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Method for preparing lithium iron phosphate from vivianite

A technology of lithium iron phosphate and cyanite, which is used in electrical components, battery electrodes, circuits, etc., can solve the problems of difficult design and manufacture of high temperature and high pressure reactors, affecting the chemical and electrochemical properties of products, and large equipment investment. , to achieve the effect of good electrochemical performance, low cost and high resource utilization

Active Publication Date: 2014-04-09
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are often iron dislocations in the prepared product structure, resulting in metastable FePO 4 , affecting the chemical and electrochemical properties of the product
At the same time, there are also disadvantages of impure phase, large investment in equipment (the design and manufacture of high temperature and high pressure reactors is difficult and expensive), or the process is relatively complicated.

Method used

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  • Method for preparing lithium iron phosphate from vivianite
  • Method for preparing lithium iron phosphate from vivianite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] This embodiment includes the following steps:

[0019] (1) Weigh 5.0 kg of blue iron ore and add it to a horizontal ball mill for mechanical ball milling and crushing. The ball milling time is 4 hours and the ball milling speed is 180r / min;

[0020] (2) With 25kg of deionized water as the medium, add 5.0kg of crushed blue iron ore, 2.5kg of oxalic acid and 2.5kg of ascorbic acid into the stirred reactor, and pass through 0.05 dm 3 / h High-purity nitrogen with a purity of 99.999%, after stirring at a speed of 400 r / min for 6 h, then add 3.34 kg lithium phosphate dodecahydrate to the reaction kettle, and adjust the molar ratio of iron, phosphorus, lithium and carbon in the mixture The ratio is 1:1:1.05:5.0, and the stirring is continued for 8 hours to obtain 14.2 kg of lithium iron phosphate precursor;

[0021] (3) The lithium iron phosphate precursor obtained in step (2) was pretreated at 300°C for 6 hours in a high-purity nitrogen atmosphere with a purity of more than ...

Embodiment 2

[0024] This embodiment includes the following steps:

[0025] (1) Weigh 5.0 kg of blue iron ore, add it to a horizontal ball mill for mechanical ball milling and crushing, the ball milling time is 0.5h, and the ball milling speed is 50r / min;

[0026] (2) With 25kg of deionized water as the medium, add 5.0 kg of crushed blue iron ore, 1 kg of acetic acid and 1.5 kg of citric acid into the stirred reactor, and feed 0.01 dm 3 / h of high-purity nitrogen with a purity of 99.999%, after stirring for 4 hours at a speed of 200 r / min, add 3.178 kg of lithium phosphate dodecahydrate to the reaction kettle, and adjust the molar ratio of iron, phosphorus, lithium and carbon in the mixture 1: 1: 1.0: 1.0, continue to stir for 4 hours to obtain 14.0 kg of lithium iron phosphate precursor;

[0027] (3) The lithium iron phosphate precursor obtained in step (2) was pretreated at 200°C for 2 hours in a high-purity nitrogen atmosphere with a purity of more than 99.999%, and then 0.35 kg of citr...

Embodiment 3

[0030] This embodiment includes the following steps:

[0031] (1) Weigh 5.0 kg of blue iron ore and add it to a horizontal ball mill for mechanical ball milling and crushing. The ball milling time is 8 hours and the ball milling speed is 250r / min;

[0032] (2) With 25kg of deionized water as the medium, add 5.0 kg of crushed blue iron ore, 2.5 kg of oxalic acid, 2.5 kg of acetic acid and 2.5 kg of malic acid into the stirred reactor, and pass through 1.0 dm 3 / h of high-purity nitrogen with a purity of 99.999%, stirred at a speed of 600 r / min for 8 h, then added 3.496 kg of lithium phosphate dodecahydrate to the reaction kettle, and adjusted the molar ratio of iron, phosphorus, lithium and carbon in the mixture The ratio is 1:1:1.1:10.0, and the stirring is continued for 8 hours to obtain 13.8 kg of lithium iron phosphate precursor;

[0033](3) The lithium iron phosphate precursor obtained in step (2) was pretreated at 400°C for 8 hours under a high-purity nitrogen atmosphere...

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Abstract

The invention relates to a method for preparing lithium iron phosphate from vivianite. The method comprises the following steps that (1) the vivianite is broken; (2) deionized water is used as media, the vivianite and composite reducing organic acid are added into a stirring reaction kettle, high-purity nitrogen gas is introduced, the stirring is carried out for 4 to 8 hours, then, lithium phosphate dodecahydrate is added, the stirring is continuously carried out for 4 to 20 hours, and lithium iron phosphate precursors are obtained; (3) the lithium iron phosphate precursors are pretreated for 2 to 8 hours at 200 to 400 DEG C in high-purity protecting atmosphere, then, composite carbon sources are added, the mechanical ball milling is carried out, the drying is carried out for 8 to 18 hours under the temperature condition being 100 to 140 DEG C, the baking is carried out for 4 to 16 hours at 500 to 700 DEG C in high-purity protecting atmosphere, and the lithium iron phosphate is obtained. The method for preparing lithium iron phosphate from vivianite has the advantages that the resource utilization rate is high, the requirements on equipment in the production process are lower, the cost is low, the energy consumption is small, and the environment is protected. The lithium iron phosphate prepared by the method has the advantages that the particle size distribution is uniform, the tap density is high, and the electrochemical performance is good.

Description

technical field [0001] The invention relates to a method for preparing lithium iron phosphate, in particular to a method for preparing lithium iron phosphate by using blue iron ore. Background technique [0002] LiFePO 4 It is a new type of cathode material for lithium-ion batteries. It has the advantages of excellent charging and discharging platform, good cycle performance, high theoretical capacity, environmental friendliness, and low price. On electric vehicles, its prospects are immeasurable. The preparation of lithium iron phosphate cathode material can be simply divided into solid-phase method and liquid-phase method. The existing solid phase methods mainly include high temperature solid phase sintering method and carbothermal reduction method. Among them, the high-temperature solid-phase sintering method uses ferrous iron as a raw material and sinters it into a finished product. The disadvantages are that the particle size and shape are not good, the particle si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 张宝张佳峰彭春丽郑俊超王健龙袁新波
Owner CENT SOUTH UNIV
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