CN102887508A - Method for preparing high-strength graphite oxide aerogel - Google Patents
Method for preparing high-strength graphite oxide aerogel Download PDFInfo
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- CN102887508A CN102887508A CN201210376937XA CN201210376937A CN102887508A CN 102887508 A CN102887508 A CN 102887508A CN 201210376937X A CN201210376937X A CN 201210376937XA CN 201210376937 A CN201210376937 A CN 201210376937A CN 102887508 A CN102887508 A CN 102887508A
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Abstract
The invention discloses a method for preparing high-strength graphite oxide aerogel. The method is characterized by comprising the following processes of: 1) matching graphite oxide powder and deionized water into a water solution with the concentration being 0.1-10mg/ml, carrying out ultrasonic oscillation for 0.1-5 hours, and obtaining a graphite oxide water solution with good dispersion; 2) adding 10-500ml graphite oxide water solution which is allocated in a water heat kettle, treating for 1-24 hours under the temperature of being 90-200 DEG C, and preparing the graphite oxide aerogel; and 3) putting the prepared graphite oxide aerogel into ammonia water, dipping for 1-36 hours under the temperature being 0-150 DEG C, freezing and drying, and obtaining the high-strength graphite oxide aerogel. The method disclosed the invention has the advantages that the preparing method is simple, the mechanical strength of the graphite oxide aerogel can be increased through simple ammonia water treatment on the basis of the graphite oxide aerogel, the energy consumption is low, no pollution exists, a microcosmic porous structure is matched, and the graphite oxide aerogel has a great application prospect in adsorption and catalysis.
Description
Technical field
The invention discloses a kind of preparation method of high strength graphene oxide aerogel, relate to the three-dimensional self-assembly preparing technical field of graphene oxide.
Background technology
Graphene oxide prepares intermediate product in the Graphene as chemical method, except possessing the peculiar laminate structure of Graphene, self also has some special performances.Multiple oxygen-containing functional group on graphene oxide basal plane and the edge (hydroxyl and carboxyl etc.) is given its higher chemically reactive, the graphene oxide negatively charged ion that carboxy moiety ionization produces makes the sheet interlayer form stable graphene oxide hydrogel with electrostatic interaction.There is research to find, graphene oxide can be regarded amphipathic flexible molecule as, and the six-membered carbon ring of its conjugation is given its hydrophobic nature, and the oxygen-containing functional group on its basal plane makes it have good wetting ability [Franklin Kim, Laural J.Cote, JiaxingHuang, Advanced Materials, 2010,22,1954-1958], can form the graphene oxide hydrogel by liquid-gas interface, make Graphene turn to three-dimensional independent utility by two dimensional application.
Three-dimensional grapheme is broken through the application limitations of traditional zero dimension, peacekeeping two dimension Graphene, can directly apply to electrode of super capacitor, sorbent material, catalyzer with its three-dimensional structure of independently assembling, and greatly be better than itself and binding agent etc. in conjunction with after electrochemical properties.The high congruent people of stone carries out the reduction of self-assembly forming section by hydrothermal method graphene oxide hydrogel [Yuxi Xu, GaoquanShi, et al.AcsNano, 2010,4324-4330].The people such as Zhang Hua have obtained cavernous three-dimensional structure Graphene [Xiehong Cao, Yumeng Shi, et al.Small, 2011,3163-3168] by vapour deposition process is grown in Graphene in the nickel foam substrate.Hydrogel by the assembling of graphene oxide lamella has eco-friendly characteristics, can be applied in useful for drug delivery and the bioengineered tissue, also has great application potential in fields such as catalysis, absorption and electrochemical energy storages.As a kind of novel porous structure material, its porosity rate reaches 80-99.8%, and bore hole size concentrates on 50 μ m, 5 μ m and 5nm, and specific surface area is up to 200-1200m2/g.Because structure and characteristics free from worldly cares, graphene aerogel has a wide range of applications in a lot of fields.But the intensity of the graphene oxide aerogel of preparation is very low at present, thereby restricts its further application.The present invention proposes a kind of preparation method of high strength graphene oxide aerogel, has no at present relevant report.
Summary of the invention
The invention discloses a kind of preparation method of high strength graphene oxide aerogel, with remedy the intensity that present graphene oxide aerogel exists low, limit the defective that it is further used.The inventive method is on the basis of graphene oxide hydrogel preparation, carrying out ammoniacal liquor soaks, not only preparation process is simple, the operating process nontoxic pollution-free, and the gel that makes has preferably physical strength, cooperate its microcosmic vesicular structure, have larger application prospect aspect absorption and the catalysis.
The present invention is achieved by the following technical solutions:
A kind of preparation method of high strength graphene oxide aerogel is characterized in that comprising following process:
1) graphene oxide powder and deionized water being made into concentration is the 0.1-10mg/ml aqueous solution, ultrasonic concussion 0.1-5 hour, obtains finely disseminated graphite oxide aqueous solution;
2) the graphite oxide aqueous solution that configures is got 10-500ml and added in the water heating kettle, processed 1-24 hour under the 90-200 ℃ of temperature, prepare the graphene oxide hydrogel;
3) the graphene oxide hydrogel of preparing is put into ammoniacal liquor, 0-150 ℃, to soak 1-36 hour, lyophilize obtains high-intensity graphene oxide aerogel.
The invention has the advantages that, according to the graphene oxide aerogel of present method preparation except the good conductivity with general gel, also has the larger specific surface area of Graphene, energy consumption is low pollution-free, and this gel shape is controlled, has good mechanical property, its microcosmic vesicular structure, having larger application prospect aspect absorption and the catalysis, also can be used as electrode of super capacitor and further study its excellent conductivity.
Description of drawings
Fig. 1 is the SEM figure of embodiment 1 prepared graphene oxide aerogel;
Fig. 2 is the graphene oxide aerogel XRD figure spectrum that different preparation conditions make;
Fig. 3 is the graphene aerogel Raman spectrum test result that different preparation conditions make;
Fig. 4 is the graphene aerogel examination of infrared spectrum result that different preparation conditions make.
Embodiment
Below by embodiment the present invention is specifically described; following examples are only for the present invention will be further described; can not be interpreted as protection domain restriction of the present invention; improvement and the adjustment of some non-intrinsically safes that those skilled in the art makes according to the content of foregoing invention all belong to protection domain of the present invention.
Embodiment 1
Graphene oxide is mixed with the aqueous solution that concentration is 2mg/ml, and ultrasonic concussion 2h obtains finely disseminated graphite oxide aqueous solution.50ml graphite oxide aqueous solution is added in the water heating kettle, and 180 ℃ of lower processing 20h prepare the graphene oxide hydrogel.Its SEM figure as shown in Figure 1.The graphene oxide hydrogel of preparing is put into ammoniacal liquor, 90 ℃, to soak 1 hour, lyophilize obtains the graphene oxide aerogel of high mechanical strength.
Embodiment 2
Graphene oxide is mixed with the aqueous solution that concentration is 1mg/ml, and ultrasonic concussion 1h obtains finely disseminated graphite oxide aqueous solution.10ml graphite oxide aqueous solution is added in the water heating kettle, and 150 ℃ of lower processing 5h prepare the graphene oxide hydrogel.The graphene oxide hydrogel of preparing is put into ammoniacal liquor, 60 ℃ of lower immersions 5 hours, lyophilize obtains the graphene oxide aerogel of high mechanical strength.
Embodiment 3
Graphene oxide is mixed with the aqueous solution that concentration is 5mg/ml, and ultrasonic concussion 3h obtains finely disseminated graphite oxide aqueous solution.200ml graphite oxide aqueous solution is added in the water heating kettle, and 90 ℃ of lower processing 20h prepare the graphene oxide hydrogel.The graphene oxide hydrogel of preparing is put into ammoniacal liquor, 0 ℃, to soak 36 hours, lyophilize obtains the graphene oxide aerogel of high mechanical strength.
Embodiment 4
Graphene oxide is mixed with the aqueous solution that concentration is 10mg/ml, and ultrasonic concussion 5h obtains finely disseminated graphite oxide aqueous solution.500ml graphite oxide aqueous solution is added in the water heating kettle, and 200 ℃ of lower processing 20h prepare the graphene oxide hydrogel.The graphene oxide hydrogel of preparing is put into ammoniacal liquor, 150 ℃, to soak 18 hours, lyophilize obtains the graphene oxide aerogel of high mechanical strength.
With the graphene oxide aerogel that different preparation conditions obtain, ammoniacal liquor is analyzed its specific surface area and pore structure before and after soaking, and finds that its specific surface area reduces, and mean pore size increases.
With the graphene oxide aerogel that different preparation conditions obtain, before and after ammoniacal liquor soaks, carry out the X-ray diffraction test, find that its interlamellar spacing becomes large to original about 2 times, as shown in Figure 2.
Graphene oxide aerogel with different preparation conditions obtain carries out simple and mechanical strength test, finds that it can support the weight of itself 600 times of quality.
Graphene oxide aerogel with different preparation conditions obtain carries out Raman spectrum and detects before and after ammoniacal liquor soaks, find that the destructiveness to Graphene does not increase before and after soaking.Raman spectrum detects collection of illustrative plates as shown in Figure 3.
The graphene oxide aerogel that different preparation conditions are obtained and detect through the aerogel censorship Fourier infrared spectrum that ammoniacal liquor soaks finds that starting material have had the adding of C-N key, as shown in Figure 4 in immersion process.
Claims (1)
1. the preparation method of a high strength graphene oxide aerogel is characterized in that comprising following process:
1) graphene oxide powder and deionized water being made into concentration is the 0.1-10mg/ml aqueous solution, ultrasonic concussion 0.1-5 hour, obtains finely disseminated graphite oxide aqueous solution;
2) the graphite oxide aqueous solution that configures is got 10-500ml and added in the water heating kettle, processed 1-24 hour under the 90-200 ℃ of temperature, prepare the graphene oxide hydrogel;
3) the graphene oxide hydrogel of preparing is put into ammoniacal liquor, 0-150 ℃, to soak 1-36 hour, lyophilize obtains high-intensity graphene oxide aerogel.
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Cited By (26)
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| CN103626154A (en) * | 2013-12-03 | 2014-03-12 | 南开大学 | Carbon material, and preparation method and use thereof |
| CN103831103A (en) * | 2014-03-14 | 2014-06-04 | 哈尔滨工业大学 | Graphene aerogel catalyst and preparation method thereof |
| CN103991864A (en) * | 2014-05-16 | 2014-08-20 | 中国科学技术大学 | Preparation method of graphene aerogel |
| CN104445162A (en) * | 2014-11-12 | 2015-03-25 | 东莞市青麦田数码科技有限公司 | Graphene oxide aqueous solution and graphene oxide thin film as well as preparation method of graphene oxide thin film |
| CN104973594A (en) * | 2015-06-26 | 2015-10-14 | 江苏大学 | Preparation method and applications of graphene aerogel |
| CN105032354A (en) * | 2015-07-29 | 2015-11-11 | 北京石油化工学院 | Silver nanowire/graphene composite elastic aerogel, and preparation method and application thereof |
| CN105384165A (en) * | 2015-12-18 | 2016-03-09 | 首都师范大学 | Spongy-like lightweight graphene aerogel preparation method |
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| CN106006620A (en) * | 2016-05-27 | 2016-10-12 | 中国科学院城市环境研究所 | Graphene oxide aerogel and graphene aerogel, as well as preparation methods and environmental application of graphene oxide aerogel and graphene aerogel |
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| CN107539980A (en) * | 2017-09-07 | 2018-01-05 | 马鞍山中粮生物化学有限公司 | A kind of novel graphite alkene aerogel material and preparation method thereof |
| CN108101041A (en) * | 2018-03-01 | 2018-06-01 | 济南开发区星火科学技术研究院 | A kind of preparation method of the graphite oxide aerogel of PH sensibility |
| CN108178146A (en) * | 2018-02-02 | 2018-06-19 | 贵州大学 | A kind of method for efficiently preparing high-energy density graphene aerogel |
| CN108715443A (en) * | 2018-08-23 | 2018-10-30 | 燕山大学 | A kind of preparation method of graphene hydrogel |
| CN108878914A (en) * | 2018-06-20 | 2018-11-23 | 西北工业大学 | Oxygen reduction catalyst agent and preparation method thereof based on nitrogen-doped graphene aeroge |
| CN109158129A (en) * | 2018-09-07 | 2019-01-08 | 常州大学 | A kind of preparation of three-dimensional grapheme load C oCu-MOF composite electrocatalyst |
| CN110152599A (en) * | 2018-03-01 | 2019-08-23 | 济南开发区星火科学技术研究院 | It is a kind of can efficient process petroleum desorption liquid graphite oxide aerogel preparation method |
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| CN111001394A (en) * | 2019-12-26 | 2020-04-14 | 武汉工程大学 | Graphene oxide/sodium alginate composite aerogel efficient adsorbent and preparation method and application thereof |
| CN111517774A (en) * | 2020-04-28 | 2020-08-11 | 青岛迦南美地家居用品有限公司 | Preparation method of magnetic graphene oxide aerogel |
| CN111569899A (en) * | 2020-06-03 | 2020-08-25 | 苏州科技大学 | MnFe2O4-TiO2-preparation method of graphene aerogel |
| CN114621011A (en) * | 2022-03-12 | 2022-06-14 | 西北工业大学 | Flaky amorphous Si-C-O aerogel and preparation method thereof |
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