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Preparation method of high purity superfine ferrous oxalate

A technology of ferrous oxalate and ferrous sulfate, applied in the direction of carboxylate preparation, etc., to achieve the effect of simple process, narrow particle size distribution range, and easy industrialized large-scale production

Inactive Publication Date: 2012-02-08
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to overcome the particle diameter is difficult to control in the existing ferrous oxalate preparation method, the shortcoming that product purity is lower, provides a kind of technique simple, cost is lower , the preparation method of high-purity ultra-fine ferrous oxalate that is easy to industrialized production

Method used

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  • Preparation method of high purity superfine ferrous oxalate
  • Preparation method of high purity superfine ferrous oxalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Dissolve 70g of industrial-grade oxalic acid in 700ml of deionized water under the action of mechanical stirring, completely dissolve 156g of industrial-grade ferrous sulfate in 320ml of deionized water under the action of mechanical stirring, and vacuum the obtained solution Remove impurities by suction filtration;

[0026] (2) Spray the purified ferrous sulfate solution into the oxalic acid solution with a dispersant (a mixture of sodium polyacrylate, methanol, ethanol and propanol) under the action of a high-speed centrifugal sprayer. The amount of dispersant added is the same as that of oxalic acid The solution ratio is 0.001mol / L until the molar ratio of ferrous sulfate and oxalic acid in the solution reaches 1:1;

[0027] (3) The reaction temperature of the sprayed ferrous sulfate solution and oxalic acid solution is always controlled at 20°C, and the two react for 10 minutes under the action of ultrasonic cavitation at an ultrasonic frequency of 40kHz to obta...

Embodiment 2

[0030] (1) Completely dissolve 70g of industrial grade oxalic acid in 180ml of deionized water under the action of mechanical stirring, completely dissolve 156g of industrial grade ferrous sulfate in 300ml of deionized water under the action of mechanical stirring, and vacuum the obtained solution Remove impurities by suction filtration;

[0031] (2) Spray the purified ferrous sulfate solution into the oxalic acid solution with ethanol dispersant under the action of a high-speed centrifugal sprayer. The ratio of the dispersant to the oxalic acid solution is 0.09 mol / L until the solution The molar ratio of ferrous sulfate to oxalic acid reaches 1:1;

[0032] (3) The reaction temperature of the sprayed ferrous sulfate solution and oxalic acid solution was always controlled at 0°C, and the two reacted for 10 minutes under the action of ultrasonic cavitation at an ultrasonic frequency of 40kHz to obtain a ferrous oxalate suspension;

[0033] (4) Leave the ferrous oxalate suspensi...

Embodiment 3

[0035] (1) Dissolve 70g of industrial grade oxalic acid in 180ml of deionized water under the action of mechanical stirring, completely dissolve 156g of industrial grade ferrous sulfate in 300ml of deionized water under the action of mechanical stirring, and use the obtained solution Remove impurities by vacuum filtration;

[0036] (2) Spray the purified ferrous sulfate solution into the oxalic acid solution with ethanol dispersant under the action of a high-speed centrifugal sprayer. The ratio of the dispersant to the oxalic acid solution is 0.1mol / L until the solution The molar ratio of ferrous sulfate to oxalic acid reaches 1:1;

[0037] (3) The reaction temperature of the sprayed ferrous sulfate solution and oxalic acid solution was always controlled at -20°C, and the two reacted for 10 minutes under the action of ultrasonic cavitation at an ultrasonic frequency of 59kHz to obtain a ferrous oxalate suspension;

[0038] (1) Leave the ferrous oxalate suspension to stand, th...

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Abstract

The invention provides a preparation method of high purity superfine ferrous oxalate. Oxalate and ferrous sulfate solids are respectively completely dissolved into deionized water under the action of mechanical agitation, impurities in the obtained solution are removed by adopting a vacuum filtration method; purified ferrous sulfate solution is sprayed into oxalate solution added with dispersant under the action of a high-speed centrifugal sprayer; reaction temperature of the sprayed ferrous sulfate solution and the oxalate solution is controlled to be minus 40 to 20 DEG C, the ferrous sulfate solution and the oxalate solution completely react under the action of ultrasonic cavitation; and generated ferrous oxalate suspension is subjected to separating, washing and drying to obtain ferrous oxalate powder. The purity of synthesized material reaches up to more than 99.5%, average particle size is 0.1-3Mum, and distribution range of the particle size is narrow; meanwhile, process flow is simple, cost is low, and industrialized mass production is easy to realize.

Description

Technical field: [0001] The invention relates to a preparation method of high-purity ultrafine ferrous oxalate, belonging to the technical field of powder material preparation. Background technique: [0002] Lithium-ion batteries have the advantages of high voltage, high energy density, no pollution, no memory effect, long life, etc., and are widely used in portable electrical devices such as mobile phones, digital cameras, and notebook computers. At present, with the increasingly prominent energy and environmental issues, lithium-ion power batteries, as an alternative energy source for petroleum, will also be widely used in electric vehicles, electric tools, and large-scale energy storage equipment. Among various cathode materials for lithium-ion batteries, olivine-like lithium iron phosphate (LiFePO 4 ) has received widespread attention due to its wide source of raw materials, low cost, high safety, and environmental friendliness, and is considered to be the preferred c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/07C07C51/41
Inventor 姚耀春戴卫平杨斌戴永年谢惠吴鉴速斌李永梅黄瑞安方海升易惠华马文会刘大春徐宝强
Owner KUNMING UNIV OF SCI & TECH
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