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Ammonium ferrous phosphate as well as preparation method and application thereof

A technology of ammonium ferrous phosphate and ferrous pyrophosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high raw material requirements, difficult doping, and low batch stability of lithium iron phosphate. , to achieve the effect of scientific preparation method, low roasting temperature, uniformity of doping and related performance improvement

Active Publication Date: 2020-05-08
DALIAN RONGKE ENERGY STORAGE GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to propose a ferrous ammonium phosphate, which has a stable iron-phosphorus ratio and lattice structure, and can It is used for batch and stable production of lithium iron phosphate, and the ammonium ferrous phosphate of the present invention introduces doping elements into its crystal structure, which is beneficial to the uniformity of doping, and has obvious effects on the uniformity of doping and related properties of lithium iron phosphate. promotion

Method used

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  • Ammonium ferrous phosphate as well as preparation method and application thereof
  • Ammonium ferrous phosphate as well as preparation method and application thereof
  • Ammonium ferrous phosphate as well as preparation method and application thereof

Examples

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Embodiment 1

[0050] This embodiment discloses a ferrous ammonium phosphate whose general formula is NH 4 FePO 4 .

[0051] The preparation method of ferrous ammonium phosphate comprises the following steps: take by weighing 27.8g ferrous sulfate heptahydrate and 11.54g concentrated phosphoric acid (85%) and be dissolved in 200mL secondary water, be placed in 70 ℃ of water baths and stir 30min, stir to Dissolve, pass argon gas for atmosphere protection, prevent ferrous iron from being oxidized by air, use a peristaltic pump to add concentrated ammonia water to the reaction system dropwise, adjust the reaction pH=7, maintain the reaction system pH and continue the reaction for 10 minutes, filter and wash the precipitate 3 times After drying, obtain ferrous ammonium phosphate. Such as figure 1 As shown, the obtained XRD spectrum of ammonium ferrous phosphate is compared with the standard spectrum in the spectral library, and it is determined that the compound obtained is ferrous ammonium p...

Embodiment 2

[0058] This embodiment discloses a ferrous ammonium phosphate whose general formula is NH 4 FePO 4 .

[0059] The preparation method of ferrous ammonium phosphate comprises the following steps: take by weighing 27.8g ferrous sulfate heptahydrate and 11.54g concentrated phosphoric acid (85%) and be dissolved in 200mL secondary water, be placed in 90 ℃ of water baths and stir 10min, stir to Dissolve, pass argon gas for atmosphere protection, prevent ferrous iron from being oxidized by air, use a peristaltic pump to drop concentrated ammonia water into the reaction system, adjust the reaction pH=6, maintain the reaction system pH and continue the reaction for 30 minutes, filter and wash the precipitate 3 times After drying, obtain ferrous ammonium phosphate.

[0060] The method for preparing lithium iron phosphate by using the above-mentioned ferrous ammonium phosphate comprises the following steps:

[0061] Place the dried ammonium ferrous phosphate in a tube furnace and roas...

Embodiment 3

[0066] This embodiment discloses a ferrous ammonium phosphate whose general formula is NH 4 Fe 0.8 V 0.2 PO 4 .

[0067] The preparation method of ammonium ferrous phosphate comprises the following steps: take by weighing 0.5g vanadyl sulfate, 27.8g ferrous sulfate heptahydrate and 11.54g concentrated phosphoric acid (85%) and dissolve in 200mL secondary water, place it in a 90°C water bath Stir in the medium for 10 minutes, stir until dissolved, pass argon for atmosphere protection, prevent iron and vanadium from being oxidized by air, use a peristaltic pump to drop concentrated ammonia water into the reaction system, adjust the reaction pH=7, maintain the reaction system pH and continue the reaction for 60 minutes. The precipitate was filtered and washed three times and then dried to obtain vanadium-doped ferrous ammonium phosphate.

[0068] The method for preparing lithium iron phosphate by using the above-mentioned ferrous ammonium phosphate comprises the following ste...

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Abstract

The invention provides ammonium ferrous phosphate as well as a preparation method and application thereof, the general formula of the ammonium ferrous phosphate is NH4FexM(1-x)PO4, and x is greater than 0 and less than or equal to 1; and M is selected from one or more of V, K, Co, Mn, Zn, Mg, Ni, Al, Ti, Nb, Zr and Cu. The invention also discloses a method for preparing lithium iron phosphate fromthe ammonium ferrous phosphate, and the method comprises the following steps: mixing ferrite, a phosphorus source and ammonia water, regulating the pH value of the reaction system to 6-7, and reacting to generate the ammonium ferrous phosphate, wherein the molar ratio of the ferrite to the phosphorus source is (0.95-1.03): (0.95-1.03); reducing and calcining the ammonium ferrous phosphate at hightemperature under inert atmosphere protection to obtain ferrous pyrophosphate; mixing the ferrous pyrophosphate with lithium salt and a carbon source, crushing and ball-milling; performing calciningand coating carbon, and synthesizing to obtain the lithium iron phosphate. The method is simple in production process, low in production precision requirement and easy to prepare and dope.

Description

technical field [0001] The invention relates to the preparation technology of lithium iron phosphate, in particular to a ferrous ammonium phosphate, its preparation method and application. Background technique [0002] At present, lithium iron phosphate is mostly prepared by the iron phosphate method. The iron phosphate method is to use iron phosphate and lithium carbonate mixed ball mill, and use the carbon coating produced by the high-temperature carbonization of the carbon source to reduce ferric iron to divalent at high temperature. Lithium iron phosphate is formed. However, the performance of lithium iron phosphate produced by this method depends heavily on the quality of raw material iron phosphate, including its moisture content, iron-phosphorus ratio, morphology and particle size, and it is difficult to obtain iron phosphate produced by precipitation on the market. This is also one of the reasons for the poor stability of commercially available lithium iron phosphat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58
CPCC01B25/451H01M4/5825C01P2002/72C01P2004/03C01P2006/40Y02E60/10
Inventor 宋明明王璐赵丹丹孟昭扬李宗麟
Owner DALIAN RONGKE ENERGY STORAGE GRP CO LTD
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