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A kind of preparation method of se-doped vulcanized polyacrylonitrile material

A technology for vulcanizing polyacrylonitrile and polyacrylonitrile, which is applied to structural parts, lithium batteries, electrical components, etc., can solve the problems of low yield, low sulfur utilization rate, complex synthesis process, etc. Conductivity, effect of simple preparation method

Active Publication Date: 2022-04-01
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the above defects or improvement needs of the prior art, the object of the present invention is to provide a preparation method of Se-doped vulcanized polyacrylonitrile material, wherein by improving the environment and atmosphere of the preparation method, reaction raw materials, reaction mechanism, etc. , directly using S, Se and PAN as raw materials, one-step heat treatment synthesis in a closed environment (such as closed air), compared with the existing technology for preparing Se-doped vulcanized polyacrylonitrile, it can effectively solve the complex synthesis process and low sulfur utilization rate. , low yield, etc., the preparation method of the present invention is simple (especially the preparation environmental conditions are simple), the yield is high, and the environment is friendly

Method used

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  • A kind of preparation method of se-doped vulcanized polyacrylonitrile material
  • A kind of preparation method of se-doped vulcanized polyacrylonitrile material
  • A kind of preparation method of se-doped vulcanized polyacrylonitrile material

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Example 1 (this example corresponds to SPAN without Se doping)

[0042] Preparation of sulfur active material S1#: Weigh PAN and sublimated sulfur powder in a mass ratio of 1:1.8, add an appropriate amount of ethanol as a dispersant for ball milling and mixing, and the obtained mixture is dried at 80 °C, and dried in an air atmosphere. The powder was placed in a closed reaction kettle and heat-treated at 300°C for 500min, and the obtained black powder was the vulcanized polyacrylonitrile composite material SPAN material.

[0043] Preparation of positive electrode sheet P1#: take 800mg SPAN, 100mg conductive agent (Super P) and 2500mg PAA (4wt% PAA / H 2 O solution), mixed, homogenized, coated with a 300 μm thick doctor blade, vacuum dried at 60 °C, cut into discs with a diameter of Φ10 mm, and then dried at 80 °C under vacuum for 4 hours to obtain a single-sided loading of 6 mg / cm 2 Vulcanized polyacrylonitrile composite material SPAN positive plate.

[0044] Preparat...

Embodiment 2

[0045] Example 2 (this example corresponds to Se-doped SPAN)

[0046] Preparation of sulfur active material S2#: take 0.96g Se, 13.44g S, 8g PAN, then add an appropriate amount of ethanol as a dispersant for ball milling and mixing, the obtained mixture is dried at 80 °C, and the dried The powder was placed in a closed reactor and heat-treated at 300 °C for 500 min, and the obtained black powder was the Se-doped vulcanized polyacrylonitrile composite material S. 1-x Se x PAN material.

[0047] Preparation of positive electrode sheet P2#: take 800mg SPAN, 100mg conductive agent (Super P) and 2500mg PAA (4wt% PAA / H 2 O solution), mixed, homogenized, coated with a 300 μm thick doctor blade, vacuum dried at 60 °C, cut into discs with a diameter of Φ10 mm, and then dried at 80 °C under vacuum for 4 hours to obtain a single-sided loading of 6 mg / cm 2 Se-doped vulcanized polyacrylonitrile composite S 1-x Se x PAN cathode sheet.

[0048] Preparation of lithium secondary batte...

Embodiment 3

[0050] Preparation of sulfur active material S3#: the same process as described in Example 2, except that the mass ratio of Se:S was replaced from 1:14 to 1:2.5.

[0051] Preparation of the positive electrode sheet P3#: the same as the preparation method of the positive electrode sheet described in Example 2.

[0052] Preparation of lithium secondary battery C3#: the same process as described in Example 2.

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Abstract

The invention belongs to the technical field of lithium secondary batteries, and discloses a preparation method of Se-doped vulcanized polyacrylonitrile material. The method is to mix polyacrylonitrile PAN with S element and Se element to form a mixture in a closed environment. Heat treatment, thereby preparing the Se-doped vulcanized polyacrylonitrile material in one step; wherein, the heat treatment temperature is 250-380° C., and the heat treatment time is 1-24 hours. The present invention improves the environment and atmosphere of the preparation method, reaction raw materials, reaction mechanism, etc., directly uses S, Se and PAN as raw materials, and synthesizes them by one-step heat treatment in a closed environment (such as closed air). Compared with the vulcanized polyacrylonitrile technology, it can effectively solve the problems of complex synthesis process, low sulfur utilization rate and low yield. The preparation method of the present invention is simple, high in yield and friendly to the environment.

Description

technical field [0001] The invention belongs to the technical field of lithium secondary batteries, and more particularly relates to a preparation method of Se-doped vulcanized polyacrylonitrile material. The preparation method prepares Se-doped vulcanized polyacrylonitrile material by a one-step method, and can further utilize The resulting active material constructs a positive electrode sheet and a corresponding lithium secondary battery. Background technique [0002] With the growing demand for advanced energy storage technologies, research on lithium-ion batteries has become more and more extensive. The energy density of traditional lithium-ion batteries is close to the theoretical upper limit, and it has been difficult to meet the increasing energy density requirements in the field of power batteries. [0003] Sulfurized polyacrylonitrile (SPAN) cathode material has high theoretical specific capacity, good chemical compatibility with commercial carbonate electrolytes, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L33/20C08K3/06C08K3/02H01M4/60H01M10/052
CPCC08K3/06C08K3/02H01M4/604H01M10/052C08L33/20Y02E60/10
Inventor 孙永明王伶月段祥瑞
Owner HUAZHONG UNIV OF SCI & TECH
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