made of ferrophosphorus in co 2 prepared in atmosphere li x fe y p z o 4 Methods

A ferrophosphorus and atmosphere technology, applied in the field of material manufacturing process, can solve the problems of high cost of atmosphere manufacturing and single variety, and achieve the effects of simple and convenient reaction, short production process and reduced manufacturing cost.

Inactive Publication Date: 2017-12-15
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is in order to overcome the deficiency of existing reaction atmosphere, has opened up Li x Fe y P z o 4 A new preparation process method, providing a line made of ferrophosphorus in CO 2 The Li x Fe y P z o 4 The unique process route of the finished product replaces the shortcomings of high manufacturing cost and single variety in the traditional process production

Method used

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  • made of ferrophosphorus in co <sub>2</sub> prepared in atmosphere li <sub>x</sub> fe <sub>y</sub> p <sub>z</sub> o <sub>4</sub> Methods
  • made of ferrophosphorus in co <sub>2</sub> prepared in atmosphere li <sub>x</sub> fe <sub>y</sub> p <sub>z</sub> o <sub>4</sub> Methods
  • made of ferrophosphorus in co <sub>2</sub> prepared in atmosphere li <sub>x</sub> fe <sub>y</sub> p <sub>z</sub> o <sub>4</sub> Methods

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Ferrophosphorus was prepared by solid-phase synthesis in CO 2 Preparation of Li in atmosphere x Fe y P z o 4 method, first iron phosphorus FeP 1.5 Grinding to 1000-2000 mesh powder, using ferrophosphorus as Li x Fe y P z o 4 Provide all iron elements and some phosphorus elements, and add the required lithium source Li according to the molar ratio of total lithium elements, total iron elements and total phosphorus elements (0.9~1.1): 1: 1 2 CO 3 and supplementary phosphorus source H 3 PO 4 Mixed ingredients with ferrophosphorus to form a precursor, ball milled and dried in CO 2 atmosphere 800 o C roasted for 6 hours, cooled and ground to obtain the product, and the reaction equation is as follows:

[0021]

[0022] The XRD pattern of the sample prepared from the reaction ( figure 2 ), the sample has four main crystal plane diffraction peaks (011), (201), (211) and (221) around 2θ=20.7°, 25.5°, 29.7° and 35.6°, which is similar to LiFePO produced by Vale...

Embodiment 2

[0024] On the basis of Example 1, change supplementary phosphorus source, H 3 PO 4 Change to NH 4 h 2 PO 4 Compared with phosphoric acid solution, the price of ammonium dihydrogen phosphate powder is lower, which further reduces the manufacturing cost.

[0025] Ferrophosphorus was prepared by solid-phase synthesis in CO 2 Preparation of Li in atmosphere x Fe y P z o 4 , first crush ferrophosphorus to a certain particle size, then weigh ferrophosphorus, Li 2 CO 3 and NH 4 h 2 PO 4 (Li: Fe: P molar ratio (0.9~1.1): 1:1) mixed, dispersed and ground with alcohol to the rheological phase, dried in CO 2 atmosphere 650 o C firing for 10 hours. The response equation is as follows:

[0026]

[0027] This reaction converts the H in Example 1 3 PO 4 Changed to NH 4 h 2 PO 4 Repeated preparation, it can be seen that LiFePO can still be generated 4 The positive electrode material also has the advantages of Embodiment 1, and further reduces the cost.

Embodiment 3

[0029] The lithium source in the preparation can be replaced by other lithium compounds that do not introduce impurities except lithium carbonate, and LiOH is taken as an example below. Ferrophosphorus was prepared by solid-phase synthesis in CO 2 Preparation of Li in atmosphere x Fe y P z o 4 , first crush ferrophosphorus to a certain particle size, then weigh ferrophosphorus, LiOH and H 3 PO 4 (Li: Fe: P molar ratio (0.9~1.1): 1:1) mixed, dispersed and ground with alcohol to the rheological phase, dried in CO 2 atmosphere 850 o C firing for 4 hours. The reaction equation is as follows:

[0030]

[0031] This reaction will Li in the embodiment 1 2 CO 3 Changed to LiOH for repeated preparation, it can be seen that LiFePO can still be generated 4 The positive electrode material also possesses the characteristics of Example 1.

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Abstract

The present invention relates to by ferrophosphorus in CO 2 Preparation of Li in atmosphere x Fe y P z o 4 method, using iron phosphorus as Li x Fe y P z o 4 Provide all iron elements and some phosphorus elements, according to the molar ratio of total lithium elements, total iron elements and total phosphorus elements (0.9~1.1):1:1, add the required lithium source and supplement the insufficient phosphorus source and phosphorus Iron was mixed and batched to form a precursor, and after ball milling and drying, the 2 Calcined in atmosphere to obtain Li x Fe y P z o 4 finished product. This method overcomes the shortcomings of high cost and single variety caused by the existing reaction atmosphere, and effectively utilizes CO 2 Exhaust gas, so that it provides an oxygen source for oxidation of P in ferrophosphorus while serving as a protective atmosphere, and one-step roasting to obtain Li x Fe y P z o 4 Finished products, turning waste into treasure. The entire reaction control conditions can remove impurities in iron phosphorus, and the tail gas CO produced by the reaction reacts with hot air to form CO 2 And recycling to realize green and clean production. In addition, the reaction process is simple and easy to control, low in cost, low in equipment requirements, and high in resource utilization.

Description

technical field [0001] The invention belongs to the technical field of material manufacturing technology, in particular to 2 Preparation of Li in atmosphere x Fe y P z o 4 new method. Background technique [0002] Currently preparing Li x Fe y P z o 4 For electrode materials, the reaction atmosphere mostly uses N 2 , Ar, H 2 , CO and other inert gases or reducing gases, these gases need to be specially manufactured and produced, and the cost is high. The present invention opens up the direct use of industrial waste gas CO 2 Preparation of Li for the reaction atmosphere x Fe y P z o 4 The new process route of the material expands the CO 2 The application approach overcomes the shortcomings of the current electrode material production atmosphere, such as high price and single raw material, and develops the CO 2 New ways of utilization and Li x Fe y P z o 4 new preparation method. The present invention innovates from the source, and creatively proposes a me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45
Inventor 闫康平崔倩王贵欣李根
Owner SICHUAN UNIV
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