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Spherical basic ammonium ferric phosphate powder with large specific surface area and preparation method thereof

A high specific surface area, ammonium iron phosphate technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of low tap density of lithium iron phosphate products, affecting the electrochemical performance of batteries, and lengthening ion diffusion paths. , to achieve the effect of short ion diffusion path, avoid wide particle distribution and simple process route

Inactive Publication Date: 2012-11-07
DALIAN MARITIME UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, if the particle size of the raw material is too large, the specific surface area of ​​the particle will be small, thereby reducing the effective reaction area, and lengthening the ion diffusion path, making the solid-state reaction difficult
On the other hand, if the particle size of the raw material is too small, the tap density of the raw material is generally low, so that the tap density of the finally obtained lithium iron phosphate product is relatively low, which ultimately affects the electrochemical performance of the battery.
[0006] At present, there is still a lack of research and reports on the morphology control technology of iron phosphate raw materials and the influence of raw material morphology on the performance of the reaction product lithium iron phosphate

Method used

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  • Spherical basic ammonium ferric phosphate powder with large specific surface area and preparation method thereof
  • Spherical basic ammonium ferric phosphate powder with large specific surface area and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Solution preparation: Prepare 1mol / L ferric citrate aqueous solution and ammonium dihydrogen phosphate aqueous solution respectively.

[0023] With above-mentioned two kinds of solutions according to molar ratio Fe:P=1:1.5, join in the reaction container under stirring respectively at the same time, reaction temperature is controlled at 50-60 ℃, after dropping, adjust with ammonia water (concentration is 20%) The pH value is adjusted until the pH value is 4 to obtain an amorphous basic ammonium ferric phosphate slurry.

[0024] The slurry is aged in the reaction liquid, and the aging temperature is controlled at 70-90°C. After aging for 10 hours, filter the slurry, wash the filter cake with deionized water, and then filter until the filtrate is neutral. Dry the filter cake in a blast drying oven at 80°C for 6-8 hours to obtain basic ammonium ferric phosphate particles. The specific surface area of ​​the particles reaches 97m 2 / g, pass the SEM test (such as figure 2...

Embodiment 2

[0027] Solution preparation: Prepare 2mol / L ferric nitrate aqueous solution and ammonium phosphate aqueous solution respectively.

[0028] With above-mentioned two kinds of solutions according to molar ratio Fe:P=1:1.6, join in the reaction vessel under stirring respectively at the same time, reaction temperature is controlled at 60-80 ℃, after dropping, adjust with ammonia water (concentration is 20%) pH value, until the pH value is 1, to obtain amorphous basic iron ammonium phosphate slurry.

[0029] The slurry is aged in the reaction liquid, and the aging temperature is controlled at 60-80°C. After aging for 12 hours, filter the slurry, wash the filter cake with deionized water, and then filter until the filtrate is neutral. Dry the filter cake in a blast drying oven at 80°C for 12 hours to obtain basic ferric ammonium phosphate. Particle specific surface area reaches 88m 2 / g, as can be seen from the SEM results, the product is a spherical petal-like particle (result and...

Embodiment 3

[0032] Solution preparation: Dissolve ferric nitrate and ferric citrate in water to prepare an iron-based mixed solution with an iron concentration of 1mol / L. Dilute the phosphoric acid solution with deionized water to prepare a phosphoric acid solution with a concentration of 1mol / L. Adjust the pH value of the phosphoric acid solution to 5-7 with ammonia water (concentration: 25%).

[0033] The above two solutions are added to the reaction vessel under stirring at the same time according to the molar ratio Fe:P=1:1.3, and the reaction temperature is controlled at 60-80°C. pH value, until the pH value is 2, to obtain amorphous basic ammonium ferric phosphate slurry.

[0034] The slurry is aged in the reaction liquid, and the aging temperature is controlled at 60-80°C. After aging for 12 hours, filter the slurry, wash the filter cake with deionized water, and then filter until the filtrate is neutral. Dry the filter cake in a blast drying oven at 80°C for 12 hours to obtain b...

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Abstract

The invention discloses spherical basic ammonium ferric phosphate powder with a large specific surface area and a preparation method. The method comprises the following steps of: dripping 1 to 2 mol / L tervalent iron salt water solution which does not contain sulfate radicals and choride ions and phosphoric acid or soluble phosphate water solution according to the Fe-to-P molar ratio of 1:(1.1 to 1.6) into a container with stirring at the temperature of between 30 and 80 DEG C; after dripping, adding ammonia water to ensure that the pH is 0.1 to 5 to obtain amorphous basic ammonium ferric phosphate slurry; aging the slurry at the temperature of between 50 and 90 DEG C for 4 to 10 hours; filtering, washing by using deionized water until the filtrate is neutral; and drying a filter cake at the temperature of between 60 and 120 DEG C for 4 to 8 hours to obtain the spherical basic ammonium ferric phosphate powder. The product is petal shaped spherical particles which are dispersed well, particles consist of a large amount of nano sheets, and have uniform sizes; the average grain size of the particles is 1 to 1 mu m; the specific surface area is 80 to 110m<2> / g; and the tap density is more than 0.9g / cm<3>. The process is reasonable and simple, and the product is suitable for large-scale production of electrode materials.

Description

technical field [0001] The invention belongs to the field of compounds containing metal iron ions, nonmetal ammonium and phosphoric acid particles in inorganic chemistry, and relates to a preparation method of basic ferric ammonium phosphate. At the same time, it involves the preparation technology of lithium-ion battery cathode materials. Background technique [0002] With the depletion of petroleum resources and the increasingly serious environmental pollution caused by automobile exhaust, the development and application of electric vehicles (EV) or hybrid electric vehicles (HEV) and corresponding power sources have been developed rapidly. Among them, lithium-ion secondary battery has the advantages of high volume energy ratio and weight energy ratio, high voltage, low self-discharge rate, no memory effect, long cycle life, etc., and has absolute advantages as EV and HEV power energy. [0003] The structure and properties of electrode materials are one of the important fa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45H01M4/58H01M4/1397
CPCY02E60/12Y02E60/122Y02E60/10
Inventor 李嵩孙俊才文钟晟季世军
Owner DALIAN MARITIME UNIVERSITY
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