A kind of nitrogen-doped carbon airgel and preparation method thereof

A technology of carbon aerogel and nitrogen doping, applied in the direction of carbon preparation/purification, etc., can solve the problems of wide explosion range, dangerous operation process, difficult to control doping amount, etc., and achieve the effect of easy control and wide application value

Active Publication Date: 2017-09-12
SINOSTEEL MAANSHAN INST OF MINING RES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ammonia gas needs to be heated at high temperature during the doping process, and its explosion range is wide, so the operation process is dangerous
In-situ doping of melamine, a large amount of decomposition occurs during the carbonization process, and its doping amount is difficult to control

Method used

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  • A kind of nitrogen-doped carbon airgel and preparation method thereof
  • A kind of nitrogen-doped carbon airgel and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1. At 40°C, prepare a trihydroxypyridine solution with a concentration of 30g / L, then add resorcinol, and after the solution is clarified, add a formaldehyde solution with a volume concentration of 38%, stir for 20min, and then add a solution with a mass concentration of 40% % potassium carbonate solution, stirred for 10min to obtain a reaction solution; the mol ratio of the trihydroxypyridine to resorcinol was 1:4.6; the mol ratio of the resorcinol to formaldehyde was 1:1.5; the resorcinol The mol ratio of hydroquinone and potassium carbonate is 1:100;

[0029] Step 2. Put the reaction solution into a high-voltage pulse treatment chamber and pretreat it with a high-voltage pulse electric field for 60 minutes, then stir it at a speed of 50 r / min for 1 hour, and then place it in a container at 40 ° C for 3 days to obtain an airgel; The glue is added into acetone and left to stand for solution exchange, and the acetone is replaced every day until the moisture content...

Embodiment 2

[0034]Step 1. At 60°C, prepare a trihydroxypyridine solution with a concentration of 90 g / L, then add resorcinol, and after the solution is clarified, add a formaldehyde solution with a volume concentration of 38%, stir for 50 minutes, and then add a solution with a mass concentration of 60 % potassium carbonate solution, stirred for 30min to obtain a reaction solution; the mol ratio of the trihydroxypyridine to resorcinol was 1:6; the mol ratio of the resorcinol to formaldehyde was 1:2.5; the resorcinol The mol ratio of hydroquinone and potassium carbonate is 1:500;

[0035] Step 2. Put the reaction solution into a high-voltage pulse treatment chamber and pretreat it with a high-voltage pulse electric field for 90 minutes, then stir it at a speed of 100 r / min for 3 hours, and then place it in a container at 60 ° C for 3 days to obtain an airgel; The glue is added into acetone and left to stand for solution exchange, and the acetone is replaced every day until the moisture con...

Embodiment 3

[0040] Step 1. At 50°C, prepare a trihydroxypyridine solution with a concentration of 60g / L, then add resorcinol, and after the solution is clarified, add an acetaldehyde solution with a volume concentration of 38%, stir for 30min, and then add a solution with a mass concentration of 50% potassium carbonate solution was stirred for 20min to obtain a reaction solution; the mol ratio of the trihydroxypyridine to resorcinol was 1:5; the mol ratio of the resorcinol to acetaldehyde was 1:1.5; The mol ratio of said resorcinol and salt of wormwood is 1:300;

[0041] Step 2. Put the reaction solution into a high-voltage pulse treatment chamber and pretreat it with a high-voltage pulse electric field for 80 minutes, then stir it at a speed of 80 r / min for 2 hours, and then place it in a container at 50 ° C for 5 days to obtain an airgel; The glue is added into acetone and left to stand for solution exchange, and the acetone is replaced every day until the moisture content in the exchan...

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Abstract

The invention discloses a nitrogen-doped carbon airgel and a preparation method thereof, comprising: (1) preparing a trihydroxypyridine solution, adding resorcinol, adding formaldehyde solution after the solution is clarified, stirring and adding potassium carbonate; 2) place to form airgel; (3) carry out solvent exchange with acetone to airgel, obtain trihydroxypyridine-resorcinol-formaldehyde gel; (4) gel trihydroxypyridine-resorcinol-formaldehyde Put the gel into a supercritical carbon dioxide extractor, and carry out supercritical carbon dioxide drying to obtain a xerogel; (5) put the xerogel in a programmed temperature-controlled carbonization furnace, sinter and carbonize it under the protection of an inert gas, and obtain a nitrogen-doped gel. Heterocarbon aerogels. The nitrogen content is not lost during the carbonization process of the preparation method of the present invention, and the nitrogen content is easier to control than the traditional doping with melamine (mostly decomposed) as the nitrogen source, and the prepared nitrogen-doped carbon airgel can be applied to supercapacitors, Non-metallic electrocatalysts, lithium-ion batteries, fuel cells and lithium-sulfur batteries and other fields.

Description

technical field [0001] The invention belongs to the field of carbon airgel preparation, and in particular relates to the preparation of a nitrogen-doped carbon airgel in which trihydroxypyridine is used as a nitrogen source and resorcinol-formaldehyde is used as a carbon source. Background technique [0002] Carbon airgel is a new type of nanoporous material with high specific surface area, wide range of density variation, adjustable pore structure and high and stable electrical conductivity in a wide temperature range. It has potential application value in the fields of mechanics, acoustics, electricity, heat and optics. Carbon aerogels generally use phenolic compounds and aldehyde compounds as raw materials, undergo polycondensation reaction under the action of sodium carbonate as a catalyst, form phenolic aerogels, and then obtain carbon foam materials with a network structure through supercritical drying and carbonization. The diameters of nitrogen and carbon atoms are ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/05
Inventor 袁磊王朝阳付志兵常丽娟范勇恒杨曦张厚琼全雪萍何永伟魏鹏郑蕾
Owner SINOSTEEL MAANSHAN INST OF MINING RES CO LTD
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