A kind of industrialized lithium iron phosphate manufacturing method and the lithium iron phosphate composite material thereof prepared

A lithium iron phosphate, iron phosphate technology, applied in the field of new energy battery materials, can solve the problems of a large amount of flushing water, poor product consistency, unstable performance, etc.

Active Publication Date: 2019-12-10
高延敏
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  • Abstract
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  • Application Information

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Problems solved by technology

However, lithium iron phosphate also has the following shortcomings: poor conductivity, low tap density, unstable performance, poor product consistency, and the preparation process is not environmentally friendly, easy to generate waste gas, requires a large amount of flushing water, and high energy consumption
Although at present, lithium iron phosphate has been in-depth research, and the performance has been greatly improved, but the nanometer control of lithium iron phosphate, electrical conductivity, tap density, grammage, and stability are still not very satisfactory. Therefore, the performance needs Further improve

Method used

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  • A kind of industrialized lithium iron phosphate manufacturing method and the lithium iron phosphate composite material thereof prepared
  • A kind of industrialized lithium iron phosphate manufacturing method and the lithium iron phosphate composite material thereof prepared
  • A kind of industrialized lithium iron phosphate manufacturing method and the lithium iron phosphate composite material thereof prepared

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preparation example Construction

[0044] A method for preparing lithium iron phosphate capable of industrialization on a large scale, the method comprising the following steps:

[0045] The step of aqueous solution preparation (abbreviation preparatory process): preparation contains the aqueous solution that concentration is 30wt% inorganic mixed acid and 10wt% contains organic acid, and inorganic mixed acid is preferably the mixture of phosphoric acid and sulfuric acid, more specifically 85wt% phosphoric acid and 98wt% concentrated sulfuric acid mixture, and the best mixing mass ratio is 10:1. More preferably, the characteristic of the organic acid described in the first reaction liquid is that it has a residual phosphorus rate of 0.1wt% or more; most preferably, the characteristic of the organic acid described in the first reaction liquid is that it also has a residual phosphorus rate of 0.1wt% % of residual carbon rate. In addition to the functions of coordinating and complexing with iron ions, controlling...

Embodiment 1

[0076] Preparation of Nano-iron Phosphate

[0077] Aqueous solution preparation process: prepare to contain the aqueous solution that concentration is 30wt% inorganic mixed acid and 10wt% containing organic acid, described mixed acid is the mixture of phosphoric acid and sulfuric acid, wherein is the mixture of 85wt% phosphoric acid and 98wt% concentrated sulfuric acid, the mass ratio of its mixing is 10:1.

[0078] Preparation of nanosheet iron phosphate

[0079] Put iron with a high-purity iron content greater than 99.8wt% into a polytetrafluoroethylene reaction tank filled with an acid solution of 30wt% inorganic mixed acid and 1wt% phytic acid, heat to 95°C, and fully react for 20 hours. At 3 o'clock, filter, demagnetize, and remove impurities to obtain a pure ferrous phosphate solution of 170g / L. Put 500L of the ferrous phosphate solution into the enamel oxidation kettle, and at the same time, add 50kg of the dissolved oxidant hydrogen peroxide into the oxidation kettle ...

Embodiment 2

[0084] Preparation of Nano-iron Phosphate

[0085] Aqueous solution preparation process: prepare to contain the aqueous solution that concentration is 30wt% inorganic mixed acid and 10wt% containing organic acid, described mixed acid is the mixture of phosphoric acid and sulfuric acid, wherein is the mixture of 85wt% phosphoric acid and 98wt% concentrated sulfuric acid, the mass ratio of its mixing is 10:1.

[0086] Preparation of Nano Spherical Iron Phosphate

[0087] Put iron with high-purity iron content greater than 99.8wt% into a reaction tank filled with 30wt% inorganic mixed acid and 5wt% phytic acid solution, heat to 90°C, fully react for 30 hours, pH = 3, filter, demagnetize, and remove impurities to obtain For ferrous phosphate solution, pour 400L of ferrous phosphate solution into the enamel oxidation kettle, and at the same time, add 58kg of hydrogen peroxide into the oxidation kettle within 15 minutes. After fully reacting, filter and wash to remove impurities, a...

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Abstract

The invention discloses an industrial lithium iron phosphate manufacturing method and a lithium iron phosphate composite material prepared thereby, the method comprises the following steps such as water solution preparing, ferrous phosphate preparing, iron phosphate preparing, lithium iron phosphate preparing and the like to obtain a lithium iron phosphate finished product, iron particles are intoa pre-prepared special mixed acid water solution to obtain a ferrous phosphate solution, and the ferrous phosphate solution is further subjected to oxidation, reaction, sintering and other steps to finally obtain the iron phosphate finished product; and the method is characterized in that in the reaction process, corresponding dispersing and nano particle control agents are added in the reactionprocess of each step, so that the morphology of each intermediate product is controlled, and the morphology and the performance of the final finished product are influenced. The lithium iron phosphatedisclosed by the invention has the advantages of high tap density, good filling property, high energy density per unit volume, low content of Fe < 3 + > phase, few impurities, improved charging and discharging cycle characteristics, environmentally-friendly process, no wastewater and waste gas, energy conservation and the like.

Description

technical field [0001] The invention belongs to the technical field of new energy battery materials, and in particular relates to an industrialized manufacturing method of lithium iron phosphate and the prepared lithium iron phosphate. Background technique [0002] Lithium iron phosphate electrode materials are mainly used in various lithium-ion batteries. AyMPO was first revealed by Japan's NTT in 1996 4 (A is an alkali metal, M is a combination of Co and Fe, for example: LiFeCoPO 4 ) Lithium battery anode material with olivine structure, in 1997, John.B.Goodenough and other research groups at Texas State University also reported LiFePO 4 The characteristics of reversibly moving in and out of lithium. The United States and Japan have simultaneously published the structure of olivine (LiMPO 4 ), making the material has received great attention, and caused extensive research and rapid development. Compared with traditional lithium-ion secondary battery cathode materials,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45H01M4/36H01M4/58H01M10/0525B82Y40/00
CPCB82Y40/00C01B25/45C01P2002/72C01P2004/03C01P2004/61C01P2004/62C01P2004/64C01P2006/12C01P2006/82H01M4/362H01M4/5825H01M10/0525H01M2004/021H01M2004/028Y02E60/10
Inventor 高延敏高一丹
Owner 高延敏
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