Three-dimensionalgraphene composite aerogel and preparation method thereof

A graphene composite and aerogel technology, applied in the directions of gel preparation, chemical instruments and methods, colloid chemistry, etc., can solve the problems of high cost of preparation methods, single structure, complicated operation, etc., and achieve rich porosity and simple equipment. , a wide range of effects

Active Publication Date: 2017-06-27
INST OF WOOD INDUDTRY CHINESE ACAD OF FORESTRY
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AI-Extracted Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of single unadjustable structure, high cost of preparation method and complicated operation in the existing prepar...
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Abstract

The invention discloses three-dimensionalgraphene composite aerogel. High-molecular material nano fiber with a biomass polysaccharide structure is compounded with oxidized graphene through a surface electrostatic-force effect, and then the composite aerogelis prepared by utilizing hydrazine hydrate reduction and a method for high-temperature pyrolysis in an inert atmosphere. The invention further discloses a preparation method of the three-dimensionalgraphene composite aerogel. The method for preparing the three-dimensionalgraphene composite aerogel is simple, easy to operate, large in specific surface area, uniform in pore size distribution and good in electrical conductivity, and the chemical reactivity is improved.

Application Domain

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  • Three-dimensionalgraphene composite aerogel and preparation method thereof
  • Three-dimensionalgraphene composite aerogel and preparation method thereof
  • Three-dimensionalgraphene composite aerogel and preparation method thereof

Examples

  • Experimental program(5)

Example Embodiment

[0045] Example 1:
[0046] 1. Rinse the bamboo material purchased in the market, dry it and pulverize it through an 80-mesh screen to obtain bamboo powder; take 1g of the pulverized bamboo powder, extract it with phenethyl alcohol at a ratio of 1:2 to remove some organic matter, and then adjust it with glacial acetic acid Add 1wt% NaClO under the condition of pH 4.5 2 Heat at 75℃ for 1h to bleach;
[0047] 2. Prepare the bleached bamboo powder into a 1wt% dispersion, and then mechanically process it to obtain a nanofiber dispersion;
[0048] 3. Stir the 1 wt% nanofiber solution obtained in step 2 on a magnetic stirrer at 500 rpm and normal temperature and pressure for 10 minutes, and then use an ultrasonic mill, 1000 W, for 20 minutes to obtain a uniformly dispersed nanofiber dispersion;
[0049] 4. The uniformly dispersed nanofibers obtained in step 3 use ion exchange methods and mechanical treatment methods to graft positively charged PEI on the surface of the nanofibers to obtain nanocellulose with positively charged groups on the surface;
[0050] 5. Add the positively charged nanofiber dispersion in step 4 to graphene oxide solution (GO) with a mass ratio of 1:5, the mass ratio of nanofibers to graphene oxide is 900:1, and 1000rpm on a magnetic stirrer , Stir at room temperature and pressure for 30 minutes, use an ultrasonic pulverizer, 1200W for 30 minutes to obtain a uniformly mixed solution of nanofibers and graphene oxide;
[0051] 6. Add N to the sample processed in step 5 at room temperature and pressure 2 H 4 ·H 2 O, where N 2 H 4 ·H 2 The mass ratio of O:GO is 1:2, after stirring and dispersing evenly, add NH 3 ·H 2 O adjust the pH of the system to 10, stir on a magnetic stirrer at 800 rpm, at room temperature and pressure for 20 minutes, seal the system after uniform dispersion, heat to 85°C, react for 180 minutes, terminate the reaction and cool to room temperature;
[0052] 7. The reaction solution obtained in step 6 is washed repeatedly with deionized water until it is neutral to obtain a composite solution of nanofibers and graphene;
[0053] 8. Replace the composite solution of nanofibers and graphene obtained in step (7) with tert-butanol to obtain a composite alcogel of nanofibers and graphene, and freeze-dry the obtained alcogel to obtain nanofibers Composite aerogel with graphene;
[0054] 9. Put the nanofiber aerogel obtained in step 8 in a tube furnace, and use a vacuum pump to vacuum it in the tube furnace. 2 In the process, heating at 5°C/min to 700°C for high temperature pyrolysis for 2 hours, and then rapidly cooling at 10°C/min to obtain a three-dimensional graphene composite aerogel with better morphology.

Example Embodiment

[0055] Example 2:
[0056] 1. The eucalyptus pulp purchased in the market is dried and then pulverized through an 80 mesh screen to obtain eucalyptus pulp powder; take 1g of the pulverized eucalyptus pulp powder and extract 1:2 with phenethyl alcohol to remove some organic matter, and then Use glacial acetic acid to adjust pH to 4.5 and add 1wt% NaClO 2 Heat at 75℃ for 1h to bleach;
[0057] 2. Prepare the bleached bamboo powder into a 1wt% dispersion, and then mechanically process it to obtain a nanofiber dispersion;
[0058] 3. Stir the 1 wt% nanofiber solution obtained in step 2 on a magnetic stirrer at 500 rpm at room temperature and pressure for 5 minutes, and then treat it with an ultrasonic mill 1200W for 10 minutes to obtain a uniformly dispersed nanofiber dispersion;
[0059] 4. The uniformly dispersed nanofibers obtained in step 3 are subjected to ion exchange and mechanical treatment methods, and surface active agent CTAB is used for surface cation modification to obtain nanocellulose with positive groups on the surface;
[0060] 5. Add the dispersed nanofibers dispersed in step 4 to graphene oxide solution (GO) with a mass ratio of 1:2.5, the mass ratio of nanofibers to graphene oxide is 500:1, 800rpm on a magnetic stirrer, at room temperature Stir at normal pressure for 40 minutes, and treat with an ultrasonic mill 1200W for 30 minutes to obtain a uniformly mixed solution of nanofibers and graphene oxide;
[0061] 6. Add N to the sample processed in step 5 at room temperature and pressure 2 H 4 ·H 2 O, where N 2 H 4 ·H 2 The mass ratio of O:GO is 1:1.5. After stirring and dispersing uniformly, stir on a magnetic stirrer at 800 rpm at room temperature and pressure for 20 minutes. After the dispersion is uniform, the system is sealed, heated to 90°C, reacted for 120 minutes, and cooled to room temperature after terminating the reaction. ;
[0062] 7. The reaction solution obtained in step 6 is repeatedly washed to neutrality by centrifugation to obtain a composite solution of nanofibers and graphene;
[0063] 8. Replace the composite solution of nanofibers and graphene obtained in step 7 with tert-butanol to obtain a composite alcogel of nanofibers and graphene, and freeze-dry the obtained alcogel to obtain nanofibers and graphite Ene composite aerogel;
[0064] 9. Place the nanofiber aerogel obtained in step 8 in a tube furnace, and use a vacuum pump to pump it into a vacuum state in the tube furnace. 2 In the process, heating at 5°C/min to 800°C for high temperature pyrolysis for 1 hour, and then rapidly cooling at 10°C/min to obtain a three-dimensional graphene composite aerogel with better morphology.

Example Embodiment

[0065] Example 3:
[0066] 1. Dry the industrial waste crab shells and crush them through an 80 mesh screen to obtain crab shell powder; take 1g of crushed crab shell powder and extract 1:2 with phenethyl alcohol to remove some organic matter, and then use glacial acetic acid Add 1wt% NaClO under the condition of adjusting pH to 4.5 2 Heat at 75℃ for 1h to bleach;
[0067] 2. Prepare the bleached crab shell powder into a dispersion with a weight fraction of 1 wt%, and then process the nanofiber dispersion with a mechanical method combined with TEMPO pre-oxidation;
[0068] 3. Stir the 1 wt% nanofiber solution obtained in step 2 on a magnetic stirrer at 300 rpm and normal temperature and pressure for 5 minutes, and then treat it with an ultrasonic mill 1200W for 10 minutes to obtain a uniformly dispersed nanofiber dispersion;
[0069] 4. The uniformly dispersed nanofibers obtained in step 3 are modified by ion exchange and mechanical treatment, and surface active agent CTAB is used for surface cation modification to obtain nanofibers with positively charged groups on the surface;
[0070] 5. Add the positively charged nanofibers dispersed in step 4 to graphene oxide solution (GO) with a mass ratio of 1:2.5, and the mass ratio of nanofibers to graphene oxide is 100:1, on a magnetic stirrer 800 rpm, normal temperature and normal pressure stirring for 40 minutes, and ultrasonic mill 1200W treatment for 30 minutes to obtain a uniformly mixed solution of nanofibers and graphene oxide;
[0071] 6. Add N to the sample processed in step 5 at room temperature and pressure 2 H 4 ·H 2 O, where N 2 H 4 ·H 2 The mass ratio of O:GO is 1:1.5, after stirring and dispersing evenly, add NH 3 ·H 2 O adjust the pH of the system to 10, stir on a magnetic stirrer at 800 rpm, at room temperature and pressure for 20 minutes, seal the system after uniform dispersion, heat to 90°C, react for 120 minutes, and cool to room temperature after terminating the reaction;
[0072] 7. The reaction solution obtained in step 6 is washed repeatedly to neutrality by the method of suction filtration to obtain a composite solution of nanofibers and graphene;
[0073] 8. Replace the composite solution of nanofibers and graphene obtained in step 7 with mannitol to obtain a composite alcogel of nanofibers and graphene, and supercritically dry the obtained alcogel to obtain nanofibers and graphite Ene composite aerogel;
[0074] 9. Put the nanofiber aerogel obtained in step 8 in a tube furnace, and use a vacuum pump to vacuum it in the tube furnace. 3 In the process, the high-temperature pyrolysis is performed at 5°C/min to 800°C for 1 hour, and then rapidly cooled at 10°C/min to obtain a three-dimensional graphene composite aerogel with rich porosity, large specific surface area and better morphology.
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the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
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