Process for preparing battery-grade high-purity nano iron phosphate

A nano-iron phosphate, battery-level technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of ultra-fine iron phosphate that is not easy to wash off, high-end recycling obstacles, and the purity of iron phosphate Low cost, fine particle size, and less waste water discharge

Active Publication Date: 2017-09-22
SICHUAN LOMON PHOSPHORUS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the present iron phosphate preparation generally adopts the reaction process of ferrous salt, oxidizing agent and phosphate, but there are problems: 1. Since ferric ions are particularly easy to be hydrolyzed and precipitated, hydrogen oxidation is easily generated during the preparation of ferric phosphate Iron and other impurities lead to low purity of ferric phosphate; 2. The purification of ferrous solution, especially the manganese, magnesium, nickel, sodium and other ions, is difficult to remove at a lower cost, so high-purity iron raw materials must be used. For example, high-purity iron powder and high-purity

Method used

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  • Process for preparing battery-grade high-purity nano iron phosphate
  • Process for preparing battery-grade high-purity nano iron phosphate
  • Process for preparing battery-grade high-purity nano iron phosphate

Examples

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Embodiment 1

[0052] (1) Add water to dissolve the titanium dioxide by-product until the total iron content in the solution is 45.5g / l, add the mixture of iron hydroxide mud and iron powder, react at 60°C, adjust the final pH of the solution to 5.2, here React at pH for 0.6 hours, filter to obtain the first filter residue and the first filtrate;

[0053] (2) the first filtrate is added acid to adjust the pH to be 1.25, then pass through air oxidation, and the pH of acid maintenance solution is 1.25 simultaneously, to the [Fe in the solution 2+ ] at 3.5g / l, then continue to stand at this pH for 1 hour, filter to obtain the second filter residue and the second filtrate;

[0054] (3) Add acid to the second filtrate, adjust the pH of the solution to be 0.12, then add gac powder, adopt a nanofiltration device to carry out depth filtration, obtain the third filtrate, and di(2-ethylhexyl) phosphoric acid with phosphoric acid and sulfuric acid Mix acid for washing, wash with pure water after washi...

Embodiment 2

[0067] (1) Add water to dissolve the titanium dioxide by-product until the total iron content in the solution is 45.5g / l, add the mixture of ferric hydroxide mud and iron powder, react at 60°C, adjust the final pH of the solution to 5.4, here React at pH for 0.6 hours, filter to obtain the first filter residue and the first filtrate;

[0068] (2) the first filtrate is added acid to adjust the pH to be 1.25, then pass through air oxidation, and the pH of acid maintenance solution is 1.25 simultaneously, to the [Fe in the solution 2+ ] at 3.5g / l, then continue to stand at this pH for 1 hour, filter to obtain the second filter residue and the second filtrate;

[0069] (3) Add acid to the second filtrate, adjust the pH of the solution to be 0.12, then add gac powder, adopt a nanofiltration device to carry out depth filtration, obtain the third filtrate, and di(2-ethylhexyl) phosphoric acid with phosphoric acid and sulfuric acid Mix acid for washing, wash with pure water after was...

Embodiment 3

[0082] (1) Add water to dissolve the titanium dioxide by-product until the total iron content in the solution is 45.5g / l, add the mixture of ferric hydroxide mud and iron powder, react at 60°C, adjust the final pH of the solution to 5.4, here React at pH for 0.6 hours, filter to obtain the first filter residue and the first filtrate;

[0083] (2) adding acid to the first filtrate to adjust the pH to be 1.15, then pass through air for oxidation, while the pH of the acid to maintain the solution is 1.25, to [Fe in the solution 2+ ] at 4.0g / l, then continue to stand at this pH for 1 hour, filter to obtain the second filter residue and the second filtrate;

[0084] (3) Add acid to the second filtrate, adjust the pH of the solution to be 0.12, then add gac powder, adopt a nanofiltration device to carry out depth filtration, obtain the third filtrate, and di(2-ethylhexyl) phosphoric acid with phosphoric acid and sulfuric acid Mix acid for washing, wash with pure water after washing...

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Abstract

The invention discloses a process for preparing battery-grade high-purity nano iron phosphate. The process comprises the steps that the pH is improved by using a titanium dioxide by-product, impurities are removed and a solution is purified by adding iron powder, then ferrous oxidization is performed to obtain ferric iron, the pH of iron sulfate is regulated, ferric ions in the iron sulfate are extracted by adopting di(2-ethylhexyl) phosphoric acid, a washed organic phase is obtained through 5-6 level counter-current extraction, 5-6 level counter-current acid solution washing and 2-3 level counter-current pure water washing, sulfonated kerosene is distilled out, the organic phase obtained after distillation is mixed with a catalyst, reaction is performed at the temperature of 300-320 DEG C for 3-4 hours, and the material obtained after reaction is washed by adding ethyl alcohol and is dried to obtain the high-purity nano iron phosphate. According to the process for preparing the high-purity nano iron phosphate, the high-purity nano iron phosphate can be prepared through the titanium dioxide by-product, the obtained iron phosphate is high in purity, small in particle size and large in specific surface area, the ferro-phosphorus ratio is 0.995-1.01, and the wastewater production amount is small.

Description

technical field [0001] The invention relates to a process for battery-grade high-purity nano-iron phosphate, which belongs to the field of new energy battery materials. Background technique [0002] Iron phosphate , also known as ferric phosphate, iron orthophosphate, molecular formula FePO4, is a white, off-white monoclinic crystal powder. It is the salt of iron salt solution and sodium phosphate, and the iron in it is positive trivalent. Its main purpose is to manufacture Lithium iron phosphate battery pool materials, catalysts and ceramics, etc. [0003] High Purity Ferric Phosphate Dihydrate color It is nearly white or light (light) yellow White Powder, with the loss of crystal water, the color gradually turns yellow, and the pure anhydrous is yellow-white powder. Phosphorus (P) in dihydrate ferric phosphate is off-white or dark off-white when it exceeds the standard; if iron exceeds the standard, it is dark yellow. The ratio of phosphorus to iron is the most...

Claims

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Application Information

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IPC IPC(8): C01B25/37B82Y30/00
CPCB82Y30/00C01B25/375C01P2006/12
Inventor 蒋央芳
Owner SICHUAN LOMON PHOSPHORUS CHEM
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