CN110655064A - Preparation method of graphene material and graphene material - Google Patents
Preparation method of graphene material and graphene material Download PDFInfo
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- CN110655064A CN110655064A CN201810691241.3A CN201810691241A CN110655064A CN 110655064 A CN110655064 A CN 110655064A CN 201810691241 A CN201810691241 A CN 201810691241A CN 110655064 A CN110655064 A CN 110655064A
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- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention discloses a preparation method of a graphene material and the graphene material, and relates to the technical field of graphene; the preparation method comprises the following steps: putting the cellulose into a preheated heating furnace, introducing inert gas into the heating furnace for protection, and heating at constant temperature; putting the obtained carbonized material into crushing equipment, and then grinding and crushing; washing the sieved carbonized material to obtain a filtered carbonized material; adding aluminum chloride into the filtered carbonized material; filtering the mixed solution, putting the filtered filter residue into an acid solution, and stirring to ensure that the acidification is uniform, so as to obtain a mixed solution of porous graphene oxide and acid; filtering the mixed solution, and putting the filtered porous graphene oxide into a reducing agent to obtain a mixed solution of a porous graphene material and the reducing agent; and filtering the mixed solution to obtain the porous graphene material. The preparation of porous graphene materials on a large scale can be realized, the porous graphene materials can be produced and applied on a large scale, and the practicability is stronger.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a preparation method of a graphene material and the graphene material.
Background
Graphene (Graphene) is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future. Common powder production methods of graphene are a mechanical stripping method, an oxidation-reduction method and a SiC epitaxial growth method, and a thin film production method is a Chemical Vapor Deposition (CVD) method.
At present, the processing method for the graphene material is only suitable for manufacturing a small amount of graphene materials, and meanwhile, the manufacturing process for the porous graphene is complex, and needs to be improved.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene material and the graphene material, which are simple in structure, reasonable in design and convenient to use, aiming at the defects and shortcomings of the prior art, and can realize the preparation of a large-scale porous graphene material, large-scale production and application and higher practicability.
In order to achieve the above purpose, the preparation method of the graphene material of the invention comprises the following steps:
1. putting cellulose into a preheated heating furnace, introducing inert gas into the heating furnace for protection, heating the heating furnace to 250 ℃, heating for 1.5-3h at constant temperature, heating to 300 ℃, heating for 2-4h at constant temperature, heating to 460 ℃, and heating for 0.5-2h at constant temperature to obtain a carbonized material;
2. cooling the obtained carbonized materials to normal temperature, putting the carbonized materials into crushing equipment, grinding and crushing, sieving, grinding and sieving again until all the carbonized materials are sieved completely;
3. washing the sieved carbonized material, and filtering the washed mixed solution to obtain a filtered carbonized material;
4. adding aluminum chloride into the filtered carbonized material, and introducing ammonia gas while stirring until no precipitate is generated;
5. filtering the mixed solution generated in the step 4, putting the filtered filter residue into an acid solution, and stirring to ensure that the acidification is uniform, so as to obtain a mixed solution of porous graphene oxide and acid;
6. filtering the mixed solution obtained in the step 5, and putting the filtered porous graphene oxide into a reducing agent to obtain a mixed solution of a porous graphene material and the reducing agent;
7. and (4) filtering the mixed solution obtained in the step (6) to obtain the porous graphene material.
Further, the cellulose is one or a mixture of two of plant straws or wood chips.
Further, the preheating temperature of the heating furnace is 200-210 ℃.
Further, in the step 1, when the temperature of the heating furnace is raised to 250 ℃, starch is put into the heating furnace, and the starch and the cellulose are uniformly stirred by a stirring rod in the heating furnace.
Further, the acid solution is hydrochloric acid, and the pH value of the acid solution is 5-6.
Further, the reducing agent is a tea polyphenol water solution.
Further, the weight of the cellulose is 100-200 kg.
The graphene material is prepared by the graphene material preparation method.
After the process is adopted, the invention has the beneficial effects that: the preparation method of the graphene material and the graphene material can realize the preparation of the large-scale porous graphene material, can be used for large-scale production and application, and have stronger practicability.
Detailed Description
The preparation method of the graphene material according to the present embodiment (example one) is as follows:
1. putting 100kg of plant straws (corn straws and wheat straws) into a preheated heating furnace (210 ℃), introducing inert gas into the heating furnace for protection, heating the heating furnace to 250 ℃, adding starch into the heating furnace at the moment, uniformly stirring the added starch and cellulose by a stirring rod in the heating furnace, heating at a constant temperature for 1.5h, heating to 300 ℃, heating at a constant temperature for 4h, heating to 460 ℃, and heating at a constant temperature for 0.5h to obtain a carbonized material;
2. cooling the obtained carbonized materials to normal temperature, putting the carbonized materials into crushing equipment, grinding and crushing the carbonized materials, sieving the crushed carbonized materials with a 800-mesh sieve, and grinding and sieving the crushed carbonized materials until all the carbonized materials are sieved;
3. washing the sieved carbonized material by using distilled water, and filtering the washed mixed solution to obtain a filtered carbonized material;
4. adding aluminum chloride into the filtered carbonized material, and introducing ammonia gas while stirring until no precipitate is generated;
5. filtering the mixed solution generated in the step 4, putting the filtered filter residue into a hydrochloric acid solution with the pH value of 5, and stirring to ensure that the acidification is uniform, so as to obtain a mixed solution of porous graphene oxide and hydrochloric acid;
6. filtering the mixed solution obtained in the step 5, and putting the filtered porous graphene oxide into a tea polyphenol aqueous solution to obtain a mixed solution of a porous graphene material and the tea polyphenol aqueous solution;
7. and (4) filtering the mixed solution obtained in the step (6) to obtain the porous graphene material.
The graphene material is prepared by the graphene material preparation method.
After the process is adopted, the specific embodiment has the beneficial effects that: the preparation method of the graphene material and the graphene material can realize the preparation of the large-scale porous graphene material, can be used for large-scale production and application, and have stronger practicability.
Example two:
the preparation method of the graphene material in this embodiment is as follows:
1. putting 150kg of sawdust into a preheated heating furnace (200 ℃), introducing inert gas into the heating furnace for protection, heating the heating furnace to 250 ℃, heating at a constant temperature for 2.5 hours, then heating to 300 ℃, heating at a constant temperature for 2 hours, heating to 460 ℃, and heating at a constant temperature for 1 hour to obtain a carbonized material;
2. cooling the obtained carbonized materials to normal temperature, putting the carbonized materials into crushing equipment, grinding and crushing the carbonized materials, sieving the crushed carbonized materials with a 800-mesh sieve, and grinding and sieving the crushed carbonized materials until all the carbonized materials are sieved;
3. washing the sieved carbonized material by using distilled water, and filtering the washed mixed solution to obtain a filtered carbonized material;
4. adding aluminum chloride into the filtered carbonized material, and introducing ammonia gas while stirring until no precipitate is generated;
5. filtering the mixed solution generated in the step 4, putting the filtered filter residue into a hydrochloric acid solution with the pH value of 6, and stirring to ensure that the acidification is uniform, so as to obtain a mixed solution of porous graphene oxide and hydrochloric acid;
6. filtering the mixed solution obtained in the step 5, and putting the filtered porous graphene oxide into a tea polyphenol aqueous solution to obtain a mixed solution of a porous graphene material and the tea polyphenol aqueous solution;
7. and (4) filtering the mixed solution obtained in the step (6) to obtain the porous graphene material.
Example three:
the preparation method of the graphene material in this embodiment is as follows:
1. putting 200kg of corn straws and saw dust (the mass ratio of the corn straws to the saw dust is 2:1) into a preheated heating furnace (210 ℃), introducing inert gas into the heating furnace for protection, heating the heating furnace to 250 ℃, heating at a constant temperature for 1.5h, heating to 300 ℃, heating at a constant temperature for 2.5h, heating to 460 ℃, and heating at a constant temperature for 1.5h to obtain a carbonized material;
2. cooling the obtained carbonized materials to normal temperature, putting the carbonized materials into crushing equipment, grinding and crushing the carbonized materials, sieving the crushed carbonized materials by a 800-wood sieve, and grinding and sieving the crushed carbonized materials until all the carbonized materials are sieved;
3. washing the sieved carbonized material by using distilled water, and filtering the washed mixed solution to obtain a filtered carbonized material;
4. adding aluminum chloride into the filtered carbonized material, and introducing ammonia gas while stirring until no precipitate is generated;
5. filtering the mixed solution generated in the step 4, putting the filtered filter residue into a hydrochloric acid solution with the pH value of 5.5, and stirring to ensure that the acidification is uniform, so as to obtain a mixed solution of porous graphene oxide and hydrochloric acid;
6. filtering the mixed solution obtained in the step 5, and putting the filtered porous graphene oxide into a tea polyphenol aqueous solution to obtain a mixed solution of a porous graphene material and the tea polyphenol aqueous solution;
7. and (4) filtering the mixed solution obtained in the step (6) to obtain the porous graphene material.
The above description is only for the purpose of illustrating the technical solutions of the present invention and not for the purpose of limiting the same, and other modifications or equivalent substitutions made by those skilled in the art to the technical solutions of the present invention should be covered within the scope of the claims of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. A preparation method of a graphene material is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) putting cellulose into a preheated heating furnace, introducing inert gas into the heating furnace for protection, heating the heating furnace to 250 ℃, heating for 1.5-3h at constant temperature, heating to 300 ℃, heating for 2-4h at constant temperature, heating to 460 ℃, and heating for 0.5-2h at constant temperature to obtain a carbonized material;
(2) cooling the obtained carbonized materials to normal temperature, putting the cooled carbonized materials into crushing equipment, grinding and crushing the materials, sieving the materials, and grinding and sieving the materials until all the carbonized materials are sieved;
(3) washing the sieved carbonized material, and filtering the washed mixed solution to obtain a filtered carbonized material;
(4) adding aluminum chloride into the filtered carbonized material, and introducing ammonia gas while stirring until no precipitate is generated;
(5) filtering the mixed solution generated in the step (4), putting the filtered filter residue into an acid solution, and stirring to ensure that the acidification is uniform, so as to obtain a mixed solution of porous graphene oxide and acid;
(6) filtering the mixed solution obtained in the step (5), and putting the filtered porous graphene oxide into a reducing agent to obtain a mixed solution of a porous graphene material and the reducing agent;
(7) and (5) filtering the mixed solution obtained in the step (6) to obtain the porous graphene material.
2. The method for preparing the graphene material according to claim 1, wherein the method comprises the following steps: the cellulose is one or a mixture of two of plant straws or wood chips.
3. The method for preparing the graphene material according to claim 1, wherein the method comprises the following steps: the preheating temperature of the heating furnace is 200-210 ℃.
4. The method for preparing the graphene material according to claim 1, wherein the method comprises the following steps: and (2) when the temperature of the heating furnace is raised to 250 ℃, adding starch into the heating furnace, and uniformly stirring the added starch and cellulose through a stirring rod in the heating furnace.
5. The method for preparing the graphene material according to claim 1, wherein the method comprises the following steps: the acid solution is hydrochloric acid, and the pH value of the acid solution is 5-6.
6. The method for preparing the graphene material according to claim 1, wherein the method comprises the following steps: the reducing agent is tea polyphenol water solution.
7. The method for preparing the graphene material according to claim 1, wherein the method comprises the following steps: the weight of the cellulose is 100-200 kg.
8. A graphene material, characterized in that: the graphene material prepared by the graphene material preparation method in claim 1.
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Citations (5)
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| CN104045077A (en) * | 2014-05-27 | 2014-09-17 | 陈永 | Graphene three-dimensional hierarchical porous carbon material and preparation method thereof |
| CN106467298A (en) * | 2016-05-04 | 2017-03-01 | 济南圣泉集团股份有限公司 | A kind of grapheme material and preparation method thereof |
| US20180037460A1 (en) * | 2015-03-04 | 2018-02-08 | Jinan Shengquan Group Share Holding Co., Ltd. | Method for preparing biomass graphene by using cellulose as raw material |
| CN107686106A (en) * | 2017-08-22 | 2018-02-13 | 杨子中 | The method that biomass graphene is prepared with wheat straw extraction cellulose |
| CN108163845A (en) * | 2018-03-21 | 2018-06-15 | 吴亚良 | A kind of preparation method of porous graphene material |
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- 2018-06-28 CN CN201810691241.3A patent/CN110655064A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045077A (en) * | 2014-05-27 | 2014-09-17 | 陈永 | Graphene three-dimensional hierarchical porous carbon material and preparation method thereof |
| US20180037460A1 (en) * | 2015-03-04 | 2018-02-08 | Jinan Shengquan Group Share Holding Co., Ltd. | Method for preparing biomass graphene by using cellulose as raw material |
| CN106467298A (en) * | 2016-05-04 | 2017-03-01 | 济南圣泉集团股份有限公司 | A kind of grapheme material and preparation method thereof |
| CN107686106A (en) * | 2017-08-22 | 2018-02-13 | 杨子中 | The method that biomass graphene is prepared with wheat straw extraction cellulose |
| CN108163845A (en) * | 2018-03-21 | 2018-06-15 | 吴亚良 | A kind of preparation method of porous graphene material |
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Application publication date: 20200107 |