CN113184820A - Method for preparing iron phosphate by using titanium dioxide byproduct ferrous sulfate - Google Patents
Method for preparing iron phosphate by using titanium dioxide byproduct ferrous sulfate Download PDFInfo
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- CN113184820A CN113184820A CN202110448673.3A CN202110448673A CN113184820A CN 113184820 A CN113184820 A CN 113184820A CN 202110448673 A CN202110448673 A CN 202110448673A CN 113184820 A CN113184820 A CN 113184820A
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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
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
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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
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for preparing iron phosphate by using a titanium dioxide byproduct ferrous sulfate. The method utilizes the pH regulator to regulate the pH of the solution, thereby realizing the removal of impurity ions; preparing ferric hydroxide by oxidizing with an oxidant and controlling the pH value of the solution; then controlling the pH value and selecting phosphoric acid to re-dissolve to prepare the iron phosphate. The preparation process is simple in process, does not need to additionally add additives, ensures the purity of the solution, and simultaneously realizes the removal of impurities in the raw material ferrous sulfate to obtain the high-purity ferric phosphate. Meanwhile, the filtrate generated in the impurity removal process is evaporated and crystallized to be used as a fertilizer, so that the benefit is increased.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a method for preparing iron phosphate by using a titanium dioxide byproduct ferrous sulfate.
Background
The by-product ferrous sulfate of titanium dioxide is widely used in the manufacture of iron phosphate, and the general process firstly oxidizes the ferrous sulfate into ferric sulfate and then is used for synthesizing the iron phosphate. However, the titanium dioxide byproduct ferrous sulfate has high impurity content, such as 0.2-1% of magnesium, 0.07-0.15% of manganese, 0.1-0.5% of titanium, 10-100 ppm of aluminum, 10-70 ppm of zinc and 10-60 ppm of nickel, and the high-purity ferric sulfate solution is difficult to prepare due to the difficulty in removing impurities from the ferrous sulfate. Ferric sulfate impurities directly affect the quality of the subsequently synthesized ferric phosphate.
At present, the ferric sulfate is prepared by oxidizing ferrous sulfate, and the ferrous sulfate is prepared into the ferric sulfate by adding an oxidizing agent under the acidic condition. And the purification of the byproduct ferrous sulfate of the titanium dioxide is mainly carried out by adjusting the pH value and adding sulfide and fluoride for removing impurities, but the impurities of magnesium and manganese can not be completely removed. The high-impurity ferric sulfate further has great influence on the impurities of the synthesized ferric phosphate, so that the contents of magnesium and manganese in the synthesized ferric phosphate are 350ppm and the content of nickel impurities is 15-20 ppm.
Therefore, a method for preparing iron phosphate by using a titanium dioxide byproduct ferrous sulfate is needed, and the iron phosphate prepared by the method has low impurity content.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: a method for preparing ferric phosphate by using a titanium dioxide byproduct ferrous sulfate is disclosed, and the ferric phosphate prepared by the method is low in impurity 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 a titanium dioxide byproduct ferrous sulfate comprises the following steps:
s1, dissolving the titanium white byproduct solid ferrous sulfate to obtain a ferrous sulfate solution I;
s2, adding a pH regulator under a heating condition, and regulating the pH of the ferrous sulfate solution to 4-6; performing solid-liquid separation, and collecting a liquid phase to obtain a ferrous sulfate solution II;
s3, under the heating condition, enabling the oxidant mixed solution and the ferrous sulfate solution II to be mixed in a parallel flow mode, controlling the pH value of the solution to be 4-7, carrying out solid-liquid separation after reaction, and collecting a solid phase to obtain ferric hydroxide;
s4, reacting the ferric hydroxide material with a mixed acid solution, controlling the reaction pH to be 1.0-2.0, controlling the temperature, performing solid-liquid separation, collecting a solid phase, washing and drying to obtain ferric phosphate;
wherein the mixed acid is a mixture of phosphoric acid solution and sulfuric acid solution.
The pH value of titanium hydroxide formed by completely hydrolyzing titanium is 2.3, the pH value of aluminum hydroxide formed by completely hydrolyzing aluminum is 4.7, the pH value of ferric hydroxide formed by completely hydrolyzing ferric iron is 4, the pH value of ferrous iron initially hydrolyzed to be 7 and the pH value of ferric hydroxide formed by completely hydrolyzing ferrous iron is 9, under the condition, the titanium, the aluminum and the ferric iron are completely precipitated, but the ferrous iron is not precipitated, and then the solution is filtered to obtain a ferrous sulfate solution.
The reaction of the ferrous sulfate solution, the oxidant and the alkali liquor is as follows:
2Fe2++4OH-+H2O2＝2Fe(OH)3↓。
because the pH value of manganese begins to hydrolyze is 8.1, the pH value of manganese hydroxide formed by complete hydrolysis is 10.4, the pH value of magnesium begins to hydrolyze is 9.4, the pH value of magnesium hydroxide formed by complete hydrolysis is 11.1, the pH value of nickel begins to hydrolyze is 7.2, the pH value of nickel hydroxide formed by complete hydrolysis is 9.5, the pH value of zinc begins to hydrolyze is 6.1, and the pH value of zinc hydroxide formed by complete hydrolysis is 8.4, under the condition of the pH value of 4-7, the magnesium, the manganese, the nickel and the zinc cannot form hydroxide precipitates and can be continuously remained in the solution, and pure ferric hydroxide is obtained after filtering and washing.
According to some embodiments of the invention, the ferrous sulfate solution I has a mass concentration of 150g/L to 300 g/L.
According to some embodiments of the invention, the heating temperature in the step S2 is 60 ℃ to 90 ℃; the heating time in the step S2 is 30-60 min. According to some embodiments of the invention, the pH adjusting agent comprises an ammonia-containing solution; preferably, the ammoniated solution comprises aqueous ammonia; preferably, the mass concentration of the ammonia water is 15-30%.
According to some embodiments of the invention, the oxidant mixture solution comprises a lye and an oxidant.
According to some embodiments of the invention, the lye comprises ammonia and a strong base.
According to some embodiments of the invention, the strong base comprises at least one of potassium hydroxide and sodium hydroxide.
According to some embodiments of the invention, the oxidizing agent comprises a peroxide.
According to some embodiments of the invention, the peroxide comprises at least one of a metal peroxide, hydrogen peroxide and a persulfate.
According to some embodiments of the invention, the metal peroxide comprises an alkali metal peroxide and an alkaline earth metal peroxide; preferably, the alkali metal peroxide comprises at least one of sodium peroxide and potassium peroxide.
According to some embodiments of the invention, the persulfate protects at least one of potassium persulfate, sodium persulfate, and ammonium persulfate.
According to some embodiments of the invention, the ratio of the amounts of the substances of the lye and the oxidant is 1:0.3 to 0.4.
According to some embodiments of the invention, the ammonia concentration in the lye is between 25g/L and 70g/L by mass.
According to some embodiments of the invention, the total mass concentration of the oxidant in the oxidant mixture solution is in the range of 0.4mol/L to 1.5 mol/L.
According to some embodiments of the invention, the ratio of the amount of the substance of ferrous ions, the amount of the substance of ammonia in the alkaline solution and the amount of the substance of the oxidizing agent in the ferrous sulfate solution II is 1:1.8 to 2.2:0.5 to 0.63.
According to some embodiments of the invention, the heating temperature in the step S3 is 60 ℃ to 90 ℃; the heating time in the step S3 is 2-7 h.
According to some embodiments of the invention, the time for the cocurrent mixing in step S3 is 1 to 2 hours.
According to some embodiments of the invention, the ratio of the amounts of the iron hydroxide, sulfuric acid and phosphoric acid is 1:0.05 to 0.1:1.0 to 1.2.
According to some embodiments of the invention, the reaction in step S4 is a stirred reaction; preferably, the stirring reaction time is 60min to 120 min.
According to some embodiments of the invention, the temperature in the step S4 is 90 ℃ to 100 ℃; the time for controlling the temperature is 2-4 h.
The method for preparing the iron phosphate by utilizing the ferrous sulfate as the titanium white byproduct, disclosed by the embodiment of the invention, has at least the following beneficial effects: the method utilizes a pH regulator (ammonia-containing solution) to regulate the pH of the solution, thereby realizing the removal of impurity ions; preparing ferric hydroxide by oxidizing the mixed solution of the oxidant and controlling the pH value of the solution; and then phosphoric acid is selected to be re-dissolved to prepare the iron phosphate. The preparation process is simple in process, does not need to additionally add additives, ensures the purity of the solution, and simultaneously realizes the removal of impurities in the raw material ferrous sulfate to obtain high-purity iron phosphate; meanwhile, the ferric phosphate prepared by the method has high tap density. Meanwhile, the filtrate (ammonium sulfate filtrate) generated in the impurity removal process is evaporated and crystallized to be used as a fertilizer, so that the benefit is increased.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
The impurity contents of the solid ferrous sulfate raw materials selected in the examples of the present invention and the comparative examples are shown in table 1 below.
TABLE 1 impurity content (unit: ppm) in solid ferrous sulfate raw materials selected in examples of the present invention and comparative examples
| Ca | Mg | Na | Ni | Zn | Cu | Mn | Cr | K | Co | Al | Ti | |
| Raw material I | 30 | 7119 | 15 | 29 | 66 | 0 | 1042 | 2 | 4 | 54 | 39 | 2379 |
| Feedstock II | 25 | 3891 | 13 | 43 | 50 | 0 | 744 | 4 | 5 | 34 | 16 | 1884 |
| Starting materials III | 47 | 5557 | 19 | 44 | 47 | 0 | 1230 | 1 | 0 | 37 | 13 | 1627 |
The first embodiment of the invention is as follows: a method for preparing iron phosphate by using a titanium dioxide byproduct ferrous sulfate comprises the following steps: the method comprises the following steps:
s1, stirring and fully dissolving the byproduct solid ferrous sulfate (raw material I) of the titanium dioxide factory in water at the dissolving temperature of 40 ℃, and then filtering to obtain a ferrous sulfate solution I with the concentration of 200 g/L.
And S2, heating the obtained ferrous sulfate solution to 70 ℃, starting stirring, adding ammonia water with the concentration of 30%, adjusting the pH value of the solution to 5.5, continuing to react for half an hour, and then filtering to obtain a ferrous sulfate solution II.
S3, mixing ammonia water with the mass concentration of 30% and hydrogen peroxide solution with the mass concentration of 28% and then adding the mixture into water to prepare mixed solution; the mass concentration of ammonia in the solution is controlled to be 44.5g/L, and the mass concentration of hydrogen peroxide is controlled to be 25 g/L.
S4, adding pure water into the reaction kettle, starting stirring, and then adding the mixed solution and the ferrous sulfate solution II into the reaction kettle in a cocurrent manner; and after the feeding is finished, heating the solution to 70 ℃, controlling the pH to be 6.0-6.5, reacting for 3 hours, filtering, collecting a filter cake, and washing the filter cake with pure water to obtain the reddish brown ferric hydroxide.
S5, adding pure water into the ferric hydroxide material to prepare slurry, then adding a mixed solution of phosphoric acid and sulfuric acid into the slurry, stirring and reacting for 60 minutes, then heating to 90 ℃, keeping the temperature for 2 hours, filtering, washing a filter cake with the pure water, and drying to obtain low-impurity ferric phosphate; wherein the concentration of the phosphoric acid is 1.2mol/L, the concentration of the sulfuric acid is 0.05mol/L, and the ratio of the ferric hydroxide to the sulfuric acid to the phosphoric acid is 1:0.05: 1.2.
The second embodiment of the invention is as follows: a method for preparing iron phosphate by using a titanium dioxide byproduct ferrous sulfate comprises the following steps: the method comprises the following steps:
s1, stirring and fully dissolving the byproduct solid ferrous sulfate (raw material I) of the titanium dioxide factory in water at the dissolving temperature of 60 ℃, and then filtering to obtain ferrous sulfate solution I with the concentration of 180 g/L.
And S2, heating the obtained ferrous sulfate solution I to 70 ℃, starting stirring, adding ammonia water with the mass concentration of 25%, adjusting the pH of the solution to 5.5, continuing to react for half an hour, and filtering to obtain a ferrous sulfate solution II.
S3, mixing ammonia water with the mass concentration of 25% with hydrogen peroxide solution with the mass concentration of 28%, and then adding pure water to prepare a mixed solution; the mass concentration of ammonia in the mixed solution is controlled to be 41g/L, and the mass concentration of hydrogen peroxide is controlled to be 21 g/L.
And S4, adding pure water into the reaction kettle, starting stirring, and then adding the prepared mixed solution of ammonia water and hydrogen peroxide and ferrous sulfate solution II into the reaction kettle in a concurrent flow manner. And heating the solution to 70 ℃, controlling the pH value to be 5.5-6.0, reacting for 4 hours, filtering, and washing a filter cake with pure water to obtain the reddish brown ferric hydroxide.
S5, adding pure water into the ferric hydroxide material to prepare slurry, then adding a mixed solution of phosphoric acid and sulfuric acid into the slurry, stirring and reacting for 60 minutes, then heating to 90 ℃, keeping the temperature for 3 hours, filtering, washing a filter cake with the pure water, and drying to obtain low-impurity ferric phosphate; wherein the concentration of the phosphoric acid is 1.1mol/L, the concentration of the sulfuric acid is 0.05mol/L, and the ratio of the ferric hydroxide to the sulfuric acid to the phosphoric acid is 1:0.05: 1.1.
The third embodiment of the invention is as follows: a method for preparing iron phosphate by using a titanium dioxide byproduct ferrous sulfate comprises the following steps: the method comprises the following steps:
s1, stirring and fully dissolving the byproduct solid ferrous sulfate (raw material I) of the titanium dioxide factory in water at the dissolving temperature of 50 ℃, then filtering, and collecting the liquid phase to obtain ferrous sulfate solution I with the concentration of 250 g/L.
And S2, heating the obtained ferrous sulfate solution I to 80 ℃, starting stirring, adding ammonia water with the mass concentration of 20%, adjusting the pH of the solution to 5.0, continuing to react for half an hour, filtering, and collecting a liquid phase to obtain a ferrous sulfate solution II.
S3, mixing ammonia water with the mass concentration of 20% and hydrogen peroxide with the mass concentration of 28%, and then adding the mixture into water to prepare a mixed solution; the mass concentration of ammonia in the mixed solution is controlled to be 56g/L, and the mass concentration of hydrogen peroxide is controlled to be 32 g/L.
And S4, adding pure water into the reaction kettle, starting stirring, and then adding the mixed solution and the ferrous sulfate solution II into the reaction kettle in a concurrent flow manner. And heating the solution to 80 ℃, controlling the pH to be 6.0-6.5, reacting for 4 hours, filtering, and washing a filter cake with pure water to obtain the reddish brown ferric hydroxide.
S5, adding pure water into the obtained ferric hydroxide material to prepare slurry, adding the pure water into the ferric hydroxide material to prepare slurry, then adding a mixed solution of phosphoric acid and sulfuric acid into the slurry, stirring and reacting for 60 minutes, then heating to 90 ℃, keeping the temperature for 2 hours, filtering, washing a filter cake with the pure water, and drying to obtain low-impurity ferric phosphate; wherein the concentration of the phosphoric acid is 1.1mol/L, the concentration of the sulfuric acid is 0.08mol/L, and the ratio of the ferric hydroxide to the sulfuric acid to the phosphoric acid is 1:0.08: 1.1.
The fourth embodiment of the invention is as follows: a method for preparing ferric sulfate by using a titanium dioxide byproduct ferrous sulfate comprises the following steps: the method comprises the following steps:
s1, stirring and fully dissolving the byproduct solid ferrous sulfate (raw material I) of the titanium dioxide factory in water at the dissolving temperature of 40 ℃, and then filtering to obtain a ferrous sulfate solution with the concentration of 300 g/L.
S2, heating the obtained ferrous sulfate solution to 50 ℃, starting stirring, adding ammonia water with the concentration of 20%, adjusting the pH value of the solution to 6.0, continuing to react for half an hour, and then filtering to obtain a clear ferrous sulfate solution.
S3, mixing the ammonia water with the concentration of 20% and the hydrogen peroxide with the concentration of 28% and adding the mixture into pure water to prepare a solution. Wherein the concentration of ammonia is 67g/L, and the concentration of hydrogen peroxide is 38 g/L.
And S4, adding pure water into the reaction kettle, starting stirring, and then adding the prepared mixed solution of ammonia water and hydrogen peroxide and ferrous sulfate solution into the reaction kettle in a concurrent flow manner. Heating the solution to 80 ℃, controlling the pH value to be 5.5-6.0, reacting for 2 hours, filtering, and washing a filter cake by pure water to obtain the reddish brown ferric hydroxide.
S5, adding the ferric hydroxide material into pure water to prepare slurry, adding a mixed solution of phosphoric acid and sulfuric acid, stirring and reacting for 60 minutes, heating to 90 ℃, preserving heat for 4 hours, filtering, washing a filter cake with the pure water, and drying to obtain low-impurity ferric phosphate; wherein the concentration of the phosphoric acid is 1.2mol/L, the concentration of the sulfuric acid is 0.1mol/L, and the ratio of the ferric hydroxide to the sulfuric acid to the phosphoric acid is 1:0.05: 1.2.
The first comparative example of the present invention is: a method for preparing ferric sulfate by using a titanium dioxide byproduct ferrous sulfate comprises the following steps: the method comprises the following steps:
s1, stirring and fully dissolving the byproduct solid ferrous sulfate (raw material II) of the titanium dioxide factory in water at the dissolving temperature of 40 ℃, and then filtering to obtain a ferrous sulfate solution with the concentration of 200 g/L.
S2, heating the obtained ferrous sulfate solution to 80 ℃, starting stirring, adding ammonia water with the concentration of 20%, adjusting the pH value of the solution to 6.0, continuing to react for half an hour, and then filtering to obtain the ferrous sulfate solution.
S3, adding the ferrous sulfate solution into the reaction kettle, starting stirring, and then adding the prepared monoammonium phosphate solution and hydrogen peroxide into the reaction kettle. And heating the solution to 90 ℃, reacting for 3 hours, filtering, washing a filter cake with pure water, and drying to obtain the iron phosphate.
The iron phosphate samples prepared in examples one to four of the present invention and comparative example one were dissolved in hydrochloric acid, and then impurities were detected using an ICP instrument, and the results thereof are shown in table 2.
Table 2 impurity ion contents of iron phosphates prepared in examples one to four of the present invention and comparative example one
As shown in Table 2, the impurities of magnesium, manganese, nickel, zinc, aluminum and titanium in the ferric phosphate product can be greatly reduced by adding ammonia water to adjust the pH value and controlling the pH value range, so that the effect of purifying the solution to reduce the impurities is achieved.
The results of the tap density test of the iron phosphates prepared in the examples one to four of the present invention and the comparative example one are shown in table 3.
Table 3 tap densities of iron phosphates prepared in examples one to four of the present invention and comparative example one
| Example one | Example two | EXAMPLE III | Practice ofExample four | Comparative example 1 | |
| Tap density (g/cm)3) | 1.17 | 1.14 | 1.09 | 1.18 | 0.87 |
As can be seen from Table 3, the tap densities of the iron phosphates prepared in examples one to four of the present invention were 1.09g/cm3The above; much higher than comparative example one (0.87g/cm 3).
In conclusion, the method provided by the invention utilizes the pH regulator (ammonia-containing solution) to regulate the pH of the solution, so as to remove impurity ions; preparing ferric hydroxide by oxidizing with an oxidant and controlling the pH value of the solution; then sulfuric acid is selected to be re-dissolved to prepare ferric sulfate. The preparation process is simple in process, does not need to additionally add additives, ensures the purity of the solution, and simultaneously realizes the removal of impurities in the raw material ferrous sulfate to obtain the high-purity ferric phosphate. Meanwhile, the filtrate (ammonium sulfate filtrate) generated in the impurity removal process is evaporated and crystallized to be used as a fertilizer, so that the benefit is increased.
While the embodiments of the present invention have been described in detail in the foregoing specification, the present invention is not limited to the above-described embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A method for preparing iron phosphate by using a titanium dioxide byproduct ferrous sulfate is characterized by comprising the following steps: the method comprises the following steps:
s1, dissolving the titanium white byproduct solid ferrous sulfate to obtain a ferrous sulfate solution I;
s2, adding a pH regulator under a heating condition, and regulating the pH of the ferrous sulfate solution to 4-6; performing solid-liquid separation, and collecting a liquid phase to obtain a ferrous sulfate solution II;
s3, under the heating condition, enabling the oxidant mixed solution and the ferrous sulfate solution II to be mixed in a parallel flow mode, controlling the pH value of the solution to be 4-7, carrying out solid-liquid separation after reaction, and collecting a solid phase to obtain ferric hydroxide;
s4, reacting the ferric hydroxide material with a mixed acid solution, controlling the reaction pH to be 1.0-2.0, controlling the temperature to be 85-95 ℃, carrying out solid-liquid separation, collecting a solid phase, washing and drying to obtain ferric phosphate;
wherein the mixed acid is a mixture of a phosphoric acid solution and a sulfuric acid solution;
the mass ratio of sulfuric acid to phosphoric acid in the mixed acid is 1: 12-20.
2. The method for preparing iron phosphate by using the titanium dioxide byproduct ferrous sulfate as claimed in claim 1, which is characterized in that: the mass concentration of the ferrous sulfate solution I is 150 g/L-300 g/L.
3. The method for preparing iron phosphate by using the titanium dioxide byproduct ferrous sulfate as claimed in claim 1, which is characterized in that: the heating temperature in the step S2 is 60-90 ℃; the heating time in the step S2 is 30-60 min.
4. The method for preparing iron phosphate by using the titanium dioxide byproduct ferrous sulfate as claimed in claim 1, which is characterized in that: the pH regulator comprises an ammonia-containing solution; preferably, the ammoniated solution comprises aqueous ammonia; preferably, the mass concentration of the ammonia water is 15-30%.
5. The method for preparing iron phosphate by using the titanium dioxide byproduct ferrous sulfate as claimed in claim 1, which is characterized in that: the oxidant mixed solution comprises alkali liquor and an oxidant; preferably, the alkali solution comprises at least one of ammonia water or strong alkali; preferably, the strong base comprises at least one of a potassium hydroxide solution and a sodium hydroxide solution; preferably, the oxidizing agent comprises a peroxide; preferably, the peroxide comprises at least one of a metal peroxide, a persulfate, and hydrogen peroxide; preferably, the metal peroxide comprises at least one of an alkali metal peroxide and an alkaline earth metal peroxide; preferably, the mass ratio of the alkaline solution to the oxidant is 1: 0.3-0.4.
6. The method for preparing iron phosphate by using the titanium dioxide byproduct ferrous sulfate as claimed in claim 5, which is characterized in that: the mass concentration of ammonia in the alkali liquor is 25g/L-70 g/L.
7. The method for preparing iron phosphate by using the titanium dioxide byproduct ferrous sulfate as claimed in claim 5, which is characterized in that: the total mass concentration of the oxidant in the oxidant mixed solution is 0.4-1.5 mol/L.
8. The method for preparing iron phosphate by using the titanium dioxide byproduct ferrous sulfate as claimed in claim 5, which is characterized in that: the ratio of the amount of the ferrous ion substances in the ferrous sulfate solution II, the amount of the ammonia substances in the alkali liquor and the amount of the oxidant substances is 1: 1.8-2.2: 0.5-0.63.
9. The method for preparing iron phosphate by using the titanium dioxide byproduct ferrous sulfate as claimed in claim 1, which is characterized in that: the heating temperature in the step S3 is 60-90 ℃; the heating time in the step S3 is 2-7 h; preferably, the time for the cocurrent mixing in the step S3 is 1h to 2 h.
10. The method for preparing iron phosphate by using the titanium dioxide byproduct ferrous sulfate as claimed in claim 1, which is characterized in that: the ratio of the amount of the ferric hydroxide, the sulfuric acid and the phosphoric acid is 1: 0.05-0.1: 1.0-1.2.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113816354A (en) * | 2021-11-04 | 2021-12-21 | 四川省盈达锂电新材料有限公司 | Method for preparing iron phosphate by using wastes in titanium dioxide production process |
| CN113968578A (en) * | 2021-12-06 | 2022-01-25 | 紫金矿业集团股份有限公司 | Method for synthesizing iron phosphate by using ferrous sulfate as titanium dioxide byproduct |
| CN114180546A (en) * | 2021-12-30 | 2022-03-15 | 江西赣锋循环科技有限公司 | Method for preparing anhydrous iron phosphate from titanium-containing lithium iron phosphate waste |
| CN114906830A (en) * | 2022-07-19 | 2022-08-16 | 昆明川金诺化工股份有限公司 | Method for controllably preparing battery-grade iron phosphate from pyrite cinder |
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| CN111847416A (en) * | 2020-07-24 | 2020-10-30 | 中南大学 | Method for preparing hydrated iron phosphate from ferrous sulfate serving as titanium dioxide byproduct |
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