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Iron phosphate precursor as well as preparation method and application thereof

An iron phosphate and precursor technology, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of low tap density of iron phosphate precursors, difficult crushing procedures, and reduced production efficiency, etc. The effect of low cost, good processing performance and high production efficiency

Inactive Publication Date: 2021-08-13
GUANGDONG BRUNP RECYCLING TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the tap density of the current iron phosphate precursors is not high, generally not exceeding 1.0g / cm 3
In addition, the specific surface area of ​​the current iron phosphate precursor is relatively high, usually 50m 2 / g or so, in order to reduce the specific surface area, most iron phosphate manufacturers use high temperature above 800°C and prolong the sintering time to melt the iron phosphate, so that the specific surface area of ​​anhydrous iron phosphate is 1.5-3m 2 / g, to reduce the internal pores of iron phosphate, but this process leads to increased energy consumption, and at the same time, the material will be sintered and agglomerated seriously, and the subsequent crushing process is difficult, which greatly reduces the production efficiency of the enterprise.

Method used

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  • Iron phosphate precursor as well as preparation method and application thereof
  • Iron phosphate precursor as well as preparation method and application thereof
  • Iron phosphate precursor as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0040] The preparation method of the iron phosphate precursor of the present embodiment comprises the following steps:

[0041] S1. Select ferric nitrate and phosphoric acid as the iron source and phosphorus source respectively. According to the molar ratio of iron in the iron source and phosphorus in phosphoric acid as 0.965:1, add phosphoric acid to ferric nitrate, adjust the pH to 0 with sulfuric acid, and configure Fe 3+ Liquid metal with a concentration of 50g / L;

[0042] S2. Add 50L of molten metal into the reaction kettle, raise the temperature to 90°C at 400r / min, and react for 10h to obtain a slurry;

[0043] S3, filtering the slurry to obtain a filter residue, and then repeatedly washing the filter residue 3 times with pure water to obtain a washed filter residue;

[0044] S4. Dry the obtained filter residue at 100°C. The drying process needs to be turned several times to obtain the iron phosphate dihydrate precursor.

[0045] The physicochemical result of embodime...

Embodiment 2

[0049] The preparation method of the iron phosphate precursor of the present embodiment comprises the following steps:

[0050] S1. Select ferric nitrate and phosphoric acid as the iron source and phosphorus source respectively. According to the molar ratio of iron in the iron source and phosphorus in phosphoric acid as 0.965:1, add phosphoric acid to ferric nitrate, adjust the pH to 0 with sulfuric acid, and configure Fe 3+ Liquid metal with a concentration of 50g / L;

[0051] S2. Add 50L of molten metal into the reaction kettle, raise the temperature to 85°C at 400r / min, and react for 15h to obtain a slurry;

[0052] S3, filtering the slurry to obtain a filter residue, and then repeatedly washing the filter residue 3 times with pure water to obtain a washed filter residue;

[0053] S4. Dry the obtained filter residue at 100°C. The drying process needs to be turned several times to obtain the iron phosphate dihydrate precursor.

Embodiment 3

[0055] The preparation method of the iron phosphate precursor of the present embodiment comprises the following steps:

[0056]S1. Select ferrous sulfate and phosphoric acid as the iron source and phosphorus source respectively. According to the molar ratio of iron and phosphoric acid elements of 0.97:1, add phosphoric acid to ferric nitrate and hydrogen peroxide, adjust the pH to 0.5 with sulfuric acid, and configure Fe 3+ Liquid metal with a concentration of 56g / L;

[0057] S2. Add 50L of molten metal into the reaction kettle, raise the temperature to 90°C at 400r / min, and react for 12h to obtain a slurry;

[0058] S3, filtering the slurry to obtain a filter residue, and then repeatedly washing the filter residue 3 times with pure water to obtain a washed filter residue;

[0059] S4. Dry the obtained filter residue at 100°C. The drying process needs to be turned several times to obtain the iron phosphate dihydrate precursor.

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Abstract

The invention belongs to the field of lithium ion battery materials, and discloses an iron phosphate precursor and a preparation method and application thereof. The microstructure of the iron phosphate precursor is spherical, the particle size D50 is 10-20 [mu] m, the specific surface area is 1-3 m < 2 > / g, and the tap density is 1-1.5 g / cm < 3 >. According to the method, ferric iron is selected as an iron source, then phosphoric acid is added into a ferric iron solution, and the morphology and the particle size distribution of primary particles of ferric phosphate are controlled by controlling the pH and the reaction temperature. The initial pH of the system is very low by adding phosphoric acid into ferric iron salt. Then, the reaction temperature is controlled to be 70-100 DEG C. Spherical dense primary particles can be formed and stacked, iron phosphate dehydrate with low specific surface area and no internal gap can be obtained after the primary particles are dried, and the tap density of the iron phosphate dehydrate is high and can reach 1-1.5 / cm < 3 >.

Description

technical field [0001] The invention belongs to the field of lithium ion battery materials, and in particular relates to an iron phosphate precursor and a preparation method and application thereof. Background technique [0002] With the hot market of new energy vehicles, lithium iron phosphate occupies a large part in the battery supporting of new energy special vehicles (including new energy logistics vehicles, new energy sanitation vehicles, and other new energy special vehicles) due to its high safety. Proportion. Lithium iron phosphate has the advantages of good safety performance, long cycle life, environmental protection and safety, low manufacturing cost, and high energy density, especially good safety performance. The electrochemical performance of the cathode material of lithium iron phosphate battery is relatively stable. During the charging and discharging process, the structure of the battery is not easy to change, and combustion and explosion rarely occur. Eve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37H01M4/58H01M10/0525
CPCC01B25/375H01M4/5825H01M10/0525C01P2004/61C01P2004/32C01P2006/11C01P2006/12Y02E60/10H01M4/58
Inventor 李玲李长东阮丁山唐盛贺秦存鹏殷磊
Owner GUANGDONG BRUNP RECYCLING TECH
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