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Method for preparing nitrogen-oxygen codoped biomass porous carbon material through two-step pre-carbonation

A porous carbon material and pre-carbonization technology, applied in the fields of carbon compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of single material composition, easy loss of heteroatoms, loss of heteroatoms, etc. Enhanced chemical adsorption capacity, high repetition rate effect

Active Publication Date: 2018-12-11
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent with the publication number CN108069423A discloses a method for preparing porous materials from marine biomass. The method uses shrimp shells and crab shells to prepare porous carbon materials through the template method. The process is simple and the price is low. However, during the high-temperature carbonization process, nitrogen, Heteroatoms such as oxygen and sulfur are easily lost, so that the composition of the material tends to be single
The conventional one-step activation method is obviously flawed. When the conventional method is used to prepare biomass carbon materials, a relatively simple pre-carbonization method is often used, and the loss of heteroatoms contained in the biomass is relatively serious.

Method used

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  • Method for preparing nitrogen-oxygen codoped biomass porous carbon material through two-step pre-carbonation
  • Method for preparing nitrogen-oxygen codoped biomass porous carbon material through two-step pre-carbonation
  • Method for preparing nitrogen-oxygen codoped biomass porous carbon material through two-step pre-carbonation

Examples

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Effect test

Embodiment 1

[0016] Wash and dry the corn granules, put them in a rigid airtight container to heat up and pressurize, then open the container to communicate with the outside world, so that the corn granules are puffed; put the puffed corn granules into a 50 ml reaction kettle, and heat to 160 ℃ and kept for 24 hours. After cooling down, the product was taken out from the reactor and transferred to a tube furnace. Nitrogen was continuously passed as a protective gas. The temperature was raised to 450°C at a heating rate of 2°C / min and reacted for 2 hours to obtain pre-carbonized Product: Grind the pre-carbonized product and potassium hydroxide in a mortar at a mass ratio of 1:3 to make it evenly mixed, then transfer the mixture to a tube furnace, and heat up to 700°C under nitrogen for 2.5 hours , the obtained product was washed to neutrality and dried to prepare a nitrogen-oxygen co-doped biomass porous carbon material.

Embodiment 2

[0018] Wash and dry the rice granules, put them in a rigid airtight container to heat up and pressurize, and then open the container to communicate with the outside world to make the rice granules puff; put the puffed rice granules into a 50ml reaction kettle and heat to 240 ℃ and keep it warm for 12 hours. After cooling down, the product is taken out from the reaction kettle and transferred to a tube furnace. The nitrogen gas is continuously passed as a protective gas, and the temperature is raised to 450°C at a heating rate of 2°C / min and reacted for 5 hours to obtain the pre-carbonized Product: Grind the pre-carbonized product and potassium hydroxide in a mortar at a mass ratio of 1:3 to make it evenly mixed, then transfer the mixture to a tube furnace, and heat up to 800°C under nitrogen for 1.5 hours , the obtained product was washed to neutrality and dried to prepare a nitrogen-oxygen co-doped biomass porous carbon material.

Embodiment 3

[0020] Wash and dry the soybean granules, put them into a rigid airtight container to heat up and pressurize, then open the container to communicate with the outside world to make the soybean granules puff; put the puffed soybean granules into a 50ml reaction kettle and heat to 200 ℃ and kept for 24 hours. After cooling down, the product was taken out from the reaction kettle and transferred to a tube furnace. The nitrogen gas was continuously passed as a protective gas, and the temperature was raised to 450°C at a heating rate of 2°C / min for 3 hours to obtain the pre-carbonized Product: Grind the pre-carbonized product and potassium hydroxide in a mortar with a mass ratio of 1:3 to make it evenly mixed, then transfer the mixture to a tube furnace, and heat up to 900°C under nitrogen for 2 hours , the obtained product was washed to neutrality and dried to prepare a nitrogen-oxygen co-doped biomass porous carbon material.

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Abstract

The invention discloses a method for preparing a nitrogen-oxygen codoped biomass porous carbon material through two-step pre-carbonation. Crop particles are cleanly cleaned and dried, and are put intoa rigid sealed container for temperature rise and pressurization; after puffing, the crop particles are charged into a reaction kettle for low-temperature pre-carbonation, and are then transferred into a nitrogen gas protection tubular furnace for secondary pre-carbonation; a pre-carbonation product and potassium hydroxide are uniformly mixed; after high-temperature treatment in nitrogen gas, thenitrogen-oxygen codoped biomass porous carbon material is prepared. Through substep pre-carbonation, the biomass multilevel structure and contained heteroatoms are effectively reserved; the biomass carbon material has superhigh specific surface area and richly contains micropore and mesoporous structures and rich nitrogen-oxygen doping sites; when the biomass porous carbon material is applied tolithium-sulfur batteries, the ion and electron transmission rate can be effectively accelerated; the adsorption capacity on polysulfides is enhanced; the shuttle effect is inhibited; the battery performance is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of synthesis of inorganic functional materials, and in particular relates to a method for preparing nitrogen and oxygen co-doped biomass porous carbon materials by two-step pre-carbonization. Background technique [0002] Due to the large pore structure and huge specific surface area, porous carbon materials have the characteristics of strong adsorption capacity, good stability of physical and chemical properties, and convenient regeneration after failure, and have potential and huge applications in the fields of catalysis, separation, and electrode material preparation. value has become a hotspot in material science research. At present, the way of using biomass to prepare carbon materials has received extensive attention. In the existing literature, starch (X. Li, et al. ACS Appl. Mater. Interfaces2017, 9, 10717-10729.), soybean (G.F. Ren, et al . J. Mater. Chem. A 2016, 4, 16507-16515.) The carbon materi...

Claims

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Application Information

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IPC IPC(8): C01B32/324C01B32/348B01J20/20H01M4/62H01M10/052
CPCB01J20/20C01B32/324C01B32/348H01M4/62H01M10/052Y02E60/10
Inventor 武大鹏陈俊良杨勇刚高志永徐芳王红菊曹锟蒋凯
Owner HENAN NORMAL UNIV
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