Preparation method of cell grade ferric orthophosphate

A technology of ferric orthophosphate and its production method, which is applied in the field of phosphorus chemical industry, can solve the problems of high cost of battery-grade ferric orthophosphate, and achieve the effects of environmental protection, cost reduction, and improvement of recycling rate

Active Publication Date: 2012-07-18
KUNMING CHUAN JINNUO CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the production of high-power batteries has always been troubled by factors such as cost. The cost of producing battery-grade iron orthophosphate in the existing technology is too high, which has become one of the obstacles restricting the development of my country's electric vehicles and other related industries.

Method used

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  • Preparation method of cell grade ferric orthophosphate
  • Preparation method of cell grade ferric orthophosphate

Examples

Experimental program
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Embodiment 1

[0026] The clarified liquid (containing P 2 o 5 8~12%) as raw material, pour into the reaction vessel, control the temperature at 80°C, add 3.5% industrial grade NaOH by weight while stirring, and fully dissolve it. In the sodium phosphate salt solution after the reaction, the molar ratio is 1:1 Join FeSO 4 ·7H 2 O solution, adding 2% catalyst H by weight 2 o 2 , control the pH value at the end point to ≈1.5, and maintain the reaction for 1 hour to obtain a crude ferric phosphate slurry, which is filtered through a plate and frame filter press and washed repeatedly with water to obtain a ferric phosphate filter cake; Min mechanical stirring to carry out crystal conversion, and adjust the acidity and P with the raw material liquid 2 o 5 Concentration, maintain H +1 0.7g / L and P 2 o 5 At 80°C, age and crystallize for 1 hour; filter and wash the aged residue repeatedly with water until the free phosphoric acid in the filter cake is ≤0.05%, sulfuric acid ≤0.0015%, and a...

Embodiment 2

[0028] The clarified liquid (containing P 2 o 5 8~12%) as raw material, pour into the reaction vessel, control the temperature at 80°C, add 3.2% industrial grade NaOH by weight while stirring, and fully dissolve it. In the sodium phosphate salt solution after the reaction, the molar ratio is 1:2 Join FeSO 4 ·7H 2 O solution, adding 5% catalyst H by weight 2 o 2 , control the end-point pH value to ≈1.5, and maintain the reaction for 1.5 hours to obtain crude ferric phosphate slurry, which is filtered through a plate and frame filter press and washed repeatedly with water to obtain a ferric phosphate filter cake; the filter cake is put into an aging tank and heated at 200 r / min under mechanical stirring for crystal conversion, and adjust the acidity and P with the raw material solution 2 o 5 Concentration, maintain H +1 0.9g / L and P 2 o5 22g / L, aged and crystallized at 90°C for 5 hours; the aged slag was repeatedly filtered and washed with water until the free phospho...

Embodiment 3

[0030] The clarified liquid (containing P 2 o 5 8~12%) as raw material, inject into the reaction vessel, control the temperature at 85°C, add 4% by weight industrial grade NaOH while stirring, fully dissolve, in the sodium phosphate salt solution after the reaction, the molar ratio is 1:2 Join FeSO 4 ·7H 2 O solution, adding 3% catalyst H by weight 2 o 2 , control the end-point pH value to ≈1.5, and maintain the reaction for 1.2 hours to obtain crude ferric phosphate slurry, which is filtered through a plate and frame filter press and washed repeatedly with water to obtain a ferric phosphate filter cake; the filter cake is put into an aging tank and heated at 150 r / min under mechanical stirring for crystal conversion, and adjust the acidity and P with the raw material solution 2 o 5 Concentration, maintain H +1 0.75g / L and P 2 o 5 At 85°C, age and crystallize for 4 hours; filter and wash the aged slag repeatedly with water until the free phosphoric acid in the filt...

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Abstract

The invention discloses a preparation method of cell grade ferric orthophosphate, which comprises processes of hybrid reaction, filtering and washing, aging, washing and separating of aging slag, drying and smashing. A clarified liquid after a two sections of neutralization of feed-grade calcium hydrogen phosphate produced by wet-process phosphoric acid serves as a raw material. The method comprises the steps of injecting the clarified liquid into a reaction container, adding sodium hydroxide, a ferrous sulfate-water (1 / 7) solution and hydrogen peroxide, preparing coarse ferric phosphate after the reaction, throwing the coarse ferric phosphate to a aging tank, converting crystal, using a raw material liquid to adjust acidity and phosphorus pentoxide concentration, crystallizing and aging the mixture for 1-5 hours, subjecting aging slag to filter and wash so that free phosphoric acid is up to <=0.05% and sulphuric acid is up to <=0.0015%, drying the obtained filtered masses so that free water is up to <=1.0%, smashing and sieving the filtered masses, and obtaining cell grade ferric orthophosphate dihydrate products or anhydrous ferric orthophosphate products. The clarified liquid after the two sections of neutralization of feed-grade calcium hydrogen phosphate produced by wet-process phosphoric acid serves as phosphor resources to produce cell grade ferric orthophosphate. The cost is low and quality is good. The method uses industrial grade ferrous sulfate-water (1 / 7) to replace ferric salts with high purities, so that the source is abundant and resource cycling usage rate is high. According to the method, yield coefficient of phosphorus pentoxide can reach to more than 89% and content of various impurities can meet requirements.

Description

technical field [0001] The invention belongs to the technical field of phosphorus chemical industry, and in particular relates to a method for producing battery-grade iron orthophosphate by using wet-process phosphoric acid. Background technique [0002] Battery-grade iron orthophosphate is an important raw material for a new type of battery. It plays an important role in protecting the battery from explosion and flame retardancy in high-temperature environments and during overcharge and discharge, and provides a reliable guarantee for the safe use of batteries. This material can not only produce low-power batteries but also widely produce high-power batteries for industries such as electric vehicles. At present, most of the phosphorus required for the production of battery-grade iron orthophosphate comes from high-purity fine phosphate or high-purity refined phosphoric acid, resulting in high production costs. At present, most of them are limited to the production of low-p...

Claims

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Application Information

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IPC IPC(8): C01B25/37H01M4/58
CPCY02E60/12Y02E60/10
Inventor 孙位成刘国标曾润国刘薨魏家贵
Owner KUNMING CHUAN JINNUO CHEM IND
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