CN109399615B - Preparation method of 3D-graphene material with biomass resource as carbon source - Google Patents
Preparation method of 3D-graphene material with biomass resource as carbon source Download PDFInfo
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- CN109399615B CN109399615B CN201811423554.7A CN201811423554A CN109399615B CN 109399615 B CN109399615 B CN 109399615B CN 201811423554 A CN201811423554 A CN 201811423554A CN 109399615 B CN109399615 B CN 109399615B
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- C01—INORGANIC CHEMISTRY
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
Abstract
The invention relates to a preparation method of a 3D-graphene material by using biomass resources as a carbon source, which comprises the following steps: the biomass is dissolved in an aqueous solution, water-soluble inorganic salt is added after the biomass is stirred to be dissolved, the mixture is continuously stirred until the mixture forms a uniform solution, the liquid is titrated into an organic solvent to obtain a white solid, and the white solid is dried in a vacuum drying oven to obtain a mixture of the biomass and the salt; and secondly, putting the materials into a tubular furnace for carbonization, dispersing the carbonized sample in water, and filtering to obtain black solids, namely the 3D-graphene material. The 3D graphene material prepared by the method disclosed by the invention is good in water solubility, large in specific surface area, high in conductivity, uniform in material lamella thickness of about 1-2nm, strong in adsorption performance on pollutants in dye wastewater, strong in adsorption performance on organic dye methyl violet or methylene blue, good in absorptivity on near infrared light and capable of converting the near infrared light into heat energy.
Description
Technical Field
The invention belongs to the technical field of preparation of functional materials, and particularly relates to a preparation method of a 3D-graphene material using biomass resources as a carbon source.
Background
Graphene is a honeycomb-shaped 2D planar carbon material formed by sp2 hybridized carbon, and is widely applied to the fields of batteries, water purification and the like due to good physical or chemical properties such as high conductivity, good flexibility, large specific surface area and near-infrared photothermal conversion. The 3D graphene is a three-dimensional network structure formed by mutually connecting graphene sheets, and the three-dimensional structure solves the problem of stacking of the graphene sheets and simultaneously generates a large number of multi-layer channels, thereby being very beneficial to mass transfer, adsorption and loading.
Currently, methods for preparing 3D graphene are diverse, including Chemical Vapor Deposition (CVD) with metal foam as a template and self-assembly into 3D structures by Graphene Oxide (GO). However, these methods are complicated to operate and have high manufacturing costs. In recent years, the preparation of graphene by using biomass as a carbon source becomes a new member in the preparation of graphene, but no relevant product in the market at present is the preparation of graphene with a three-dimensional structure by using biomass as a carbon source, so that the preparation of 3D-graphene by using a biomass resource as a carbon source is very necessary.
Through searching, no patent publication related to the present patent application has been found.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the preparation method of the 3D-graphene material by using the biomass resource as the carbon source, the method is good in biocompatibility and simple, and the prepared 3D-graphene material has high conductivity, good absorptivity for near infrared light and good adsorptivity for methyl violet and methylene blue dyes.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a 3D-graphene material using biomass resources as a carbon source comprises the following steps:
the biomass is dissolved in an aqueous solution, water-soluble inorganic salt is added after the biomass is stirred to be dissolved, the mixture is continuously stirred until the mixture forms a uniform solution, the liquid is titrated into an organic solvent to obtain a white solid, and the white solid is dried in a vacuum drying oven to obtain a mixture of the biomass and the salt;
wherein the biomass: the mass ratio of the salt is 1: 1-1: 10;
the method comprises the steps of putting a mixture of biomass and salt in the step into a tube furnace for carbonization, dispersing carbonized samples in water, and filtering to obtain black solids, so that the 3D-graphene material is obtained.
In the first step, the biomass is water-soluble biomolecules.
Furthermore, the water-soluble biomolecule is an amino acid or a sugar.
In the first step, the stirring temperature is normal temperature, and is 20-30 ℃.
In the first step, the water-soluble inorganic salt is copper sulfate, sodium sulfate, potassium chloride or sodium chloride.
In the first step, the organic solvent is an organic solvent which is miscible with water.
And the organic solvent which is mutually soluble with water is ethanol, isopropanol or methanol.
And titrating into the organic solvent by using a syringe pump during titration, wherein the titration speed of the syringe pump is 200-1000 ul/min.
The drying in the first step is carried out under the specific conditions of 80-120 ℃ for 4-12 hours.
And in the step, when the tubular furnace is carbonized, the temperature rising program of the tubular furnace is as follows:
heating the mixture from room temperature to 200-500 ℃ at a rate of 1-5 ℃/min and maintaining the temperature for 1-2 hours, and then heating the mixture to 500-900 ℃ at a rate of 1-5 ℃/min and maintaining the temperature for 1-2 hours.
The invention has the advantages and positive effects that:
1. the 3D graphene material prepared by the method has good water solubility, large specific surface area, high conductivity and uniform material lamella thickness of about 1-2nm, has strong adsorption performance on pollutants in dye wastewater, has strong adsorption performance on organic dye methyl violet or methylene blue, has good absorptivity on near infrared light, and can be converted into heat energy; in addition, the method selects the biomass as the carbon source, can realize large-scale production, has low cost, greatly saves the production cost, and has wide application prospect.
2. The method has the advantages of simple synthetic process, good biocompatibility and easily controlled conditions, and the prepared material has uniform structure, good conductivity, near-infrared photothermal conversion, water solubility and specific surface area, can be used as a battery electrode material, a heating film and an adsorbent, realizes multiple purposes of one material, and has wide application prospect.
3. The 3D graphene prepared by the method has a simple synthesis process, the subsequent template salt removal process is simple to operate, only water is needed for dissolving, and the water-soluble inorganic salt can be recycled, so that the method has a wide application prospect.
4. The 3D structure of the 3D graphene formed by the method can be obtained by only one-step reaction, the reaction process is simple, and the working efficiency is improved.
5. The carbon source of the 3D graphene prepared by the method disclosed by the invention is biomass, such as amino acid and sugar, so that the production cost is greatly saved, and the method has a wide application prospect.
Drawings
FIG. 1 is a scanning electron microscope image of a 3D-graphene material prepared by using a biomass source as a carbon source, and it can be seen from FIG. 1 that the thickness of the sheets prepared by the method is uniform, and the sheets are connected with each other to form a 3D structure;
FIG. 2 is a transmission electron microscope image of a 3D-graphene material prepared by using a biomass source as a carbon source, and it can be seen from FIG. 2 that the material sheet prepared by the method of the present invention is very thin, and the thickness of the sheet layer is 1-2 nm;
fig. 3 is an XRD chart of the 3D-graphene material prepared by using a biomass source as a carbon source according to the present invention, and it can be seen from fig. 3 that the crystal form of the material prepared by the method of the present invention is very good.
Detailed Description
The following detailed description of the embodiments of the present invention is provided for the purpose of illustration and not limitation, and should not be construed as limiting the scope of the invention.
The raw materials used in the invention are conventional commercial products unless otherwise specified; the methods used in the present invention are conventional in the art unless otherwise specified.
Example 1
A preparation method of a 3D-graphene material using protein as a carbon source comprises the following steps:
dissolving bovine serum albumin in an aqueous solution, stirring at 20 ℃ to dissolve the bovine serum albumin, adding sodium sulfate, continuously stirring until the solution forms a uniform solution, titrating the liquid into ethanol by using an injection pump (the titration speed is 200ul/min) to obtain a white solid, and drying in a vacuum drying oven at 80-120 ℃ for 4-12 hours to obtain a mixture of the bovine serum albumin and salt;
wherein the mass ratio of the bovine serum albumin to the salt is 1: 3;
the method comprises the following steps of putting a mixture of the protein and the salt in the step into a tube furnace for carbonization, dispersing a carbonized sample in water, and filtering to obtain a black solid, namely the 3D-graphene material.
The temperature raising procedure comprises the following steps: the temperature was raised from room temperature to 300 ℃ at 2 ℃/min for 2 hours, and then to 500 ℃ at 3 ℃/min for 1 hour.
Example 2
A preparation method of a 3D-graphene material with glycine as a carbon source comprises the following steps:
dissolving glycine in an aqueous solution, stirring at 20 ℃ to dissolve the glycine, adding potassium chloride, continuously stirring to form a uniform solution, titrating the liquid into isopropanol by using an injection pump (the titration speed is 300ul/min) to obtain a white solid, and drying in a vacuum drying oven at 80-120 ℃ for 4-12 hours to obtain a mixture of glycine and salt;
wherein the mass ratio of the glycine to the salt is 1: 5;
the method comprises the following steps of putting a mixture of glycine and salt into a tube furnace for carbonization, dispersing carbonized samples into water, and filtering to obtain black solids, so that the 3D-graphene material is obtained.
The temperature raising procedure comprises the following steps: heating from room temperature to 200 ℃ at a speed of 3 ℃/min and maintaining for 1-2 hours, then heating to 600 ℃ at a speed of 1 ℃/min and maintaining for 1-2 hours.
Example 3
A preparation method of a 3D-graphene material with glutamic acid as a carbon source comprises the following steps:
dissolving glutamic acid in an aqueous solution, stirring at normal temperature (25 ℃) to dissolve the glutamic acid, adding copper sulfate, continuously stirring until the glutamic acid is dissolved to form a uniform solution, titrating the solution into isopropanol by using an injection pump (the titration speed is 500ul/min), obtaining a white solid, and drying in a vacuum drying oven at 80-120 ℃ for 4-12 hours to obtain a mixture of glutamic acid and salt;
wherein the mass ratio of the glutamic acid to the salt is 1: 8;
the method comprises the following steps of putting a mixture of glutamic acid and salt in a tube furnace for carbonization, dispersing a carbonized sample in water, and filtering to obtain a black solid, namely the 3D-graphene material.
The temperature raising procedure comprises the following steps: heating from room temperature to 350 ℃ at a speed of 2 ℃/min and maintaining for 1-2 hours, and then heating to 700 ℃ at a speed of 3 ℃/min and maintaining for 1-2 hours.
Example 4
A preparation method of a 3D-graphene material with sugar as a carbon source comprises the following steps:
dissolving glucose in deionized water, stirring at normal temperature to dissolve the glucose, adding sodium chloride, stirring to form a uniform solution, titrating the liquid into ethanol by using an injection pump (the titration speed is 300ul/min) to obtain a white solid, and drying in a vacuum drying oven at 80-120 ℃ for 4-12 hours to obtain a mixture of the glucose and the sodium chloride;
wherein the mass ratio of the glucose to the salt is 1: 5;
the method comprises the following steps of putting a mixture of glucose and salt in a tube furnace for carbonization, dispersing carbonized samples in water, and filtering to obtain black solids, so that the 3D-graphene material is obtained.
The temperature raising procedure comprises the following steps: heating from room temperature to 300 ℃ at a speed of 5 ℃/min and maintaining for 1-2 hours, and then heating to 600 ℃ at a speed of 3 ℃/min and maintaining for 1-2 hours.
Example 5
A preparation method of a 3D-graphene material with sugar as a carbon source comprises the following steps:
dissolving glucose in deionized water, stirring at normal temperature to dissolve the glucose, adding sodium chloride, stirring to form a uniform solution, titrating the solution into methanol by using an injection pump (the titration speed is 600ul/min), centrifuging to obtain a white solid, and drying in a vacuum drying oven to obtain a mixture of the glucose and the sodium chloride;
wherein the mass ratio of the glucose to the sodium chloride is 1: 6;
the method comprises the following steps of putting a mixture of glucose and potassium chloride into a tube furnace for carbonization, dispersing a carbonized sample in water, and filtering to obtain a black solid, namely the 3D-graphene material.
The temperature raising procedure comprises the following steps: heating from room temperature to 500 ℃ at a rate of 3 ℃/min and maintaining for 1-2 hours, and then heating to 900 ℃ at a rate of 5 ℃/min and maintaining for 1-2 hours.
The invention relates to the detection of 3D-graphene materials with biomass sources as carbon sources:
1. according to the invention, a scanning electron microscope image test of the 3D-graphene material with a biomass source as a carbon source shows that the result is shown in figure 1, and the sheets of the invention are uniform in thickness and are connected with each other to form a 3D structure in figure 1;
2. the transmission electron microscope image detection of the 3D-graphene material with the biomass source as the carbon source shows that the result is shown in FIG. 2, and the lamella of the material is very thin and can be seen from FIG. 2, and the thickness of the lamella is 1-2 nm;
3. the XRD pattern of the 3D-graphene material using the biomass source as the carbon source is shown in figure 3, and the result is shown in figure 3, so that the crystal form of the material is good.
Although the embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the disclosure of the embodiments and the accompanying drawings.
Claims (1)
1. A preparation method of a 3D-graphene material using biomass resources as a carbon source is characterized by comprising the following steps: the method comprises the following steps:
wherein the biomass: the mass ratio of the salt is 1: 1-1: 10;
said step (c) is
The medium biomass is water-soluble biomolecule;
the water-soluble biomolecule is amino acid or sugar;
said step (c) is
The medium water-soluble inorganic salt is copper sulfate or sodium sulfate or potassium chloride or sodium chloride;
said step (c) is
The medium organic solvent is an organic solvent mutually soluble with water;
said step (c) is
The specific conditions of medium drying are 80-120 ℃ and 4-12 hours;
said step (c) is
When carbonizing in the medium-tube furnace, the temperature rising procedure of the tube furnace is as follows:
heating the mixture from room temperature to 200-500 ℃ at a speed of 1-5 ℃/min and maintaining the temperature for 1-2 hours, then heating the mixture to 500-900 ℃ at a speed of 1-5 ℃/min and maintaining the temperature for 1-2 hours;
said step (c) is
The medium stirring temperature is 20-30 ℃;
the organic solvent which is mutually soluble with water is ethanol or isopropanol or methanol;
said step (c) is
In the middle titration, the mixture is titrated into the organic solvent by using a syringe pump, and the titration speed of the syringe pump is 200-1000 mu L/min.
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| CN111547709A (en) * | 2020-05-09 | 2020-08-18 | 九江学院 | Biomass three-dimensional porous graphene and preparation method thereof |
| WO2024006663A2 (en) * | 2022-06-24 | 2024-01-04 | University Of Virginia Patent Foundation | Graphene and methods of making graphene |
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| CN103715430B (en) * | 2013-12-23 | 2015-09-09 | 天津大学 | Three-dimensional grapheme network structure load carbon covered stannum rice material and preparation and application |
| US10766772B2 (en) * | 2016-11-04 | 2020-09-08 | Electronics And Telecommunications Research Institute | Method for preparing three-dimensional graphene structure and energy storage device |
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