Preparation method of battery-grade iron phosphate

An iron phosphate, battery-grade technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of complex production process of iron phosphate, unreusable raw materials, high cost of sewage treatment, and improve resource utilization, The effect of reduced production cycle and low cost

Pending Publication Date: 2020-04-17
博创宏远新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the prior art, the iron phosphate production process is relatively complicated, the energy consumption is high, and the water consumption during washing is large, and the cost of sewage treatment is high; secondly, the raw materials cannot be reused, such as neutralizer liquid alkali or ammonia water, which cannot be reused, and finally form a solid Salt, or even if it is reused, a large amount of calcium sulfate will be produced, and the amount of solid waste will be large; moreover, due to the use of more raw materials in the prior art, and the complicated process, there are many opportunities to introduce impurities, resulting in the purity of the product not tall

Method used

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  • Preparation method of battery-grade iron phosphate
  • Preparation method of battery-grade iron phosphate
  • Preparation method of battery-grade iron phosphate

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Experimental program
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Effect test

Embodiment 1

[0039] Concentrated hydrochloric acid with a concentration of 37% was prepared with deionized water to form 547.5kg of a 20% solution, and then 57.14kg of high-purity iron powder with a fineness of 100 mesh and a purity of 98% was added to fully react, and the reaction temperature was controlled to 65°C through jacket heat exchange , until the iron powder no longer dissolves.

[0040] After filtering, take the filtrate, add 74.18kg of 27.5% hydrogen peroxide, control the temperature at 55°C, and react for 3 hours, detect the absence of ferrous ions in the iron solution by the o-phenanthroline indicator method, and obtain the oxidizing solution.

[0041] Add 117kg of 85% phosphoric acid, mix evenly, and transport it to the spray dryer, control the air inlet temperature to 195°C, and the air outlet temperature to 105°C, and the solid collected after evaporation is ferric phosphate dihydrate, and the water vapor and hydrogen chloride condensate are recovered for storage spare.

...

Embodiment 2

[0046] Concentrated hydrochloric acid with a concentration of 37% was configured with deionized water to form 547.5kg of a 20% solution, and then 57.14kg of high-purity iron powder with a fineness of 100 mesh and a purity of 98% was added to fully react, and the reaction temperature was controlled by a heat exchanger to be 55 °C until no longer dissolved.

[0047]After filtering, take the filtrate, add 92.72 kg of 27.5% hydrogen peroxide, control the temperature at 65° C., react for 2 hours, detect the absence of ferrous ions in the iron solution by potassium permanganate titration, and obtain the oxidized solution.

[0048] Add 118.7kg of 85% phosphoric acid, mix well and transport to the spray dryer, control the inlet air temperature to 200°C, and the outlet air temperature to 105°C, and collect the solid obtained after evaporation as ferric phosphate dihydrate, recover water vapor and hydrogen chloride condensate for storage spare.

[0049] Send the ferric phosphate dihydr...

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Abstract

The invention provides a preparation method of battery-grade iron phosphate. The preparation method comprises the following steps: adding high-purity iron powder into hydrochloric acid with a proper concentration, and carrying out a reaction until the iron powder is not dissolved any more; filtering, adding a proper amount of hydrogen peroxide, and reacting until no ferrous ions exist in the reaction solution; adding phosphoric acid, uniformly stirring, and carrying out spray drying to obtain iron phosphate dihydrate; and sintering at a high temperature to remove crystal water to obtain anhydrous iron phosphate. According to the invention, the method comprises the steps of ferrous solution synthesis, oxidation, ferric phosphate dihydrate synthesis and high-temperature sintering, so that the procedures of ferric phosphate precipitation, aging, filtering, washing and the like are reduced, the procedures are reduced, the flow is shortened, the production period is shortened, the production efficiency is improved, water resources are saved, and the cost is low; the raw materials are recycled, no solid waste is generated, and the cost is reduced; and a neutralizer is not needed, the useof raw materials is reduced, the opportunity of impurity introduction is reduced, the obtained product is high in purity and low in impurity content, and the market requirements of battery-grade rawmaterials can be well met.

Description

technical field [0001] The invention belongs to the technical field of preparation of lithium-ion battery materials, and in particular relates to a method for preparing battery-grade iron phosphate. Background technique [0002] The synthesis process routes of lithium iron phosphate, the cathode material of lithium ion batteries, include hydrothermal process, ferrous oxalate process, iron red process, and iron phosphate process. The iron phosphate process has gradually become the mainstream route for lithium iron phosphate production due to its good batch stability and excellent electrochemical performance. The ferric phosphate in the prior art is a conventional chemical precipitation method, and the production process is: batching—ferrous oxidation—ferric phosphate precipitation—filtering and washing—low temperature drying—high temperature sintering, etc. For example, CN201910630953.9 discloses a method for preparing battery-grade iron phosphate. The preparation method co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
CPCC01B25/375C01P2002/72
Inventor 赵杰龙锦
Owner 博创宏远新材料有限公司
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