Preparation method of amorphous iron phosphate

An iron phosphate and amorphous technology, applied in the field of preparation of amorphous iron phosphate, can solve the problems of poor electrochemical performance of lithium iron phosphate, poor batch stability and high cost, and achieve improved process reliability and product stability. , the effect of high product purity

Active Publication Date: 2012-10-24
徐源庆
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  • Abstract
  • Description
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Problems solved by technology

Batch production of iron phosphate is complicated, high cost, difficult to control the proportion of product components, poor batch stability, poor electrochemical performance of subsequent synthesis of lithium iron phosphate

Method used

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  • Preparation method of amorphous iron phosphate
  • Preparation method of amorphous iron phosphate

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Experimental program
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Embodiment 1

[0017] According to the stoichiometric ratio Fe:P=1:1.03, take ferric chloride and phosphoric acid to form Fe 3+ For a metal mixed solution with an ion concentration of 1.5 mol / L, prepare a 4 mol / L ammonia solution as a precipitant. First add deionized water to the reactor and adjust the pH to 1.8 with hydrochloric acid solution. The metal mixed solution was continuously fed into the 10L reactor at a flow rate of 300mL / h, and at the same time, the ammonia solution was added in parallel to control the pH=2.3 for reaction. The reaction process temperature was 50° C., and the stirring speed was 200 rpm. When the average particle size of ferric phosphate particles is D50=6-8μm and the particle size distribution is 3-20μm, adjust the flow rate of ammonia solution to control pH=3.0 and react for 30 minutes, then adjust the flow rate of metal mixed solution to restore pH=2.3 for continuous reaction. The obtained white suspension was filtered and washed, and the filter cake was drie...

Embodiment 2

[0019] According to the stoichiometric ratio Fe:P=1:1.03, take ferric chloride and phosphoric acid to form Fe 3+ For a metal mixed solution with an ion concentration of 1.5 mol / L, prepare a 4 mol / L ammonia solution as a precipitant. First add deionized water to the reactor and adjust the pH to 1.8 with hydrochloric acid solution, and the additive gelatin is added in an amount of 10mg / L. The metal mixed solution was continuously fed into the 10L reactor at a flow rate of 300mL / h, and at the same time, the ammonia solution was added in parallel to control the pH=2.3 for reaction. The reaction process temperature was 50° C., and the stirring speed was 360 rpm. When the average particle size of ferric phosphate particles is D50=6-8μm and the particle size distribution is 3-20μm, adjust the flow rate of ammonia solution to control pH=3.0 and react for 30 minutes, then adjust the flow rate of metal mixed solution to restore pH=2.3 for continuous reaction. The obtained white suspen...

Embodiment 3

[0021] According to the stoichiometric ratio Fe:P=1:1.03, take ferric chloride and phosphoric acid to form Fe 3+ For a metal mixed solution with an ion concentration of 1.5 mol / L, prepare a 4 mol / L ammonia solution as a precipitant. First add deionized water to the reactor and adjust the pH to 1.8 with hydrochloric acid solution, and the additive gelatin is added in an amount of 10mg / L. The metal mixed solution was continuously fed into the 10L reactor at a flow rate of 300mL / h, and at the same time, the ammonia solution was added in parallel to control the pH=2.3 for reaction. The reaction process temperature was 50° C., and the stirring speed was 200 rpm. When the average particle size of iron phosphate particles is D50=6-8μm and the particle size distribution is 3-20μm, adjust the flow rate of ammonia solution to control pH=3.0 and react for 120 minutes, then adjust the flow rate of metal mixed solution to restore pH=2.3 for continuous reaction. The obtained white suspens...

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Abstract

A preparation method of amorphous iron phosphate is disclosed. According to the method, phosphoric acid or a phosphate is adopted as a phosphorus source, an iron salt or a ferrous salt is adopted as an iron source, and ammonia water is adopted as a precipitating agent; the phosphorus source and the iron source are weighed according to a stoichiometric ratio and are added with deionized water to prepare a mixed metal solution; the mixed metal solution and the ammonia water are respectively continuously added to a stirred reactor with the flow being 200-600mL / h, and a chemical reaction for precipitating the iron phosphate is continuously carried out under conditions comprising a reaction temperature being 40-80DEG C and a reaction pH value being 1.8-3.5; and an overflow slurry of the reactor is filtered, washed and dried to obtain the powdery amorphous iron phosphate. The crystal form of the prepared iron phosphate is amorphous, the average particle size D50 of the prepared iron phosphate is 7-15mum, and the tap density of the prepared iron phosphate is equal to or greater than 0.95g / cm<3>.

Description

technical field [0001] The invention relates to the preparation technology of amorphous iron phosphate. Background technique [0002] Iron phosphate is a widely used chemical raw material, which can be used as a food thickener and iron supplement, and can also be used as a pigment, ceramic metal glaze color glaze. In recent years, iron phosphate has been widely researched and applied as a high-quality raw material for the production of lithium iron phosphate, a cathode material for lithium-ion batteries. [0003] The traditional industrial production method of ferric phosphate is made by reacting phosphoric acid and ferric chloride in a closed container at 180-190°C for 2-3 hours; another method is to add phosphoric acid to ferrous salt in the presence of an oxidizing agent. . In addition, the Chinese patent (publication number CN101172594) discloses a method for preparing iron phosphate for the preparation of lithium iron phosphate materials. It is an anionic surfactant ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 朱福良
Owner 徐源庆
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