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Preparation method suitable for industrial production and used for nano lithium titanate

A technology of nano-lithium titanate and lithium titanate, which is applied in the direction of electrochemical generators, electrical components, battery electrodes, etc., can solve the problem of unsuitable industrial production of nano-lithium titanate materials, unsuitable for industrial production, and difficult control of process conditions, etc. problems, to achieve the effect of short electron conduction path, cheap raw materials, and environmental friendliness

Inactive Publication Date: 2016-11-23
RISESUN MENGGULI NEW ENERGY SCIENCE & TECHNOLOGY CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sol-gel method has uniform chemical reaction, can achieve atomic-level distribution, controllable stoichiometric ratio, low heat treatment temperature, and can be made into nano-powder; disadvantages: high raw material cost, low yield, large water consumption, and waste water pollution Environment, long process flow, high requirements on equipment; hydrothermal ion exchange synthesis method uses a low-temperature hydrothermal reactor at 100-200 °C to achieve ion exchange, and the reaction takes 24-48 hours; the preparation conditions are not easy to control and are not suitable for industrial production
The self-propagating combustion method also has the problem that the process conditions are not easy to control, and is not suitable for industrial production.
[0005] The above three methods of synthesizing nanomaterials have their own advantages and disadvantages, but none of them are suitable for the industrial production of nano-lithium titanate materials.

Method used

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  • Preparation method suitable for industrial production and used for nano lithium titanate
  • Preparation method suitable for industrial production and used for nano lithium titanate
  • Preparation method suitable for industrial production and used for nano lithium titanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Such as figure 1 Process flow shown. Get the amorphous Ti of 50kg particle average particle size 50nm 0.99 Zr 0.01 o 2 as titanium source, Li 2 CO 3 Lithium source, according to the ratio Li:(Ti 0.99 Zr 0.01 ) (mol%)=4:5; glucose is the carbon source, and the raw materials are weighed according to the carbon content accounting for 2wt% of the final synthesized lithium titanate; pure water is added as a dispersant, and the solid content is adjusted to 50wt%, and the ball mill is mixed evenly Finally, the mixed slurry of the precursor was obtained; using spray drying equipment, the inlet temperature of the hot gas nozzle was 120°C, the outlet temperature was 100°C, the flow rate of the slurry inlet was 20ml / min, and the flow rate of the gas inlet was 30m 3 / h, spray-dry the slurry to obtain dry and loose lithium titanate precursor powder; the gained powder is placed in an atmosphere furnace and fed with N 2 Insulate at 750°C for 8 hours, naturally cool to room tem...

Embodiment 2

[0044] Such as figure 1 Process flow shown. Use 200kg of anatase Ti with an average particle size of 100nm 0.98 al 0.02 o 2 as titanium source, Li 2 CO 3 Lithium source, according to the ratio Li:(Ti 0.98 al 0.02 ) (mol%)=4:5; carboxymethyl cellulose is the carbon source, and each raw material is weighed according to the carbon content accounting for 0.5wt% of the synthesized lithium titanate; distilled water is added as a dispersant, and the solid content is adjusted to 40wt%. Mix uniformly by ball milling to obtain the mixed slurry of the precursor; use spray drying equipment, the inlet temperature of the hot gas nozzle is 180°C, the outlet temperature is 100°C, the flow rate of the slurry inlet is 30ml / min, and the flow rate of the gas inlet is 40m 3 / h, spray-dry the slurry to obtain dry and loose lithium titanate precursor powder; the gained powder is placed in an atmosphere furnace and fed with N 2 Insulate at 780°C for 12 hours, cool naturally to room temperatur...

Embodiment 3

[0046] Such as figure 1 Process flow shown. Use 500kg of anatase Ti with an average particle size of 60nm 0.995 Na 0.005 o 2 as titanium source, Li 2 CO 3 Lithium source, according to the ratio Li:(Ti 0.995 Na 0.005 ) (mol%)=4:5; polyethylene glycol is the carbon source, and each raw material is weighed according to the carbon content accounting for 1wt% of the synthesized lithium titanate; ultrapure water is added as a dispersant, and the solid content is adjusted to 55wt%, Mix uniformly by ball milling to obtain the mixed slurry of the precursor; using spray drying equipment, the inlet temperature of the hot gas nozzle is 200°C, the outlet temperature is 120°C, the slurry inlet flow rate is 25ml / min, and the gas inlet flow rate is 50m 3 / h, spray-dry the slurry to obtain dry and loose lithium titanate precursor powder; the gained powder is placed in an atmosphere furnace and fed with N 2 Insulate at 770°C for 16 hours, cool naturally to room temperature and sieve. Th...

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Abstract

The invention provides a preparation method suitable for industrial production and used for a lithium ion battery anode material nano lithium titanate. The preparation method comprises steps as follows: nanoscale Ti<1-x>MxO2(M is Al, Mg, Ag, Zr, Na, K, Zn or Ca; x is larger than or equal to 0 and smaller than or equal to 0.2) is selected as a titanium source, a lithium source and organic carbon source are added in proportion, water is adopted as a dispersant, wet ball milling and mixing are performed, a precursor is obtained with a pray drying technology, and a doped nano spinel lithium titanate material is obtained through high-temperature treatment. The method adopts cheap raw materials, adopts a simple technology and short processes, is environment-friendly, has low equipment requirement and is suitable for industrial production of the nano lithium titanate material.

Description

technical field [0001] The invention relates to the preparation of a lithium ion battery negative electrode material, in particular to an industrial preparation method of a lithium ion battery negative electrode material nanometer lithium titanate. Background technique [0002] With the widespread application of lithium-ion batteries in hybrid and pure electric vehicles, people have put forward higher requirements for the safety, rate performance and service life of lithium-ion electrode materials. Lithium titanate (Li 4 Ti 5 o 12 ) has the characteristic of "zero strain", during the charging and discharging process of the battery, Li + The insertion and extraction of Li 4 Ti 5 o 12 The crystal structure of the material has little effect and has good cycle performance. At the same time, compared with the currently widely used carbon anode materials for lithium-ion batteries, Li 4 Ti 5 o 12 It also has a high lithium intercalation potential (1.55V Li + / Li), so tha...

Claims

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Application Information

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IPC IPC(8): H01M4/485H01M10/0525
CPCH01M4/485H01M10/0525Y02E60/10
Inventor 刘建红王兴勤王赛高云吴宁宁
Owner RISESUN MENGGULI NEW ENERGY SCIENCE & TECHNOLOGY CO LTD
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