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Preparation method of sulfur modified polyacrylonitrile material

A polyacrylonitrile and sulfur modification technology, which is applied in the preparation/purification of sulfur, carbon preparation/purification, chemical instruments and methods, etc., can solve the problem that the rate characteristics of sulfur-modified polyacrylonitrile composite materials are not enough for power batteries , The quality of polyacrylonitrile powder is different, etc., to achieve the effect of improving capacity and rate characteristics, improving electrochemical performance, and simple operation

Pending Publication Date: 2021-12-24
ZHEJIANG CHINT ELECTRIC CO LTD
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method can theoretically obtain good rate characteristics, it is limited by the quality of commercially available polyacrylonitrile powders, which makes the current rate characteristics of sulfur-modified polyacrylonitrile composites not enough to be used in power batteries.

Method used

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  • Preparation method of sulfur modified polyacrylonitrile material
  • Preparation method of sulfur modified polyacrylonitrile material

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preparation example Construction

[0030] A preparation method of sulfur-modified polyacrylonitrile material, comprising the following steps:

[0031] In step S1, mixing the acrylonitrile monomer and the emulsifier in deionized water to obtain a first mixed solution, and then adding an initiator for initiating the polymerization reaction to generate polyacrylonitrile solid particles and vacuum drying to obtain polyacrylonitrile solid particles;

[0032] In step S2, mixing polyacrylonitrile solid particles and sublimated sulfur powder in a ball mill tank to obtain a sulfur-polyacrylonitrile mixture;

[0033] In step S3, under nitrogen protection, the sulfur-polyacrylonitrile mixture is heated for carbonization reaction, and the sulfur-modified polyacrylonitrile material is obtained after cooling.

[0034] The preparation method of a sulfur-modified polyacrylonitrile material of the present invention uses acrylonitrile monomers, emulsifiers and initiators to obtain polyacrylonitrile solid particles through the me...

Embodiment 1

[0046] The synthesis of step S1 polyacrylonitrile:

[0047] S1.1 Weigh 20g of acrylonitrile monomer, 1.8g of sodium lauryl sulfate, and 160g of deionized water into the reaction flask and stir evenly to obtain the first mixed liquid. The stirring time is about 30 minutes. Weigh 0.15 g of ammonium persulfate and dissolve it in 20 g of deionized water to make an initiator solution, and add the initiator solution into a constant pressure funnel. It should be noted that the polymerization of acrylonitrile belongs to free radical polymerization, and the initiator solution cannot be added to the flask together with acrylonitrile monomer and sodium lauryl sulfate as an emulsifier, because directly adding ammonium persulfate is easy to cause If the concentration of the initiator in the inner solution is too high, the local polymerization reaction will be violent and exothermic, especially the free radical polymerization self-acceleration phenomenon will be easily strengthened, which w...

Embodiment 2

[0058] Steps S1-S2 are the same as steps S1-S2 in embodiment 1, and the difference from embodiment 1 is in step S3.

[0059] In step S3, 20 g of the ground mixture was weighed and placed in a quartz tube, and heated at 450° C. for 6 hours under nitrogen protection (carbonization process), and a black sulfur-modified polyacrylonitrile material was obtained after natural cooling.

[0060] After testing, the 0.1C cycle for 3 weeks, the discharge gram capacity reached 1288.9mAh·g-1, the capacity retention rate after 0.5C cycle for 80 cycles was 80.1%, and the rate characteristic 1C capacity retention rate was 95.6%.

[0061] As an organic polymer with high nitrogen content, polyacrylonitrile material itself does not have electrical conductivity, but carbonized polyacrylonitrile material has certain electrical conductivity, which is attributed to the molecular structure of polyacrylonitrile material after carbonization. Pyridine ring structure linked composition. The carbonization...

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Abstract

A preparation method of a sulfur modified polyacrylonitrile material comprises the following steps of: S1, mixing an acrylonitrile monomer and an emulsifier well in deionized water, then adding an initiator for initiating a polymerization reaction to generate polyacrylonitrile solid particles, and drying the polyacrylonitrile solid particles under vacuum; S2, ball-milling and mixing the polyacrylonitrile solid particles and sublimed sulfur powder in a ball-milling tank to obtain a sulfur-polyacrylonitrile mixture; and S3, under the protection of nitrogen, heating the sulfur-polyacrylonitrile mixture for a carbonization reaction, and cooling to obtain the sulfur modified polyacrylonitrile material. According to the preparation method of the sulfur-modified polyacrylonitrile material, polyacrylonitrile solid particles are obtained by using the acrylonitrile monomer, the emulsifier and the initiator through an emulsion preparation method, the operation is simple, the raw materials are cheap and easy to obtain, the chemical quality stability of the product is good, and large-scale production is easy.

Description

technical field [0001] The invention relates to the field of positive electrode active materials for lithium secondary batteries, in particular to a preparation method of a sulfur-modified polyacrylonitrile material. Background technique [0002] Compared with traditional secondary batteries, lithium secondary batteries have advantages such as small size and light weight, so lithium secondary batteries have been widely used in various fields. However, with the development of the power battery industry in recent years, traditional lithium-ion batteries have gradually exposed some shortcomings such as low energy density and potential safety hazards. Among many high-energy-density battery material systems, lithium-sulfur battery systems have attracted a large number of With the attention and research of scientific researchers, in addition to elemental sulfur-based composite materials, sulfur-containing polyacrylonitrile materials are ideal materials for lithium-sulfur batteries...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/02C01B32/05C08F220/46C08F222/02H01M4/38H01M4/62H01M10/052
CPCC01B17/0243C01B32/05C08F220/46H01M4/38H01M4/62H01M4/625H01M10/052C08F222/02Y02E60/10
Inventor 涂玉祖倪文彬孙庆娜
Owner ZHEJIANG CHINT ELECTRIC CO LTD
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