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Preparation method of iron phosphate for preparing lithium iron phosphate and iron phosphate

A technology of lithium iron phosphate and iron phosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as uneven distribution, uneven particle size of iron orthophosphate, etc., to improve the rate and cycle performance , prevent agglomeration and excessive growth, good crystallinity effect

Active Publication Date: 2012-08-01
深圳市毓丰新材料有限公司
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Problems solved by technology

[0005] The patent application with the publication number CN101891176A discloses a method for preparing iron orthophosphate for lithium-ion battery materials with non-ionic surfactants, but the particle size of the prepared iron orthophosphate is large and uneven (50-300nm), indicating that Simple non-ionic surfactants can not play a good dispersion effect, this method is not suitable for the preparation of lithium iron phosphate precursor iron phosphate
The patent application with the publication number CN10695998A discloses a preparation method for preparing nanoscale iron phosphate. Although the particle size of the prepared iron phosphate is small, the distribution is uneven (10~100nm), and the rotating packed bed reactor used Complicated to use, not suitable for mass production
In the patent application with the publication number CN1021101662A, ferrous oxalate and phosphoric acid are used as raw materials to prepare anhydrous crystalline ferric phosphate. Because of the high temperature treatment at 500°C in the process, the energy consumption is large and the ferric phosphate is easy to grow. The performance of lithium has adverse effects on

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  • Preparation method of iron phosphate for preparing lithium iron phosphate and iron phosphate
  • Preparation method of iron phosphate for preparing lithium iron phosphate and iron phosphate
  • Preparation method of iron phosphate for preparing lithium iron phosphate and iron phosphate

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preparation example Construction

[0032] In one embodiment, the method for preparing iron phosphate for preparing lithium iron phosphate comprises the following steps:

[0033] (1) Prepare cationic surfactant aqueous solution;

[0034] (2) Prepare soluble iron salt aqueous solution and soluble phosphate aqueous solution with a concentration of 0.1~5mol / L respectively;

[0035] (3) Slowly add the soluble iron salt aqueous solution and soluble phosphate aqueous solution to the cationic surfactant in sequence according to Fe:P=1:0.8~1.2 (molar ratio) under the condition of 25~50°C, ultrasound and stirring In the aqueous solution, the addition rate is not more than 60ml / min, and the concentration of the cationic surfactant in the reaction solution obtained after all the soluble iron salt aqueous solution and soluble phosphate aqueous solution are added is 1~10g / L, preferably 3~10g / L. 6g / L.

[0036] (4) Add ammonia water to the reaction solution to adjust the pH of the solution to 0-3 at 25-50°C under ultrasonic ...

Embodiment 1

[0047] (1) dissolving cetyltrimethylammonium bromide in deionized water to prepare a cationic surfactant aqueous solution;

[0048] (2) Use deionized water to prepare ferric chloride aqueous solution and diammonium hydrogen phosphate aqueous solution with a concentration of 1mol / L;

[0049] (3) Under the conditions of 25~50°C (in this example, the water bath is heated to 40°C), ultrasonic and stirring, according to Fe:P=1:1 (molar ratio), ferric chloride aqueous solution and diammonium hydrogen phosphate aqueous solution are respectively Slowly add in the cationic surfactant aqueous solution in sequence, the concentration of the cationic surfactant in the reaction solution obtained after the ferric chloride aqueous solution and the diammonium hydrogen phosphate aqueous solution are all added is 4g / L; the adding speed is 30ml / min , the preferred ultrasonic frequency is 30~100KHZ, in this example, the ultrasonic frequency is 50KHZ;

[0050] (4) Add ammonia water to the reaction s...

Embodiment 2

[0055] (1) dissolving cetyltrimethylammonium chloride in distilled water to prepare an aqueous cationic surfactant solution;

[0056] (2) Use deionized water to prepare ferric nitrate aqueous solution and ammonium dihydrogen phosphate aqueous solution with a concentration of 3 mol / L;

[0057] (3) Under the conditions of 25~50°C (in this example, the water bath is heated to 40°C), ultrasonic and stirring, slowly add the ferric nitrate aqueous solution and the ammonium dihydrogen phosphate aqueous solution to the cationic surfactant solution in sequence. The concentration of the cationic surfactant in the reaction solution obtained after adding all the ferric nitrate aqueous solution and the ammonium dihydrogen phosphate aqueous solution is 5g / L; the adding speed is not more than 60ml / min, and the preferred ultrasonic frequency is 30~100KHZ. In this example, the ultrasonic frequency Choose 100KHZ;

[0058] (4) Add ammonia water to the reaction solution in step (3) to adjust the...

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Abstract

The invention discloses a preparation method of iron phosphate for preparing lithium iron phosphate. The preparation method comprises the following steps of: (1) preparing cationic surfactant aqueous solution; (2) preparing soluble iron salt aqueous solution and soluble phosphate aqueous solution of 0.1-5 mol / L respectively; (3) adding the soluble iron salt aqueous solution and the soluble phosphate aqueous solution into the cationic surfactant aqueous solution in sequence at 25-50 DEG C under ultrasonic treatment and stirring according to a molar ratio of Fe: P of 1:0.8-1.2, wherein the speed is less than or equal to 60 ml / min, and the concentration of a cationic surfactant in reaction solution formed after all materials are added is 1-10 g / L; (4) adding ammonia water at 25-50 DEG C under ultrasonic treatment and stirring to adjust the pH of the solution to be 0-3, performing ultrasonic treatment for a time and continuously stirring for 30-180 minutes; and (5) washing the liquid obtained by the step (4) with de-ionized water or absolute ethanol and then drying at 70-90 DEG C to obtain powdery iron phosphate.

Description

technical field [0001] The invention belongs to the field of inorganic materials, and in particular relates to a method for preparing iron phosphate used for preparing lithium iron phosphate and iron phosphate. Background technique [0002] At this stage, energy and environmental problems are becoming more and more serious, the development and use of clean energy is imminent, and the development of electric vehicles is the trend of future development. The large-scale application of green energy such as wind energy, solar energy, and geothermal energy has put forward higher requirements for energy storage devices, especially for the service life of energy storage batteries. [0003] Lithium iron phosphate, the cathode material of lithium-ion batteries, has good safety performance, low price, high thermal stability, good cycle performance, high theoretical capacity (170mAh / g), and high charge and discharge platform (3.4V~3.6V) , no memory effect, environmental friendliness an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 李宝华邢玉涛褚晓东杜鸿达杨全红康飞宇
Owner 深圳市毓丰新材料有限公司
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