CN104817075B - A kind of preparation method of highly dispersed graphene oxide nanobelt liquid - Google Patents
A kind of preparation method of highly dispersed graphene oxide nanobelt liquid Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 41
- 239000007788 liquid Substances 0.000 title claims abstract description 20
- 239000002127 nanobelt Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 14
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 33
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 33
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000002074 nanoribbon Substances 0.000 claims abstract description 18
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000007787 solid Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000005520 cutting process Methods 0.000 claims description 11
- 230000010355 oscillation Effects 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002109 single walled nanotube Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000002079 double walled nanotube Substances 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 239000002048 multi walled nanotube Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 238000002156 mixing Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 238000004146 energy storage Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000011232 storage material Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 238000005406 washing Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
本发明提供一种高度分散的氧化石墨烯纳米带液的制备方法，属于碳纳米材料技术领域。该方法主要包含以下步骤：将碳纳米管加入到浓硫酸和高锰酸钾混合搅拌进行物理化学反应，然后将混合液中的固体残余物加入无水乙醇与水的混合液中，在超临界状态下对石墨烯纳米带进行剥离与分散，最后得到高度分散的石墨烯碳纳米带液。本方法操作简便，生产成本低，环境友好，适合工业大规模生产，制备出的石墨烯纳米带比表面积大、孔结构发达、导电性强，可以广泛用作电池、超级电容器的储能材料，也可用作导电导热、吸附、催化剂载体、涂料等应用领域。
The invention provides a method for preparing a highly dispersed graphene oxide nanobelt liquid, which belongs to the technical field of carbon nanomaterials. The method mainly comprises the following steps: adding carbon nanotubes to concentrated sulfuric acid and potassium permanganate and mixing and stirring to carry out a physical and chemical reaction; The graphene nanobelts are exfoliated and dispersed in the state, and finally a highly dispersed graphene carbon nanobelt liquid is obtained. The method is easy to operate, low in production cost, environmentally friendly, and suitable for industrial large-scale production. The prepared graphene nanoribbons have large specific surface area, developed pore structure and strong electrical conductivity, and can be widely used as energy storage materials for batteries and supercapacitors. It can also be used in electrical and thermal conductivity, adsorption, catalyst carrier, coating and other application fields.
Description
Technical Field
The invention relates to the technical field of carbon nano materials.
Background
In 2004, graphene was invented due to its high strength (2.9 μ N/100 nm)2) And high hardness (Young's modulus can approach 1.0TPa, breaking strength up to 130GPa), extremely high carrier movement rate (about 200,000 cm)2·V-1s-1) And a thermal conductivity (5300 W.m) ten times that of copper and better than that of carbon nanotubes-1K-1) Extraordinary specific surface area (up to 2630 m)2Theoretical value of/g) and the like, and has wide application prospect, thereby arousing great interest of people in the method.
The graphene nanoribbon is a ribbon-shaped graphene with a large aspect ratio, inherits the excellent properties of graphene, and has the specific semiconductor performance. Therefore, the graphene nanoribbon has wide application prospects in the fields of novel electronic devices such as super capacitors, solar cells, lithium ion batteries and sensing devices, nano electronic devices, integrated circuits, composite materials and the like.
The existing preparation method for preparing the graphene nanoribbon mainly comprises methods such as alkali metal nanoparticle cutting and temperature difference cutting. The alkali metal nanoparticle cutting method is to cut graphene under the etching action in the annealing process to prepare the graphene nanoribbon. The method has complex production technology, low yield and high cost, and is not suitable for the requirement of industrial macro preparation. The temperature difference cutting method is to prepare the graphene nanoribbon by sequentially processing the carbon nanotube by acid and alkali through high temperature and low temperature. The method needs strong acid, strong alkali, high temperature and low temperature environment, has high requirements on production equipment and high production cost, and is not suitable for industrial production.
Disclosure of Invention
The invention aims to solve the problems that the existing preparation method of the graphene nanoribbon is low in yield, difficult to prepare massively and too complicated to operate, and provides the preparation method of the graphene nanoribbon liquid, which is easy to operate and easy for large-scale production.
The technical scheme adopted for achieving the purpose of the invention is that the preparation method of the graphene nanobelt solution is characterized by comprising the following steps of:
1) cutting the carbon nano tube:
1-1) adding a carbon nano tube into concentrated sulfuric acid, stirring at room temperature for 1-24 hours to obtain a suspension I, wherein the mass (g) of the carbon nano tube is as follows: the volume (ml) of the sulfuric acid is 1: 50-2000.
1-2) adding potassium permanganate into the suspension I, and stirring to obtain a suspension II. The mass ratio of the carbon nano tube (g) to the potassium permanganate (g) is 1: 1-20.
1-3) separating the solid residue from the suspension II.
2) Supercritical dispersion of graphene nanoribbons:
2-1) preparing a mixed solution of absolute ethyl alcohol and water. The ratio of the absolute ethyl alcohol to the water is 1-10: 1
2-2) adding the solid obtained in the step 1) into the mixed solution, and carrying out ultrasonic oscillation for 0.5-2h to uniformly disperse the solid to obtain a suspension III.
2-3) placing the suspension III in a high-pressure container, heating the suspension III, and reacting for 1-8 hours under a supercritical condition to obtain the highly dispersed graphene nanobelt solution.
Further, in the step 1-1), the carbon nanotubes are selected from single-walled carbon nanotubes, double-walled carbon nanotubes or multi-walled carbon nanotubes.
Further, the concentrated sulfuric acid in the step 1-1) has a concentration of 70 wt% -98 wt%,
further, in the step 1-2), after potassium permanganate is added into the suspension I, in the stirring process of the suspension I-potassium permanganate system, the system is stirred at room temperature, then the system is stirred at 60-90 ℃ after being heated, and finally the system is stirred at zero degree of ice bath.
Further, in the step 1-3), the specific process of separating the solid from the suspension II is as follows:
and (3) separating solid residues from the suspension II by suction filtration, and then repeatedly washing the suspension II by deionized water until the pH value of the filtrate is 7.
Further, the high-pressure container in the step 2-3) is filled with supercritical fluid with the pressure of 6-30 MPa.
And after the suspension III is heated, the pressure in the high-pressure container is 6-30MPa, and the temperature is 300-650 ℃.
Compared with the prior art, the invention provides a preparation method of the highly dispersed graphene nanobelt liquid, which comprises the steps of performing physical and chemical cutting on a carbon nano tube by using oxidizing acid and an oxidant, and performing supercritical dispersion on a cut product by using a water-ethanol-carbon dioxide supercritical system to prepare the highly dispersed graphene nanobelt liquid. Compared with the prior art, the whole production process is beneficial to industrial production, the equipment is simple, and the cost is low. The water, carbon dioxide and ethanol used in the supercritical dispersion process are easy to obtain, environment-friendly, nontoxic and harmless. The method disclosed by the invention is simple and convenient to operate, low in production cost and environment-friendly, and the prepared graphene nanoribbon has excellent electrical properties and has a great application prospect particularly in energy storage materials, adsorption materials and microelectronic devices.
Drawings
Fig. 1 is a photograph of the highly dispersed graphene nanobelt liquid prepared in example 1.
Fig. 2 is a scanning electron micrograph of the graphene nanoribbon prepared in example 1.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and examples, but it should not be construed that the scope of the above-described subject matter is limited to the examples. Various substitutions and alterations can be made without departing from the technical idea of the invention and the scope of the invention is covered by the present invention according to the common technical knowledge and the conventional means in the field.
Example 1:
1) cutting the carbon nano tube:
1-1) adding carbon nanotubes into concentrated sulfuric acid, stirring at room temperature for 24 hours to obtain a suspension I, wherein the mass (g) of the carbon nanotubes is as follows: the volume (ml) of the sulfuric acid is 1: 400; the carbon nanotubes are selected from single-walled carbon nanotubes. The concentrated sulfuric acid concentration is 70 wt%.
1-2) adding potassium permanganate into the suspension I, mixing and stirring for 10 hours at room temperature, then heating the mixed solution to 85 ℃, continuously stirring for 4 hours, and then transferring the mixed solution into an ice bath environment, and stirring for 1 hour under a zero-temperature condition to obtain a suspension II; the mass ratio of the carbon nano tube to the potassium permanganate is 1: 7.95;
1-3) filtering the suspension II with suction to separate a solid residue, and washing the obtained solid residue with distilled water until the pH value of the filtrate is 7;
2) supercritical dispersion of graphene nanoribbon liquid:
2-1) mixing the solution according to the volume ratio of anhydrous ethanol to water of 10: 1;
2-2) adding the solid substance obtained in the step 1) into a mixed solution of absolute ethyl alcohol and water, and performing ultrasonic oscillation for 2 hours at room temperature under the condition that the oscillation frequency is 100Hz to uniformly disperse the solid substance to obtain a suspension III;
2-3) placing the suspension III in a high-pressure container filled with carbon dioxide, heating the suspension III until the pressure in the high-pressure container is 7.4MPa, keeping the supercritical reaction at the temperature of 304 ℃ for 6 hours, and then naturally cooling to obtain the highly dispersed graphene nanobelt solution.
Example 2:
1) cutting the carbon nano tube:
1-1) adding carbon nanotubes into concentrated sulfuric acid, stirring at room temperature for 1 hour to obtain a suspension I, wherein the mass (g) of the carbon nanotubes is as follows: the volume (ml) of the sulfuric acid is 1: 50; the carbon nanotubes are selected from single-walled carbon nanotubes. The concentrated sulfuric acid concentration is 80 wt%.
1-2) adding potassium permanganate into the suspension I, mixing and stirring for 1 hour at room temperature, then heating the mixed solution to 60 ℃, continuously stirring for 1 hour, and then transferring the mixed solution into an ice bath environment to stir for 10min under the zero-temperature condition to obtain a suspension II; the mass ratio of the carbon nano tube to the potassium permanganate is 1: 1;
1-3) filtering the suspension II with suction to separate a solid residue, and washing the obtained solid residue with distilled water until the pH value of the filtrate is 7;
2) supercritical dispersion of graphene nanoribbon liquid:
2-1) mixing the solution according to the volume ratio of absolute ethyl alcohol to water of 0: 1;
2-2) adding the solid substance obtained in the step 1) into a mixed solution of absolute ethyl alcohol and water, and performing ultrasonic oscillation for 1h at the room temperature under the condition that the oscillation frequency is 1000Hz to uniformly disperse the solid substance to obtain a suspension III;
2-3) placing the suspension III in a high-pressure container filled with water vapor, heating the suspension III until the pressure in the high-pressure container is 22MPa and the temperature is 647 ℃, maintaining the supercritical reaction for 1 hour, and then naturally cooling to obtain the highly dispersed graphene nanobelt liquid;
example 3:
the preparation method of the graphene nanoribbon liquid is characterized by comprising the following steps:
1) cutting the carbon nano tube:
1-1) adding carbon nanotubes into concentrated sulfuric acid, stirring at room temperature for 24 hours to obtain a suspension I, wherein the mass (g) of the carbon nanotubes is as follows: the volume (ml) of the sulfuric acid is 1: 1000; the carbon nanotubes are selected from multi-walled carbon nanotubes. The concentrated sulfuric acid concentration is 98 wt%.
1-2) adding potassium permanganate into the suspension I, mixing and stirring for 10 hours at room temperature, then heating the mixed solution to 90 ℃, continuously stirring for 10 hours, and then transferring the mixed solution into an ice bath environment, and stirring for 2 hours under a zero-temperature condition to obtain a suspension II; the mass ratio of the carbon nano tube to the potassium permanganate is 1: 10;
1-3) filtering the suspension II with suction to separate a solid residue, and washing the obtained solid residue with distilled water until the pH value of the filtrate is 7;
2) supercritical dispersion of graphene nanoribbon liquid:
2-1) mixing the solution according to the volume ratio of the absolute ethyl alcohol to the water of 5: 1
2-2) adding the solid substance obtained in the step 1) into a mixed solution of absolute ethyl alcohol and water, and performing ultrasonic oscillation for 0.5h at room temperature under the condition that the oscillation frequency is 1MHz to uniformly disperse the solid substance to obtain a suspension III;
2-3) placing the suspension III in a high-pressure container filled with ethanol, heating the suspension III until the pressure in the high-pressure container is 6.4MPa, keeping the supercritical reaction at 516 ℃ for 8 hours, and then naturally cooling to obtain the highly dispersed graphene nanobelt liquid;
example 4:
1) cutting the carbon nano tube:
1-1) adding carbon nanotubes into concentrated sulfuric acid, and stirring at room temperature for 13.5 hours to obtain a suspension I, wherein the mass (g) of the carbon nanotubes is as follows: the volume (ml) of the sulfuric acid is 1: 600; the carbon nanotubes are selected from a mixture of single-walled carbon nanotubes and double-walled carbon nanotubes. The concentrated sulfuric acid concentration is 85%.
1-2) adding potassium permanganate into the suspension I, mixing and stirring for 6 hours at room temperature, then heating the mixed solution to 80 ℃, continuously stirring for 7 hours, and then transferring the mixed solution into an ice bath environment, and stirring for 80min under a zero-temperature condition to obtain a suspension II; the mass ratio of the carbon nano tube to the potassium permanganate is 1: 7;
1-3) filtering the suspension II with suction to separate a solid residue, and washing the obtained solid residue with distilled water until the pH value of the filtrate is 7;
2) supercritical dispersion of graphene nanoribbon liquid:
2-1) mixing the solution according to the volume ratio of the absolute ethyl alcohol to the water of 1: 1;
2-2) adding the solid substance obtained in the step 1) into a mixed solution of absolute ethyl alcohol and water, and performing ultrasonic oscillation for 0.5h at room temperature under the condition that the oscillation frequency is 1MHz to obtain a suspension III;
2-3) placing the suspension III in a high-pressure container filled with nitrogen, heating the suspension III until the pressure in the high-pressure container is 30MPa and the temperature is 800 ℃, maintaining the supercritical reaction for 7 hours, and then naturally cooling to obtain the highly dispersed graphene nanobelt solution.
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| CN106185878A (en) * | 2016-06-06 | 2016-12-07 | 重庆大学 | A kind of graphene nanobelt preparation method |
| CN108622890A (en) * | 2018-04-04 | 2018-10-09 | 北京石墨烯技术研究院有限公司 | A kind of method of graphene oxide separation |
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