CN108163841B - A method of graphene is prepared using tar - Google Patents
A method of graphene is prepared using tar Download PDFInfo
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- CN108163841B CN108163841B CN201810046031.9A CN201810046031A CN108163841B CN 108163841 B CN108163841 B CN 108163841B CN 201810046031 A CN201810046031 A CN 201810046031A CN 108163841 B CN108163841 B CN 108163841B
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
Abstract
The invention belongs to carbon material technical fields, more particularly to a kind of method for preparing graphene using tar, it obtains sample the following steps are included: 1) tar to be uniformly applied to nickel foil surface, and sample is coated with the one side of tar being placed in reacting furnace upward；It 2) will be closed after the full protective gas of filling in reacting furnace；3) sample is subjected to high-temperature process in reacting furnace under the atmosphere of protection gas, cooling after high-temperature process obtains graphene.This method simple process, raw material are simple and easy to get, greatly reduce the production cost of graphene, and realize the higher value application of tar.
Description
Technical field
The invention belongs to carbon material technical fields, and in particular to a method of graphene is prepared using tar.
Background technique
Graphene is a kind of Carbon Materials for extremely having application prospect, is most thin, maximum intensity material known today, tool
There are excellent conduction, the capacity of heat transmission and optical property.Graphene still can not achieve the industrialized production of large-scale low-cost at present,
Its key is preparation process and cost.Graphene is mainly by graphite or small molecule hydrocarbon gas in exacting terms such as high temperature
Under be prepared, higher cost is not suitable for producing in enormous quantities.Cheap carbon source and relatively mild preparation condition are found, is to promote
Into the key of graphene large-scale low-cost industrialized production.
Tar is the liquid product that the solid fuels such as coal or biomass obtain after pyrolysis or gasification, and price is low, obtains way
It is a kind of common chemical raw material through simple.However, since structure is complicated, stability is poor, calorific value is low for tar chemistry, it is conventional
Direct burning, gasification or the methods of upgrading there is a problem of corresponding, therefore, developing new tar using technique is extremely must
It wants.
Summary of the invention
To solve the deficiencies in the prior art, the present invention provides a kind of methods for preparing graphene using tar.This method
Simple process, raw material are simple and easy to get, greatly reduce the production cost of graphene, and realize the high-valued benefit of tar
With.
Technical solution provided by the present invention is as follows:
A method of graphene is prepared using tar, comprising the following steps:
1) tar is uniformly applied to nickel foil surface and obtains sample, and sample is coated with the one side of tar putting upward
It is placed in reacting furnace；
It 2) will be closed after the full protective gas of filling in reacting furnace；
3) sample is subjected to high-temperature process in reacting furnace under the atmosphere of protection gas, cooling after high-temperature process obtains
To graphene.
Based on the above-mentioned technical proposal, graphene can be prepared by tar, and method and process is simple, raw material are simply easy
.
Specifically, the tar is the tar prepared by solid carbonaceous fuels in step 1).
Specifically, the tar is coal tar, biomass coke tar or sludge tar in step 1).
Preferably, in step 1), the thickness that tar is smeared is no more than 3mm.
In above-mentioned technical proposal, tar sample is obtained by raw materials such as coal, biomass through pyrolysis or vaporizing system, tar sample throughput
It is abundant, cheap, cheap, sustainable, free of contamination alternative materials are provided for the production of graphene.
Specifically, the protection gas is nitrogen, helium or argon gas in step 2).
In above-mentioned technical proposal, it is full of inert gas in reacting furnace, can avoid the Oxidative inactivation of nickel foil, avoid tar sample
Oxidation, also can avoid reaction process in graphene predecessor oxidation, improve the yield and quality of graphene, also avoid
The Oxidative inactivation of nickel foil.
Specifically, the high-temperature process is not low to be warming up to the heating rate no more than 20 DEG C/min in step 3)
In 800 DEG C of final temperature, and keep being not less than 3 minutes under final temperature.
In above-mentioned technical proposal, lower heating rate can provide longer high-temperature heat treatment process, more to guarantee
The process that the particle participation graphene of metallic catalyst is formed, the yield and quality of the graphene of guarantee, under an inert atmosphere certainly
So damage of the cooling temperature-fall period also avoided to graphene.
Specifically, in step 3), cooling procedure natural cooling under the atmosphere of protection gas.
Provided by the invention to prepare the method for graphene compared with conventional method using tar, this preparation method has following
A little:
1, carbon source is tar, cheap and easy to get；
2, preparation method and reacting furnace are simple, easily operated, convenient for large-scale production；
3, preparation temperature is low, without the treatment process of superhigh temperature, consumes energy low.
Detailed description of the invention
Fig. 1 is the flow chart of the method provided by the present invention that graphene is prepared using tar.
Fig. 2 is the Raman spectrogram for the graphene sample that the embodiment of the present invention 1 obtains.
Fig. 3 is the atomic force microscopy diagram for the graphene sample that the embodiment of the present invention 1 obtains.
Specific embodiment
The principles and features of the present invention are described below, and illustrated embodiment is served only for explaining the present invention, is not intended to
It limits the scope of the invention.
Embodiment 1
Include: using the method that tar prepares graphene
1) 1g coal tar is uniformly applied to nickel foil surface and obtains sample, coal tar smear with a thickness of 2mm, and by sample
Product are coated with the one side of tar being placed in reacting furnace upward；
It 2) will be closed after the full nitrogen of filling in reacting furnace；
3) sample is carried out to high-temperature process under the atmosphere of nitrogen in reacting furnace, high-temperature process is with the liter of 3 DEG C/min
Warm rate is warming up to 800 DEG C of final temperature, and is kept for 3 minutes under final temperature, and cooling after high-temperature process, cooling procedure is in nitrogen
Atmosphere under natural cooling, obtain the target product of lamelliform, the specific productivity of graphene is 9%.
Product is measured by following methods:
Make to be washed with deionized water and remove soluble inorganic salt in product, then is successively successively cleaned using hydrochloric acid and hydrofluoric acid
Indissoluble inorganic salt impurities are removed, graphene sample 0.5g is obtained.
Raman spectrogram shows, which has the distinctive peak G of grapheme material, the peak D and the peak 2D (Fig. 2)；
Atomic force microscope shows that sample has the pattern of graphene to made sample topography, and produces difference
The graphene (Fig. 3) of the number of plies；
Nitrogen adsorption is analysis shows that its specific surface area is 2420m2/ g illustrates that product has biggish specific surface area.
Embodiment 2
Include: using the method that tar prepares graphene
1) 1g biomass coke tar is uniformly applied to nickel foil surface and obtains sample, biomass coke tar smear with a thickness of
2mm, and sample is coated with the one side of tar being placed in reacting furnace upward；
It 2) will be closed after the full helium of filling in reacting furnace；
3) sample is carried out to high-temperature process under the atmosphere of helium in reacting furnace, high-temperature process is with the liter of 5 DEG C/min
Warm rate is warming up to 800 DEG C of final temperature, and is kept for 5 minutes under final temperature, and cooling after high-temperature process, cooling procedure is in helium
Atmosphere under natural cooling, obtain the target product of lamelliform, the specific productivity of graphene is 7%.
Embodiment 3
Include: using the method that tar prepares graphene
1) 1g sludge tar is uniformly applied to nickel foil surface and obtains sample, sludge tar smear with a thickness of 1.5mm,
And sample is coated with the one side of tar being placed in reacting furnace upward；
It 2) will be closed after the full argon gas of filling in reacting furnace；
3) sample is carried out to high-temperature process under the atmosphere of argon gas in reacting furnace, high-temperature process is with the liter of 3 DEG C/min
Warm rate is warming up to 800 DEG C of final temperature, and is kept for 3 minutes under final temperature, and cooling after high-temperature process, cooling procedure is in argon gas
Atmosphere under natural cooling, obtain the target product of lamelliform, the specific productivity of graphene is 5%.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of method for preparing graphene using tar, which comprises the following steps:
1) tar is uniformly applied to nickel foil surface and obtains sample, and sample is coated with the one side of tar being placed in upward
In reacting furnace；
It 2) will be closed after the full protective gas of filling in reacting furnace；
3) sample is subjected to high-temperature process in reacting furnace under the atmosphere of protection gas, cooling after high-temperature process obtains stone
Black alkene, the high-temperature process are to be warming up to the final temperature not less than 800 DEG C no more than the heating rate of 20 DEG C/min, and at end
Temperature is lower to be kept being not less than 3 minutes.
2. the method according to claim 1 for preparing graphene using tar, it is characterised in that: described in step 1)
Tar is the tar prepared by solid carbonaceous fuels.
3. the method according to claim 2 for preparing graphene using tar, it is characterised in that: described in step 1)
Tar is coal tar, biomass coke tar or sludge tar.
4. the method according to claim 3 for preparing graphene using tar, it is characterised in that: in step 1), tar is applied
The thickness smeared is no more than 3mm.
5. the method according to claim 1 for preparing graphene using tar, it is characterised in that: cooled in step 3)
Journey natural cooling under the atmosphere of protection gas.
6. the method according to any one of claims 1 to 5 for preparing graphene using tar, it is characterised in that: in step 2),
The protection gas is nitrogen, helium or argon gas.
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| CN201810046031.9A CN108163841B (en) | 2018-01-17 | 2018-01-17 | A method of graphene is prepared using tar |
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| CN201810046031.9A CN108163841B (en) | 2018-01-17 | 2018-01-17 | A method of graphene is prepared using tar |
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| CN108163841A CN108163841A (en) | 2018-06-15 |
| CN108163841B true CN108163841B (en) | 2019-11-08 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205622B (en) * | 2018-09-20 | 2020-11-10 | 中国科学院广州能源研究所 | Preparation method of biomass tar derived porous carbon material |
| CN110203908B (en) * | 2019-05-30 | 2021-07-02 | 华中科技大学 | Method for preparing graphene by using biomass pyrolysis oil and product |
| CN110240147B (en) * | 2019-05-30 | 2021-03-26 | 华中科技大学 | Device for preparing graphene by using biomass pyrolysis oil |
| CN112225203B (en) * | 2020-10-19 | 2022-03-22 | 中南大学 | Method for preparing thin-layer graphene negative active material by using antibiotic fungi residues |
| CN114604859B (en) * | 2022-04-06 | 2024-03-22 | 昆明理工大学 | Method and device for continuously preparing graphene by one-stage pyrolysis of coal tar |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502593A (en) * | 2011-10-11 | 2012-06-20 | 中国石油大学(北京) | Preparation method of grapheme or doped graphene or graphene complex |
| CN102800774A (en) * | 2011-05-27 | 2012-11-28 | 浦项工科大学校产学协力团 | Method of preparing carbon thin film, and electronic device and electrochemical devices each including the carbon thin film |
| CN105236394A (en) * | 2015-08-31 | 2016-01-13 | 安徽工业大学 | Method of preparing mutually-connected graphene nano sheet used for supercapacitor |
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- 2018-01-17 CN CN201810046031.9A patent/CN108163841B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102800774A (en) * | 2011-05-27 | 2012-11-28 | 浦项工科大学校产学协力团 | Method of preparing carbon thin film, and electronic device and electrochemical devices each including the carbon thin film |
| CN102502593A (en) * | 2011-10-11 | 2012-06-20 | 中国石油大学(北京) | Preparation method of grapheme or doped graphene or graphene complex |
| CN105236394A (en) * | 2015-08-31 | 2016-01-13 | 安徽工业大学 | Method of preparing mutually-connected graphene nano sheet used for supercapacitor |
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