Preparation method of iron manganese phosphate

A technology of ferromanganese phosphate and ferromanganese, which is applied in the field of lithium battery new energy materials, can solve the problems of high iron hydroxide content, low phosphorus content, and low purity, and achieve low iron hydroxide content, sulfate radical and chloride ion content The effect of low, uniform particle size distribution

Active Publication Date: 2018-07-20
蒋央芳
View PDF7 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The precursor of lithium manganese iron phosphate is generally ferromanganese phosphate, but the conventional preparation process, such as the coprecipitation reaction of phosphate and ferrous salt, manganese salt and oxidant, has the following problems: due to the low pH of ferric phosphate precipitation, and The pH of manganese phosphate precipitation is higher, and at higher pH, ferrous salt reacts with oxidant to get ferric hydroxide, resulting in high content of ferric hydroxide, low purity and low phosphorus content

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of iron manganese phosphate
  • Preparation method of iron manganese phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of ferromanganese phosphate, which comprises the following steps:

[0034] (1) prepare bottom liquid, bottom liquid is ammonium bicarbonate solution, and the pH of bottom liquid is 7.08, and manganese sulfate and ammonium ferrous sulfate are made into solution, then mix to obtain ferromanganese mixed solution, prepare ammonium bicarbonate solution, then Add ferromanganese mixed solution and ammonium bicarbonate solution to the bottom solution under stirring, maintain the pH of the process at 7.08, the temperature at 53.5°C, the stirring speed at 220r / min, the total adding time is 145min, and the first 30 minutes of feeding The speed is 1.25 times of the subsequent feeding speed. After the feeding is completed, continue to stir and react for 80 minutes, then raise the temperature to 72.5°C, add ammonia water to adjust the pH of the solution to 7.75, and continue to react for 25 minutes to obtain carbonate slurry;

[0035] (2) The carbonate slurry obt...

Embodiment 2

[0046] A preparation method of ferromanganese phosphate, which comprises the following steps:

[0047] (1) prepare bottom liquid, bottom liquid is ammonium bicarbonate solution, and the pH of bottom liquid is 7.11, and manganese sulfate and ferrous ammonium sulfate are made into solution, mixes then and obtains ferromanganese mixed solution, prepares ammonium bicarbonate solution, and then Add ferromanganese mixed solution and ammonium bicarbonate solution to the bottom solution under stirring, maintain the pH of the process at 7.11, the temperature at 51°C, the stirring speed at 240r / min, the total adding time is 130min, and the first 30 minutes of feeding The speed is 1.45 times of the subsequent feeding speed. After the feeding is completed, continue to stir and react for 80 minutes, then raise the temperature to 73.5°C, add ammonia water to adjust the pH of the solution to 7.75, and continue to react for 18 minutes to obtain carbonate slurry;

[0048] (2) The carbonate slu...

Embodiment 3

[0060] A preparation method of ferromanganese phosphate, which comprises the following steps:

[0061] (1) prepare bottom liquid, bottom liquid is ammonium bicarbonate solution, and the pH of bottom liquid is 7.11, and manganese sulfate and ferrous ammonium sulfate are made into solution, mixes then and obtains ferromanganese mixed solution, prepares ammonium bicarbonate solution, and then Add ferromanganese mixed solution and ammonium bicarbonate solution to the bottom solution under stirring, maintain the pH of the process at 7.11, the temperature at 53.5°C, the stirring speed at 240r / min, the total addition time is 140min, and the first 30 minutes of feeding The speed is 1.35 times of the subsequent feeding speed. After the feeding is completed, continue to stir and react for 80 minutes, then raise the temperature to 72°C, add ammonia water to adjust the pH of the solution to 7.72, and continue to react for 20 minutes to obtain carbonate slurry;

[0062] (2) The carbonate s...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
magnetic flux densityaaaaaaaaaa
magnetic flux densityaaaaaaaaaa
Login to view more

Abstract

The invention discloses a preparation method of iron manganese phosphate. The preparation method comprises the steps of preparing a base solution, and adding a ferromanganese mixed solution and an ammonium hydrogen carbonate solution to the base solution in a stirring condition, and after adding is completed, continuously performing a stirring reaction to obtain carbonate paste; performing solid liquid separation on the carbonate paste, washing the filtering residue by hot pure water, and then adding the product into the pure water to be subjected to slurrying, and next, adding a phosphoric acid solution and hydrogen peroxide into the slurry material at the unfirm speed synchronously, and next, performing heating to obtain iron manganese phosphate paste; performing solid liquid separationon the iron manganese phosphate paste, washing the filtering residue by hot pure water, and then performing vacuum drying, screening and iron removing to obtain iron manganese phosphate; and adding iron manganese phosphate into a mixed solution of anhydrous alcohol and butyl titanate, performing grinding, and next carrying out spray drying on the paste to obtain titanium-coated iron manganese phosphate. The titanium-coated iron manganese phosphate material obtained in the invention has small grain diameter, high tap density, small specific surface, and uniform grain diameter distribution, without causing a ferromanganese segregation phenomenon.

Description

technical field [0001] The invention relates to a preparation method of ferromanganese phosphate, which belongs to the field of lithium battery new energy materials. Background technique [0002] LiMnPO4 (LMP) has the advantages of cheap raw materials, relatively stable structure, high theoretical specific capacity and high discharge voltage platform, and is one of the positive electrode materials for lithium-ion power batteries with great development prospects. However, LMP materials have defects such as low electronic conductivity and ionic conductivity, which limit their large-scale application. Doping Fe in LMP can improve the kinetic performance of the material during charge and discharge. In recent years, methods such as nano-composite carbon coating have been used to greatly improve the electrochemical performance of iron-doped lithium manganese phosphate (LFMP) materials. The latest report shows that PHOSTCH also has the ability to mass produce LFMP, and LFMP materi...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525C01B25/45
CPCC01B25/45C01P2004/32C01P2004/62C01P2004/64C01P2004/80C01P2006/11C01P2006/12C01P2006/80H01M4/366H01M4/5825H01M4/62H01M10/0525Y02E60/10
Inventor 蒋央芳
Owner 蒋央芳
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products