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Low-temperature continuous production process for lithium iron phosphate and dedicated device therefor

A lithium iron phosphate and production process technology, applied in the field of preparation of in, ion-doped lithium iron phosphate materials, can solve the problem of poor high current discharge capability of synthetic materials, limiting large-scale industrialization of lithium iron phosphate, and powder preparation process time. Long and other problems, to achieve the effect of excellent electrochemical performance, wide application range of raw materials, and fine particles

Active Publication Date: 2011-09-07
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have some inherent disadvantages, such as: high powder synthesis temperature, long powder preparation process time, harsh control conditions, high cost, poor stability between batches, and poor high-current discharge capability of the synthesized materials. Restricting the large-scale industrialization of lithium iron phosphate

Method used

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  • Low-temperature continuous production process for lithium iron phosphate and dedicated device therefor
  • Low-temperature continuous production process for lithium iron phosphate and dedicated device therefor
  • Low-temperature continuous production process for lithium iron phosphate and dedicated device therefor

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Experimental program
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Effect test

Embodiment 1

[0018] Embodiment 1: the structure of special equipment.

[0019] The horizontal stirring dryer 2 of this embodiment is equipped with a heat transfer oil circulating agitator 4 . Make the material evenly heated. The feed pump 1 communicates with the feed inlet 2-1 of the horizontal stirring dryer 2, and the upper end of the feed inlet has a sealing cover 3, and the gas outlet valve 2-3 on the upper side of the horizontal stirring dryer is connected to the slow flow of the solvent recovery system. One end of the tube 5 is connected, and ten axially extending spiral baffles are arranged in the slow-flow tube as the turbulence device 6, and its function is to reduce the air velocity of solvent volatilization. device7. The filter device consists of two layers of screen mesh and cotton wool to form a filter cloth. The main function is to prevent the passage of fine material particles.

[0020] The other end of the slow flow tube communicates with the condenser 9, and the conden...

Embodiment 2

[0024] (1) Weigh 8.64 kg of ferrous oxalate, 7.68 kg of iron oxide, 10.40 kg of lithium dihydrogen phosphate, 0.820 kg of glucose, 17.240 kg of oxalic acid, 0.226 kg of yttrium oxide, and 0.266 kg of niobium oxide. The solvent methanol was added to the stirrer with a circulating reflux device, stirred at room temperature for 0.5h, and the stirring speed was 400r / min, and a light yellow lithium iron phosphate precursor slurry was obtained; the obtained slurry was added to a dryer. Fluidized drying, compressed air is blown into the drying process with a flow rate of 80m 3 / h, the drying temperature is 80°C, and the drying time is 2h. After drying, a lithium iron phosphate precursor powder containing a composite carbon source and a composite metal compound is obtained; the volatilized solvent is recycled by condensation. The obtained lithium iron phosphate precursor powder is ultrafinely pulverized to obtain a fine powder with a particle size of 200 mesh, and then mechanically c...

Embodiment 3

[0028] (2) Weigh 8.82 kg of ferrous oxalate, 7.84 kg of iron oxide, 10.40 kg of lithium dihydrogen phosphate, 0.480 kg of chitosan, 0.420 kg of fruit acid, 17.240 kg of oxalic acid, 0.062 kg of magnesium fluoride, and 0.151 kg of tin oxide , first mixed, and then added together with the solvent methanol into a stirrer with a circulating reflux device, stirred at room temperature for 0.2h, and the stirring speed was 200r / min, to obtain a light yellow lithium iron phosphate precursor slurry; the obtained The slurry is added to the dryer for fluidized drying, and the compressed air is blown into the drying process with a flow rate of 40m 3 / h, the drying temperature is 70°C, and the drying time is 4h. After drying, a lithium iron phosphate precursor powder containing a composite carbon source and a composite metal compound is obtained; the volatilized solvent is recycled by condensation. The obtained lithium iron phosphate precursor powder is ultrafinely pulverized to obtain a f...

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Abstract

The invention discloses a low-temperature continuous production process for lithium iron phosphate and a dedicated device therefor. The process comprises the following steps: preparing ferrous oxalate, lithium dihydrogen phosphate, an organic composite carbon source and a composite metal compound which are used as raw materials; mechanically stirring the raw materials in a way of circulation reflux in methanol which is used as a medium; performing fluidized drying on the resulting slurry to obtain a lithium iron phosphate precursor containing the composite carbon source and the composite metal compound; performing micronization and mechanical compaction and then calcining at a low temperature in a protective atmosphere with extremely-low oxygen content; and performing air flow classification and vibratory screening to obtain fine-particle lithium iron phosphate which has uniform grain-size distribution and excellent electrochemical properties and is used as an anode material for lithium ion batteries. The process is simple and easy to operate. The lithium iron phosphate product has excellent electrochemical properties, high tap density and good processing properties. The dedicateddevice has a high production capacity, is suitable for continuous industrial production, does not produce waste, and is environment-friendly and significant in application value.

Description

Background technique [0001] The preparation of lithium iron phosphate cathode materials can be simply divided into solid-phase method and liquid-phase method. The existing solid-phase methods mainly include the following types: high-temperature solid-phase sintering method and carbothermal reduction method. The former generally uses divalent iron as a raw material and is sintered to make a finished product; In the process of material reduction, ferric iron is reduced to ferrous iron through carbothermal reduction reaction at high temperature to make lithium iron phosphate finished product. The liquid phase method refers to the reaction of ions in the solution to generate lithium iron phosphate or a precursor, and then heat treatment to make a finished product. The liquid phase method is especially suitable for the preparation of ion-doped lithium iron phosphate materials. However, these methods have some inherent disadvantages, such as: high powder synthesis temperature, lon...

Claims

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Application Information

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IPC IPC(8): C01B25/45
Inventor 张宝张佳峰彭春丽沈超陈核章
Owner CENT SOUTH UNIV
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