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A method for preparing battery-grade iron phosphate from industrial iron-containing waste

An iron phosphate, battery-level technology, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problems of inconvenient residual carbon content and high cost of ferrous oxalate, achieve excellent electrochemical performance, improve commercial value, and maintain consistency sexual effect

Active Publication Date: 2017-05-03
湖北高博科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Use ferrous oxalate (or ferric oxide) as iron source, phosphoric acid (or ammonium phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate) has been widely used as the technical route of phosphorus source, but the iron source of this technical route and The phosphorus source comes from two different raw materials, especially the cost of using ferrous oxalate is relatively high, and using it as an iron source will easily bring inconvenience to the control of residual carbon content in the product

Method used

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  • A method for preparing battery-grade iron phosphate from industrial iron-containing waste
  • A method for preparing battery-grade iron phosphate from industrial iron-containing waste
  • A method for preparing battery-grade iron phosphate from industrial iron-containing waste

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Embodiment 1

[0032] Take 500mL of iron-containing waste acid, filter it, add 20g of waste iron slag to the obtained solution, and react at 30°C for 48h until the solution pH=5. Subsequently, the above solution was filtered twice to obtain a green clear solution; under stirring conditions, 80 mL of hydrogen peroxide and 100 mL of phosphoric acid were added to the above clear solution for 18 hours of reaction. Finally, when the water bath is heated to 92°C, add 110mL of phosphoric acid and 250mL of sodium hydroxide solution, and react for 5 hours to form a yellow suspension; filter and wash to pH = 6 and dry at 100°C for 10 hours to obtain ferric phosphate dihydrate (FePO 4 2H 2 O) Samples.

[0033] Accurately weigh Li 2 CO 3 、FePO 4 2H 2 O (Example 1) and glucose were ball milled in absolute ethanol medium for 12 hours, mixed evenly, transferred to an oven at 50°C for about 12 hours, and after drying, they were sintered in a tube furnace under a nitrogen atmosphere and sieved to obtain...

Embodiment 2

[0035]Take 500mL of iron-containing waste acid, filter it, add 20g of waste iron slag to the obtained solution, and react at 30°C for 48h until the solution pH=5. Subsequently, the above solution was filtered twice to obtain a green clear solution; under stirring conditions, 80 mL of hydrogen peroxide and 100 mL of phosphoric acid were added to the above clear solution for 18 hours of reaction. Finally, when the water bath is heated to 87°C, add 110mL of phosphoric acid and 250mL of sodium hydroxide solution, and react for 5 hours to form a yellow suspension; filter and wash to pH=6 and dry at 100°C for 10 hours to obtain ferric phosphate dihydrate (FePO 4 2H 2 O) Samples.

Embodiment 3

[0037] Take 500mL of iron-containing waste acid, filter it, add 20g of waste iron slag to the obtained solution, and react at 30°C for 48h until the solution pH=5. Subsequently, the above solution was filtered twice to obtain a green clear solution; under stirring conditions, 80 mL of hydrogen peroxide and 100 mL of phosphoric acid were added to the above clear solution for 18 hours of reaction. Finally, when the water bath is heated to 92°C, add 80g of ammonium dihydrogen phosphate and 250mL of sodium hydroxide solution, and react for 5 hours to form a yellow suspension; filter and wash to pH = 6 and dry at 100°C for 10 hours to obtain phosphoric acid dihydrate Iron (FePO 4 2H 2 O) Samples.

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Abstract

The invention provides a method for preparing battery-grade FePO4 from industrial iron-containing waste. The method comprises steps as follows: iron-containing waste acid is taken and filtered, and waste iron residues are added to a filtrate and react at 30-35 DEG C for 24-48 h until the pH of a solution is 5-6; the solution is filtered 1-3 times, a green settled solution is obtained, hydrogen peroxide and a phosphorous source are added under the stirring condition, and the solution is subjected to a reaction for 12-18 h; the solution is heated to 85-95 DEG C in a water bath, the phosphorus source and a sodium hydroxide solution are added, the solution is subjected to a reaction for 3-6 h, and a yellow suspension is produced; the yellow suspension is filtered, washed and dried, and battery-grade FePO4, namely, FePO4*2H2O, is obtained and is in a regular sheet shape. The FePO4 is synthesized at the low temperature; no impurities are produced during synthesis, and pure-phase FePO4*2H2O can be obtained. The prepared FePO4*2H2O has stable properties, and all indexes meet the requirement of battery-grade FePO4.

Description

technical field [0001] The invention relates to a battery-grade iron phosphate dihydrate and a preparation method thereof. The battery-grade iron phosphate is an ideal raw material for preparing lithium iron phosphate, a cathode material of a lithium ion battery, and belongs to the technical field of energy material preparation. Background technique [0002] Energy is the basis for the existence of human society and the source of all development. With the advancement of science and technology, human beings are increasingly dependent on energy. Coal, oil, and natural gas have been developed and used as energy. These non-renewable energy sources are the development of the earth. Generated during evolution, the cycle is long, and human predatory development makes these non-renewable energy sources gradually exhausted. Although wind energy and solar energy are inexhaustible new renewable energy sources, these energy sources are largely affected by the natural environment and are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37H01M4/58
CPCC01B25/375C01P2002/72C01P2004/03H01M4/5805Y02E60/10
Inventor 张露露孙华斌杨学林徐风李振周英贤丁晓凯
Owner 湖北高博科技有限公司