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Method for preparing carbon doped high-pressure solid iron phosphate

A technology of iron phosphate and real phosphoric acid, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of low energy density, poor capacity, large size, etc., achieve dense particle growth, simple preparation method, one-time The effect of large particle size

Active Publication Date: 2020-01-14
王敏
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] As we all know, the main bottleneck affecting the application of lithium iron phosphate is the low energy density. The main reason is that the current mainstream process of lithium iron phosphate is still carbon-coated lithium iron phosphate, but this process has the following problems: carbon-coated lithium iron phosphate particles , the conductivity between particles increases, but the conductivity of a single particle of lithium iron phosphate does not improve significantly; at the same time, because the coated carbon is flocculent amorphous carbon, this part of carbon affects the compaction density of lithium iron phosphate , because if the particles of lithium iron phosphate are made larger, although the compaction density is high, the size of the particles is too large, which leads to a long migration distance of lithium ions and poor capacity. In order to ensure the capacity, the particle size can only be reduced, which affects the The compaction of lithium iron phosphate, capacity and compaction are the same as a seesaw, and cannot have both

Method used

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  • Method for preparing carbon doped high-pressure solid iron phosphate
  • Method for preparing carbon doped high-pressure solid iron phosphate
  • Method for preparing carbon doped high-pressure solid iron phosphate

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Embodiment 1

[0040] A kind of preparation method of carbon-doped high compacted iron phosphate, it is the following steps:

[0041] 1) Dissolve disodium EDTA in water, prepare a solution with a concentration of 0.26mol / L at 30°C, add ferric nitrate solution to disodium EDTA solution, then add an acid-base regulator until the pH of the mixed solution is 1.25, and stir Mix evenly, then add the mixed solution of phosphoric acid and ammonium dihydrogen phosphate, the addition time is 1.5h, then stir and react for 20min to obtain the reaction slurry;

[0042] 2) Add alkali to the reaction slurry obtained in step (1), adjust the pH of the solution to 2.5, raise the temperature to 93°C, then stir and react for 25 minutes, then cool down to the material temperature of 55°C, then filter, wash and dry Dry to obtain dried material;

[0043] 3) The dried material is calcined in a rotary furnace under a nitrogen atmosphere, the calcining temperature is 625° C., and the calcining time is 3 hours to obt...

Embodiment 2

[0057] A kind of preparation method of carbon-doped high compacted iron phosphate, it is the following steps:

[0058] 1) Dissolve disodium EDTA in water, prepare a solution with a concentration of 0.28mol / L at 32°C, add ferric nitrate solution to disodium EDTA solution, then add an acid-base regulator until the pH of the mixed solution is 1.2, and stir Mix evenly, then add the mixed solution of phosphoric acid and ammonium dihydrogen phosphate, the addition time is 1.5h, then stir and react for 20min to obtain the reaction slurry;

[0059] 2) Add alkali to the reaction slurry obtained in step (1), adjust the pH of the solution to 2.5, raise the temperature to 90°C, then stir and react for 25 minutes, then cool down to the material temperature of 55°C, then filter, wash and dry Dry to obtain dried material;

[0060] 3) The dried material is calcined in a rotary furnace under a nitrogen atmosphere, the calcining temperature is 645° C., and the calcining time is 2.5 hours to ob...

Embodiment 3

[0072] A kind of preparation method of carbon-doped high compacted iron phosphate, it is the following steps:

[0073] 1) Dissolve disodium EDTA in water, prepare a solution with a concentration of 0.3mol / L at 35°C, add ferric nitrate solution to disodium EDTA solution, then add an acid-base regulator until the pH of the mixed solution is 1, and stir Mix evenly, then add the mixed solution of phosphoric acid and ammonium dihydrogen phosphate, the addition time is 1.5h, then stir and react for 20min to obtain the reaction slurry;

[0074] 2) Add alkali to the reaction slurry obtained in step (1), adjust the pH of the solution to 2.8, raise the temperature to 90°C, then stir and react for 25 minutes, then cool down to the material temperature of 55°C, then filter, wash and dry Dry to obtain dried material;

[0075] 3) The dried material is calcined in a rotary furnace under a nitrogen atmosphere, the calcining temperature is 635° C., and the calcining time is 2.5 hours to obtai...

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Abstract

The invention discloses a method for preparing carbon doped high-pressure solid iron phosphate. The method comprises the following steps: dissolving EDTA (ethylene diamine tetraacetic acid) disodium into water, preparing a 0.25-0.3mol / L solution at 30-35 DEG C, adding a solution of ferric nitrate to the EDTA disodium solution, adding an acid-base regulator to the mixed solution till the pH value is 1-1.5, performing uniform stirring and mixing, adding a mixed solution of phosphoric acid and ammonium dihydrogen phosphate for an addition time of 1-2 hours, and performing a stirring reaction for15-30 minutes so as to obtain reaction slurry; further adding an alkali into the reaction slurry, adjusting the pH value of the solution, performing heating, performing a stirring reaction, performingcooling, and performing filtering, washing and drying so as to obtain a dried material; and calcining the dried material in a rotary furnace in a nitrogen atmosphere, so as to obtain the carbon dopedhigh-pressure solid iron phosphate. The preparation method disclosed by the invention is simple, iron phosphate doped with carbon is obtained, granules grow densely, the aperture is small, and the primary particle size is large.

Description

technical field [0001] The invention relates to a preparation method of carbon-doped high-pressure compacted iron phosphate, which belongs to the technical field of lithium batteries. Background technique [0002] Lithium batteries are gradually developing with the development of new energy vehicles. At present, the mainstream lithium batteries are divided into lithium iron phosphate batteries, lithium manganese oxide batteries and ternary batteries. [0003] In 2018, the total output of new energy vehicles in China was 1.23 million, accounting for 60% of the total global sales, and the installed capacity of power batteries was 56Gwh, a year-on-year increase of 68%. Against the background of the overall decline in the auto market in 2018, new energy vehicles still delivered a perfect answer with the support of subsidies. [0004] At present, the price of lithium iron phosphate of mainstream manufacturers has dropped to about 53,000 yuan / ton, which has dropped by more than 6...

Claims

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Application Information

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IPC IPC(8): C01B25/37H01M4/58H01M4/62H01M10/052
CPCC01B25/375C01P2002/72C01P2004/03C01P2004/61C01P2006/10C01P2006/11C01P2006/12H01M4/5825H01M4/62H01M10/052Y02E60/10
Inventor 王敏
Owner 王敏