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Method for preparation of lithium iron phosphate material in static mixing tube type reactor

A tubular reactor, static mixing technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of difficult industrial production, large product particle size, uneven distribution, etc., to achieve easy continuous industrial production, particle size The effect of narrow distribution and simple process

Active Publication Date: 2012-04-04
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the preparation of lithium iron phosphate materials mainly adopts high-temperature solid-phase synthesis method. The advantage of this method is that the process is simple and easy to realize industrialization. However, because the reactants are not easy to mix uniformly, the particle size of the product is large and unevenly distributed, and the shape is irregular. Therefore, there is a problem of insufficient batch stability
Compared with the high-temperature solid-phase synthesis method, the hydrothermal method does not require the protection of an inert atmosphere and can be directly synthesized to obtain LiFeP. 4 , and it is also easy to control the shape and particle size of the material, but the hydrothermal method requires high temperature and high pressure equipment, and industrial production is difficult
The traditional liquid-phase co-precipitation method usually adopts a batch reactor to operate as a batch method. Due to the limitation of the amount of reaction materials, the reaction process is long-lasting, which is not conducive to large-scale production. With the progress of the reaction process, the reaction conditions (such as concentration , pH value) are constantly changing, which affects the particle size and distribution of the micropowder

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  • Method for preparation of lithium iron phosphate material in static mixing tube type reactor
  • Method for preparation of lithium iron phosphate material in static mixing tube type reactor
  • Method for preparation of lithium iron phosphate material in static mixing tube type reactor

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Embodiment 1

[0025] (1) Prepare a ferrous ammonium sulfate solution with a concentration of 0.05mol / L and an ammonium dihydrogen phosphate solution with a concentration of 0.05mol / L, and then mix them to form the solution A to be reacted; prepare a 0.1mol / L solution of lithium hydroxide and Ammonia solution, it is mixed, is made into solution B to be reacted;

[0026] (2) Use two feeding pumps to inject the solutions A and B in step (1) from one end of the static mixing tube reactor at an equal volume flow rate of 2.5 L / min, and perform a mixing reaction to form an emulsion. The molar ratio of iron ions, phosphorus ions, and lithium ions is required to be 1:1:1, and the pH value in the reactor should be controlled between 7.3 and 7.8 by adjusting the amount of ammonia water in solution B;

[0027] (3) After aging the emulsion in step (2) for 2 hours, perform membrane washing to obtain a slurry solution from which impurity ions are removed;

[0028] (4) Dissolving sucrose and adding it to ...

Embodiment 2

[0033] (1) Prepare ferrous sulfate solution with a concentration of 0.5mol / L and ammonium monohydrogen phosphate solution with a concentration of 0.5mol / L, and then mix them to make solution A to be reacted; prepare lithium hydroxide 1mol / L solution and ammonia solution , mix them to form the solution B to be reacted;

[0034] (2) Use two feeding pumps to inject solutions A and B in step (1) at an equal volume flow rate of 0.5 L / min from one end of the static mixing tube reactor, and perform a mixing reaction to form an emulsion. The molar ratio of iron ions, phosphorus ions, and lithium ions is required to be 1:1:1, and the pH value in the reactor is controlled between 7.8 and 8.3 by adjusting the amount of ammonia water in solution B;

[0035] (3) After aging the emulsion in step (2) for 4 hours, perform membrane washing to obtain a slurry solution from which impurity ions are removed;

[0036] (4) Dissolving glucose and adding it to the slurry liquid in step (3), and fully...

Embodiment 3

[0041] (1) Prepare a ferrous ammonium nitrate solution with a concentration of 0.8mol / L, and an ammonium phosphate solution with a concentration of 0.8mol / L, and then mix them to make the solution A to be reacted; mix lithium hydroxide 1.6mol / L solution and ammonia solution , mix them to form the solution B to be reacted;

[0042](2) Use two feeding pumps to inject solutions A and B in step (1) from one end of the static mixing tube reactor at an equal volume flow rate of 0.1 L / min, and perform a mixing reaction to form an emulsion. The molar ratio of iron ions, phosphorus ions, and lithium ions is required to be 1:1:1. By adjusting the amount of ammonia water in solution B, the pH value in the reactor is controlled between 8.4 and 8.9;

[0043] (3) After aging the emulsion in step (2) for 3 hours, perform membrane washing to obtain a slurry solution from which impurity ions are removed;

[0044] (4) Dissolving fructose and adding it to the slurry liquid in step (3), and full...

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Abstract

The invention discloses a method for preparation of a lithium iron phosphate material in a static mixing tube type reactor, which mainly comprises the following steps: filling of mixed solution of a divalent iron source and a phosphorous source and mixed solution of lithium hydroxide and ammonia of the same volume flow from one end of the static mixing tube type reactor, liquid-phase mixing reaction in the static mixing tube type reactor to prepare emulsion, film washing after aging to remove impurity ions, mixing with a carbon source, spray drying to obtain carbon-containing LiFePO4 precursor powder, placing the precursor powder in a tube type furnace, and sintering for 3-10h at 600-750 DEG C in the protective atmosphere of inert gases to obtain the finished product. The obtained material has a small particle size and narrow particle size distribution, the costs of raw materials are low, the process is simple, and continuous chemical production can be facilitated.

Description

technical field [0001] The invention relates to a method for preparing a positive electrode material of a lithium ion battery, in particular to a method for preparing a lithium iron phosphate material in a static mixing tube reactor, and belongs to the technical field of battery material preparation. Background technique [0002] Olivine-type lithium iron phosphate (LiFeP0 4 ) As a new generation of lithium-ion batteries, it has the advantages of high specific energy, high power, long service life, no memory effect, and high cost performance, and has become the main choice for rechargeable power supplies for portable electronic products. LiFeP0 4 It has relatively high theoretical specific capacity (about 170 mAh / g) and theoretical specific energy (about 550 Wh / kg), good chemical stability and thermal stability, and stable charge and discharge voltage platform, making organic electrolytes more suitable for battery applications. Because of the advantages of safety, abundant...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 何学刚刘大军杨续来
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY