Preparation method for lithium titanate

A technology of lithium titanate and lithium titanate, applied in chemical instruments and methods, titanium compounds, inorganic chemistry, etc., can solve the problems of poor material performance, high equipment requirements, long process flow, etc., to improve conductivity and follow-up Processability, improvement of ionic conductivity, and improvement of process performance

Active Publication Date: 2013-12-25
四川新锂想能源科技有限责任公司
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Problems solved by technology

The solid-phase method is to mix the solid raw materials with ball milling and then roast them at high temperature, relying on the solid-phase diffusion between the various components of the raw materials to realize the synthesis. Chinese patent 200610109497.6 uses this method to grind various solid raw materials to a uniformly mixed solid powder, which is placed in a horse Calcination is carried out in a Furnace, the reaction temperature is 500-1200 ° C, and the reaction time is 6-16 hours. The advantages of the solid-phase method are that the process flow is short, simple and easy, and it is easy to produce on a large scale; the disadvantage is that the produced materials have poor performance. High-quality products are not easily available
The chemical precipitation method is to control the appropriate conditions in the aqueous solution of metal salts to make the precipitant react with metal ions to produce hydrated oxides or insoluble compounds, so that the solute is converted into a precipitate, and then separated, dried or calcined to obtain a super Particles, Wu Xianming et al. in "Preparation of Li by Solution Deposition 4/3 Ti 5/3 o 4 Thin films and their properties" disclosed in the preparation of Li 4 Ti 5 o 12 The method: dissolve the lithium acetate of stoichiometric ratio in ethylene glycol methyl ether, then add tetrabutyl titanate dropwise and keep stirring, filter the obtained solution to remove insoluble matter and other impurities, and obtain Li 4/3 Ti 5/3 o 4 Precursor solution, this method has a long process flow and high raw material cost, and the Li obtained by this method 4/3 Ti 5/3 o 4 There are technical defects such as poor conductivity and rapid specific capacity decay when working in a high-rate environment
Nano-Li prepared by sol-gel method 4/3 Ti 5/3 o 4 Potentially improved, but difficult to scale up
The hydrothermal method is one of the solvothermal methods. It is a method in which raw materials are placed in water to react at a higher temperature and pressure to synthesize products. This method can produce nano-scale Li 4 Ti 5 o 12 , the initial electrochemical performance has been improved, and the Chinese invention patent application CN102259911A involves the synthesis of nano-Li by hydrothermal method 4 Ti 5 o 12 : In step 1, fully mix nano-titanium dioxide and lithium hydro

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  • Preparation method for lithium titanate
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  • Preparation method for lithium titanate

Examples

Experimental program
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Effect test

Embodiment 1

[0036] (1) The raw materials (see Table 1 for the specific ratio, Li weight in LiOH: TiO 2 Medium Ti weight = 4:5) Accurately weigh with a 600g electronic balance (accuracy: 0.01g), put it into a stirring grinder with a capacity of 3L, add 1400mL of deionized water, stir and grind at a speed of 1200 rpm for 2 hours made into slurry;

[0037] (2) When the spray dryer is preheated to an outlet temperature of 140°C, add the prepared slurry above to the nozzle for atomization and drying. 92-95°C, 478.00 g of pale white powder was obtained;

[0038] (3) Put the above-mentioned powder into the tubular rotary furnace, close the furnace mouth and pass in nitrogen-hydrogen mixed gas containing 10% (volume fraction) of hydrogen, and start the rotary furnace after 20 minutes (set the rotary speed of the rotary furnace at 2 to 5 revolutions per minute, no special requirements for other parameters), power on and heat up (heating rate 3-5°C / s, other no special requirements) to 790-810°C a...

Embodiment 2

[0042] (1) The raw materials (see Table 1 for the specific ratio, Li weight in LiOH: TiO 2 Medium Ti weight = 4.02:5) Accurately weigh 600 grams of electronic balance (accuracy 0.01 grams), put it into a stirring grinder with a capacity of 3 L, add 2600 mL of distilled water, stir and grind for 3 hours at a speed of 500 rpm slurry;

[0043] (2) When the spray dryer is preheated to an outlet temperature of 160°C, add the prepared slurry above to the nozzle for atomization and drying. 95-98°C, 492.00 g of pale white powder was obtained;

[0044] (3) Put the above-mentioned powder into the tubular rotary furnace, close the furnace mouth and pass in nitrogen-hydrogen mixed gas containing 8% (volume fraction) of hydrogen, and start the rotary furnace after 20 minutes (set the rotary speed of the rotary furnace at 2 to 5 revolutions per minute, no special requirements for other parameters), power on and heat up (heating rate 3-5°C / s, other no special requirements) to 790-810°C and...

Embodiment 3

[0048] (1) The raw materials (see Table 1 for the specific ratio, Li weight in LiOH: TiO 2 Medium Ti weight=4.05:5) Weigh accurately with 600g electronic balance (accuracy 0.01g), put it into a stirring grinder with a capacity of 3L, add 1350mL of deionized water, stir and grind at 1500 rpm for 4.5 hours made into slurry;

[0049] (2) When the spray dryer is preheated to an outlet temperature of 150°C, add the prepared slurry above to the nozzle for atomization and drying. 95-100°C, 498.00 g of pale white powder was obtained;

[0050] (3) Put the above-mentioned powder into the tubular rotary furnace, close the furnace mouth and pass in nitrogen-hydrogen mixed gas containing 12% (volume fraction) of hydrogen, and start the rotary furnace after 20 minutes (set the rotary speed of the rotary furnace at 2-5 revolutions per minute, no special requirements for other parameters), power on and heat up (heating rate 3-5°C / s, other no special requirements) to 790-810°C and keep warm ...

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Abstract

The invention discloses a preparation method for lithium titanate. The preparation method comprises the following steps: (1) preparing a slurry by using a titanium source, a lithium source, an inorganic additive, an organic additive and water; (2) atomizing and drying the slurry prepared by the first step into powder in an atomizing dryer; (3) roasting the powder prepared by the second step at the atmosphere of a hydrogen and nitrogen gas mixture for 5 to 10 hours; (4) cooling the roasted powder obtained by the third step at the atmosphere of the hydrogen and nitrogen gas mixture to room temperature, thereby obtaining the lithium titanate. The lithium titanate prepared by the preparation method is stable in quality; meanwhile, the product has high-rate discharge performance and cycling performance, and is an excellent lithium ion battery anode material.

Description

technical field [0001] The invention relates to a preparation method of lithium titanate, which belongs to the field of lithium ion battery materials. Background technique [0002] With the rapid development of transportation, communication and information industrialization, products such as electric vehicles, notebook computers and mobile communication tools have put forward higher and very urgent requirements for the development of new chemical power sources. The development of new secondary green batteries has become an inevitable need. Compared with the traditional secondary battery, lithium-ion battery has rapidly developed into one of the most Important and state-of-the-art secondary batteries. It has become an ideal power source for small and lightweight electronic devices such as cameras, mobile phones, notebook computers, and portable measuring instruments, and it is also the preferred power source for lightweight high-energy power batteries for future electric ve...

Claims

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Application Information

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IPC IPC(8): H01M4/485C01G23/00
CPCY02E60/10
Inventor 岳波凌睿向中林
Owner 四川新锂想能源科技有限责任公司
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