Iron phosphate preparation method

A technology of ferric phosphate and ferrous phosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as difficulty in meeting the requirements of battery-grade and food-grade ferric phosphate, low purity of ferric phosphate, etc., and reduce environmental pollution. The effect of carrying pressure, avoiding iron-containing waste residue, and ensuring purity

Pending Publication Date: 2021-04-16
SICHUAN UNIV
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  • Description
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Problems solved by technology

[0003] In the current industrialization path of lithium iron phosphate, the process route of iron phosphate has become the mainstream; , manganese, titanium, zinc, copper, chromium and cadmium and other heavy metal elements, magnesium, titanium and manganese all reach thousands of ppm, resulting in low purity of iron phosphate, which is difficult to meet the requirements of battery grade and food grade iron phosphate

Method used

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Embodiment 1

[0034] Please combine figure 1 , figure 2 , the present embodiment provides a method for preparing ferric phosphate, comprising the steps of:

[0035] Take 120 mL of ferrous sulfate solution with a molar concentration of 1.3 mol / L, add it to 80 mL of diammonium hydrogen phosphate solution with a molar concentration of 1.3 mol / L, stir and add NH 3 ·H 2 O, adjust the pH value to 7, and after 60 minutes of reaction, ferrous phosphate precipitation is obtained.

[0036] After filtering and washing, transfer ferrous phosphate to a beaker, add 100g of water for beating, and then add 1.3mol / L of FeSO 4 Solution 24mL and 0.05g dithiocarbamate capture agent, add 0.4mol phosphoric acid to the residue after filtration, add H 2 o 2 About 3.35g, with NH 3 -H 2 O (1:3) adjusted the pH of the system to 2.0, raised the temperature to 95°C for 180 minutes, filtered and dried the precipitate to obtain FePO4·2H2O (ferric phosphate dihydrate) powder.

[0037] Weigh FePO4·2H2O powder to a...

Embodiment 2

[0041] Add 420 mL of ferrous sulfate solution with a molar concentration of 0.5 mol / L to 140 mL of diammonium hydrogen phosphate solution with a molar concentration of 1.0 mol / L, add 0.2 g of dispersant CTAB to the solution, and add 32% NaOH to adjust When the pH value reaches 5.0, filter and wash after reacting for 20 minutes to obtain ferrous phosphate precipitate;

[0042]Add ferrous phosphate to 40% of the solid content and add water for beating, then add 20g of sulfuric acid, 5g of sodium sulfate and 1g of xanthate capture agent, add 0.5mol of phosphoric acid, filter after 0.5 hours of reaction, and then pour into the residue Add H to 2 o 2 About 4.15g and use 16% NaOH to adjust the pH of the system to 1.5. After 2 hours of reaction, raise the temperature to 80 degrees and age for 6 hours to obtain FePO 4 .2H 2 O (ferric phosphate dihydrate) powder.

[0043] Weigh FePO4·2H2O powder to analyze its purity, the purity of ferric phosphate dihydrate is 99.6%, and the conte...

Embodiment 3

[0047] 40 mL of diammonium hydrogen phosphate (NH 4 h 2 PO 4 ), added to 120mL molar concentration of 1.3mol / L ferrous sulfate (FeSO 4 ) solution, ammonia monohydrate (NH 3 .H 2 (0), adjust its pH value to 4.0, after reacting for 10min, filter and wash to obtain ferrous phosphate precipitation.

[0048] After ferrous phosphate was beaten with water according to 30% solid content, 5 g of hydrochloric acid, 10 g of ammonium sulfate and 0.05 g of octahydroxyquinoline were added, and then 0.5 mol of phosphoric acid and 0.04 mol of ammonium dihydrogen phosphate were added. The reaction was filtered for 0.5 h, and H was added to the residue 2 o 2 A total of 3.28g, with NH 3 ·H 2 O to adjust the pH of the system to 3.0, after aging for 40 minutes, raise the temperature to 90°C for 3 hours, filter and dry to obtain FePO 4 .2H 2 O powder. .

[0049] Weigh FePO4 2H2O powder to analyze its purity, the purity of ferric phosphate dihydrate is 99.5%, and the content of impurity ...

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Abstract

An iron phosphate preparation method relates to the field of new energy material preparation, and comprises the following steps: mixing a ferrous sulfate solution and a phosphorus source in proportion, performing stirring to react for 10-120 min, adding an adjusting solution, adjusting the pH value to 3-7, performing filtering and washing to obtain ferrous phosphate; transferring ferrous phosphate into a reaction kettle, adding an impurity removing agent and a complexing agent, supplementing a phosphorus source according to a ratio of P to Fe of 1: 1-1.5: 1, then adding an oxidizing agent which is obtained by oxidizing ferrous iron into ferric iron with a stoichiometric ratio of 1.0-1.5 times, adding an adjusting solution, adjusting the pH value to 1.5-3.5, carrying out heat preservation for 30-90 minutes, heating to 80-100 DEG C, performing forming for 30-180 minutes, and carrying out precipitating, filtering, washing and drying to obtain finished ferric phosphate dihydrate; and carrying out heat preservation on the Ferric phosphate dihydrate at the temperature of 400 DEG C- and 750 DEG C for 30-360 minutes to obtain an anhydrous iron phosphate finished product. Heavy metal ions can be efficiently removed, so that the purity of iron phosphate is effectively ensured.

Description

technical field [0001] The invention relates to the field of preparation of new energy materials, in particular to a method for preparing iron phosphate. Background technique [0002] In the current positive electrode material family, lithium iron phosphate LiFePO4 with an olivine structure has become a commercially available material because of its high theoretical specific capacity (170mAh / g), good cycle performance, good thermal stability, low process cost, and no pollution to the environment. One of the most mature cathode materials for lithium-ion batteries. [0003] In the current industrialization path of lithium iron phosphate, the process route of iron phosphate has become the mainstream; , manganese, titanium, zinc, copper, chromium and cadmium and other heavy metal elements, magnesium, titanium and manganese all reach thousands of ppm, resulting in low purity of iron phosphate, which is difficult to meet the requirements of battery grade and food grade iron phosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 王倩吴昊张玥莹
Owner SICHUAN UNIV
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