CN111439745A - Preparation method of single-layer or few-layer biomass graphene - Google Patents
Preparation method of single-layer or few-layer biomass graphene Download PDFInfo
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Abstract
The invention discloses a preparation method of single-layer or few-layer biomass graphene. Taking natural crop straws as raw materials, and preparing single-layer biomass graphene by firstly carrying out a stripping process and then carrying out a carbonization process; the few-layer biomass graphene can be prepared by firstly carrying out a carbonization process and then carrying out a stripping process. The number of layers, the microscopic size and the defects on the surface of the prepared graphene can be regulated and controlled by regulating the process parameters. Compared with the prior art, the graphene preparation method takes cheap and easily-obtained crop straws as raw materials to prepare single-layer and few-layer graphene. The preparation method of the biomass graphene has the advantages of mild process conditions, simple and easy operation process, low equipment requirement, low production cost and the like, can realize large-scale batch production, and has good application prospect.
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. Thus, graphene is considered to be an infinite extension of aromatic macromolecules in a two-dimensional plane, and is also considered to be an infinite extension of aromatic macromolecules in a two-dimensional planeBasic composition units of graphite-based materials such as fullerene and one-dimensional carbon nanotubes. 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 100m L of water, stirring at normal temperature until the strong oxidant is completely dissolved, adding 1-30 m L 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 100m L of water, stirring at normal temperature until the strong oxidant is completely dissolved, adding 1-30 m L 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 100m L of water, stirring at normal temperature until the potassium dichromate is completely dissolved, adding 12m L 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 100m of L water, stirring at normal temperature until the sodium hypochlorite is completely dissolved, adding 10m of L 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 100m L of water, stirring at normal temperature until the potassium permanganate is completely dissolved, adding 8m L 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 100m L of water, stirring at normal temperature until the sodium persulfate is completely dissolved, adding 18m L of concentrated sulfuric acid, and uniformly stirring to obtain stripping liquid 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 100m L of water, stirring at normal temperature until the potassium dichromate is completely dissolved, adding 11m L of concentrated nitric 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 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 100m L of water, stirring at normal temperature until the sodium bismuthate is completely dissolved, adding 16m L 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 (10)
1. A single-layer or few-layer biomass graphene is characterized in that: taking natural crop straw cores as raw materials, firstly carrying out a stripping process, and then carrying out a carbonization process to prepare single-layer biomass graphene; and the few-layer biomass graphene can be prepared by performing a carbonization process and then performing a stripping process.
2. The method for preparing single-layer biomass graphene according to claim 1, 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 100m L of water, stirring at normal temperature until the strong oxidant is completely dissolved, adding 1-30 m L 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 method for preparing few-layer biomass graphene according to claim 1, 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 100m L of water, stirring at normal temperature until the strong oxidant is completely dissolved, adding 1-30 m L 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.
3. The method for preparing single-layer biomass graphene according to claim 2, wherein the natural crop straw husks are removed in step (1), and the straw core is mechanically crushed into powder, and the particle size is controlled to be in a range of 20 meshes to 160 meshes.
4. The preparation method of single-layer biomass graphene according to claim 2, 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, 0.1-20 g of the strong oxidant is added into 100m L of water and stirred at normal temperature until the strong oxidant is completely dissolved, 1-30 m L of the strong acid is added and stirred uniformly, and then the stripping solution A is prepared.
5. The preparation method of single-layer biomass graphene as claimed in claim 2, wherein 1-30 g of straw core powder is added into the stripping solution and soaked for 0.5-20 h, solid matter is filtered out, the filtrate is washed with clear water, and then the solid matter is put into an oven and dried for 0.5-4 h at 40-100 ℃.
6. The preparation method of single-layer biomass graphene according to claim 2, wherein the dried solid substance in the step (4) is carbonized in a tube furnace, the temperature rise rate of the tube furnace is controlled to be 5-25 ℃/min, the temperature is raised to 200-650 ℃, and the temperature is maintained for 1-8 hours, so that the single-layer biomass graphene is prepared.
7. The method for preparing few-layer biomass graphene according to claim 2, wherein the natural crop straw husks are removed in step (1), and the straw core is mechanically crushed into powder, and the particle size is controlled to be in the range of 20 meshes to 160 meshes.
8. The preparation method of few-layer biomass graphene according to claim 2, 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, 0.1-20 g of the strong oxidant is added into 100m L of water and stirred at normal temperature until the strong oxidant is completely dissolved, 1-30 m L of the strong acid is added and stirred uniformly, and the stripping solution A is prepared.
9. The preparation method of few-layer biomass graphene according to claim 2, wherein 1-30 g of straw core powder is put into a tube furnace for carbonization in the step (3), the temperature rise rate of the tube furnace is controlled to be 5-25 ℃/min, the temperature is raised to 200-650 ℃, and the temperature is kept for 1-8 hours, so that a carbonized product is obtained.
10. The method for preparing few-layer biomass graphene according to claim 2, wherein 1-30 g of carbonized product is added into stripping liquid and soaked for 0.5-20 h in step (4), solid matter is filtered out, the filtrate is washed with clear water, the solid matter is put into an oven and dried at 40-100 ℃ for 0.5-4 h, and then the few-layer biomass graphene is prepared.
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