at least one of sodium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, potassium phosphate, dipotassium hydrogen phosphate, and potassium dihydrogen phosphate.
In the process, the initiator is used as a nucleus, so that ferric trichloride and phosphoric acid continuously grow on the surface of the initiator in a water environment, and an iron phosphate product with a corresponding particle size is obtained according to the requirement.
Preferably, the iron phosphate prepared by the method has a particle size of 0.3-0.5 μm, and is particularly suitable for further preparing an electrode material lithium iron phosphate.
In the application, after the reaction of an initiator, a precipitator and the organic phase containing ferric trichloride, standing and layering are carried out, the upper organic phase can be recycled, and the lower suspension is filtered, separated, washed, dried and calcined to obtain the final ferric phosphate.
In alternative embodiments, the calcination can be performed at 500-600 deg.C (e.g., 500 deg.C, 550 deg.C, 600 deg.C, etc.) for 20-40min (e.g., 20min, 25min, 30min, 35min, 40min, etc.). The calcination under these conditions was sufficient to remove the bound water from the iron phosphate.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
Mixing ilmenite and hydrochloric acid with the concentration of 15vt% in a mass ratio of 1: 5 reacting for 15h at 20 ℃. Subsequently, the reaction product was filtered to obtain a clear liquid and a solid. The titanium content in the clear liquid is not more than 0.1 wt%, and the titanium content in the solid is not less than 30 wt%.
And (3) carrying out iron extraction on the obtained clear liquid by using an iron extraction agent, and directionally transferring ferric trichloride in the clear liquid into an extraction reagent to obtain an organic phase containing ferric trichloride. Wherein the volume ratio of the extraction reagent to the clear liquid is 4: 1, extracting a reagent prepared from trioctylamine and sulfonated kerosene according to a volume ratio of 2: 1.
Mixing an initiator and water, heating to 65 ℃, adjusting the pH value to 1.5-2.0, simultaneously dropwise adding a precipitator and an organic phase containing ferric trichloride, and keeping the pH value at 1.5-2.0 till obtaining the iron phosphate precursor with the preset particle size (0.3-0.5 mu m). Wherein, the initiator is a commercially available nano-scale ferric phosphate substance, the precipitator is sodium phosphate, and the pH is adjusted by sodium hydroxide.
Standing and layering a system obtained after reacting an initiator, a precipitator and an organic phase containing ferric trichloride, recycling an upper layer of the organic phase, filtering a lower layer of suspension, washing, drying, and calcining at 550 ℃ for 30min to obtain the final ferric phosphate, wherein an SEM picture of the final ferric phosphate is shown in figure 1, and the size of ferric phosphate particles is concentrated to be about 0.2-0.3 mu m.
Example 2
Mixing ilmenite and hydrochloric acid with the concentration of 10 vt% in a mass ratio of 1: 1 at 10 ℃ for 24 h. Subsequently, the reaction product was filtered to obtain a clear liquid and a solid. The titanium content in the clear liquid is not more than 0.1 wt%, and the titanium content in the solid is not less than 30 wt%.
And (3) carrying out iron extraction on the obtained clear liquid by using an iron extraction agent, and directionally transferring ferric trichloride in the clear liquid into the extraction agent to obtain an organic phase containing ferric trichloride. Wherein, the volume ratio of the extraction reagent to the clear liquid is 3: 1, extracting a reagent prepared from trioctylamine and sulfonated kerosene according to a volume ratio of 1: 1.
Mixing an initiator and water, heating to 60 ℃, adjusting the pH value to 1.5-2.0, simultaneously dropwise adding a precipitator and an organic phase containing ferric trichloride, and keeping the pH value at 1.5-2.0 till obtaining the iron phosphate precursor with the preset particle size (0.3-0.5 mu m). Wherein, the initiator is a commercially available nano-scale ferric phosphate substance, the precipitator is sodium phosphate, and the pH is adjusted by sodium hydroxide.
Standing and layering a system obtained after reacting an initiator, a precipitator and an organic phase containing ferric trichloride, recycling the upper layer of the organic phase, filtering the lower layer of suspension, washing, drying, and calcining at 500 ℃ for 40min to obtain the final iron phosphate.
Example 3
Mixing ilmenite and hydrochloric acid with the concentration of 12.5 vt% in a mass ratio of 1: 10 at 35 ℃ for 10 h. Subsequently, the reaction product was filtered to obtain a clear liquid and a solid. The titanium content in the clear liquid is not more than 0.1 wt%, and the titanium content in the solid is not less than 30 wt%.
And (3) carrying out iron extraction on the obtained clear liquid by using an iron extraction agent, and directionally transferring ferric trichloride in the clear liquid into an extraction reagent to obtain an organic phase containing ferric trichloride. Wherein, the volume ratio of the extraction reagent to the clear liquid is 5: 1, extracting a reagent by using trioctylamine and sulfonated kerosene according to a volume ratio of 3: 1.
Mixing an initiator and water, heating to 70 ℃, adjusting the pH value to 1.5-2.0, simultaneously dropwise adding a precipitator and an organic phase containing ferric trichloride, and keeping the pH value at 1.5-2.0 till obtaining the iron phosphate precursor with the preset particle size (0.3-0.5 mu m). Wherein, the initiator is a commercially available nano-scale ferric phosphate substance, the precipitator is sodium phosphate, and the pH is adjusted by sodium hydroxide.
Standing and layering a system obtained after reacting an initiator, a precipitator and an organic phase containing ferric trichloride, recycling the upper layer of the organic phase, filtering the lower layer of suspension, washing, drying, and calcining at 600 ℃ for 20min to obtain the final iron phosphate.
Example 4
This example differs from example 1 in that: the iron extractant is tributyl phosphate, and the oil phase solvent is sulfonated kerosene.
Example 5
This example differs from example 1 in that: the iron extractant is trioctylamine, and the oil phase solvent is toluene.
Example 6
This example differs from example 1 in that: the iron extractant is secondary carbon primary amine and methyl phosphonic acid di (1-methyl heptyl) ester, and the volume ratio is 1: 1, and the oil phase solvent is isoamyl alcohol and sulfonated kerosene according to the volume ratio of 1: 1 mixing the above components.
Example 7
The present embodiment 1 differs from embodiment 1 in that: the initiator is an iron phosphate substance prepared by water, ferric trichloride and phosphoric acid, the precipitator is potassium phosphate, and the pH is adjusted by potassium hydroxide.
Comparative example 1
Leaching 500 g of ilmenite with sulfuric acid, filtering, and dissolving a certain amount of hematite and ferric sulfate in the filtrate to ensure that the concentration of Fe in the mixed solution is 0.1mol/L and the molar ratio of Ti to Fe is 0.3; adding sufficient sodium peroxide solution (1mol/L), adding phosphoric acid (1mol/L) which is equimolar with Fe, adjusting the pH value to be 2.5 +/-0.1 by using sodium hydroxide solution (0.5mol/L), reacting for 5min in a stirring reactor at 40 ℃, washing and filtering the obtained precipitate, and drying at 100 ℃ to obtain a mixture of precursor of lithium iron phosphate, namely ferric phosphate and doped phosphate of the lithium ion battery cathode material.
Test examples
The results of measuring the content of metal ions in the products obtained in example 1 and comparative example 1 are shown in Table 1, wherein the national standard is HG/T4701-2014, the unit of iron and phosphorus is ppm, and the unit of the rest of metal ions is ppm.
TABLE 1 Metal ion content of iron phosphate
As can be seen from Table 1, the method for synthesizing iron phosphate by using ilmenite provided by the application can obtain iron phosphate with higher purity, and meets the national standard requirements.
In summary, the liquid obtained by solid-liquid separation after the reaction of ilmenite and hydrochloric acid is subjected to iron extraction to obtain an organic phase containing ferric trichloride. And then reacting the initiator, the precipitator and the organic phase containing ferric trichloride to obtain a ferric phosphate precursor, and calcining to obtain the high-purity ferric phosphate. The method can directly obtain the iron phosphate with higher purity from the ilmenite, does not need an oxidation step in the synthesis process, simplifies the working procedures compared with the prior art, reduces the production cost, and is suitable for industrial production. The iron phosphate is suitable for further preparing an electrode material lithium iron phosphate.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. A method for synthesizing battery-grade iron phosphate by utilizing ilmenite is characterized by comprising the following steps of: reacting ilmenite with hydrochloric acid, and performing iron extraction on liquid obtained by solid-liquid separation to obtain an organic phase containing ferric trichloride;
reacting an initiator with a precipitating agent and the organic phase containing ferric trichloride, separating out a precipitate obtained by the reaction, and then calcining;
the concentration of the hydrochloric acid is 10-15vt%, and the mass ratio of the hydrochloric acid to the ilmenite is 1-10: 1; the reaction of the ilmenite and the hydrochloric acid is carried out at the temperature of 10-20 ℃ for 10-24 h;
the reaction of the initiator, the precipitator and the organic phase containing ferric trichloride is carried out under the conditions that the pH is 1.5-2.0 and the temperature is 60-70 ℃;
dropwise adding the precipitator and the organic phase containing ferric trichloride into a mixture obtained by mixing the initiator and water for reaction;
the initiator is ferric phosphate crystal;
the precipitating agent comprises at least one of phosphoric acid and phosphate;
the volume ratio of the extraction reagent used for iron extraction to the liquid is 3-5: 1; the extraction reagent comprises an iron extraction reagent; the iron extractant comprises at least one of trioctylamine, secondary primary amine, tributyl phosphate and bis (1-methylheptyl) methylphosphonate;
the extraction reagent also comprises an oil phase solvent, wherein the oil phase solvent comprises at least one of toluene, isoamyl alcohol and sulfonated kerosene; the volume ratio of the extraction reagent to the oil phase solvent is 1-3: 1.
2. the method as claimed in claim 1, wherein the calcination is carried out at 500-600 ℃ for 20-40 min.
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