Method for synthesizing iron phosphate by utilizing titanium dioxide byproduct ferrous sulfate

A technology of ferrous sulfate and ferric phosphate, used in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of neglecting the control of sulfur content, potential safety hazards, complicated operations, etc., to improve the utilization rate and increase the concentration. Effect

Inactive Publication Date: 2021-03-12
HUNAN YACHENG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The precipitation method is to remove the impurity manganese and magnesium in ferrous sulfate by adding sulfide and fluoride respectively, and realize the removal of magnesium ions by using the low solubility of manganese sulfide. Poor, at the same time improper operation will also produce hydrogen sulfide gas, this method has serious potential safety hazards; resin adsorption method is to use resin to different ion adsorption capacity difference to ferrous sulfate to remove impurities, but due to a large amount of divalent Iron ions will be preferentially adsorbed by the resin, and impurities such as manganese and magnesium cannot be effectively removed
Though said method can reduce impurity manganese, magnesium content in ferrous sulfate to a certain extent, thereby make the lower ferric phosphate finished product of manganese, magnesium content, but most methods (as countercurrent extraction, recrystallization, sulfide impurity removal, etc.) has the disadvantages of cumbersome steps and complicated operations
At the same time, these methods only focus on the control of impurity manganese and magnesium in the finished product of iron phosphate, while ignoring the control of sulfur content

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  • Method for synthesizing iron phosphate by utilizing titanium dioxide byproduct ferrous sulfate
  • Method for synthesizing iron phosphate by utilizing titanium dioxide byproduct ferrous sulfate
  • Method for synthesizing iron phosphate by utilizing titanium dioxide byproduct ferrous sulfate

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Embodiment 1

[0046] Embodiment 1 of the present invention is: a method for synthesizing ferric phosphate by using ferrous sulfate, a by-product of titanium dioxide, comprising the following steps:

[0047] S1: Pretreatment: Control the temperature at 70°C, add ammonia water with a mass concentration of 30% to the titanium dioxide by-product ferrous sulfate solution, adjust the pH value to 4.2, and press filter to obtain a mass concentration of iron element of 101g / The ferrous sulfate raw material solution of L;

[0048] Add a hydrogen peroxide solution with a mass concentration of 30% into the ferrous sulfate raw material solution, control the molar ratio of hydrogen peroxide and iron element in the ferrous sulfate raw material solution to be 0.6:1, and oxidize all ferrous ions into iron ions Finally, add an appropriate amount of pure water to obtain a ferric sulfate raw material solution with a mass concentration of iron element of 56g / L;

[0049] According to the solid-to-liquid ratio ...

Embodiment 2

[0053] Embodiment 2 of the present invention is: a method for synthesizing ferric phosphate by using titanium dioxide by-product ferrous sulfate, comprising the following steps:

[0054] S1: Pretreatment: Control the temperature at 80°C, add a sodium hydroxide solution with a mass concentration of 25% to the titanium dioxide by-product ferrous sulfate solution, adjust the pH value to 5.0, and press filter to obtain the mass concentration of iron element as The ferrous sulfate raw material liquid of 87g / L;

[0055] Add a hydrogen peroxide solution with a mass concentration of 30% into the ferrous sulfate raw material solution, control the molar ratio of hydrogen peroxide and iron element in the ferrous sulfate raw material solution to be 0.6:1, and oxidize all ferrous ions into iron ions Finally, add an appropriate amount of pure water to obtain a ferric sulfate raw material solution with a mass concentration of iron element of 67g / L;

[0056] According to the solid-to-liquid ...

Embodiment 3

[0060] Embodiment three of the present invention is: a method for synthesizing ferric phosphate by using ferrous sulfate as a by-product of titanium dioxide, comprising the following steps:

[0061] S1: Pre-treatment: Control the temperature of the titanium dioxide by-product ferrous sulfate solution to 60°C, add ammonia water with a mass concentration of 30% to the ferrous sulfate solution, adjust the pH value to 3.8, and press filter to obtain the quality of iron element Concentration is the ferrous sulfate raw material solution of 105g / L;

[0062] Add a hydrogen peroxide solution with a mass concentration of 30% into the ferrous sulfate raw material solution, control the molar ratio of hydrogen peroxide and iron element in the ferrous sulfate raw material solution to be 0.6:1, and oxidize all ferrous ions into iron ions Finally, add an appropriate amount of pure water to obtain a ferric sulfate raw material solution with a mass concentration of iron element of 44.8g / L;

[...

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Abstract

The invention discloses a method for synthesizing iron phosphate by utilizing a titanium dioxide byproduct ferrous sulfate. According to the method, the titanium dioxide byproduct ferrous sulfate is used as a raw material, through pretreatment, oxidation of ferrous sulfate in advance, partial substitution of phosphoric acid with sulfuric acid or hydrogen chloride and other inorganic acids to serveas acidizing fluid, generation of Mn3(PO4)2 and Mg3(PO4)2 precipitates in the iron phosphate preparation process is effectively inhibited, therefore the iron phosphate finished product with the low impurity Mn, Mg and S element content is prepared. Meanwhile, the utilization rate of iron ions is increased, and the iron-phosphorus ratio of the prepared iron phosphate is obviously higher than thatof the related technology. According to the method, complex and tedious operations such as extraction, recrystallization and sulfide precipitation are avoided, the titanium dioxide byproduct ferrous sulfate is successfully utilized to prepare the iron phosphate with low impurity content and high iron-phosphorus ratio, the process is simple, and the effect is remarkable.

Description

technical field [0001] The invention relates to the technical field of lithium-ion battery materials, in particular to a method for synthesizing ferric phosphate by using ferrous sulfate, a by-product of titanium dioxide. Background technique [0002] Due to the advantages of large theoretical discharge capacity, long cycle life, high safety, and environmental friendliness, lithium iron phosphate is considered to be one of the most promising cathode materials for lithium-ion batteries, and is widely used in various mobile communication devices and vehicles. . Among them, iron phosphate is an important precursor for the production of lithium iron phosphate, and the purity and quality of iron phosphate have an extremely important impact on the electrochemical performance of lithium iron phosphate batteries. For iron phosphate production enterprises, in the face of the plight of continuous rising raw material prices, how to reduce the cost of raw and auxiliary materials and en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
CPCC01B25/375C01P2002/72C01P2004/03C01P2006/12C01P2006/80C01P2004/52C01P2004/30
Inventor 林奕颜志雄万文治李万罗强
Owner HUNAN YACHENG NEW MATERIAL CO LTD
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