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A method for rapid preparation of graphene airgel by heteropolyacid catalysis

A graphene aerogel, heteropolyacid technology, applied in the direction of graphene, chemical instruments and methods, carbon compounds, etc., can solve the problems of not meeting the requirements of rapid large-scale production, not suitable for large-scale production, and unable to be practically applied. , to achieve the effect of high mechanical strength, mild process conditions and short time consumption

Active Publication Date: 2020-05-22
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the hydrothermal method has problems such as time-consuming and high energy consumption, which does not meet the requirements of rapid large-scale production
For example, Song Ximing et al reported "a three-dimensional structure graphene airgel composite and its preparation method and application" in the patent CN1068428246A, which is prepared by hydrothermal method, but it takes a long time (12 to 18 hours) and consumes energy High (120-180°C), and generally need to be synthesized under high temperature and high pressure, not suitable for large-scale production, and cannot be practically applied
For another example, Liu Chenyang et al. disclosed "a kind of graphene airgel and its hybrid composite material and its preparation method and application" in CN106422995A, which adopts a relatively mild oil bath heating method (70-100 ° C), but Requires repeated oil baths for up to 18 hours, also has the problem of high energy consumption and long time

Method used

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  • A method for rapid preparation of graphene airgel by heteropolyacid catalysis
  • A method for rapid preparation of graphene airgel by heteropolyacid catalysis
  • A method for rapid preparation of graphene airgel by heteropolyacid catalysis

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Experimental program
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Effect test

Embodiment 1

[0045] (1) First, 0.05 g, 0.025 mmol of phosphomolybdic acid yellow crystals (McLean Biochemical Technology Co., Ltd.) were dissolved in 2 mL of deionized water to form a yellow clear solution, which was designated as solution A;

[0046] (2) Dissolve 0.027 g and 0.25 mmol of p-phenylenediamine powder (McLean Biochemical Technology Co., Ltd.) in 2 mL of deionized water to form a red clear solution, which is designated as solution B.

[0047](3) The two were evenly stirred and mixed to obtain a suspension, which was transferred to a 10 mL glass bottle after ultrasonication at 30 kW for 1 min.

[0048] (4) 3 mL of graphene oxide dispersion with a concentration of 5 mg / mL was injected into a glass vial with a pipette gun, and the graphene hydrogel was obtained after standing for 1 min.

[0049] (5) After the obtained graphene hydrogel is soaked in deionized water to remove unreacted substances, it is pre-frozen at -30°C, and then freeze-dried at -50°C and <10Pa pressure environme...

Embodiment 2

[0053] (1) First, 0.05 g, 0.025 mmol of phosphomolybdic acid crystals (McLean Biochemical Technology Co., Ltd.) were dissolved in 2 mL of deionized water to form a yellow clear solution, which was recorded as solution A;

[0054] (2) Dissolve 0.027 g and 0.25 mmol of 2,6-diaminopyridine powder (McLean Biochemical Technology Co., Ltd.) in 2 mL of deionized water to form a red clear solution, which is designated as solution B.

[0055] (3) The two were evenly stirred and mixed to obtain a suspension, which was transferred to a 10 mL glass bottle after 30 kW ultrasound for 1 min.

[0056] (4) 3 mL of graphene oxide dispersion with a concentration of 5 mg / mL was injected into a glass vial with a pipette gun, and the graphene hydrogel was obtained after standing for 1 min.

[0057] (5) After the obtained graphene hydrogel is soaked in deionized water to remove unreacted substances, it is pre-frozen at -30°C, and then freeze-dried at -50°C and image 3 As shown, a three-dimensional ...

Embodiment 3

[0060] (1) First, 0.05 g, 0.025 mmol of phosphomolybdic acid crystals (McLean Biochemical Technology Co., Ltd.) were dissolved in 2 mL of deionized water to form a yellow clear solution, which was recorded as solution A;

[0061] (2) Dissolve 0.036 g and 0.25 mmol of melamine powder (McLean Biochemical Technology Co., Ltd.) in 2 mL of deionized water to form a red clear solution, which is designated as solution B.

[0062] (3) The two were evenly stirred and mixed to obtain a suspension, which was transferred to a 10 mL glass bottle after ultrasonication at 30 kW for 1 min.

[0063] (4) 3 mL of graphene oxide dispersion with a concentration of 5 mg / mL was injected into a glass vial with a pipette gun, and the graphene hydrogel was obtained after standing for 1 min.

[0064] (5) After the obtained graphene hydrogel is soaked in deionized water to remove unreacted substances, it is pre-frozen at -30°C, and then freeze-dried at -50°C and Figure 5 As shown, a three-dimensional po...

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Abstract

The invention discloses a method for quickly preparing graphene aerogel through heteropoly acid catalysis. The method comprises the following steps: uniformly mixing a phosphomolybdic acid solution with an aromatic amine solution, thus obtaining a mixed solution; then adding a graphene oxide dispersion solution in the mixed solution, and standing, thus obtaining graphene hydrogel; prefreezing after soaking and washing the graphene hydrogel by using water, and then carrying out freeze drying, thus obtaining the graphene aerogel. The method disclosed by the invention is simple in preparation technology, easy to operate, short in consumed time, low in energy consumption, wide in source of raw materials and relatively low in price, graphene aerogel blocks in different sizes can be produced toa large scale, and the obtained graphene aerogel has excellent performance in aspect of supercapacitor electrodes.

Description

[0001] (1) Technical field [0002] The invention relates to a method for rapidly preparing graphene airgel by heteropolyacid catalysis. [0003] (2) Background technology [0004] As a new type of three-dimensional material, graphene airgel has attracted great attention, which is mainly composed of graphite sheets interlaced and connected in three-dimensional space. Graphene airgel has a low density (1 ~ 50mg / cm 3 ), high porosity (>50%), large specific surface area, good mechanical properties, good electrical conductivity and chemical stability. It can be used as a dielectric material for clean energy storage such as hydrogen and natural gas, and an electric energy storage such as an electrode material for supercapacitors. It also has important application prospects in the fields of heterogeneous catalysis, sewage treatment and sensors. [0005] Graphene aerogels are generally prepared from graphene hydrogels by low-temperature freeze-drying or supercritical drying techn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184H01G11/24H01G11/36
CPCC01B32/184C01B2204/22H01G11/24H01G11/36Y02E60/13
Inventor 高静佟明兴金秋阳刘书杰李国华
Owner ZHEJIANG UNIV OF TECH