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Preparation method of nano spherical ferric phosphate as well as nano ferric phosphate prepared by the method, lithium ferric phosphate and lithium battery

A technology of lithium iron phosphate and iron phosphate, which is applied in the field of new energy material preparation, can solve the problems of complex components, affecting production efficiency, and long time consumption, and achieve the effects of mild synthesis conditions, controllable particle size, and excellent electrical properties

Active Publication Date: 2017-12-29
YOSHIHIRO COMM EQUIP GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the obtained industrialization results, the post-treatment of nano-scale spherical iron phosphate obtained by phosphoric acid has a good effect by controlling the pH and aging, but the outstanding defect of this method is that it takes a long time and takes 2-3 days. time, affecting productivity
For example, the patent application number 201080011745.8 uses phosphoric acid and citric acid to control together. This method is not only time-consuming and affects production efficiency, but also because phosphoric acid is prone to have multi-level anions, such as: dihydrogen phosphate, monophosphate A variety of anions such as hydrogen radicals and phosphate radicals lead to complex components. During the precipitation process, oxides, hydroxide compounds, and precipitates of different grades of phosphate radicals will be included. These inclusions will affect the quality of iron phosphate and lead to the preparation of lithium iron phosphate materials. The purity is affected, which in turn affects the performance of the cathode material lithium iron phosphate

Method used

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  • Preparation method of nano spherical ferric phosphate as well as nano ferric phosphate prepared by the method, lithium ferric phosphate and lithium battery
  • Preparation method of nano spherical ferric phosphate as well as nano ferric phosphate prepared by the method, lithium ferric phosphate and lithium battery
  • Preparation method of nano spherical ferric phosphate as well as nano ferric phosphate prepared by the method, lithium ferric phosphate and lithium battery

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preparation example Construction

[0043] A kind of FePO containing general formula 4 ·nH 2 The preparation method of the nano-spherical ferric phosphate of O (n≤2.5), described nano-spherical ferric phosphate refers to that particle is spherical or quasi-spherical, particle size is in 1-300nm ferric phosphate particle; Described method comprises the following steps:

[0044] 1) mix : drop the mixed solution of the phosphorus source compound solution and the oxidizing agent solution in the soluble ferrous compound solution, the dropping speed is 1d / min, add the nano-spherical control agent and stir and mix at the same time;

[0045] The ferrous compound is at least one of ferrous sulfate, ferrous sulfite, ferrous chloride, ferric nitrate and ferrous dihydrogen phosphate;

[0046] The phosphorus source compound is at least one of phosphoric acid, ammonium monohydrogen phosphate, ammonium dihydrogen phosphate and ammonium phosphate;

[0047] Described oxidizing agent is hydrogen peroxide and / or ammonium persul...

specific Embodiment

[0062] How to measure electrical conductivity

[0063] The method for measuring the electrical conductivity is that firstly the mold is pressed into a solid body through the obtained ferric phosphate, the diameter of the molded body is 12 mm, the thickness of the molded body is about 3 mm, and the final thickness is measured by a micron thread gauge. The multifunctional measuring device of the voltage source is a digital multimeter (M4660), which measures the electrode voltage and the resistance through the test body.

Embodiment 1

[0065] In the solution containing 1 mole of ferrous sulfate, drop the mixed solution of ammonium phosphate solution and hydrogen peroxide solution; the mixed solution contains 1 mole of ammonium phosphate solution, and the quality of hydrogen peroxide is 30% of the theoretical output of ferric phosphate, and the dropping speed is 1d / min, add nano-spherical control agent (1) simultaneously and mix, stir, stirring speed is 300 revs / min, and the control agent add-on is 10wt% of the ferric phosphate theoretical output; The chemical equation of reaction is:

[0066] FeSO 4 +NH 4 h 2 PO 4 +H 2 O+ control agent (1)------FePO 4 (Spherical Nano Iron Phosphate)

[0067] The nano-spherical control agent (1) is:

[0068]

[0069] Under reflux condition, in the reactor of 500ml, react for 8 hours, reaction temperature is 60 ℃, adopt high magnetic filter to filter then, remove magnetic substance (iron oxide and iron hydroxide), then press filter, press filter The obtained ferric ...

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Abstract

The invention discloses a preparation method of nano spherical ferric phosphate as well as nano ferric phosphate prepared by the method, lithium ferric phosphate and a lithium battery. The method comprises the following steps: mixing: dropwise adding a mixed solution consisting of a phosphorus source compound solution and an oxidant solution into a soluble ferrous compound solution, adding a nano spherical control agent, and stirring and mixing; reacting: stirring at 50 to 100 DEG C under a refluxing condition, and reacting for 5 to 10 h; filtering: magnetically filtering the mixed solution after the reaction by adopting a high magnetic filter, press filtering the filtered solution, and obtaining a ferric phosphate crude product; and calcining: calcining for 24h at 650 to 850 DEG C under the protection of inert gas, and cooling to obtain a final ferric phosphate product. By adopting the method, the morphology of the ferric phosphate product can be controlled, and the performance of the lithium ferric phosphate can be improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of new energy materials, in particular to a method for LiFePO 4 The preparation method of the nano-spherical iron phosphate of the prepared precursor raw material and the nano-iron phosphate, lithium iron phosphate and lithium battery prepared by the method. Background technique [0002] Lithium (sub)iron phosphate is an important cathode material for lithium batteries. It has a voltage of 3.5V and a theoretical capacity of 170mAh / g. Compared with lithium cobalt batteries, it is not only temperature resistant, but also has higher safety. Inexpensive lithium iron phosphate (LiFePO 4 ) compounds are attracting attention as positive electrode active materials for lithium secondary batteries. With the development of electric vehicles, the research on their preparation technology and morphology control methods has been developed rapidly. Among many materials for the preparation of lithium iron ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37C01B25/45H01M4/58H01M10/052B82Y40/00
CPCC01B25/375C01B25/45C01P2002/72C01P2004/03C01P2004/32C01P2004/62C01P2004/64C01P2006/40H01M4/5825H01M10/052H01M2220/20Y02E60/10
Inventor 高延敏
Owner YOSHIHIRO COMM EQUIP GRP CO LTD
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