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Nitrogen-doped carbon aerogel and preparation method thereof

A carbon aerogel and nitrogen doping technology, which is applied in the field of preparation of nitrogen-doped carbon aerogel, can solve the problems of wide explosion range, dangerous operation process, difficult control of doping amount, etc., and achieves easy control and wide application. effect of value

Active Publication Date: 2015-12-16
SINOSTEEL MAANSHAN INST OF MINING RES
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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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  • Nitrogen-doped carbon aerogel and preparation method thereof

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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 nitrogen-doped carbon aerogel and a preparation method thereof. The preparation method of the nitrogen-doped carbon aerogel comprises the following steps: (1) preparing a trihydroxy pyridine solution, adding resorcinol, adding a formaldehyde solution after the solution is clear, and adding potassium carbonate while stirring; (2) leaving the mixture to stand to form aerogel; (3) performing solvent exchange on the aerogel by using acetone, so as to obtain trihydroxy pyridine-resorcinol-formaldehyde gel; (4) putting the trihydroxy pyridine-resorcinol-formaldehyde gel into a supercritical carbon dioxide extraction instrument, and carrying out carbon dioxide supercritical drying, so as to obtain xerogel; (5) putting the xerogel into a temperature programmed control carbonization furnace, and sintering and carburizing under the inert gas protection, so as to obtain the nitrogen-doped carbon aerogel. The preparation method has the advantages that loss of nitrogen content during the carbonization process is avoided, and the nitrogen content is easier to control as compared with the nitrogen content in the traditional doping manner in which melamine (most of which is decomposed) is adopted as a nitrogen source; the prepared nitrogen-doped carbon aerogel can be applied to the fields of supercapacitors, nonmetallic electrocatalysts, lithium ion batteries, fuel cells, lithium-sulfur batteries, and the like.

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 Applications(China)
IPC IPC(8): C01B31/02
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
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