Preparation method of microporous conjugated polymer carbide lithium ion battery anode material

A technology of conjugated polymers and lithium-ion batteries, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of large mass loss, difficulty in controlling the pore structure, and affecting the electrochemical performance of negative electrode materials, achieving high specific capacity, Large magnification, easy mass production effect

Inactive Publication Date: 2013-10-23
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Application Information

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Problems solved by technology

However, most of these hard carbon precursor materials contain hydrogen and oxygen elements. During the carbonization process, the mass loss is large, and it is difficult to control the pore structure, and the developed pore structure is the main factor affecting the electrochemical performance of the negative electrode material.

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  • Preparation method of microporous conjugated polymer carbide lithium ion battery anode material
  • Preparation method of microporous conjugated polymer carbide lithium ion battery anode material
  • Preparation method of microporous conjugated polymer carbide lithium ion battery anode material

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preparation example Construction

[0012] The present invention is a method for preparing a negative electrode material of a microporous conjugated polymer carbonized lithium ion battery. The microporous conjugated polymer with a developed three-dimensional pore structure is used as a precursor, and the porous hard carbon negative electrode material is prepared through carbonization. The specific steps are as follows:

[0013] (1) Preparation of microporous conjugated polymers with three-dimensional pore structure: 1,3,5-triethynylbenzene Polymerization to obtain a microporous conjugated polymer with a rigid three-dimensional network structure; or through the Pd(II)-catalyzed Sonogashira-Hagihara coupling copolymerization of the terminal alkynyl group of the monomer and the halogenated group, the ethynyl aromatic compound monomer and Polymerization of halogenated aromatic compound monomers to obtain microporous conjugated polymers;

[0014] (2) Preparation of porous hard carbon by carbonization of microporou...

Embodiment 1

[0028] Weigh 1.2 g of 1,3,5-triethynylbenzene, 0.17 g of bis(triphenylphosphine)palladium dichloride, and 0.044 g of cuprous iodide, and put them into a container containing 8 ml of toluene and 8 ml of triethyl In the amine flask, the mixture was stirred and reacted for 24 h at 70 °C under nitrogen protection to obtain a yellow polymer. The polymer was washed several times with chloroform, acetone, water and methanol to remove unreacted monomers and residual catalysts; then methanol was used as solvent, and CMP was obtained after Soxhlet extraction of the polymer for 72 h. The prepared CMP is pretreated at a high temperature of 200-400° C. for 1-5 hours in a weakly reducing inert atmosphere to pre-carbonize the CMP. Then, raise the temperature to 600-800°C and keep it warm for 2-10 hours to fully carbonize the CMP, and then cool to room temperature to obtain the target product, the microporous conjugated polymer carbonized negative electrode material. Its SEM photos are as ...

Embodiment 2

[0031] Weigh 0.72 g of 1,3,5-triethynylbenzene, 1.74 g of 1,3,5-tris(4-bromophenyl)benzene, 0.16 g of tetrakistriphenylphosphine palladium, and 0.048 g of cuprous iodide, and put into a flask containing 8 ml of toluene and 8 ml of triethylamine, and the mixture was stirred and reacted for 24 h at 80°C under the protection of nitrogen to obtain a yellow polymer. The polymer was washed several times with chloroform, acetone, water and methanol to remove unreacted monomers and residual catalysts; then methanol was used as solvent, and CMP was obtained after Soxhlet extraction of the polymer for 72 h. The prepared CMP is pretreated at a high temperature of 200-400° C. for 1-5 hours in a weakly reducing inert atmosphere to pre-carbonize the CMP. Then, raise the temperature to 600-800°C and keep it warm for 2-10 hours to fully carbonize the CMP, and then cool to room temperature to obtain the target product, the microporous conjugated polymer carbonized negative electrode material. ...

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Abstract

The invention relates to a preparation method of microporous conjugated polymer carbide lithium ion battery anode material. The method comprises the steps of: firstly, carrying out self-coupling polymerization reaction on alkynyl at the tail end of a monomer catalyzed by Pd (II) / Cu (I), and polymerizing 1, 3, 5-tri-acetenyl benzene to obtain microporous conjugated polymer with a rigid three-dimensional network structure; or carrying out coupling copolymerization reaction on the alkynyl at the tail end of a monomer catalyzed by Pd (II) and Sonogashira-Hagihara with a halogenated group, and polymerizing acetenyl aromatic compound monomer and halogenated aromatic compound monomer to obtain the microporous conjugated polymer; then, carrying out pretreatment on precursor mixture in weak reductive inert atmosphere at the high temperature of 200-400 DEG C for 1-5h to carbonize the microporous conjugated polymer in advance; heating up to 600-800 DEG C, and carrying out heat preservation for 2-10h to fully carbonize the microporous conjugated polymer; and cooling to the room temperature to obtain the target product microporous conjugated polymer carbide anode material.

Description

technical field [0001] The invention relates to a preparation technology of a negative electrode material of a lithium ion battery. Background technique [0002] Anode materials are a key component of lithium-ion batteries, and their performance directly determines the performance of lithium-ion batteries. Traditional graphite lithium-ion battery anode materials: low specific capacity (about 300 mAh / g), poor rate charge and discharge performance, poor cycle performance (about 500 times), it is difficult to meet the requirements of lithium-ion battery development. Hard carbon materials are composed of interlaced single graphite layers; when intercalating lithium, Li + Can be embedded on both sides of a single graphite layer, so hard carbon has a higher specific capacity, up to 900 mAh / g. In addition, hard carbon has better overcharge resistance than graphite. When lithium intercalation is 110%, metal lithium will not be precipitated on the surface, and the safety performanc...

Claims

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Application Information

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IPC IPC(8): H01M4/583
CPCY02E60/12Y02E60/10
Inventor 李安张庆堂孙寒雪王晓梅
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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