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Carbon aerogel prepared from superfine nano aerogel obtained through TEMPO (2,2,6,6-tetramethylpiperidinooxy) oxidation and preparation method of carbon aerogel

A carbon aerogel, ultra-fine nano technology, applied in the field of carbon aerogel and its preparation, can solve the problems of carbon aerogel specific surface area, low porosity, non-uniform structure, etc., and achieves a simple, safe and controllable preparation process. , The effect of uniform structure and rich products

Active Publication Date: 2016-06-15
INST OF WOOD INDUDTRY CHINESE ACAD OF FORESTRY
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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 solve the problems such as low specific surface area, low porosity and uneven structure of the carbon aerogel obtained by mechanical treatment in the existing carbon aerogel preparation process, and to provide an ultra-fine nano Carbon airgel prepared from cellulose airgel and preparation method thereof

Method used

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  • Carbon aerogel prepared from superfine nano aerogel obtained through TEMPO (2,2,6,6-tetramethylpiperidinooxy) oxidation and preparation method of carbon aerogel
  • Carbon aerogel prepared from superfine nano aerogel obtained through TEMPO (2,2,6,6-tetramethylpiperidinooxy) oxidation and preparation method of carbon aerogel
  • Carbon aerogel prepared from superfine nano aerogel obtained through TEMPO (2,2,6,6-tetramethylpiperidinooxy) oxidation and preparation method of carbon aerogel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1. Extract the bamboo pulp with phenylethanol at a ratio of 1:2 to remove some organic matter, then use glacial acetic acid to adjust the pH to 4-5 and add 1wt% NaClO 2 Heating at 75°C for 1h and bleaching; the bleached bamboo powder is prepared as a 1wt% dispersion by a high-pressure homogenization method to obtain a 1wt% coarse cellulose dispersion;

[0041]2. Add phosphate buffer solution to the above dispersion liquid, adjust the pH of the dispersion liquid to 6.8 and stir on a magnetic stirrer for 5-10 minutes to better disperse the cellulose;

[0042] 3. Then add TEMPO and NaClO, disperse evenly and then add NaClO 2 , TEMPO:NaClO:NaClO 2 1:1:100 (molar ratio), quickly seal the container and heat it to 65°C for 2 hours. After the reaction, add a certain amount of ethanol to terminate the reaction. The amount of ethanol added is ethanol:NaClO 2 =1:500 (molar ratio);

[0043] 4. Repeatedly rinse the obtained dispersion with deionized water until it becomes neutral...

Embodiment 2

[0047] 1. Buy bleached bamboo pulp on the market, crush it through an 80-mesh sieve, prepare a 1wt% dispersion, and store it at 4°C

[0048] 2. Take 400ml of the above dispersion, stir it evenly, add 300ml of phosphate buffer solution, and adjust the pH of the dispersion to 6.8.

[0049] 3. Then add TEMPO and NaClO, disperse evenly and then add NaClO 2 , TEMPO:NaClO:NaClO 2 The molar ratio is 1:13:100, and the container is quickly sealed and heated to 70°C for 1-2 hours. After the reaction, a certain amount of ethanol is added to terminate the reaction. The amount of ethanol added is ethanol: NaClO 2 =1:300 (molar ratio);

[0050] 4. Repeatedly rinse the obtained dispersion with deionized water until it becomes neutral, and then use an ultrasonic pulverizer (1500W) to sonicate the dispersion for 1 hour;

[0051] 5. Substitute the dispersion with tert-butanol to obtain a gel, freeze the obtained gel at -20°C for 4 hours, and obtain nanocellulose airgel after freeze-drying; ...

Embodiment 3

[0054] 1. Buy bleached bamboo pulp on the market, crush it through an 80-mesh sieve, prepare a 1wt% dispersion, and store it at 4°C

[0055] 2. Take 400ml of the above dispersion, stir it evenly, add 0.064g of TEMPO and 0.4g of NaBr, after the dispersion is uniform, add 2mol / LNaClO, use 0.5mol / LNaOH to control the pH of the dispersion at 10.2, react for 1h, then add 25ml of ethanol to terminate reaction;

[0056] 3. Repeatedly rinse the obtained dispersion with deionized water until it becomes neutral, and then use an ultrasonic pulverizer (1500W) to sonicate the dispersion for 2 hours;

[0057] 4. Replace the dispersion with tert-butanol to obtain a gel, freeze the obtained gel at -80°C for 4 hours, and obtain nanocellulose airgel after freeze-drying;

[0058] 5. Heat the nanocellulose airgel in a tube furnace Ar 2 Under protection, heat at 5°C / min to 800°C and hold for 1.5h, then rapidly cool down at 8°C / min to obtain carbon aerogels with better morphology.

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Abstract

The invention discloses carbon aerogel prepared from superfine nano aerogel obtained through TEMPO (2,2,6,6-tetramethylpiperidinooxy) oxidation. The superfine nano aerogel is prepared with a TEMPO oxidation method, then, preoxidation at the high temperature is performed, and the carbon aerogel is prepared with a carbonization method under the inert gas shielding condition. Used TEMPO is an environment-friendly solvent and has high safety, and therefore, the prepared carbon aerogel cannot have toxicity and cannot corrode instrument equipment or pollute the environment. TEMPO as an oxidizing agent can be recycled, and the condition of environment pollution caused by metal ions serving as a catalyst can be avoided.

Description

technical field [0001] The invention relates to carbon airgel, in particular to a carbon airgel prepared by using TEMPO-oxidized ultrafine nano-airgel and a preparation method thereof. Background technique [0002] Nanocellulose airgel is a new type of material, with a particle size ranging from 1 to 100 nm, and is a typical three-dimensional nanomaterial. The raw materials for the synthesis of nanocellulose aerogels come from a wide range of sources, such as cotton, plant roots, fruit skins, tunicates, mollusk shells, some microorganisms, etc. (Angew.Chem.Int.Ed.2012,51,1–6). The raw materials selected by the method are wood pulp, bamboo pulp and crop stalks. These raw materials are biodegradable, non-toxic, and are the largest natural polymers in the world. The airgel made of TEMPO oxidized nanocellulose has a higher aspect ratio (diameter of 3-5nm, length of 500-700nm) compared to airgel directly obtained by other mechanical and chemical treatments. , and the surface c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
CPCC01P2002/82C01P2004/03C01P2004/04
Inventor 卢芸叶贵超郭娟闫晓美刘波殷亚方袁绯玭张毛毛
Owner INST OF WOOD INDUDTRY CHINESE ACAD OF FORESTRY
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