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A method of synthesizing nitrogen-containing sulfur-containing multistage porous charcoal through a solid phase process

A solid-phase method, nitrogen-sulfur technology, applied in the preparation/purification of carbon, electrical components, electrochemical generators, etc., can solve the problems of poor controllability of the pore structure and morphology of carbon materials, and achieve good electrochemical performance , the effect of good electronic conductivity

Active Publication Date: 2017-06-23
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

Usually, the preparation of such carbon materials needs to first obtain melamine resin in a complicated way, and the controllability of the pore structure and morphology of the prepared carbon materials is also poor.

Method used

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  • A method of synthesizing nitrogen-containing sulfur-containing multistage porous charcoal through a solid phase process
  • A method of synthesizing nitrogen-containing sulfur-containing multistage porous charcoal through a solid phase process
  • A method of synthesizing nitrogen-containing sulfur-containing multistage porous charcoal through a solid phase process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 0.6 g of melamine and 0.7 g of terephthalaldehyde, grind and mix them in a mortar, and at the same time, take 0.6 g of lithium oxide, add it to the above solid mixture, and grind for 30 minutes. The solid mixture was kept under an inert atmosphere at 3°C ​​for min -1 Raise the temperature to 150°C, keep the temperature constant for 240min, then raise the temperature to 550°C at the same heating rate, and keep the constant temperature for 240min. The water and ethanol solution (3:1 volume ratio) of hydrochloric acid with a mass concentration of 10% was used for acid washing at 60°C for 24 hours, and then washed with water and dried at 90°C for 24 hours.

[0025] The scanning electron microscope of present example gained porous carbon material is as figure 1 shown. The sample has a honeycomb-like morphology, and the thickness of the through-hole wall of the honeycomb is about 5nm. The prepared hierarchical porous carbon has macropores of 80-200nm. The resulting ni...

Embodiment 2

[0027] Take 0.6g of melamine and 0.7g of isophthalaldehyde, grind and mix them in a mortar, and at the same time, take 2.1g of lithium oxide, and add it to the above solid mixture, and grind for 30min. The solid mixture was kept under an inert atmosphere at 3°C ​​for min -1 Raise the temperature to 100°C, keep the temperature constant for 240min, then raise the temperature to 600°C at the same heating rate, and keep the constant temperature for 240min. Use 10% hydrochloric acid water and ethanol solution (3:1 volume ratio) to acid wash at 60°C for 24h, then wash with water and dry at 90°C for 24h.

Embodiment 3

[0029]The bulk nitrogen-containing porous carbon prepared in Example 1 was used as the negative electrode material of the lithium-ion battery. Grind carbon, acetylene black, and PVDF at a mass ratio of 8:1:1, add an appropriate amount of N-methylpyrrolidone, mix well, and coat aluminum foil to prepare pole pieces. The electrode sheet (size 1cm×1cm, about 25-50μm thick) lithium sheet and separator were assembled into a button battery, and its electrochemical performance was tested at a rate current density of 100mA g-1. image 3 is the electrochemical cycling stability curve of the material. The first reversible specific capacity is 1035mAh g -1 , the specific capacity reached 798mAh g after 35 cycles -1 Above, has good cycle stability.

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Abstract

The invention relates to a method of synthesizing porous charcoal containing nitrogen, sulfur and other hetero atoms based on Schiff base chemistry and by utilizing an in-situ solid phase process. A Schiff base reaction between an amino-containing aromatic ring compound (melamine, sulfanilic acid, and the like) and an aromatic-ring-containing aldehyde (terephthalaldehyde, 1,3-benzenedialdehyde or 4,4'-biphenyldicarboxaldehyde) is utilized to generate a nitrogen-containing sulfur-containing polymer. Through a gas-solid phase reaction between a reducing atmosphere such as carbon oxide compounds generated in a pyrolysis process of the polymer and lithium oxide, carbonate is generated in an in-situ manner and adopted as a template for preparing the charcoal material, and acid washing is performed to remove the template to obtain the honeycomb porous charcoal material containing nitrogen, sulfur and the like. According to the method, the method is simple to operate, equipment is simple, and the template is generated by an in-situ reaction, thus further preparing the porous structured charcoal material. Through regulating and controlling experiment parameters, the multistage porous charcoal material which contains nitrogen, sulfur and other hetero atoms, which has controllable morphology and an adjustable pore channel structure can be prepared.

Description

technical field [0001] The invention relates to a preparation method for synthesizing nitrogen-containing and sulfur-containing hierarchical porous carbon by a solid-phase method. The honeycomb nitrogen-containing and sulfur-containing hierarchical porous carbon material can be synthesized by using this process, which belongs to the preparation and application of novel heteroatom-doped carbon materials. Its electrode application field. Background technique [0002] Porous carbon is a porous carbonaceous material with ultra-fine particles and surface solid properties in the range of nano-micron and other spatial scales. The nanostructured porous carbon material can be directional modulated in its pore structure and surface chemistry, making it suitable for adsorption Materials, catalyst supports, electrode materials and other fields have shown good application prospects. [0003] In the application field of electrode materials, it is believed that macroporous-mesoporous-micr...

Claims

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Application Information

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IPC IPC(8): C01B32/05H01M4/583H01M4/133H01M4/1393H01M10/0525
CPCC01P2004/03C01P2004/90C01P2006/12C01P2006/16C01P2006/40H01M4/133H01M4/1393H01M4/583H01M10/0525Y02E60/10
Inventor 郭德才陈剑陶韬孙春水
Owner 中科派思储能技术有限公司
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