CN111439745B - Preparation method of single-layer or few-layer biomass graphene - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 51
- 239000010410 layer Substances 0.000 title claims abstract description 25
- 239000002028 Biomass Substances 0.000 title claims abstract description 22
- 239000002356 single layer Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000010902 straw Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000003763 carbonization Methods 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000007800 oxidant agent Substances 0.000 claims description 12
- 230000001590 oxidative effect Effects 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 claims description 6
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 6
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000010923 batch production Methods 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 240000006394 Sorghum bicolor Species 0.000 description 5
- 235000011684 Sorghum saccharatum Nutrition 0.000 description 5
- 240000008042 Zea mays Species 0.000 description 5
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 5
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 235000005822 corn Nutrition 0.000 description 5
- 235000014676 Phragmites communis Nutrition 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005411 Van der Waals force Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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Abstract
本发明公开了一种单层或少层生物质石墨烯的制备方法。以天然农作物秸秆为原材料，通过先进行剥离工艺，再进行碳化工艺，可制得单层生物质石墨烯；通过先进行碳化工艺，再进行剥离工艺，可制得少层生物质石墨烯。通过调节工艺参数，可以调控所制得的石墨烯的层数、微观尺寸大小以及石墨烯表面的缺陷。与现有技术相比，本发明的石墨烯制备方法以廉价易得的农作物秸秆为原料，制得单层和少层石墨烯。本发明采用的生物质石墨烯的制备方法具有工艺条件温和、工艺简单易操作、设备要求低、生产成本低等优点，能实现大规模批量生产，具有良好的应用前景。The invention discloses a preparation method of single-layer or few-layer biomass graphene. Using natural crop straws as raw materials, single-layer biomass graphene can be obtained by first performing a peeling process and then a carbonization process; by first performing a carbonization process and then performing a peeling process, few-layer biomass graphene can be obtained. By adjusting the process parameters, the number of layers, the microscopic size and the defects of the graphene surface can be regulated. Compared with the prior art, the graphene preparation method of the present invention uses cheap and easily available crop straws as raw materials to prepare single-layer and few-layer graphene. The preparation method of biomass graphene adopted in the present invention has the advantages of mild process conditions, simple and easy operation, low equipment requirements, low production cost, etc., can realize large-scale batch production, and has good application prospects.
Description
Technical Field
The invention belongs to the technical field of low-dimensional material preparation, and relates to a method for preparing single-layer or few-layer graphene by using natural crop straws.
Background
(1) Graphene is a carbon atom sp2The hybridized six-membered rings are arranged to form the two-dimensional carbon material with honeycomb crystal lattices. Graphene sheets can be stacked by pi-pi to form graphite with an interlayer spacing of about 0.335 nm. Therefore, graphene is considered as an infinite extension of an aromatic macromolecule on a two-dimensional plane, and is also considered as a basic constituent unit of a graphite-based material such as fullerene, one-dimensional carbon nanotube, or the like. The graphene has excellent electrical properties, thermal conductivity, mechanical properties, optical properties and the like, so that the graphene has wide application prospects in the aspects of novel electronic devices, sensors, energy conversion and storage devices, catalysts, adsorbents, structural reinforcing agents and the like.
(2) Graphene can be prepared by two ways of from bottom to top and from top to bottom at present. The bottom-up method is to use silicon carbide or organic micromolecules as a carbon source and rearrange or connect carbon atoms under certain conditions to prepare the graphene. The chemical vapor deposition method is the most studied method for preparing graphene from bottom to top. The graphene with complete structure and few layers can be prepared by a chemical vapor deposition method. However, the chemical vapor deposition method requires the use of expensive metal catalysts and involves the subsequent removal of the catalysts, the reaction is carried out at a high temperature of 600 to 1000 ℃ in the presence of combustible gases, the preparation process is energy-intensive, has a safety hazard, and requires expensive hardware equipment. Therefore, the chemical vapor deposition method for preparing graphene is high in cost and not beneficial to large-scale batch production.
(3) The "top-down" method generally uses high-purity graphite as a raw material, and weakens the van der waals force between graphite layers by means of stripping, so that the bulk graphite is stripped into single-layer or few-layer graphene. Due to the van der waals force between graphite layers, it is very difficult to completely peel off a large area of single-layer graphene by a top-down method. Common "top-down" methods include ultrasonic exfoliation, electrochemical, chemical, ball milling, and the like. The graphene prepared by the ultrasonic stripping method and the electrochemical method has fewer layers, mild preparation conditions and lower production cost than that of the chemical vapor deposition method. However, such preparation methods are time-consuming, and the prepared graphene has more defects.
(4) The straw of natural crops such as sorghum, corn, rape, reed and the like has a porous loose structure core inside. The straw cores are used for conveying nutrients and water for plant growth. The main components of the straw core are cellulose and hemicellulose. Due to the special microstructure and chemical composition of the crop straw core, the graphene material can be prepared through carbonization and stripping processes. The invention provides a method for preparing graphene under mild conditions by taking crop straw cores as raw materials, which can prepare single-layer graphene and few-layer graphene by controlling process parameters, and has the advantages of simple preparation method, low equipment requirement and low production cost.
Disclosure of Invention
The invention aims to provide a method for preparing single-layer or few-layer graphene by taking natural crop straw cores as raw materials. Preparing single-layer graphene by performing a stripping process and then performing a carbonization process; the few-layer graphene is prepared by firstly carrying out a carbonization process and then carrying out a stripping process. The preparation method has the advantages that stripping process and carbonization process related to the preparation method are mild in condition and short in preparation period, are not affected by the types of raw materials, and biomass graphene with different layers is obtained by changing the process sequence so as to meet the use requirements of different occasions.
The preparation method of the single-layer biomass graphene comprises the following steps:
(1) removing the outer shell of the natural crop straw, and mechanically crushing the straw core into powder, wherein the particle size is controlled within the range of 20 meshes to 160 meshes;
(2) adding 0.1-20 g of strong oxidant into 100mL of water, stirring at normal temperature until the strong oxidant is completely dissolved, adding 1-30 mL of strong acid, and uniformly stirring to obtain stripping liquid A;
(3) adding 1-30 g of straw core powder into stripping liquid, soaking for 0.5-20 h, filtering out solid matter, washing the filtrate with clear water, putting the solid matter into an oven, and drying at 40-100 ℃ for 0.5-4 h;
(4) and putting the dried solid matter into a tubular furnace for carbonization, controlling the temperature rise rate of the tubular furnace to be 5-25 ℃/min, raising the temperature to 200-650 ℃, and preserving the temperature for 1-8 h to obtain the single-layer biomass graphene.
The strong oxidant in the step (2) is one of sodium persulfate, potassium dichromate, potassium permanganate, sodium hypochlorite and sodium bismuthate. The strong acid in the step (2) is one of concentrated nitric acid, concentrated sulfuric acid and concentrated hydrochloric acid.
The preparation method of the few-layer biomass graphene comprises the following steps:
(1) removing the outer shell of the natural crop straw, and mechanically crushing the straw core into powder, wherein the particle size is controlled within the range of 20 meshes to 160 meshes;
(2) adding 0.1-20 g of strong oxidant into 100mL of water, stirring at normal temperature until the strong oxidant is completely dissolved, adding 1-30 mL of strong acid, and uniformly stirring to obtain stripping liquid A;
(3) putting 1-30 g of straw core powder into a tubular furnace for carbonization, controlling the temperature rise rate of the tubular furnace to be 5-25 ℃/min, raising the temperature to 200-650 ℃, and preserving the temperature for 1-8 h to obtain a carbonized product;
(4) adding 1-30 g of carbonized product into stripping liquid, soaking for 0.5-20 h, filtering out solid matter, washing the filtered matter with clear water, putting the solid matter into an oven, and drying at 40-100 ℃ for 0.5-4 h to obtain the few-layer biomass graphene.
The strong oxidant in the step (2) is one of sodium persulfate, potassium dichromate, potassium permanganate, sodium hypochlorite and sodium bismuthate. The strong acid in the step (2) is one of concentrated nitric acid, concentrated sulfuric acid and concentrated hydrochloric acid.
Compared with the prior art, the method has the following beneficial effects:
(1) according to the preparation method provided by the invention, graphene with different layers can be prepared by changing the sequence of stripping and carbonization processes;
(2) the method for preparing the graphene has the advantages of cheap and easily-obtained raw materials, mild process conditions, low equipment requirements, simplicity in operation, low production cost and suitability for large-scale production.
Drawings
Fig. 1 is a scanning electron microscope image of single-layer graphene prepared in example 1 of the present invention. Fig. 2 is a scanning electron microscope image of few-layer graphene prepared in example 4 of the present invention.
Detailed Description
The invention is further illustrated by the following examples, which are intended only for a better understanding of the contents of the invention and do not limit the scope of the invention.
Example 1:
(1) removing the hull of the sorghum straw, and mechanically crushing the sorghum straw core into powder with the size of 40 meshes;
(2) adding 2g of potassium dichromate into 100mL of water, stirring at normal temperature until the potassium dichromate is completely dissolved, adding 12mL of concentrated sulfuric acid, and uniformly stirring to obtain a stripping solution A;
(3) adding 3g of straw core powder into the stripping liquid, soaking for 4 hours, filtering out solid matters, washing the filtrate with clear water, putting the solid matters into a drying oven, and drying at 40 ℃ for 0.5 hour;
(4) and putting the dried solid matter into a tubular furnace for carbonization, controlling the temperature rise rate of the tubular furnace to be 5 ℃/min, raising the temperature to 450 ℃, and preserving the temperature for 4h to obtain the single-layer biomass graphene.
Example 2:
(1) removing the shells of the corn straws, and mechanically crushing the corn straw cores into powder with the size of 60 meshes;
(2) adding 3g of sodium hypochlorite into 100mL of water, stirring at normal temperature until the sodium hypochlorite is completely dissolved, adding 10mL of concentrated nitric acid, and uniformly stirring to obtain a stripping solution A;
(3) adding 2g of straw core powder into the stripping liquid, soaking for 3h, filtering to obtain solid matter, washing the filtrate with clear water, putting the solid matter into an oven, and drying at 50 ℃ for 0.5 h;
(4) and putting the dried solid matter into a tubular furnace for carbonization, controlling the temperature rise rate of the tubular furnace at 10 ℃/min, raising the temperature to 500 ℃, and preserving the temperature for 6 hours to obtain the single-layer biomass graphene.
Example 3:
(1) removing shells of the rape straws, and mechanically crushing the rape straw cores into powder with the size of 100 meshes;
(2) adding 2g of potassium permanganate into 100mL of water, stirring at normal temperature until the potassium permanganate is completely dissolved, adding 8mL of concentrated hydrochloric acid, and uniformly stirring to obtain stripping liquid A;
(3) adding 1g of straw core powder into the stripping liquid, soaking for 5h, filtering to obtain solid matter, washing the filtrate with clear water, putting the solid matter into a drying oven, and drying at 40 ℃ for 1 h;
(4) and putting the dried solid matter into a tubular furnace for carbonization, controlling the temperature rise rate of the tubular furnace at 15 ℃/min, raising the temperature to 600 ℃, and preserving the temperature for 5 hours to obtain the single-layer biomass graphene.
Example 4:
(1) removing the shells of the reed straws, and mechanically crushing the reed straw cores into powder with the grain size of 160 meshes;
(2) adding 5g of sodium persulfate into 100mL of water, stirring at normal temperature until the sodium persulfate is completely dissolved, adding 18mL of concentrated sulfuric acid, and uniformly stirring to obtain a stripping solution A;
(3) putting 10g of straw core powder into a tubular furnace for carbonization, controlling the temperature rise rate of the tubular furnace at 20 ℃/min, raising the temperature to 650 ℃, and preserving the temperature for 3 hours to obtain a carbonized product;
(4) and adding 6g of carbonized product into the stripping solution, soaking for 6h, filtering to obtain solid matter, washing the filtered matter with clear water, putting the solid matter into an oven, and drying at 100 ℃ for 2h to obtain the few-layer biomass graphene.
Example 5:
(1) removing the outer shell of the corn straw, and mechanically crushing the corn straw core into powder with the particle size of 80 meshes;
(2) adding 4g of potassium dichromate into 100mL of water, stirring at normal temperature until the potassium dichromate is completely dissolved, adding 11mL of concentrated nitric acid, and uniformly stirring to obtain a stripping solution A;
(3) putting 30g of straw core powder into a tubular furnace for carbonization, controlling the temperature rise rate of the tubular furnace at 10 ℃/min, raising the temperature to 550 ℃, and preserving the temperature for 7 hours to obtain a carbonized product;
(4) and adding 5g of carbonized product into the stripping solution, soaking for 8h, filtering to obtain solid matter, washing the filtrate with clear water, putting the solid matter into an oven, and drying at 80 ℃ for 4h to obtain the few-layer biomass graphene.
Example 6:
(1) removing the hull of the sorghum straw, and mechanically crushing the sorghum straw core into powder with the particle size of 100 meshes;
(2) adding 6g of sodium bismuthate into 100mL of water, stirring at normal temperature until the sodium bismuthate is completely dissolved, adding 16mL of concentrated hydrochloric acid, and uniformly stirring to obtain stripping liquid A;
(3) putting 30g of straw core powder into a tubular furnace for carbonization, controlling the temperature rise rate of the tubular furnace at 5 ℃/min, raising the temperature to 500 ℃, and preserving the temperature for 6 hours to obtain a carbonized product;
(4) and adding 3g of carbonized product into the stripping solution, soaking for 4h, filtering to obtain solid matter, washing the filtered matter with clear water, putting the solid matter into an oven, and drying at 100 ℃ for 1h to obtain the few-layer biomass graphene.
Claims (3)
1. A preparation method of single-layer biomass graphene is characterized by comprising the following steps:
(1) removing the outer shell of the natural crop straw, and mechanically crushing the straw core into powder, wherein the particle size is controlled within the range of 20 meshes to 160 meshes;
(2) adding 0.1-20 g of strong oxidant into 100mL of water, stirring at normal temperature until the strong oxidant is completely dissolved, adding 1-30 mL of strong acid, and uniformly stirring to obtain stripping liquid A;
(3) adding 1-30 g of straw core powder into stripping liquid, soaking for 0.5-20 h, filtering out solid matter, washing the filtrate with clear water, putting the solid matter into an oven, and drying at 40-100 ℃ for 0.5-4 h;
(4) and putting the dried solid matter into a tubular furnace for carbonization, controlling the temperature rise rate of the tubular furnace to be 5-25 ℃/min, raising the temperature to 200-650 ℃, and preserving the temperature for 1-8 h to obtain the single-layer biomass graphene.
2. The method for preparing single-layer biomass graphene according to claim 1, wherein the strong oxidant in the step (2) is one of sodium persulfate, potassium dichromate, potassium permanganate, sodium hypochlorite and sodium bismuthate; the strong acid is one of concentrated nitric acid, concentrated sulfuric acid and concentrated hydrochloric acid.
3. A preparation method of few-layer biomass graphene is characterized by comprising the following steps:
(1) removing the outer shell of the natural crop straw, and mechanically crushing the straw core into powder, wherein the particle size is controlled within the range of 20 meshes to 160 meshes;
(2) adding 0.1-20 g of strong oxidant into 100mL of water, stirring at normal temperature until the strong oxidant is completely dissolved, adding 1-30 mL of strong acid, and uniformly stirring to obtain stripping liquid A; the strong oxidant is one of sodium persulfate, potassium dichromate, potassium permanganate, sodium hypochlorite and sodium bismuthate; the strong acid is one of concentrated nitric acid, concentrated sulfuric acid and concentrated hydrochloric acid;
(3) putting 1-30 g of straw core powder into a tubular furnace for carbonization, controlling the temperature rise rate of the tubular furnace to be 5-25 ℃/min, raising the temperature to 200-650 ℃, and preserving the temperature for 1-8 h to obtain a carbonized product;
(4) adding 1-30 g of carbonized product into the stripping solution A, soaking for 0.5-20 h, filtering out solid matter, washing the filtered matter with clear water, putting the solid matter into an oven, and drying at 40-100 ℃ for 0.5-4 h to obtain the few-layer biomass graphene.
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