A kind of ferrous ammonium phosphate, its preparation method and application

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

Active Publication Date: 2022-06-28
DALIAN RONGKE ENERGY STORAGE GRP CO LTD
View PDF6 Cites 0 Cited by
  • 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

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
  • A kind of ferrous ammonium phosphate, its preparation method and application
  • A kind of ferrous ammonium phosphate, its preparation method and application
  • A kind of ferrous ammonium phosphate, its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] This embodiment discloses a kind of ferrous ammonium phosphate, and its general formula is NH 4 FePO 4 .

[0047] The preparation method of ferrous ammonium phosphate includes the following steps: Weigh 27.8g of ferrous sulfate heptahydrate and 11.54g of concentrated phosphoric acid (85%) and dissolve it in 200mL of secondary water, place it in a 70°C water bath and stir for 30min, and stir until Dissolve, pass argon 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=7, maintain the pH of the reaction system and continue the reaction for 10min, filter and wash the precipitate 3 times After drying, ferrous ammonium phosphate is obtained. like figure 1 As shown, the obtained XRD pattern of ferrous ammonium phosphate is compared with the standard spectrum in the spectrum library, and it is determined that the obtained compound is ferrous am...

Embodiment 2

[0054] This embodiment discloses a kind of ferrous ammonium phosphate, and its general formula is NH 4 FePO 4 .

[0055] The preparation method of ferrous ammonium phosphate includes the following steps: weigh 27.8g of ferrous sulfate heptahydrate and 11.54g of concentrated phosphoric acid (85%) and dissolve it in 200mL of secondary water, place it in a 90°C water bath and stir for 10min, and stir until Dissolve, pass argon 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 pH of the reaction system and continue the reaction for 30min, filter and wash the precipitate for 3 times After drying, ferrous ammonium phosphate is obtained.

[0056] The method for preparing lithium iron phosphate using above-mentioned ferrous ammonium phosphate, comprises the following steps:

[0057] After drying, the ferrous ammonium phosphate was plac...

Embodiment 3

[0062] This embodiment discloses a kind of ferrous ammonium phosphate, and its general formula is NH 4 Fe 0.8 V 0.2 PO 4 .

[0063] The preparation method of ferrous ammonium phosphate includes the following steps: weigh 0.5g vanadyl sulfate, 27.8g ferrous sulfate heptahydrate and 11.54g concentrated phosphoric acid (85%), dissolve them in 200mL secondary water, and place them in a 90°C water bath. Stir for 10min, 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 pH of the reaction system and continue the reaction for 60min, the The precipitate is filtered and washed three times and then dried to obtain vanadium-doped ferrous ammonium phosphate.

[0064] The method for preparing lithium iron phosphate using above-mentioned ferrous ammonium phosphate, comprises the following steps:

[0065...

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

No PUM Login to view more

Abstract

The invention provides a ferrous ammonium phosphate, its preparation method and application, the general formula of ferrous ammonium phosphate is: NH 4 Fe x m (1‑x) PO 4 , wherein x=greater than 0 and less than or equal to 1; 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 from ferrous ammonium phosphate, which includes the following steps: mixing ferrous salt, phosphorus source and ammonia water, adjusting the pH of the reaction system to 6-7, and reacting to generate ferrous ammonium phosphate; the ferrous The molar ratio of the salt to the phosphorus source is 0.95-1.03:0.95-1.03; the ammonium ferrous phosphate is reduced and calcined at a high temperature under the protection of an inert atmosphere to obtain ferrous pyrophosphate; the ferrous pyrophosphate is mixed with lithium salt and carbon source, Crushing, ball milling; calcining, carbon coating, and synthesis to obtain lithium iron phosphate. The production process of the invention is simple, the production precision is low, and the preparation and doping are easy.

Description

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

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 Patents(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
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