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Method for preparing battery-grade ferric phosphate through multistage reactions

A multi-stage reaction, iron phosphate technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high viscosity of iron phosphate products, incomplete utilization of raw materials, difficult washing, etc., to reduce viscosity and speed up. Washing speed, the effect of promoting complete reaction

Active Publication Date: 2017-10-24
CNSG ANHUI HONG SIFANG NEW ENERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the deficiencies of the prior art, the present invention provides a method for preparing battery-grade iron phosphate by a multi-stage reaction, which solves the problem of high viscosity of the iron phosphate product in the preparation process of the prior art, difficulty in washing, incomplete utilization of raw materials, and subsequent waste water Technical problems with a lot of waste residue

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Weigh industrial-grade ferric sulfate and diammonium hydrogen phosphate, dissolve them in deionized water, and prepare solution A and solution B with a concentration of 1.2mol / L. Add solution A and solution B simultaneously at 1:1.02, add sodium hydroxide at the same time, adjust the pH to 0.8, and the resulting precipitated suspension flows into container 2 continuously, according to the iron content in the suspension as a reference, according to the volume ratio of 1:1.2 and 1:3.5 Add solution B and hypochlorous acid simultaneously, and add neutralizing agent sodium hydroxide at the same time, adjust the reaction pH to 2, control the reaction temperature at 40°C, press filter the obtained precipitate suspension, and use 40-60°C Repeated washing with deionized water and pressure filtration until the pH of the discharged water is 4.5, and the obtained iron phosphate precipitate is dried to obtain anhydrous iron phosphate crystals

[0047]Compared with the original prepa...

Embodiment 2

[0049] Weigh industrial-grade ferric chloride and ammonium dihydrogen phosphate and dissolve them in deionized water to form solution A and solution B with a concentration of 1.4mol / L. Add solution A and solution B simultaneously at a ratio of 1:1.01, and add sodium hydroxide at the same time to adjust the pH to 1.0, and the resulting sediment suspension continuously flows into container 2, taking the iron content in the suspension as a reference, and according to the volume ratio of 1:1 Add ammonium dihydrogen phosphate and potassium permanganate synchronously with 1:3 respectively, and add neutralizing agent sodium hydroxide at the same time, the pH of the price adjustment reaction is 1.5, and the reaction temperature is controlled at 55°C. The obtained precipitate suspension is press-filtered and then used Repeated washing with deionized water at 40-60°C and pressure filtration until the pH of the discharged water is 4.5, and the obtained iron phosphate precipitate is dried ...

Embodiment 3

[0052] Weigh industrial-grade ferric nitrate and sodium dihydrogen phosphate and dissolve them in deionized water to form solution A and solution B with a concentration of 1.5mol / L. Add solution A and solution B simultaneously at a ratio of 1:1.02, and at the same time add neutralizing agent ammonium acetate to adjust the pH to 1.2, and the resulting precipitate suspension continuously flows into container 2, taking the iron content in the suspension as a reference, and according to the volume ratio of 1 : 1.5 and 1: 4 respectively add sodium dihydrogen phosphate and hydrogen peroxide synchronously, and add neutralizing agent ammonium acetate at the same time, the pH of the price adjustment reaction is 2, and the reaction temperature is controlled at 60°C. Repeated washing with deionized water at 60°C and pressure filtration until the pH of the discharged water is 4.5, and the obtained ferric phosphate precipitate is dried to obtain anhydrous ferric phosphate crystals.

[0053...

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PUM

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Abstract

The invention provides a method for preparing battery-grade ferric phosphate through multistage reactions, belonging to the field of preparation of battery materials. The method comprises the following steps: (1) preparing a ferric salt solution and a phosphorous salt solution with certain concentrations; (2) synchronously adding the ferric salt solution and the phosphorous salt solution into a stirring container 1 in proportion, controlling the pH value of a reaction and allowing a produced precipitate suspension to continuously flow into a container 2; (3) adding a phosphorus salt, an oxidizing agent and a neutralizer into the container 2 in proportion and controlling a pH value to obtain another precipitate suspension; (4) subjecting the obtained precipitate suspension to press filtration and washing so as to obtain a ferric phosphate precipitate; and (5) drying the ferric phosphate precipitate so as to obtain an anhydrous ferric phosphate crystal. The method provided by the invention overcomes the technical problems of great viscosity of a ferric phosphate product, difficulty in washing, incomplete utilization of raw materials and a great amount of waste residues in subsequent waste water in the prior art. The method for preparing ferric phosphate in the invention accelerates the washing speed of the ferric phosphate product, improves the utilization rate of raw materials and reduces the content of waste residues in waste water.

Description

technical field [0001] The invention relates to the field of battery material preparation, in particular to a method for preparing battery-grade iron phosphate by multistage reaction. Background technique [0002] Lithium iron phosphate (LiFePO 4 ) has rapidly developed into a positive electrode material for lithium ions due to its good charge-discharge efficiency and cycle stability. Due to its good stability, low loss on ignition rate, and easy control of the preparation process, iron phosphate is widely recognized in the industry as an ideal precursor for the synthesis of lithium iron phosphate. [0003] The production of iron phosphate in the prior art is to use trivalent or divalent iron salt as raw material, add phosphoric acid or phosphorus salt, adjust the pH to form iron phosphate precipitate, and then wash, precipitate and dry to obtain the finished iron phosphate product. [0004] However, in the prior art, in the iron phosphate production process, due to the hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
CPCC01B25/375C01P2006/82
Inventor 陈凯张景訾洪静程祥文陆剑波郝成婷吴雪芳单成龙张立鹏何健任开法王长平
Owner CNSG ANHUI HONG SIFANG NEW ENERGY TECH
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