CN110668430A - Method for preparing graphene by fermenting graphene with graphene - Google Patents

Method for preparing graphene by fermenting graphene with graphene Download PDF

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Publication number
CN110668430A
CN110668430A CN201911098126.6A CN201911098126A CN110668430A CN 110668430 A CN110668430 A CN 110668430A CN 201911098126 A CN201911098126 A CN 201911098126A CN 110668430 A CN110668430 A CN 110668430A
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CN
China
Prior art keywords
graphene
temperature
graphite
peptide
steps
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Pending
Application number
CN201911098126.6A
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Chinese (zh)
Inventor
刘宏伟
姜国文
王丽华
姜钧奇
周诗博
李晓峰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHENYANG ZHONGKE CORROSION CONTROL ENGINEERING TECHNOLOGY CENTER
Institute of Metal Research of CAS
Original Assignee
SHENYANG ZHONGKE CORROSION CONTROL ENGINEERING TECHNOLOGY CENTER
Institute of Metal Research of CAS
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Priority to CN201911098126.6A priority Critical patent/CN110668430A/en
Publication of CN110668430A publication Critical patent/CN110668430A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/22Electronic properties
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/30Purity
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/32Size or surface area

Abstract

The invention belongs to the technical field of biomass new energy, and particularly relates to a method for preparing graphene by fermenting graphene with graphite peptide, which comprises the following steps: mixing graphite peptide and graphene, adding a chemical solvent, and adding a catalyst; heating the obtained product at high temperature, and then carrying out ultrahigh pressure treatment to obtain graphene; the high-temperature heating process comprises the steps of heating to 18-25 ℃ per minute and controlling the temperature to 350-400 ℃; heating to about 20-30 ℃ per minute, and controlling the temperature to 900-1400 ℃; the chemical solvent is one or a mixture of two solvents of nitric acid or sulfuric acid; the catalyst is silicic acid, and the mass ratio of the addition amount of the silicic acid to the total amount of the graphite peptide and the grapheme is as follows: (0.001-0.01): 1. the invention has the advantages of little environmental pollution, simple process, low cost and large specific surface area.

Description

Method for preparing graphene by fermenting graphene with graphene
Technical Field
The invention belongs to the technical field of biomass new energy, and particularly relates to a method for preparing graphene by fermenting graphene with graphite peptide.
Background
Graphene (Graphene) is a two-dimensional carbon nanomaterial composed of carbon atoms in sp hybridized orbitals into a hexagonal honeycomb lattice. 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. Physicists of manchester university, england, adenle, cameo and consutant, norwochoff, succeeded in isolating graphene from graphite by micromechanical exfoliation. 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. Among these methods, the mechanical lift-off method and the epitaxial growth method have low production efficiency and are difficult to satisfy large-scale demands. Although the chemical vapor deposition method can obtain a large-size continuous graphene film, the chemical vapor deposition method is suitable for micro-nano electronic devices or transparent conductive films, and cannot meet the large-scale requirements in the fields of energy storage materials and functional composite materials.
Graphene is currently the thinnest and hardest nanomaterial in the world, and is almost completely transparent, absorbing only 2.3% of light; the thermal conductivity coefficient is as high as 5300W/m.K, higher than that of carbon nano tube and diamond, the electron mobility is higher than that of carbon nano tube or silicon crystal at normal temperature, and the resistivity is only about 10-6 omega.cm, lower than that of copper or silver, and is the material with the smallest resistivity in the world at present. Because of its extremely low resistivity and high electron transfer rate, it is expected to be used for developing a new generation of thinner and faster-conducting electronic devices or transistors. Since graphene is essentially a transparent and good conductor, it is also suitable for manufacturing transparent touch screens, optical panels, and even solar cells.
The oxidation-reduction method for preparing the graphene material powder is easy to implement and is a common method for preparing the graphene material powder, but the method uses a large amount of strong acid and oxidant in the process of preparing the graphene, so that the surface of the graphene is seriously damaged, and the environment is easily polluted, so that the method is not suitable for large-scale industrialized graphene preparation.
Disclosure of Invention
The invention provides a method for preparing graphene by fermenting graphene with graphite peptide, which has the advantages of small environmental pollution, simple process, low cost and large specific surface area.
In order to solve the technical problem, the invention is realized as follows:
the method for preparing graphene by fermenting graphene with graphite peptide is characterized by comprising the following steps: mixing graphite peptide and graphene, adding a chemical solvent, and adding a catalyst; and heating the obtained product at high temperature, and then carrying out ultrahigh pressure treatment to obtain the graphene.
As a preferred scheme, the high-temperature heating process comprises the steps of heating to 18-25 ℃ per minute and controlling the temperature to 350-400 ℃; and then the temperature is raised to about 20-30 ℃ per minute, and the temperature is controlled to 900-1400 ℃.
Further, the chemical solvent is one or a mixture of two solvents of nitric acid or sulfuric acid.
Further, the catalyst is silicic acid, and the mass ratio of the addition amount of the silicic acid to the total amount of the graphite peptide and the grapheme is as follows: 0.001-0.01: 1.
further, the ultrahigh pressure condition of the invention is as follows: the pressure is 450-700 MPa; the pressure maintaining time is 27-65 min, and the pressurizing temperature is 53-83 ℃.
The invention has the advantages of little environmental pollution, simple process, low cost and large specific surface area. The specific surface area of the graphene prepared by the preparation method provided by the scheme of the invention is 2100-3500 cm3The aperture of the graphene is 3-22 nm. According to the method, the graphene is prepared by taking the graphene as the raw material, so that the biomass is well treated, the additional value of the biomass is greatly improved, and the method is beneficial to the rapid promotion of rural economy in China. Conductivity (S/m): 25100 and 29000; raman Spectroscopy (IG/ID): not less than 5.0; C/O: not less than 30; ash (%): 2.0 to 4.0; fe (%): 0.2 to 0.8; si (%): 0.06 to 0.9.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the described embodiments are merely a few embodiments of the invention and are not to be taken as the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The method for preparing graphene by fermenting graphene with graphite peptide comprises the following steps: mixing graphite peptide and graphene, adding a chemical solvent, and adding a catalyst; and heating the obtained product at high temperature, and then carrying out ultrahigh pressure treatment to obtain the graphene. The high-temperature heating process comprises the steps of heating up to 18 ℃ per minute and controlling the temperature to be 350 ℃; then the temperature is raised by about 20 ℃ per minute, and the temperature is controlled to be 900 ℃. The chemical solvent is nitric acid. The catalyst is silicic acid, and the mass ratio of the addition amount of the silicic acid to the total amount of the graphite peptide and the graphene is as follows: 0.001: 1. the ultrahigh pressure condition of the invention is as follows: the pressure is 450 MPa; the pressure maintaining time is 27min, and the pressurizing temperature is 53 ℃.
Example 2
The method for preparing graphene by fermenting graphene with graphite peptide comprises the following steps: mixing graphite peptide and graphene, adding a chemical solvent, and adding a catalyst; and heating the obtained product at high temperature, and then carrying out ultrahigh pressure treatment to obtain the graphene. The high-temperature heating process comprises the steps of heating up to 25 ℃ per minute and controlling the temperature to be 400 ℃; then the temperature is raised by about 30 ℃ per minute, and the temperature is controlled to be 1400 ℃. The chemical solvent is sulfuric acid. The catalyst is silicic acid, and the mass ratio of the addition amount of the silicic acid to the total amount of the graphite peptide and the graphene is as follows: 0.01: 1. the ultrahigh pressure condition of the invention is as follows: the pressure is 700 MPa; the dwell time is 65min, and the pressurizing temperature is 83 ℃.
Example 3
The method for preparing graphene by fermenting graphene with graphite peptide comprises the following steps: mixing graphite peptide and graphene, adding a chemical solvent, and adding a catalyst; and heating the obtained product at high temperature, and then carrying out ultrahigh pressure treatment to obtain the graphene. The high-temperature heating process comprises the steps of heating up to 20 ℃ per minute and controlling the temperature to be 380 ℃; then the temperature is raised to about 25 ℃ per minute, and the temperature is controlled to be 1000 ℃. The chemical solvent is nitric acid. The catalyst is silicic acid, and the mass ratio of the addition amount of the silicic acid to the total amount of the graphite peptide and the graphene is as follows: 0.005: 1. the ultrahigh pressure condition of the invention is as follows: the pressure is 650 MPa; the pressure maintaining time is 35min, and the pressurizing temperature is 63 ℃.
Example 4
The method for preparing graphene by fermenting graphene with graphite peptide comprises the following steps: mixing graphite peptide and graphene, adding a chemical solvent, and adding a catalyst; and heating the obtained product at high temperature, and then carrying out ultrahigh pressure treatment to obtain the graphene. The high-temperature heating process comprises the steps of heating up to 19 ℃ per minute and controlling the temperature to be 380 ℃; then the temperature is raised by about 25 ℃ per minute, and the temperature is controlled to be 960 ℃. The chemical solvent is a mixture of nitric acid or sulfuric acid. The catalyst is silicic acid, and the mass ratio of the addition amount of the silicic acid to the total amount of the graphite peptide and the graphene is as follows: 0.009: 1. the ultrahigh pressure condition of the invention is as follows: the pressure is 690 MPa; the pressure maintaining time is 59min, and the pressurizing temperature is 71 ℃.

Claims (5)

1. The method for preparing graphene by fermenting graphene with graphite peptide is characterized by comprising the following steps: mixing graphite peptide and graphene, adding a chemical solvent, and adding a catalyst; and heating the obtained product at high temperature, and then carrying out ultrahigh pressure treatment to obtain the graphene.
2. The method for preparing graphene by fermenting graphene with graphite peptide according to claim 1, wherein the method comprises the following steps: the high-temperature heating process comprises the steps of heating to 18-25 ℃ per minute and controlling the temperature to 350-400 ℃; and then the temperature is raised to about 20-30 ℃ per minute, and the temperature is controlled to 900-1400 ℃.
3. The method for preparing graphene by fermenting graphene with graphite peptide according to claim 2, wherein the method comprises the following steps: the chemical solvent is one of nitric acid or sulfuric acid or a mixture of two solvents.
4. The method for preparing graphene by fermenting graphene with graphite peptide according to claim 3, wherein the method comprises the following steps: the catalyst is silicic acid, and the mass ratio of the addition amount of the silicic acid to the total amount of the graphite peptide and the grapheme is as follows: (0.001-0.01): 1.
5. the method for preparing graphene by fermenting graphene with graphite peptide according to claim 4, wherein the method comprises the following steps: the ultrahigh pressure condition is as follows: the pressure is 450-700 MPa; the pressure maintaining time is 27-65 min, and the pressurizing temperature is 53-83 ℃.
CN201911098126.6A 2019-11-12 2019-11-12 Method for preparing graphene by fermenting graphene with graphene Pending CN110668430A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111748586A (en) * 2020-06-30 2020-10-09 段杨阳 Preparation method of biological graphite peptide RNA

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120329989A1 (en) * 2010-02-16 2012-12-27 Peptides & Elephants Gmbh Method for producing a graphite-based peptide purification material and method for peptide purification
CN106542521A (en) * 2016-12-28 2017-03-29 江苏中亚新材料股份有限公司 A kind of method that high efficiency, low cost prepares multi-layer graphene
CN106744835A (en) * 2016-11-30 2017-05-31 温县兴发生物科技有限公司 A kind of method that utilization maize straw prepares Graphene
CN106744836A (en) * 2016-11-30 2017-05-31 温县兴发生物科技有限公司 A kind of method that utilization biomass material prepares Graphene

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120329989A1 (en) * 2010-02-16 2012-12-27 Peptides & Elephants Gmbh Method for producing a graphite-based peptide purification material and method for peptide purification
CN106744835A (en) * 2016-11-30 2017-05-31 温县兴发生物科技有限公司 A kind of method that utilization maize straw prepares Graphene
CN106744836A (en) * 2016-11-30 2017-05-31 温县兴发生物科技有限公司 A kind of method that utilization biomass material prepares Graphene
CN106542521A (en) * 2016-12-28 2017-03-29 江苏中亚新材料股份有限公司 A kind of method that high efficiency, low cost prepares multi-layer graphene

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111748586A (en) * 2020-06-30 2020-10-09 段杨阳 Preparation method of biological graphite peptide RNA

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