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Preparation method of carbon aerogel

A carbon aerogel and aerogel technology, applied in the field of carbon aerogel preparation, can solve the problems of high toxicity of raw materials and long production cycle, and achieve the effects of reducing environmental burden, shortening cycle and reducing cost

Inactive Publication Date: 2016-10-26
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a kind of preparation method of carbon airgel, to solve the raw material toxicity existing in the prior art; The technical problem of long production cycle

Method used

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  • Preparation method of carbon aerogel
  • Preparation method of carbon aerogel
  • Preparation method of carbon aerogel

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Experimental program
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preparation example Construction

[0023] see figure 1 , the preparation method of carbon aerogel provided by the invention, comprises the following steps:

[0024] 1) Mix the cellulose pretreated by strong acid hydrolysis and additives evenly, put it in a water bath, adjust the pH of the solution to alkaline with an inorganic base, then react for 4 to 8 hours, and obtain oxidized cellulose after drying;

[0025] 2) Under acidic conditions, the oxidized cellulose is chemically cross-linked to form an oxidized cellulose airgel, and the oxidized cellulose airgel is subjected to supercritical carbon dioxide drying, high-temperature pyrolysis and carbonization to obtain a carbon aerogel;

[0026] Additives are the group consisting of oxidizing agents, accelerators and catalysts, the group consisting of oxidizing agents, accelerators and catalysts includes the first group: oxidizing agents sodium hypochlorite, accelerators 2,2,6,6-tetramethylpiperidine-1-oxide free Group consisting of base and catalyst sodium bromi...

Embodiment 1

[0057] (1) Pretreatment of cellulose: use cellulose as raw material, use a beater to perform high-speed mechanical beating for 30 minutes, then soak it in 1M sodium hydroxide solution for 2 days, then use 65% sulfuric acid in a water bath at 45°C hydrolyze in medium for 25 minutes, and finally wash it with deionized water to obtain pretreated cellulose;

[0058] According to the weight ratio in Table 1, the pretreated cellulose is mixed with oxidant, accelerator and catalyst.

[0059] Table 1 prepares the weight ratio table of each component of the additive of oxidized cellulose (parts by weight)

[0060]

[0061] Note: Combinations in the table, the first group: a, b, d and e; the second group: a, b, c and d.

[0062] (2) Preparation of oxidized cellulose: the weight ratio is 95 parts of pretreated cellulose, 3 parts of sodium hypochlorite, 1 part of 2,2,6,6-tetramethylpiperidine-1-oxide radical and sodium bromide Mix 1 part of the raw materials evenly, place it in a wat...

Embodiment 2

[0066] (1) Pretreated cellulose

[0067] Using cellulose as raw material, use a beater to mechanically beat it at high speed for 10 minutes, then soak it in a strong alkali solution for 1 day, then use a strong acid to hydrolyze it in a water bath at 45°C for 25 minutes, and finally wash it with deionized water Obtain pretreated cellulose;

[0068] The strong base is sodium hydroxide or potassium hydroxide, and the molar concentration is 0.2M; the strong acid is sulfuric acid, and the mass concentration is 60%.

[0069] (2) Preparation of oxidized cellulose

[0070] Mix the raw materials with a weight ratio of 95 parts of pretreated cellulose, 1 part of oxidant, 1 part of accelerator and 0.5 part of catalyst, and then place them in a water bath at 30 ° C. Adjust the pH of the solution to Alkaline, then react for 4 hours, and finally freeze-dry to obtain oxidized cellulose;

[0071] The oxidizing agent, accelerator and catalyst are combined according to No. 2 in Table 1, the...

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Abstract

The invention provides a preparation method of carbon aerogel. The method comprises the following steps: selectively oxidizing cellulose primary hydroxyl into carboxyl through a 2,2,6,6-tetramethyl piperidine-1-oxide free radical / sodium bromide / sodium hypochlorite catalysis system to obtain oxidized cellulose, then quickly enabling the oxidized cellulose to be subjected to chemical cross-linking under an acidic condition to form gel, and finally carrying out processes of supercritical drying via carbon dioxide and high-temperature pyrolysis carbonization to obtain a carbon aerogel material with a three-dimensional network structure. The method is short in preparation period; through the method, the carbon aerogel is prepared by taking the innocuous and unpoisonous cellulose as the raw material.

Description

technical field [0001] The invention relates to the technical field of inorganic materials, in particular to a preparation method of carbon airgel. Background technique [0002] Traditional airgel materials include silica, alumina, silica-alumina, resorcinol-formaldehyde (RF) and carbon aerogel, among which carbon aerogel is a light Nanoporous materials with high porosity, large specific surface area, wide range of density changes, and adjustable structure have broad application prospects in the fields of high temperature insulation, electrode materials, catalysts, wastewater treatment, and target materials. Research hotspots in the field of glue in recent years (either provide complete literature information or don't write). [0003] The existing carbon airgel preparation method generally uses resorcinol-formaldehyde system, phenol-formaldehyde system or phenol-furfural system as the basic raw material, and then in the alkaline catalysis of sodium carbonate, magnesium acet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/00C01B31/02
CPCB01J13/0091
Inventor 冯坚张思钊冯军宗姜勇刚
Owner NAT UNIV OF DEFENSE TECH