Preparation method of anhydrous ferric pyrophosphate

A technology of ferric orthophosphate and phosphoric acid, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as low purity of ferric phosphate, complex preparation process, and difficult component control, achieving remarkable technological progress and production process Simple, pure effect

Inactive Publication Date: 2017-06-09
SHANGHAI INSTITUTE OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the above-mentioned technical problems in the prior art, the present invention provides a method for preparing anhydrous ferric orthophosphate, and the method for preparing anhydrous ferric orthophosphate should solve the problem of preparing ferric phosphate materials in the prior art The

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  • Preparation method of anhydrous ferric pyrophosphate
  • Preparation method of anhydrous ferric pyrophosphate
  • Preparation method of anhydrous ferric pyrophosphate

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Experimental program
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Embodiment 1

[0053] Anhydrous ferric orthophosphate (FePO 4 ) preparation method, specifically comprises the following steps:

[0054] (1) The phosphoric acid of 110 weight parts is added into the deionized water of 300 weight parts to be mixed with phosphoric acid solution, control solution temperature 50 o c. Add 56 parts by weight of 300-mesh reduced iron powder under stirring, and react for 3 hours to obtain a precursor solution containing a phosphorus source and an iron source;

[0055] (2) Add the precursor solution obtained in step (1) into a nano sand mill, and ball mill for 2 hours to obtain a suspension with a D50 of 321 nm in the particle size distribution. The obtained ball mill suspension was spray-dried at 170° C. to obtain spherical precursor powder.

[0056] (3) Finally, after calcining the obtained spherical precursor powder in an air atmosphere at 600° C. for 8 hours, the anhydrous iron orthophosphate powder material is obtained.

[0057]The anhydrous ferric orthophos...

Embodiment 2

[0061] Anhydrous ferric orthophosphate (FePO 4 ) preparation method, specifically comprises the following steps:

[0062] (1) Add 115 parts by weight of phosphoric acid into 300 parts by weight of deionized water to prepare a phosphoric acid solution, and control the temperature of the solution to 65 o c. Add 56 parts by weight of 300-mesh reduced iron powder under stirring, and react for 3 hours to obtain a precursor solution containing a phosphorus source and an iron source;

[0063] (2) Add the precursor solution obtained in step (1) into a nano sand mill, and ball mill for 2 hours to obtain a suspension with a D50 of 258nm in the particle size distribution. The obtained ball mill suspension was spray-dried at 170° C. to obtain spherical precursor powder.

[0064] (3) Finally, after calcining the obtained spherical precursor powder in an air atmosphere at 700° C. for 8 hours, the anhydrous iron orthophosphate powder material is obtained.

[0065] The anhydrous ferric or...

Embodiment 3

[0069] Anhydrous ferric orthophosphate (FePO 4 ) preparation method, specifically comprises the following steps:

[0070] (1) The phosphoric acid of 120 weight parts is added into the deionized water of 300 weight parts and is mixed with phosphoric acid solution, controls solution temperature 80 o c. Add 56 parts by weight of 300-mesh reduced iron powder under stirring, and react for 3 hours to obtain a precursor solution containing a phosphorus source and an iron source;

[0071] (2) Add the precursor solution obtained in step (1) into a nano sand mill, and ball mill for 2 hours to obtain a suspension with a D50 of 217nm in the particle size distribution. The obtained ball mill suspension was spray-dried at 170° C. to obtain spherical precursor powder.

[0072] (3) Finally, after calcining the obtained spherical precursor powder in an air atmosphere at 800° C. for 8 hours, the anhydrous iron orthophosphate powder material is obtained.

[0073] The anhydrous iron orthophos...

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Abstract

The invention discloses a preparation method of anhydrous ferric pyrophosphate, wherein the method includes steps of adding 110-120 parts by weight of phosphoric acid in 300 parts by weight of de-ionized water and preparing to be phosphoric acid solution; controlling the solution temperature at 50-80 DEG C, and adding 56 parts by weight of 300 meshes-100 meshes of reduced iron powder under the stirring state and reacting for 3 hours, and then adding the acquired precursor liquid in a nanoscale sand grinding machine; performing ball milling for 2 hours and acquiring turbid liquid of which grain diameter distribution D5 is 200-400 nm; spraying and drying the acquired ball mill turbid liquid at 170 DEG C, and acquiring a spherical precursor powder body; at last, calcining the acquired spherical precursor powder body in the air at 600-800 DEG C for 8 hours, and then acquiring the anhydrous ferric pyrophosphate material. As the raw material for producing the lithium iron phosphate material, the calcining process is not existed with the dewatering process of recrystallization water, thereby overcoming the shortcoming that water and carbon are formed to be water gas and the carbon content in the product is reduced; therefore, the anhydrous ferric pyrophosphate is an ideal raw material for producing lithium iron phosphate in the industry.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to an iron phosphate, in particular to a preparation method of anhydrous iron orthophosphate. Background technique [0002] As the upstream of the new energy vehicle industry chain, the lithium battery industry has gradually entered a stage of rapid development. Among them, the cost of power lithium batteries accounts for a relatively high proportion of the cost of new energy vehicles, close to 40%. Lithium iron phosphate batteries are relatively safe, and the cost has also dropped significantly in recent years. Considering the maturity and economy of battery technology, the current power batteries for electric vehicles are mainly lithium iron phosphate batteries. [0003] Iron phosphate has a stable structure and has a similar crystal structure and unit cell parameters to lithium iron phosphate. As a precursor for the synthesis of lithium iron phosphate, it can effectively control th...

Claims

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Application Information

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IPC IPC(8): C01B25/37
CPCC01B25/375C01P2002/72C01P2004/03C01P2004/32C01P2004/52C01P2004/61
Inventor 常程康陈雪平肖鹏关利吕庭键
Owner SHANGHAI INSTITUTE OF TECHNOLOGY
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