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A method for preparing lithium iron phosphate with no pollution and zero discharge

A lithium iron phosphate, zero-emission technology, applied in the field of green chemical processes, can solve problems such as uneven particle size distribution, air pollution, water vapor emission, etc., and achieve the effects of good electrochemical performance, reduced production costs, and stable batches.

Active Publication Date: 2016-09-28
南阳逢源新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004]However, we believe that the birth of a new green energy should be green from its birth process, not to obtain a new green energy Energy has already caused serious environmental pollution before it is obtained, so it may not be worth the candle
The traditional solid-phase method and liquid-phase method or microwave-synthesized LiFePO4 not only takes a long time, but also consumes a lot of energy, has uneven particle size distribution, and unsatisfactory performance. At the same time, it emits a large amount of waste gas, waste water, and dust and other pollutants, causing serious environmental pollution
The traditional high-temperature solid-state method uses Li 2 CO 3 +2FeC 2 o 4 +2NH 4 h 2 PO 4 = 2LiFePO 4 +2NH 3 ↑+5CO 2 ↑+3H 2 O, per 1 ton of LiFePO produced 4 , it will generate about 350m 3 CO 2 gas, while also producing about 153 m 3 NH 3 Gas, these gases are very polluting to the air, and it is difficult to recover, and there is a large amount of water vapor emission

Method used

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  • A method for preparing lithium iron phosphate with no pollution and zero discharge
  • A method for preparing lithium iron phosphate with no pollution and zero discharge
  • A method for preparing lithium iron phosphate with no pollution and zero discharge

Examples

Experimental program
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Effect test

Embodiment 1

[0018] see figure 1 , a pollution-free and zero-emission lithium iron phosphate preparation method is characterized in that it comprises the following steps:

[0019] H 3 PO 4 , FeCl 2 and LiOH, weighed in a molar ratio of 1:1:3; then the weighed H 3 PO 4 , FeCl 2 and LiOH are supersaturated dissolved in deionized water to form molecular-level H 3 PO 4 Precursor solution, FeCl 2 precursor solution and LiOH precursor solution, followed by the H 3 PO 4 Add the precursor solution into the autoclave, and raise the temperature in the autoclave to 50-110°C, then slowly add FeCl 2 precursor solution to make H 3 PO 4 Precursor solution with FeCl 2 After the precursor solution is mixed evenly, an inert gas is introduced into the autoclave, and then the LiOH precursor solution is added into the autoclave, and then the temperature rise reaction starts in the autoclave, that is, FeCl 2 + H 3 PO 4 + 3LiOH→2LiCl + LiFePO 4 ↓+3H 2O, during the heating reaction pr...

Embodiment 2

[0028] In the method steps described in Example 1, further, after the temperature rise reaction is completed, the materials in the autoclave are separated from solid to liquid, and the obtained solid is lithium iron phosphate crystals, and the separated lithium iron phosphate crystals are washed to keep the washing The weight percentage of water in the final lithium iron phosphate crystal is 30-80%. After washing, a lithium iron phosphate crystal suspension is formed, and then the clathrate is added to the lithium iron phosphate crystal suspension. The added clathrate and phosphoric acid The molar ratio of lithium iron crystals is 1-2.5:1, and the clathrate is supersaturated and dissolved in the suspension of lithium iron phosphate crystals, and then the clathrate process is completed under the mechanism of saturated solution and ultrasonic dispersion interaction through physical and chemical effects. Form the lithium iron phosphate inclusion compound crystal precursor. After t...

Embodiment 3

[0030] In the method steps described in Example 2, further, the clathrate is hydroquinone or β-cyclodextrin.

[0031] Detection analysis:

[0032] Entrust Xinxiang Huanyu Group to do the detection, the lithium iron phosphate material prepared by the preparation method of a carbonitriding lithium iron phosphate material provided by the present invention, after testing, the theoretical gram capacity of lithium iron phosphate is 170mAH / g , the lithium iron phosphate material prepared by this method can stably reach 163mAH / g, see the attached gram capacity test chart for details figure 2 ; The rate performance of the lithium iron phosphate material prepared by this method, the standard of the European Union is that 1C charge and discharge is not less than 130mAH / g, and the relatively good domestic ones can reach 1C charge and discharge 135mAH / g at present, and the phosphoric acid prepared by this method For lithium iron material, the tested data is about 154mAH / g at 1C charge an...

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Abstract

The invention relates to a pollution-free and zero-discharge lithium iron phosphate preparation method. The pollution-free and zero-discharge lithium iron phosphate preparation method accords with the green chemistry and fine chemical idea of environmental friendliness, sustainable development and no pollution. According to the pollution-free and zero-discharge lithium iron phosphate preparation method, a lithium source, an iron source and a phosphorus source are dissolved and mixed in an appropriate environment, the mixture is synthesized into high-purity lithium iron phosphate crystals under the control of synthesis conditions in reaction process, different components of the product are controlled so that separation treatment is easy, a lithium iron phosphate crystal precursor is extracted and then is clathrated, the clathrated lithium iron phosphate crystal precursor is subjected to carbonization annealing heat treatment, the residual liquid and byproduct are subjected to green treatment and then be recycled, and heat produced by cooling is recovered and recycled. The lithium iron phosphate material obtained by the preparation method has good electrochemical performances, high purity and good processing performances. The preparation method realizes reasonable element content, has stable batch, no pollution and zero discharge and is convenient for large-scale production.

Description

technical field [0001] The invention belongs to the field of chemical synthetic materials, in particular the invention relates to a green chemical process for preparing lithium iron phosphate with no pollution and zero discharge. Background technique [0002] AyMPO was first revealed by Japan's NTT in 1996 4 (A is an alkali metal, M is a combination of CoFe: LiFeCOPO 4 ) Lithium battery cathode material with olivine structure, in 1997, John. B. Goodenough and other research groups at Texas State University reported LiFePO 4 The olivine structure (LiM PO 4 ), Europeans also discovered LiFePO with natural olivine structure 4 . LiFePO 4 It has also been found to have superior performance that cannot be compared with commercialized secondary battery materials such as lithium cobalt oxide, lithium nickel oxide, and ternary materials. The material has a series of advantages such as wide source of raw materials, low price, no memory effect, long cycle life, good safety perfor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58C01B25/45
CPCC01B25/45H01M4/5825H01M10/0525Y02E60/10
Inventor 孙青林汪浩魏宏政
Owner 南阳逢源新能源科技有限公司