Preparation method of ferric phosphate with high tap density

A technology of tap density and iron phosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high nucleation rate, low utilization rate of phosphorus resources, and excessive excess, so as to improve the growth of crystal nuclei rate, avoiding environmental protection treatment costs, and inhibiting the effect of nucleation rate

Active Publication Date: 2019-05-07
CENT SOUTH UNIV
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Problems solved by technology

[0003] FePO reported in the literature 4 2H 2 There are many methods for O synthesis, such as solid-phase synthesis, hydrothermal synthesis, co-precipitation, etc., but the only synthetic technology that has achieved large-scale industrial application is the co-precipitation method.
The main process is to use ferrous iron source, hydrogen peroxide and phosphate as raw materials to synthesize FePO 4 2H 2 O powder, there are following deficiencies in this technology: 1) due to Fe 2+ 、PO 4 3- and H 2 o 2 The ion concentration in the coexistence solution system is high, the nucleation rate is large, and the FePO formed by precipitation 4 2H 2 O particle diameter is small, the product tap density is low
2) To avoid Fe 3...

Method used

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  • Preparation method of ferric phosphate with high tap density
  • Preparation method of ferric phosphate with high tap density
  • Preparation method of ferric phosphate with high tap density

Examples

Experimental program
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Embodiment 1

[0043] (1) Synthesis of ferrous phosphate

[0044] Weigh 25.02g of ferrous sulfate heptahydrate and dissolve it in 100ml of boiled deionized water to form a 0.9mol / L ferrous sulfate solution; weigh 7.92g of diammonium hydrogen phosphate and dissolve it in 100ml of deionized water to form a For the diammonium hydrogen phosphate solution of L, adjust the pH of diammonium hydrogen phosphate to 9.68 with ammonia water (1+1). Add the diammonium hydrogen phosphate solution into the reaction kettle equipped with the ferrous sulfate solution with a peristaltic pump at a rate of 20ml / min. After adding the diammonium hydrogen phosphate, the pH of the mixed solution is 4.67. Heated in a water bath to 30°C for 1.0h.

[0045] (2) Preparation of ferrous phosphate suspension

[0046] Wash the precipitate obtained by the reaction in step (1) with suction filtration and water, weigh 42.36 g of ferrous phosphate after washing, add ferrous phosphate to the reaction kettle, add 423 ml of deioni...

Embodiment 2

[0052] (1) Synthesis of ferrous phosphate

[0053] Weigh 33.36g of ferrous sulfate heptahydrate and dissolve it in 100ml of boiled deionized water to form a 1.2mol / L ferrous sulfate solution; weigh 10.56g of diammonium hydrogen phosphate and dissolve it in 100ml of deionized water to form a For the diammonium hydrogen phosphate solution of L, adjust the pH of diammonium hydrogen phosphate to 9.7 with ammonia water (1+1). Add the diammonium hydrogen phosphate solution into the reaction kettle equipped with the ferrous sulfate solution with a peristaltic pump at a rate of 20ml / min. After adding the diammonium hydrogen phosphate, the pH of the mixed solution is 4.7. Heated in a water bath to 30°C for 1.0h.

[0054] (2) Preparation of ferrous phosphate suspension

[0055] Wash the precipitate obtained by the reaction in step (1) by suction filtration and water, weigh 44g of ferrous phosphate after washing, add ferrous phosphate into the reaction kettle, add 440ml of deionized wa...

Embodiment 3

[0061] (1) Synthesis of ferrous phosphate

[0062] Weigh 33.36g of ferrous sulfate heptahydrate and dissolve it in 100ml of boiled deionized water to form a 1.2mol / L ferrous sulfate solution; weigh 10.56g of diammonium hydrogen phosphate and dissolve it in 100ml of deionized water to form a For the diammonium hydrogen phosphate solution of L, adjust the pH of diammonium hydrogen phosphate to 9.72 with ammonia water (1+1). Add the diammonium hydrogen phosphate solution into the reaction kettle equipped with the ferrous sulfate solution with a peristaltic pump at a rate of 20ml / min. After adding the diammonium hydrogen phosphate, the pH of the mixed solution is 4.7. Heated in a water bath to 30°C for 1.0h.

[0063] (2) Preparation of ferrous phosphate suspension

[0064] Wash the precipitate obtained by the reaction in step (1) by suction filtration and water, weigh the mass of ferrous phosphate after washing to 42.36g, add ferrous phosphate into the reaction kettle, add 847ml...

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Abstract

The invention discloses a preparation method of ferric phosphate with high tap density. The preparation method comprises: 1) synthesizing solid ferrous phosphate by using a liquid phase precipitationmethod; 2) preparing a ferrous phosphate slurry from the solid ferrous phosphate; and 3) adding a phosphoric acid and hydrogen peroxide mixed solution to the ferrous phosphate slurry in a dropwise manner, and carry out a reaction to obtain a ferric phosphate precursor material with characteristics of large particle, nearly spherical shape and high tap density. According to the present invention, the method has characteristics of simple operation, low agent consumption, less wastewater generation and high ammonia nitrogen concentration, wherein the wastewater can be subjected to evaporation condensation treatment so as to avoid the problem of high concentration ammonia nitrogen wastewater treatment.

Description

technical field [0001] The invention relates to a method for preparing iron phosphate, in particular to a method for preparing an iron phosphate precursor with large particles, nearly spherical shape, and high tap density for the synthesis of lithium iron phosphate cathode active materials for lithium ion batteries, which belongs to new energy sources The field of material preparation technology. Background technique [0002] Lithium iron phosphate has become one of the most potential battery cathode materials due to its advantages of low price, environmental protection and pollution-free, high safety and good thermal stability, so it has attracted the attention of many scientific research institutions and commercial institutions. The conductivity, tap density and stability of lithium iron phosphate are important indicators for its quality characterization, and the iron phosphate precursor (FePO 4 2H 2 O) powder, its physical and chemical properties have a great influence ...

Claims

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Application Information

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IPC IPC(8): C01B25/37
Inventor 周康根彭长宏陈伟胡舜聪李钟山黄典一
Owner CENT SOUTH UNIV
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