Low-temperature hydrothermal method for preparing nano lithium iron phosphate

A lithium iron phosphate and lithium phosphate technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problem of low equipment requirements, and achieve the effect of reducing equipment requirements, reducing equipment investment, and improving production safety

Pending Publication Date: 2022-07-05
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The purpose of the present invention is to solve the above-mentioned defects in the prior art, and provide a method for preparing nano-lithium iron phosphate by low-temperature hydrothermal method. Aiming at the problem that the preparation of nano-lithium iron phosphate by the current hydrothermal method requires high-temperature and high-pressure reaction, by introducing additives, the The hydrothermal reaction temperature is reduced from the conventional 150-280°C to 100-120°C, with mild reaction conditions and low equipment requirements

Method used

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  • Low-temperature hydrothermal method for preparing nano lithium iron phosphate
  • Low-temperature hydrothermal method for preparing nano lithium iron phosphate
  • Low-temperature hydrothermal method for preparing nano lithium iron phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 21g of ferrous sulfate heptahydrate and dissolve it in 70ml of deionized water; add the corresponding lithium phosphate according to the ratio of iron, phosphorus and lithium elements as 1:1:3, and transfer it to the liner of the hydrothermal kettle after sonicating for 30 minutes; after sealing Incubate at 110°C for 10h; cool down naturally to room temperature after the incubation; wash with deionized water and filter until the filtrate is neutral; place the filter cake in an oven at 120°C to dry the nanolithium iron phosphate for 10h. Finally, lithium in lithium iron phosphate: iron: phosphorus = 1:0.95:1.01.

Embodiment example 2

[0035] Weigh 28g of ferrous sulfate heptahydrate and dissolve it in 70ml of deionized water; add the corresponding lithium phosphate according to the ratio of iron, phosphorus and lithium elements as 1:1:3, and transfer it to the liner of the hydrothermal kettle after 40 minutes of ultrasonication; after sealing Incubate at 100°C for 10h; cool down naturally to room temperature after the incubation; wash and filter with deionized water until the filtrate is neutral; place the filter cake in an oven at 120°C to dry the nanolithium iron phosphate for 10h. Lithium: iron: phosphorus = 1:0.98:0.99 in the final lithium iron phosphate.

Embodiment example 3

[0037] Weigh 18g of ferric nitrate and dissolve it in 70ml of deionized water; add the corresponding lithium phosphate according to the ratio of iron, phosphorus, and lithium elements as 1:1:3, and transfer it to the liner of the hydrothermal kettle after sonicating for 30 minutes; seal it and place it at 90 Incubate in ℃ for 10h; after the incubation, cool down to room temperature naturally; use deionized water to wash and filter until the filtrate is neutral; place the filter cake in an oven at 120 ℃ to dry the nanolithium iron phosphate for 10h. Lithium: iron: phosphorus = 1:0.99:1.03 in the final lithium iron phosphate.

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Abstract

The invention provides a low-temperature hydrothermal method for preparing nano lithium iron phosphate. The method comprises the following steps: weighing lithium phosphate, ferrous sulfate and a reaction aid according to a certain proportion; the preparation method comprises the following steps: dissolving ferrous sulfate in a proper amount of deionized water, transferring to a hydrothermal reaction kettle, then adding lithium phosphate and a reaction aid to obtain a solid-liquid mixed suspension, carrying out ultrasonic-assisted dispersion for a certain time, then heating the reaction kettle at a certain temperature, and carrying out heat preservation for a certain time; and washing the product obtained after hydrothermal treatment with deionized water, and drying to obtain the nano lithium iron phosphate. According to the invention, the hydrothermal reaction temperature is effectively reduced, the equipment requirement is reduced, the equipment investment is reduced, and the production safety is improved.

Description

technical field [0001] The invention belongs to the technical field of battery raw materials, and in particular relates to a method for preparing nanometer lithium iron phosphate by low-temperature hydrothermal treatment. Background technique [0002] With the consumption of fossil fuels and the increasing environmental pollution, the utilization of renewable energy (wind energy, solar energy, tidal energy, etc.) has attracted more and more attention, and the development of large-scale energy storage technology has also received more and more attention. Lithium iron phosphate cathode materials have attracted widespread attention due to their low cost and good cycle stability. The preparation methods of lithium iron phosphate mainly include solid phase method and liquid phase method. Among them, the liquid phase method has uniform mixing of raw materials, good product consistency and high cycle times. The liquid-phase process currently mainly refers to the hydrothermal proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58B82Y30/00
CPCC01B25/45H01M4/5825B82Y30/00C01P2004/64C01P2002/72C01P2004/03H01M2004/028
Inventor 吴振国朱超琼杨青张梦珂郭孝东宋扬钟本和
Owner SICHUAN UNIV
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