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A kind of preparation method of battery grade anhydrous iron phosphate

An anhydrous phosphoric acid, battery-level technology, applied in chemical instruments and methods, inorganic chemistry, phosphorus compounds, etc., can solve the problem of high iron source cost, affecting the performance of lithium iron phosphate and lithium iron phosphate batteries, high impurity content in iron phosphate, etc. problems, to achieve the effect of improving performance and eliminating differences in microscopic components

Active Publication Date: 2021-12-03
安徽丰原锂电能源有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The cost of the iron source used in the above ferric phosphate preparation method is relatively high, and there is also the problem of high content of impurities such as potassium, sodium, magnesium and heavy metals in the prepared ferric phosphate, the existence of these impurities will affect the further prepared lithium iron phosphate And the performance of lithium iron phosphate battery

Method used

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  • A kind of preparation method of battery grade anhydrous iron phosphate
  • A kind of preparation method of battery grade anhydrous iron phosphate
  • A kind of preparation method of battery grade anhydrous iron phosphate

Examples

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Embodiment 1

[0032] The method of the present embodiment was prepared battery grade anhydrous iron phosphate embodiment, see the flow chart figure 1 , The cold rolled iron automobile scrap iron source, and a concentration of 20% dilute sulfuric acid solution, the reaction under stirring for 3 hours to generate ferrous sulfate solution, ferrous sulfate solution was added to the impurity agent impurity, sediment filter, and the resulting filtrate is purified ferrous sulfate solution;

[0033] Purified ferrous sulfate solution with phosphoric acid - mixed urea solution adjusted to pH 2.0, followed by addition of impurity flocculant, the flocculant in an amount of 0.05% by mass of ferrous sulfate solution, a mixed coagulant flocculant, particularly polymerization sulfate EDTA and iron weight ratio 2: 1 mixture of flocculant is added, stirring rate 100r / min, the stirring time 5min, then the residue was removed by filtration, then purified to give a green solution of ferrous sulfate;

[0034] Puri...

Embodiment 2

[0041] The preparation method of the battery-level anhydrous phosphate of the present embodiment has a ferrous sulfate to produce titanium white powder by sulfuric acid. Specifically, Titanium iron ore is prepared at the end of sulfuric acid (SO 4 ) 2 Tioso 4 Generate FESO at the same time 4 And Fe 2 (SO 4 ) 3 , Acid solution to the generated Tioso 4 FESO 4 The mixture is removed, and the dissolved residual residue is removed by leaching and settling. The solution is added to the elbow after removing impurities, and the trivalent iron ions in the solution are present in the form of a divalent iron ion. Tioso 4 TI 2 (SO 4 ) 3 The form exists. Titanium solution treated with purification, concentrate, cooled by vacuum, so that ferrous sulfate is FESO 4 · 7h 2 O form is crystallized, centrifuged, that is, the raw material of the present embodiment.

[0042] The sulfate is dissolved in the ferrous acid method for the production of titanium white powder by the ferrous acid method. After...

Embodiment 3

[0049] The preparation method of the battery-level anhydrous phosphate in this example is based on the iron source of the automobile cold rolled iron plate, and the dilute sulfuric acid solution having a concentration is 20%, and the ferrous sulfate is formed under stirring. Solution, the ferrous sulfate solution is added to the dispense agent, and the obtained filtrate is a ferrous sulfate solution after purification.

[0050] The purified ferrous sulfate solution is mixed with phosphoric acid-urea to mix the pH to 2.0, then the flocculant is used in addition to 0.05%, the amount of ferrous sulfate is 0.05%, the flocculant is a mixed flocculant, specifically No. 3 After the flocculant and EDTA were added to a flocculant, the stirring rate was 100 r / min, stirred for 5 min, and then the residue was filtered, and a green sulfate refined solution was obtained;

[0051] Sulfate refined solution to the H 2 O 2 The solution and hydrogen peroxide is more than 10% higher than the calcul...

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Abstract

The invention belongs to the technical field of battery material preparation, and specifically discloses a method for preparing battery-grade anhydrous iron phosphate. The method adopts cold-rolled iron plate leftovers and / or beneficiation reduced iron powder as iron source to prepare ferrous solution, or adopts sulfuric acid method titanium dioxide to produce by-product ferrous sulfate to prepare ferrous solution; Iron ions are oxidized to ferric ions, mixed with a solution containing phosphate ions, added with a dispersant, and crystallized to obtain iron phosphate crystals, which are dried and roasted to obtain battery-grade anhydrous iron phosphate. The preparation method of the present invention uses low-cost cold-rolled iron plate scraps, ore-dressing reduced iron powder, or ferrous sulfate, a by-product in the production process of sulfuric acid titanium dioxide, as an iron source, and uses a flocculant to precipitate and remove impurities, and then recrystallizes to prepare The battery-grade iron phosphate has low raw material cost, high product purity, high tap density, spherical structure, and can be used as a precursor of high tap density lithium iron phosphate.

Description

Technical field [0001] The present invention relates to the technical field prepare a battery material, particularly relates to a method for preparing a battery grade anhydrous iron phosphate. Background technique [0002] Lithium iron phosphate (LiFePO 4 ) Assembling a lithium battery positive electrode material having excellent cycle characteristics, good thermal stability, wide sources of raw materials and no pollution, etc, LiFePO 4 It is considered good lithium ion battery positive electrode material. However, compared with other lithium iron phosphate cathode material, a lower tap density of lithium iron phosphate, which leads to lower energy density and volume specific capacity, and therefore can not meet the requirements of higher energy density of the battery material. Therefore, how to improve the lithium iron phosphate of a hot tap density of lithium iron phosphate present competing manufacturers to explore. Has found that if the lithium iron phosphate powder of unifor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37
CPCC01B25/375C01P2004/03C01P2004/32C01P2004/61C01P2006/11C01P2006/12C01P2006/82
Inventor 王立卓王宇飞周知斌王宝璐孙浩
Owner 安徽丰原锂电能源有限公司
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