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Method for preparing ferrous oxalate from siderite

A technology of ferrous oxalate and siderite, which is applied in carboxylate preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of high energy consumption and low purity of ferrous oxalate, and achieve a high level of clean production , high purity, and remarkable environmental benefits

Active Publication Date: 2022-05-31
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems of the technologies described above, the purpose of this invention is to provide a kind of method utilizing siderite to prepare ferrous oxalate, to solve prior art and utilize siderite to prepare Problems of high energy consumption and low purity of ferrous oxalate

Method used

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  • Method for preparing ferrous oxalate from siderite
  • Method for preparing ferrous oxalate from siderite
  • Method for preparing ferrous oxalate from siderite

Examples

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Embodiment 1

[0058] A method utilizing siderite to prepare ferrous oxalate, comprising the following steps:

[0059] (1) Ore leaching: Grind 100kg of low-grade siderite into fine particles with a particle size of 100 mesh, add it to dilute sulfuric acid solution, and conduct a leaching reaction at 80°C for 4 hours to convert the iron carbonate in the siderite into soluble ferrous ions; wherein, the liquid-solid ratio of dilute sulfuric acid solution and siderite is 8:1, and the molar ratio of iron in sulfuric acid and siderite is 1.3:1;

[0060] (2) Liquid-solid separation: the slurry obtained in step (1) is subjected to pressure filtration to obtain slag and a separating liquid containing ferrous sulfate;

[0061] (3) Precipitating iron oxalate (removing potassium and sodium): add oxalic acid to the separation liquid 1, carry out precipitation reaction for 0.5h at 30°C, and then separate solid and liquid to obtain primary ferrous oxalate and separation liquid 2; among them, oxalic acid T...

Embodiment 2

[0070] A method utilizing siderite to prepare ferrous oxalate, comprising the following steps:

[0071] (1) Ore leaching: Grind 100kg of low-grade siderite into fine particles with a particle size of 100 mesh, add it to dilute sulfuric acid solution, and conduct a leaching reaction at 70°C for 5 hours to convert the iron carbonate in the siderite into soluble ferrous ions; wherein, the liquid-solid ratio of dilute sulfuric acid solution and siderite is 1:1, and the molar ratio of iron in sulfuric acid and siderite is 1.1:1;

[0072] (2) Liquid-solid separation: the slurry obtained in step (1) is subjected to pressure filtration to obtain slag and a separating liquid containing ferrous sulfate;

[0073] (3) Precipitating iron oxalate (removing potassium and sodium): add oxalic acid to the separation liquid 1, carry out precipitation reaction at 30°C for 0.6h, and then separate solid and liquid to obtain primary ferrous oxalate and separation liquid 2; among them, oxalic acid T...

Embodiment 3

[0082] A method utilizing siderite to prepare ferrous oxalate, comprising the following steps:

[0083] (1) Ore leaching: Grind 100kg of low-grade siderite into fine particles with a particle size of 100 mesh, add it to dilute sulfuric acid solution, and conduct a leaching reaction at 100°C for 3 hours to convert the iron carbonate in the siderite into soluble ferrous ions; wherein, the liquid-solid ratio of dilute sulfuric acid solution and siderite is 10:1, and the molar ratio of iron in sulfuric acid and siderite is 1.5:1;

[0084] (2) Liquid-solid separation: the slurry obtained in step (1) is subjected to pressure filtration to obtain slag and a separating liquid containing ferrous sulfate;

[0085] (3) Precipitating iron oxalate (removing potassium and sodium): add oxalic acid to the separation liquid 1, carry out precipitation reaction for 0.5h at 30°C, and then separate solid and liquid to obtain primary ferrous oxalate and separation liquid 2; among them, oxalic acid ...

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Abstract

The invention discloses a method for preparing ferrous oxalate by using siderite, which comprises the following steps: adding siderite into an inorganic acid solution to carry out leaching reaction, and then carrying out solid-liquid separation to obtain a separated liquid I; oxalic acid is added into the first separation liquid for a precipitation reaction, then solid-liquid separation is conducted, and primary ferrous oxalate is obtained; adding the primary ferrous oxalate into an oxalic acid solution for pulping, then adding an oxidizing agent, and carrying out solid-liquid separation to obtain a separation solution III; and performing reduction treatment on the separation liquid III, then performing solid-liquid separation, and washing and drying the obtained precipitate to obtain ferrous oxalate. According to the method, the low-grade siderite is used as a raw material, the electrode-grade ferrous oxalate is directly synthesized, the obtained product is high in purity and few in by-product, meanwhile, the technological process is shortened, efficient resource utilization of the low-grade siderite is achieved, the production cost of the ferrous oxalate is reduced, in addition, the method is a closed-loop circulation process, the solution is recycled, no waste water is discharged, and the method is suitable for industrial production. The clean production level is high and the environment-friendly benefit is obvious.

Description

technical field [0001] The invention relates to the technical field of preparation of anode material precursors of lithium ion batteries, in particular to a method for preparing ferrous oxalate from siderite. Background technique [0002] Lithium-ion batteries have many advantages such as high energy density, long cycle life, less environmental pollution and no memory effect, and become an important basis for supporting the development of current electric vehicle power supplies. Lithium iron phosphate batteries have excellent performance in terms of safety and cycle life. , becoming one of the mainstream batteries in the current electric vehicle market. [0003] Ferrous oxalate is a high-quality precursor for preparing lithium iron phosphate. At present, it is mainly obtained by using commercial ferrous salt and oxalate through mixed precipitation. This type of technology first needs to undergo a complex metallurgical process to obtain ferromanganese ore. Commercialized hig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C51/42C07C55/07
CPCC07C51/412C07C51/42C07C55/07Y02P10/20
Inventor 孙维义苏仕军丁桑岚
Owner SICHUAN UNIV
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