Battery-grade ferric phosphate and preparation method

An iron phosphate, battery-grade technology, applied in phosphates, battery electrodes, phosphorus oxyacids, etc., can solve the problems of heat removal, increased energy consumption, low bulk density, etc., to improve product consistency and determine ingredients Reliable, high bulk density results

Inactive Publication Date: 2014-05-28
NINGBO UNIVERSITY OF TECHNOLOGY +1
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Problems solved by technology

[0025] One is that the reaction process produces by-product salts, such as NaNO 3 , NaCl, Na 2 SO 4 etc., by-product salts exist in the mother liquor produced by the reaction, and also exist in large quantities in the washing liquid of iron phosphate products, direct discharge will seriously pollute the environment, waste liquid treatment will cause cost increases, and by-products are low-value products;
[0026] The second is that the generated iron phosphate contains a certain amount of crystal water, usually two, that is, FePO 4 2H 2 O; In addition to crystal water, the product usually contains a small amount of adsorbed water; due to the crystal water and adsorbed water, the actual composition of iron phosphate is not very certain and reliable, which brings certain difficulties to the precise ingredients in the production of lithium iron phosphate;
The main disadvantage of low bulk density is that the product is roasted with a small amount of boat and the production capacity of the roaster is small; the solid content of the slurry is low

Method used

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  • Battery-grade ferric phosphate and preparation method
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  • Battery-grade ferric phosphate and preparation method

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preparation example Construction

[0060] The preparation method of the battery-grade iron phosphate is to use ferric nitrate as an iron source, and phosphoric acid or ammonium dihydrogen phosphate or diammonium hydrogen phosphate or ammonium phosphate as a phosphorus source; prepare a mixed aqueous solution of an iron source and a phosphorus source; Ammonia solution is added to the aqueous solution of the mixture of iron source and phosphorus source as a pH adjuster, stirred and reacted to form a crystalline complex containing ammonium, hydroxide and crystal water, and then solid-liquid separation and drying to obtain NH 4 Fe 2 (OH)(PO 4 ) 2 2H 2 O powder, in which the molar ratio of iron and phosphorus is 0.99-1.01:1, the powder is composed of monodisperse olive-shaped particles with regular appearance, and the tap density is as high as 1.2-1.3g / cm 3 ; The powder is roasted in the air atmosphere to decompose and remove ammonium, hydroxide and crystal water to obtain battery-grade anhydrous iron phosphate F...

Embodiment 1

[0070] Prepare ferric nitrate and phosphoric acid mixed aqueous solution, wherein ferric nitrate concentration is 2.0 mol / liter, phosphoric acid concentration is 2.0 mol / liter, the mol ratio of phosphorus and iron is 1: 1;

[0071] Preparation concentration is the ammonia solution of 10.0 mol / liter as pH regulator;

[0072] Add 2 liters of deionized water to the reaction kettle with a volume of 7 liters, stir vigorously, and pass constant temperature water into the jacket of the reaction kettle, and control the water temperature in the reaction kettle to 95°C;

[0073] Continuously input the mixed aqueous solution of ferric nitrate and phosphoric acid and ammonia solution into the reactor respectively with a pump, control the flow rate of the mixed aqueous solution of ferric nitrate and phosphoric acid to 20 ml / min, adjust the flow rate of ammonia solution, and control the pH value of the reaction solution in the reactor 1.60±0.05;

[0074] Through a constant temperature wate...

Embodiment 2

[0081] Prepare ferric nitrate and ammonium phosphate mixed aqueous solution, wherein ferric nitrate concentration is 0.2 mol / liter, ammonium phosphate concentration is 0.2 mol / liter, the mol ratio of phosphorus and iron is 1: 1;

[0082] Preparation concentration is the ammonia solution of 0.5 mol / liter as pH regulator;

[0083] Add 2 liters of deionized water to the reactor with a volume of 7 liters, stir vigorously, and pass constant temperature water into the jacket of the reactor, and control the water temperature in the reactor to 60°C;

[0084] The ferric nitrate and ammonium phosphate mixed aqueous solution and the ammonia solution are respectively continuously input into the reactor with a pump, the flow of the ferric nitrate and ammonium phosphate mixed aqueous solution is controlled to be 20 ml / min, the flow of the ammonia solution is adjusted, and the reaction liquid in the reactor is controlled. The pH value is 5.50±0.05;

[0085] Through a constant temperature wa...

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Abstract

The invention discloses battery-grade ferric phosphate and its preparation method. The battery-grade ferric phosphate is anhydrous ferric phosphate FePO4. The powder is composed of monodisperse olive-shaped particles with regular shapes. Bulk density is high, and tap density reaches up to 1.5-1.6 g/cm<3>. The preparation method comprises the following steps: using trivalent ferric salt ferric nitrate as an iron source, and using phosphoric acid or ammonium biphosphate or diammonium phosphate or ammonium phosphate as a phosphorus source; adding an ammonia-water solution as a pH value conditioning agent into a mixed aqueous solution of the iron source and the phosphorus source, stirring and reacting and ageing to generate high-density olive-shaped crystalline compound NH4Fe2(OH)(PO4)2.2H2O containing ammonium, hydroxide and crystal water; and carrying out solid-liquid separation, roasting and decomposing to prepare the battery-grade ferric phosphate. The battery-grade ferric phosphate is an ideal raw material for preparing the lithium ion batteries cathode material lithium iron phosphate. The preparation method is suitable for mass, economic, stable and reliable production of the high-quality high-density battery-grade ferric phosphate, has no discharge of waste water, has obvious advantages, and has practical value.

Description

technical field [0001] The invention belongs to the technical field of energy material preparation, and relates to a high-density olive-shaped battery-grade anhydrous iron phosphate and a preparation method thereof. The battery-grade iron phosphate is an ideal precursor for preparing lithium iron phosphate, a cathode material of a lithium ion battery. Background technique [0002] Lithium-ion batteries are a new generation of green high-energy batteries, which have many advantages such as high voltage, high energy density, good cycle performance, small self-discharge, no memory effect, and wide operating temperature range. They are widely used in mobile phones, notebook computers, and digital cameras. , camcorders, electronic instruments, etc., also have bright application prospects in UPS, electric tools, electric bicycles, electric vehicles, energy storage batteries and other fields. In recent years, the output of lithium-ion batteries has grown rapidly, and the applicatio...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCC01B25/26H01M4/5825Y02E60/10
Inventor 应皆荣陈韶峰王顺林沈震雷陈明锋沙金陈炼芦亚婷
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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