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A kind of preparation method of bulk nitrogen-containing multi-level porous carbon material

A carbon material and block technology, which is applied in the preparation of new heteroatom-doped carbon materials and their electrode applications, can solve problems such as complex process routes, complex powder structure molding processes, and high processing conditions, and achieve good application prospects , the effect of good cycle stability

Active Publication Date: 2019-06-11
中科派思储能技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of carbon fiber material requires high processing conditions, the process route is more complicated, and the powder structure molding process of carbon fiber material is more complicated, and the powder shape also limits it to have a high mass transfer rate.

Method used

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  • A kind of preparation method of bulk nitrogen-containing multi-level porous carbon material
  • A kind of preparation method of bulk nitrogen-containing multi-level porous carbon material
  • A kind of preparation method of bulk nitrogen-containing multi-level porous carbon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Get 1ml tetraethyl orthosilicate (TEOS) and dissolve in 3ml DMF, stir to obtain colorless transparent solution, meanwhile, prepare 125g L -1 Add 1.5ml of polyacrylonitrile-DMF solution, and add it into TEOS-DMF solution, stir well. Add 0.01728 g of 1,6-hexanediamine solution (the solvent is ethanol and water at 1:1) while stirring at 80°C, and stir evenly. The reaction system was sealed, turned to 90°C for aging for 12 hours, and dried to obtain a block polymer. And put it under the protection of inert atmosphere, 3°C min -1 Raise the temperature to 400°C, keep the temperature constant for 60 minutes, then raise the temperature to 800°C at the same heating rate, and keep the temperature constant for 120 minutes to obtain a bulk carbon-silicon oxide composite with shape retention. Use 8% sodium hydroxide solution in water and ethanol (3:1 volume ratio) to remove silicon at 50°C for 24h, then wash with water and dry at 90°C for 24h.

[0026] The scanning electron micro...

Embodiment 2

[0028] Get 1.2ml tetraethyl orthosilicate (TEOS) and dissolve in 3ml DMF, stir to obtain a colorless transparent solution, meanwhile, prepare 100g L -1Add 5ml of polyacrylonitrile-DMF solution, and add it into TEOS-DMF solution, stir evenly. Add 800ul NH 3 .H 2 O, stir well. Seal the reaction system, transfer it to a certain temperature for aging for 12 hours, and after natural cooling, perform solvent replacement (3 times with ethanol, 3 times with n-hexane and 3 times with trimethylchlorosilane), and dry at 50°C to obtain block polymerization things. And put it under the protection of inert atmosphere, 3 ℃ min -1 Raise the temperature to 400°C, keep the temperature constant for 60 minutes, then raise the temperature to 800°C at the same heating rate, and keep the temperature constant for 120 minutes to obtain a bulk carbon-silicon oxide composite with shape retention. Use 8% sodium hydroxide solution in water and ethanol (3:1 volume ratio) to remove silicon at 50°C for ...

Embodiment 3

[0030] Taking the bulk nitrogen-containing porous carbon prepared in Example 1, a carbon-sulfur composite with a sulfur content of 44% was prepared. Grind the carbon-sulfur composite, acetylene black, and PVDF at a mass ratio of 8:1:1, add an appropriate amount of N-methylpyrrolidone, mix well, and coat the aluminum foil to prepare a pole piece. The electrode sheet (size 1cm×1cm, about 25-50μm thick, containing 0.5-1.5mg of sulfur) was used as the positive electrode, and the lithium sheet was used as the negative electrode to assemble a button battery, and its electric capacity at a rate current density of 0.1C was tested. chemical properties. image 3 is the electrochemical cycling stability curve of the material. The first discharge specific capacity is 1400mAh g -1 , the specific capacity reached 750mAh g after 50 cycles at a current density of 0.1C -1 Above, has good cycle stability.

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Abstract

The invention relates to a method for preparing polyacrylonitrile-based lumpy nitrogenous porous charcoal. The method comprises the steps: taking polyacrylonitrile as a precursor, taking DMF, DMSO or DMSO / water as a solvent, and preparing a polyacrylonitrile-based lumpy polymer by a stable-system sol-gel process by using a hydrogen bonding action between polyacrylonitrile and a silicon source hydrolyzate, i.e., silicic acid obtained under base catalysis; and putting the polyacrylonitrile-based lumpy polymer in a charring furnace, carrying out charring under the protection of an inert atmosphere, and removing SiO2, thereby obtaining a lumpy nitrogenous multistage-pore-passage-structured charcoal material. According to the method disclosed by the invention, the preparation method is simple in operation, the equipment is simple, the conventional method that polyacrylonitrile-based charcoal materials are produced by electrostatic spinning is broken through, and the nitrogenous multistage-pore charcoal material with lumpy morphology and an adjustable pore passage structure can be prepared.

Description

technical field [0001] The invention relates to a preparation method of a polyacrylonitrile-based block nitrogen-containing porous carbon material. The process method can be used to synthesize a nitrogen-containing multi-level porous carbon material with a block structure, which belongs to the preparation of a new type of heteroatom-doped carbon material and its electrode application. field. Background technique [0002] Porous carbon is a porous carbonaceous material with ultrafine particles and surface solid properties in the range of nano-micron and other spatial scales. It has rich pore structure and surface chemical structure characteristics. It is used in adsorption materials, catalyst carriers and electrode materials. The field shows good application prospects. [0003] In the application field of electrode materials, it is believed that the macroporous-mesoporous-microporous series-type hierarchical porous block structure carbon material can effectively improve the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/05H01M4/1393H01M4/139
CPCY02E60/10
Inventor 郭德才陈剑陶韬陈浩
Owner 中科派思储能技术有限公司
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