CN110803695A - Method for preparing graphene by using large-sized seaweed as raw material - Google Patents
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
A method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps: (1) preparing a precursor: placing the large-scale seaweed powder which is washed by water, dried and crushed by a crusher into a vacuum tube furnace, heating to 500 ℃ under the condition of nitrogen atmosphere, and carrying out heat treatment for 1-3 hours to obtain solid biochar; (2) alkali high-temperature activation: mixing alkali with the biochar obtained in the step (1), fully soaking to uniformly mix the biochar, and carrying out heat treatment under nitrogen gas to activate the biochar at high temperature by the alkali; (3) acid treatment, water washing and drying: and (3) treating the sample obtained in the step (2) with acid liquor, then filtering, washing the obtained solid with water until the washing liquid is neutral, and drying the obtained solid to obtain the graphene. The invention aims to provide a preparation method of graphene by using large-scale seaweed with abundant resources and low cost as a raw material, and simultaneously improve the high-added-value comprehensive utilization of the large-scale seaweed.
Description
Technical Field
The invention belongs to the technical field of graphene preparation, and relates to a method for preparing graphene by using large-scale seaweed as a raw material.
Background
Graphene is a novelDue to the special two-dimensional structure of the carbon nano material, the graphene has a plurality of excellent physical properties. For example, the Young modulus and the breaking strength of the material are respectively as high as 1000GPa and 130GPa, which are equivalent to that of the carbon nano tube, so that the material has the highest strength performance at present; the thermal conductivity coefficient at room temperature is as high as 5300W/(m.K), which is higher than that of diamond and carbon nano tube; the electron mobility can reach 15000cm at normal temperature2V · s, and at the same time, its resistivity is extremely low (10)-6Ω · cm) is the material with the lowest resistivity at present. In addition, the theoretical specific surface area is up to 2630m2Per g, a theoretical thickness of 0.335nm, and is an almost transparent conductor with an absorption of only 2.3% for visible light (a transmission of up to 97.7%). Due to the excellent performance of the graphene, the graphene has wide application prospects in the aspects of electrochemistry, adsorption, catalysis, biomedicine and the like.
At present, the raw materials for preparing graphene mainly comprise graphite, land biomass resources and the like. The graphite is a non-renewable resource and has limited reserves; the land plants have large seasonal fluctuation, and the resources are dispersed and collected, so that a large amount of cost and time are needed, the continuous supply of raw materials is influenced, and the large-scale industrial production is difficult to carry out. For example, publication CN106744836A discloses a method for preparing graphene from biomass raw materials such as corn stalks, wheat stalks, shells and other waste, which requires a high time and cost for collecting raw materials. Compared with land plants, the kelp has the advantages of abundant sources, wide distribution, no occupation of arable land resources, high growth speed and the like, is a biomass resource which is not effectively developed and utilized on the earth, and has more advantages in the aspect of serving as a raw material for preparing graphene.
The preparation method of graphene mainly comprises a physical method and a chemical method. For example, the mechanical exfoliation method and the liquid phase exfoliation method both belong to physical preparation methods, wherein the mechanical exfoliation method is not easy to control the size of graphene, has poor repeatability, and is not suitable for industrial production. The main disadvantage of the liquid phase exfoliation method is that the obtained graphene has low yield. The chemical method for preparing graphene mainly comprises an oxidation-reduction method, a Chemical Vapor Deposition (CVD) method and a crystal epitaxial growth method. The redox method mainly uses graphite as a raw material and is subjected to high-temperature alkalization or graphite oxide self-assembly, and a great amount of chemical substances with high toxicity, strong corrosivity and strong oxidizing property can be consumed in the reaction process; the chemical vapor deposition method takes an organic carbon source as a preparation raw material, and the reaction conditions are harsh; the crystal epitaxial growth method has high preparation cost and low graphene yield, and is difficult to realize large-scale industrial production.
Disclosure of Invention
In order to overcome the defects of high cost and low yield of the existing preparation method of the graphene, the invention aims to provide the preparation method of the graphene by using the large-scale seaweed which is rich in resources and low in cost as the raw material, and simultaneously improve the high-added-value comprehensive utilization of the large-scale seaweed.
The purpose of the invention is realized by the following technical scheme:
a method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps:
(1) preparing a precursor: placing the large-scale seaweed powder which is washed by water, dried and crushed by a crusher into a vacuum tube furnace, heating to 500 ℃ under the condition of nitrogen atmosphere, and carrying out heat treatment for 1-3 hours to obtain solid biochar;
(2) alkali high-temperature activation: mixing alkali with the biochar obtained in the step (1), fully soaking to uniformly mix the biochar, and carrying out heat treatment under nitrogen gas to activate the biochar at high temperature by the alkali;
(3) acid treatment, water washing and drying: and (3) treating the sample obtained in the step (2) with acid liquor, then filtering, washing the obtained solid with water until the washing liquid is neutral, and drying the obtained solid to obtain the graphene.
Further, in the step (1), the water washing means washing the seaweed with water until the filtrate is transparent.
In the step (1), the drying refers to drying at 80-120 ℃ for 12 hours.
In the step (1), the crushing is carried out to 40 meshes by using a crusher.
In the step (1), the temperature is raised to 500 ℃ at a rate of 5-15 ℃/min.
Still further, in the step (2), the alkali is at least one of potassium hydroxide and sodium hydroxide.
In the step (2), the mass ratio of the alkali to the biochar is (2-5) to 1, and preferably 4 to 1.
In the step (2), the sufficient impregnation time is 1-3h, preferably 2h, and the impregnation can fully mix the biochar with alkali.
In the step (2), the flow rate of the nitrogen atmosphere is 300 mL/min.
In the step (2), the heat treatment is carried out by heating to 700-900 ℃ at a heating rate of (5-15) ° c/min in a tube furnace, and then keeping for 1-3 hours.
Furthermore, in the step (3), the acid solution is a hydrochloric acid aqueous solution, the concentration of the acid solution is 0.5 to 3mmol/L, and the acid washing time is 1 to 3 hours.
In the step (3), the drying refers to vacuum drying, and the drying conditions are as follows: the drying time is 12-24 h at 80-110 ℃.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the method, the large-scale seaweed with abundant resources and low cost is used as the raw material to prepare the graphene, the production cost is low, the preparation process is simple and controllable, a catalyst is not used in the preparation process, and the method is green and environment-friendly and is suitable for low-cost industrial production of the graphene. The prepared seaweed-based graphene is multilayer graphene (3-7 layers), has a rich pore structure and a specific surface area of (1411-2069 m)2And/g) has good application prospect in the fields of super capacitors, fuel cells, adsorption and the like.
Drawings
Fig. 1 is a raman spectrum of a multilayer graphene product prepared according to an embodiment of the present invention;
fig. 2 is a transmission electron micrograph of a multilayer graphene product prepared according to an embodiment of the present invention.
Detailed description of the invention
The following will further describe the embodiments of the present invention with reference to the examples and the accompanying drawings, wherein the macroalgae selected in the examples are Sargassum horneri.
Example 1:
a method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps:
(1) preparing a precursor: washing large seaweed-Sargassum horneri from Wenzhou, Zhejiang with clear water to remove silt and salt attached to the surface, simply air drying in the sun, drying at 105 deg.C, pulverizing the cleaned dried Sargassum horneri sample with a pulverizer, sieving with a multilayer sieve, and packaging the 40-mesh sample into a sealed transparent bag with air-pumping;
pre-carbonization: and putting the obtained sargassum horneri powder into a vacuum tube furnace, heating to 400 ℃ at the heating rate of 5 ℃/min in the nitrogen environment, and keeping the constant temperature for 2 hours to obtain the biochar.
(2) Alkali high-temperature activation: weighing 3g of the biochar obtained in the step (1) and 12g of potassium hydroxide, mixing, adding 8ml of deionized water for dissolving, stirring uniformly, dipping for 2h, and drying at 105 ℃ to remove water. And then, placing the residue in a tube furnace, controlling the heating rate to be 5 ℃/min under the nitrogen atmosphere, heating to 850 ℃, keeping the temperature for 2h, cooling to room temperature, and taking out the sample.
(3) Acid treatment, water washing and drying: washing with 1.0mol/L hydrochloric acid solution for 2h, washing with deionized water until the washing solution is neutral, washing with anhydrous ethanol for 2 times, and drying in a vacuum drying oven at 80 deg.C for 12 h.
The specific surface area of the graphene prepared by the embodiment is 1411m2(ii)/G, raman spectrogram (fig. 1) shows that the sample has a D peak, a G peak and a 2D peak which are characteristic of graphene materials; the transmission electron micrograph (FIG. 2) shows that the sample has 3-7 layers of graphene, illustrated as multi-layered porous graphene.
Example 2:
a method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps:
(1) preparing a precursor: washing large Sargassum-Sargassum horneri from Wenzhou, Zhejiang with clear water to remove silt and salt attached to the surface, simply air drying in sunlight, drying at 105 deg.C, pulverizing the cleaned dried Sargassum-Sargassum sample with pulverizer, sieving with multilayer screen, and packaging 40 mesh sample in sealed transparent bag with air-pumping.
Pre-carbonization: and putting the obtained sargassum horneri powder into a vacuum tube furnace, heating to 400 ℃ at the heating rate of 10 ℃/min in the nitrogen environment, and keeping the constant temperature for 2 hours to obtain the biochar.
(2) Alkali high-temperature activation: weighing 3g of the biochar obtained in the step (1) and 12g of potassium hydroxide, mixing, adding 8ml of deionized water for dissolving, stirring uniformly, then soaking for 3h, and drying at 105 ℃ to remove water. And then, placing the residue in a tube furnace, controlling the heating rate to be 10 ℃/min under the nitrogen atmosphere, heating to 800 ℃, keeping the temperature for 2h, cooling to room temperature, and taking out the sample.
(3) Acid treatment, water washing and drying: washing with 2.0mol/L hydrochloric acid solution for 2h, washing with deionized water until the washing solution is neutral, washing with anhydrous ethanol for 2 times, and drying in a vacuum drying oven at 100 deg.C for 15 h.
The specific surface area of the graphene prepared in the embodiment is 2095m2In terms of the Raman spectrum,/g, the Raman spectrum is similar to that of the graphene prepared in example 1, as shown in FIG. 1, and the TEM photograph is similar to that of the graphene prepared in example 1, as shown in FIG. 2.
Example 3:
a method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps:
(1) preparing a precursor: washing large Sargassum-Sargassum horneri from Wenzhou, Zhejiang with clear water to remove silt and salt attached to the surface, simply air drying in sunlight, drying at 105 deg.C, pulverizing the cleaned dried Sargassum-Sargassum sample with pulverizer, sieving with multilayer sieve, and packaging 40 mesh sample in sealed transparent bag with evacuated air.
Pre-carbonization: and putting the obtained sargassum horneri powder into a vacuum tube furnace, heating to 500 ℃ at the heating rate of 10 ℃/min in the nitrogen environment, and keeping the constant temperature for 2 hours to obtain the biochar.
(2) Alkali high-temperature activation: weighing 3g of the biochar obtained in the step (1) and 12g of potassium hydroxide, mixing, adding 8ml of deionized water for dissolving, stirring uniformly, dipping for 2h, and drying at 105 ℃ to remove water. And then, placing the residue in a tube furnace, controlling the heating rate to be 10 ℃/min under the nitrogen atmosphere, heating to 750 ℃, keeping the temperature for 2h, cooling to room temperature, and taking out the sample.
(3) Acid treatment, water washing and drying: washing with 1.0mol/L hydrochloric acid solution for 2 hr, washing with deionized water until the washing solution is neutral, washing with anhydrous ethanol for 2 times, and oven drying at 80 deg.C for 24 hr.
The specific surface area of the graphene prepared in the embodiment is 1917m2In terms of the Raman spectrum,/g, the Raman spectrum is similar to that of the graphene prepared in example 1, as shown in FIG. 1, and the TEM photograph is similar to that of the graphene prepared in example 1, as shown in FIG. 2.
Example 4:
a method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps:
(1) preparing a precursor: washing large Sargassum-Sargassum horneri from Wenzhou, Zhejiang with clear water to remove silt and salt attached to the surface, simply air drying in sunlight, drying at 105 deg.C, pulverizing the cleaned dried Sargassum-Sargassum sample with pulverizer, sieving with multilayer screen, and packaging 40 mesh sample in sealed transparent bag with air-pumping.
Pre-carbonization: and putting the obtained sargassum horneri powder into a vacuum tube furnace, heating to 500 ℃ at the heating rate of 5 ℃/min in the nitrogen environment, and keeping the constant temperature for 2 hours to obtain the biochar.
(2) Alkali high-temperature activation: weighing 3g of the biochar obtained in the step (1) and 12g of potassium hydroxide, mixing, adding 6ml of deionized water for dissolving, stirring uniformly, dipping for 2h, and drying at 105 ℃ to remove water. And then, placing the residue in a tube furnace, controlling the heating rate to be 5 ℃/min under the nitrogen atmosphere, heating to 700 ℃, keeping the temperature for 3h, cooling to room temperature, and taking out the sample.
(3) Acid treatment, water washing and drying: washing with 2.0mol/L hydrochloric acid solution for 2h, washing with deionized water until the washing solution is neutral, washing with anhydrous ethanol for 2 times, and drying in a vacuum drying oven at 100 deg.C.
The specific surface area of the graphene prepared by the embodiment is 1733m2In terms of the Raman spectrum,/g, the Raman spectrum is similar to that of the graphene prepared in example 1, as shown in FIG. 1, and the TEM photograph is similar to that of the graphene prepared in example 1, as shown in FIG. 2.
Example 5:
a method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps:
(1) preparing a precursor: washing large Sargassum-Sargassum horneri from Wenzhou, Zhejiang with clear water to remove silt and salt attached to the surface, simply air drying in sunlight, drying at 105 deg.C, pulverizing the cleaned dried Sargassum-Sargassum sample with pulverizer, sieving with multilayer screen, and packaging 40 mesh sample in sealed transparent bag with air-pumping.
Pre-carbonization: and putting the obtained sargassum horneri powder into a vacuum tube furnace, heating to 400 ℃ at the heating rate of 5 ℃/min in the nitrogen environment, and keeping the constant temperature for 2 hours to obtain the biochar.
(2) Alkali high-temperature activation: weighing 3g of the biochar obtained in the step (1) and 9g of potassium hydroxide, mixing, adding 6ml of deionized water for dissolving, stirring uniformly, dipping for 2h, and drying at 105 ℃ to remove water. And then, placing the residue in a tube furnace, controlling the heating rate to be 5 ℃/min under the nitrogen atmosphere, heating to 850 ℃, keeping the temperature for 2h, cooling to room temperature, and taking out the sample.
(3) Acid treatment, water washing and drying: washing with 1.0mol/L hydrochloric acid solution for 2h, washing with deionized water until the washing solution is neutral, washing with anhydrous ethanol for 2 times, and drying in a vacuum drying oven at 80 deg.C for 15 h.
The specific surface area of the graphene prepared in the embodiment is 2069m2In terms of the Raman spectrum,/g, the Raman spectrum is similar to that of the graphene prepared in example 1, as shown in FIG. 1, and the TEM photograph is similar to that of the graphene prepared in example 1, as shown in FIG. 2.
Example 6:
a method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps:
(1) preparing a precursor: washing large Sargassum-Sargassum horneri from Wenzhou, Zhejiang with clear water to remove silt and salt attached to the surface, simply air drying in sunlight, drying at 105 deg.C, pulverizing the cleaned dried Sargassum-Sargassum sample with pulverizer, sieving with multilayer screen, and packaging 40 mesh sample in sealed transparent bag with air-pumping.
Pre-carbonization: and putting the obtained sargassum horneri powder into a vacuum tube furnace, heating to 500 ℃ at the heating rate of 10 ℃/min in the nitrogen environment, and keeping the constant temperature for 2 hours to obtain the biochar.
(2) Alkali high-temperature activation: weighing 3g of the biochar obtained in the step (2) and 9g of potassium hydroxide, mixing, adding 6ml of deionized water for dissolving, stirring uniformly, dipping for 2h, and drying at 105 ℃ to remove water. And then, placing the residue in a tube furnace, controlling the heating rate to be 10 ℃/min under the nitrogen atmosphere, heating to 800 ℃, keeping the temperature for 2h, cooling to room temperature, and taking out the sample.
(3) Acid treatment, water washing and drying: washing with 2.0mol/L hydrochloric acid solution for 2h, washing with deionized water until the washing solution is neutral, washing with anhydrous ethanol for 2 times, and drying in a vacuum drying oven at 80 deg.C for 15 h.
The graphene prepared in the embodiment has a specific surface area of 1654m2In terms of the Raman spectrum,/g, the Raman spectrum is similar to that of the graphene prepared in example 1, as shown in FIG. 1, and the TEM photograph is similar to that of the graphene prepared in example 1, as shown in FIG. 2.
Example 7:
a method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps:
(1) preparing a precursor: washing large Sargassum-Sargassum horneri from Wenzhou, Zhejiang with clear water to remove silt and salt attached to the surface, simply air drying in sunlight, drying at 105 deg.C, pulverizing the cleaned dried Sargassum-Sargassum sample with pulverizer, sieving with multilayer screen, and packaging 40 mesh sample in sealed transparent bag with air-pumping.
Pre-carbonization: and putting the obtained sargassum horneri powder into a vacuum tube furnace, heating to 500 ℃ at the heating rate of 5 ℃/min in the nitrogen environment, and keeping the constant temperature for 2 hours to obtain the biochar.
(2) Alkali high-temperature activation: weighing 3g of the biochar obtained in the step (1) and 9g of potassium hydroxide, mixing, adding 6ml of deionized water for dissolving, stirring uniformly, dipping for 2h, and drying at 105 ℃ to remove water. And then, placing the residue in a tube furnace, controlling the heating rate to be 5 ℃/min under the nitrogen atmosphere, heating to 750 ℃, keeping the temperature for 2h, cooling to room temperature, and taking out the sample.
(3) Acid treatment, water washing and drying: washing with 1.0mol/L hydrochloric acid solution for 2h, washing with deionized water until the washing solution is neutral, washing with anhydrous ethanol for 2 times, and drying in a vacuum drying oven at 80 deg.C for 15 h.
The specific surface area of the graphene prepared by the embodiment is 1443m2In terms of the Raman spectrum,/g, the Raman spectrum is similar to that of the graphene prepared in example 1, as shown in FIG. 1, and the TEM photograph is similar to that of the graphene prepared in example 1, as shown in FIG. 2.
Example 8:
a method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps:
(1) preparing a precursor: washing large Sargassum-Sargassum horneri from Wenzhou, Zhejiang with clear water to remove silt and salt attached to the surface, simply air drying in sunlight, drying at 120 deg.C, pulverizing the dried Sargassum-Sargassum sample with pulverizer, sieving with multi-layer sieve, and packaging the 40-mesh sample in sealed transparent bag with air-pumping.
Pre-carbonization: and putting the obtained sargassum horneri powder into a vacuum tube furnace, heating to 500 ℃ at the heating rate of 5 ℃/min in the nitrogen environment, and keeping the constant temperature for 2 hours to obtain the biochar.
(2) Alkali high-temperature activation: weighing 3g of the biochar obtained in the step (1) and 12g of potassium hydroxide, mixing, adding 6ml of deionized water for dissolving, stirring uniformly, dipping for 2h, and drying at 105 ℃ to remove water. And then, placing the residue in a tube furnace, controlling the heating rate to be 5 ℃/min under the nitrogen atmosphere, heating to 700 ℃, keeping the temperature for 3h, cooling to room temperature, and taking out the sample.
(3) Acid treatment, water washing and drying: washing with 2.0mol/L hydrochloric acid solution for 2h, washing with deionized water until the washing solution is neutral, washing with anhydrous ethanol for 2 times, and drying in a vacuum drying oven at 100 deg.C.
The specific surface area of the graphene prepared by the embodiment is 1790m2In terms of the Raman spectrum,/g, the Raman spectrum is similar to that of the graphene prepared in example 1, as shown in FIG. 1, and the TEM photograph is similar to that of the graphene prepared in example 1, as shown in FIG. 2.
Example 9:
a method for preparing graphene by using large-sized seaweeds as raw materials comprises the following steps:
(1) preparing a precursor: washing large Sargassum-Sargassum horneri from Wenzhou, Zhejiang with clear water to remove silt and salt attached to the surface, simply air drying in sunlight, oven drying at 80 deg.C, pulverizing the cleaned dried Sargassum-Sargassum sample with pulverizer, sieving with multilayer sieve, and packaging 40 mesh sample in sealed transparent bag with evacuated air.
Pre-carbonization: and putting the obtained sargassum horneri powder into a vacuum tube furnace, heating to 500 ℃ at the heating rate of 15 ℃/min in the nitrogen environment, and keeping the constant temperature for 2 hours to obtain the biochar.
(2) Alkali high-temperature activation: weighing 3g of the biochar obtained in the step (1) and 12g of potassium hydroxide, mixing, adding 6ml of deionized water for dissolving, stirring uniformly, dipping for 2h, and drying at 105 ℃ to remove water. And then, placing the residue in a tube furnace, controlling the heating rate to be 15 ℃/min under the nitrogen atmosphere, heating to 700 ℃, keeping the temperature for 3h, cooling to room temperature, and taking out the sample.
(3) Acid treatment, water washing and drying: washing with 2.0mol/L hydrochloric acid solution for 2h, washing with deionized water until the washing solution is neutral, washing with anhydrous ethanol for 2 times, and drying in a vacuum drying oven at 100 deg.C.
The specific surface area of the graphene prepared by the embodiment is 1682m2In terms of the Raman spectrum,/g, the Raman spectrum is similar to that of the graphene prepared in example 1, as shown in FIG. 1, and the TEM photograph is similar to that of the graphene prepared in example 1, as shown in FIG. 2.
Claims (10)
1. A method for preparing graphene by using large-sized seaweeds as raw materials is characterized by comprising the following steps:
(1) preparing a precursor: placing the large-scale seaweed powder which is washed by water, dried and crushed by a crusher into a vacuum tube furnace, heating to 500 ℃ under the condition of nitrogen atmosphere, and carrying out heat treatment for 1-3 hours to obtain solid biochar;
(2) alkali high-temperature activation: mixing alkali with the biochar obtained in the step (1), fully soaking to uniformly mix the biochar, and carrying out heat treatment under nitrogen gas to activate the biochar at high temperature by the alkali;
(3) acid treatment, water washing and drying: and (3) treating the sample obtained in the step (2) with acid liquor, then filtering, washing the obtained solid with water until the washing liquid is neutral, and drying the obtained solid to obtain the graphene.
2. The method for preparing graphene from large-sized seaweed as claimed in claim 1, wherein in the step (1), the washing with water means washing the seaweed with water until the filtrate is transparent.
3. The method for preparing graphene from large-sized seaweed as claimed in claim 1 or 2, wherein in the step (1), the drying is carried out at 80-120 ℃ for 12 h.
4. The method for preparing graphene from large-sized seaweeds as claimed in claim 1 or 2, wherein the pulverization in the step (1) is performed by pulverizing to 40 mesh by a pulverizer.
5. The method for preparing graphene from large-sized seaweed as claimed in claim 1 or 2, wherein in the step (1), the temperature rise to 300 ℃ and 500 ℃ is controlled at a temperature rise rate of 5-15 ℃/min.
6. The method for preparing graphene from large-sized seaweed as claimed in claim 1 or 2, wherein in the step (2), the alkali is at least one of potassium hydroxide and sodium hydroxide.
7. The method for preparing graphene by using large-sized seaweeds as raw materials according to claim 1 or 2, wherein in the step (2), the mass ratio of the alkali to the biochar is (2-5): 1.
8. The method for preparing graphene by using large-sized seaweeds as raw materials according to claim 1 or 2, wherein in the step (2), the sufficient immersion time is 1-3 h; the flow rate of the nitrogen atmosphere is 300 mL/min; the heat treatment is to heat the mixture to 700-900 ℃ at a heating rate of (5-15) DEG C/min in a tube furnace and then keep the mixture for 1-3 h.
9. The method for preparing graphene from large-sized seaweed as claimed in claim 1 or 2, wherein in the step (3), the acid solution is an aqueous hydrochloric acid solution, the concentration of the acid solution is 0.5-3 mmol/L, and the acid washing time is 1-3 h.
10. The method for preparing graphene from large-sized seaweed as claimed in claim 1 or 2, wherein in the step (3), the drying is vacuum drying under the following conditions: the drying time is 12-24 h at 80-110 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112246220A (en) * | 2020-10-30 | 2021-01-22 | 井冈山大学 | Graphene-like biochar prepared from bidens tripartita and method for treating printing and dyeing wastewater by using graphene-like biochar |
| CN112279240A (en) * | 2020-10-30 | 2021-01-29 | 井冈山大学 | Graphene-like biochar prepared from allium aviculare and method for removing sulfonamide antibiotics by graphene-like biochar |
| CN112678809A (en) * | 2020-12-30 | 2021-04-20 | 安徽工程大学 | Method for synthesizing graphene with hierarchical structure by catalyzing biomass |
| CN112723343A (en) * | 2020-12-30 | 2021-04-30 | 安徽工程大学 | Method for directly preparing high-quality graphene from biomass |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105752969A (en) * | 2016-02-29 | 2016-07-13 | 武汉理工大学 | Method for preparing polyatomic self-doped graphene by using natural porous and laminated vegetables |
| CN106348274A (en) * | 2016-11-07 | 2017-01-25 | 华南农业大学 | Method for preparing graphene from agriculture and forestry waste biomass as carbon source |
| US20180126368A1 (en) * | 2016-11-07 | 2018-05-10 | Council Of Scientific & Industrial Research | Process for the production of graphene sheets with tunable functionalities from seaweed promoted by deep eutectic solvents |
| CN109292760A (en) * | 2018-11-30 | 2019-02-01 | 长江师范学院 | A method of preparing graphene |
-
2019
- 2019-10-29 CN CN201911035759.2A patent/CN110803695A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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