CN103818897B - A method of multi-layer graphene is prepared with semi-coke - Google Patents
A method of multi-layer graphene is prepared with semi-coke Download PDFInfo
- Publication number
- CN103818897B CN103818897B CN201410009735.0A CN201410009735A CN103818897B CN 103818897 B CN103818897 B CN 103818897B CN 201410009735 A CN201410009735 A CN 201410009735A CN 103818897 B CN103818897 B CN 103818897B
- Authority
- CN
- China
- Prior art keywords
- layer graphene
- semi
- coke
- highly basic
- microwave
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
Pass through the method that microwave heating directly prepares multi-layer graphene powder using semi-coke the invention discloses a kind of for raw material.The preparation method mixes semi-coke with alkali, a large amount of by the way of microwave fast heating, quickly prepare multi-layer graphene, and semi-coke is obtained multi-layer graphene under the action of highly basic by high temperature pyrolysis in preparation process, subsequent to remove impurity using washing, pickling.Effect and advantage of the invention is that obtained multi-layer graphene yield and content are higher, can obtain application in numerous areas such as lithium ion battery negative material, adsorbent material and catalyst carriers；While the features such as raw material is cheap and easy to get, simple process, excellent properties of product, the large-scale production suitable for multi-layer graphene.
Description
Technical field
The invention belongs to carbon material preparation technical fields, are related to a kind of method for preparing multi-layer graphene with semi-coke.
Background technique
Graphene (Graphene) is a kind of carbon material of novel two-dimensional structure, by sp2Carbon atom close-packed arrays form bee
Nido structure.Graphene is most thin, maximum intensity material known today, has excellent conduction, the capacity of heat transmission and optics
Performance.These excellent performances of graphene make it have potential application prospect in various fields, become recent investigation of materials
Hot spot.
The research and application of graphene propose an urgent demand to preparation method.The preparation method of graphene is main at present
There are the methods of micromechanics stripping method, thermal expansion graphite method, graphite oxide reduction method and gas phase chemical deposition.Wherein, micromechanics
Stripping method and thermal expansion graphite method low efficiency, yield are small, can only be limited to laboratory small scale experiments；Although graphite oxide reduction method
It can be prepared on a large scale, but oxidation-reduction process introduces a large amount of defects, seriously affects its physics and chemical property, especially electric conductivity
Energy；Chemical vapor deposition method complex process, preparation condition is harsh, is unsuitable for cost production in large quantity.Therefore, inexpensive at present
Obtaining large batch of graphene product, there is also certain difficulties.
Summary of the invention
The object of the present invention is to provide it is a kind of be simple to operate and friendly to environment, raw material is easy to get, high conversion rate can be used for advising greatly
The method that mould industrial production prepares multi-layer graphene.
Multi-layer graphene preparation method provided by the present invention is by semi-coke raw material and highly basic hybrid microwave heating directly system
Standby multi-layer graphene powder, comprising the following steps:
(1) semi-coke raw material and highly basic is uniform to 1:10 ball milling mixing according to mass flow ratio 1:0.1；
(2) hydroxide such as potassium hydroxide, sodium hydroxide, calcium hydroxide may be selected in highly basic；
(3) after mixing by semi-coke and highly basic, it is put into the container for absorbing microwave material preparation；
(4) container equipped with raw material is put into microwave reactor, obtains within microwave heating 5-50 minutes multi-layer graphene production
Object；
(5) product is removed the inorganic impurity in product, is finally obtained the Multi-layer graphite of high-purity using washing, pickling
Ene product.
The present invention prepares multi-layer graphene using semi-coke raw material, by analysis methods such as Raman, XRD, carries out to product
Indicator, it was demonstrated that multi-layer graphene powder can be prepared by this method.
The present invention provides a kind of methods for preparing multi-layer graphene, compared with conventional method, this preparation method have with
Lower advantage:
(1) step is simple, easily operated, is suitble to large-scale industrial production；
(2) raw material sources are extensive, cheap；
(3) microwave heating reaction speed is fast, is not necessarily to inert gas shielding, low energy consumption.
Detailed description of the invention
Fig. 1 is the microwave reactor schematic diagram of the multi-layer graphene of preparation of the embodiment of the present invention.
Fig. 2 is the Raman spectrogram of the Multi-layer graphite ene product of preparation of the embodiment of the present invention.
Fig. 3 is the XRD spectra of the Multi-layer graphite ene product of preparation of the embodiment of the present invention.
Specific embodiment
Below by specific embodiment, the present invention will be further described.
By 1.0 Crane charcoals and 2.0 grams of potassium hydroxide ground and mixeds it is uniform after, be packed into small crucible, then small crucible be put into dress
Have in the big crucible of graphite powder, then puts it into micro-wave oven.
It is reacted 30 minutes using 900 watts of microwave stove heatings, microwave is absorbed by graphite powder and quickly heats crucible and raw material,
It is naturally cooling to room temperature after reaction, collects product in crucible.
It is washed using multiple deionization and removes soluble inorganic salt in product, then successively use 1M hydrochloric acid and 0.5M hydrogen fluorine
Successively cleaning removes indissoluble inorganic salt impurities to acid.
Under the above conditions, the yield of multi-layer graphene is 0.5 gram.Fig. 1 is microwave reactor schematic diagram；Raman spectrogram
(see figure 2) shows that the sample has the distinctive peak G of grapheme material, the peak D and the peak 2D；Nitrogen adsorption is analysis shows that its specific surface area
For 2800m2/ g illustrates that product has the specific surface area of increasing；From the XRD diagram (see Fig. 3) of product it is found that product has graphene special
The diffraction maximum of some widthization.
Claims (1)
1. a kind of method for preparing multi-layer graphene with semi-coke, the method includes by the mass ratio of semi-coke powder and highly basic 1:
Between 0.1-1:10, after mixing, multi-layer graphene is prepared in microwave heating 5-50 minutes, it is characterised in that microwave in the two
After pyrolysis prepares multi-layer graphene, inorganic impurity is removed using washing, pickling, purification obtains Multi-layer graphite ene product；Using strong
Alkali auxiliary preparation, highly basic are potassium hydroxide, sodium hydroxide, calcium hydroxide；Semi-coke and highly basic are used to the mode of ball milling or grinding
Make semi-coke dusting and is uniformly mixed with highly basic；Pickling uses nitric acid, hydrochloric acid, sulfuric acid or hydrofluoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410009735.0A CN103818897B (en) | 2014-01-09 | 2014-01-09 | A method of multi-layer graphene is prepared with semi-coke |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410009735.0A CN103818897B (en) | 2014-01-09 | 2014-01-09 | A method of multi-layer graphene is prepared with semi-coke |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103818897A CN103818897A (en) | 2014-05-28 |
| CN103818897B true CN103818897B (en) | 2019-01-29 |
Family
ID=50754237
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410009735.0A Expired - Fee Related CN103818897B (en) | 2014-01-09 | 2014-01-09 | A method of multi-layer graphene is prepared with semi-coke |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103818897B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107895653B (en) * | 2017-10-27 | 2019-10-25 | 西安理工大学 | Microwave prepares cigarette filter/graphene composite material method and application thereof |
| CN109775691B (en) * | 2017-11-13 | 2024-04-05 | 新奥集团股份有限公司 | Sulfur-doped graphene, preparation method and system thereof, and solar cell |
| CN109801986A (en) * | 2017-11-17 | 2019-05-24 | 新奥（内蒙古）石墨烯材料有限公司 | Solar battery and preparation method thereof |
| CN109133036B (en) * | 2018-09-17 | 2022-08-23 | 巧鸾科技有限公司 | Green method for manufacturing nano-carbon multi-crystal mixture product by coal gangue |
| CN109351333A (en) * | 2018-12-22 | 2019-02-19 | 西安科技大学 | A kind of preparation method of the semi-coke base adsorbent for separation of methane/nitrogen |
| CN109850888A (en) * | 2019-01-31 | 2019-06-07 | 西安科技大学 | A kind of method of semicoke sub-prime coproduction porous activated carbon and class graphene aerogel |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102612490B (en) * | 2009-04-03 | 2016-05-18 | 沃尔贝克材料有限公司 | The polymer composition that contains graphene film and graphite |
| CN101850960B (en) * | 2010-05-26 | 2012-07-11 | 安徽工业大学 | Method for preparing carbon micro-spheres by using coal as raw material |
| CN102992313B (en) * | 2012-12-12 | 2015-09-30 | 常州第六元素材料科技股份有限公司 | A kind of High specific surface area graphene of mesopore prosperity, and preparation method thereof |
| CN103288076A (en) * | 2013-06-08 | 2013-09-11 | 新疆师范大学 | Method for preparing multilayer graphene from coal-base raw material |
-
2014
- 2014-01-09 CN CN201410009735.0A patent/CN103818897B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN103818897A (en) | 2014-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103771403B (en) | A method of preparing multi-layer graphene with lignite slag | |
| CN103818897B (en) | A method of multi-layer graphene is prepared with semi-coke | |
| CN108199030B (en) | Preparation method of porous silicon/graphite/carbon composite negative electrode material of lithium ion secondary battery | |
| Liu et al. | Simultaneous preparation of silica and activated carbon from rice husk ash | |
| CN104030275B (en) | A kind of preparation method of redox graphene heat conduction thin film | |
| CN103288076A (en) | Method for preparing multilayer graphene from coal-base raw material | |
| CN102167314B (en) | Method for preparing graphene | |
| CN106587017A (en) | Porous graphene and preparation method thereof | |
| CN104701498B (en) | A kind of preparation method of biological carbon/ammonium vanadate anode material for lithium-ion batteries | |
| CN104944392B (en) | A kind of method that magnanimity prepares graphite phase carbon nitride nanometer sheet | |
| CN106629689B (en) | Graphene oxide or the efficient catalytic magnanimity preparation method of its compound are removed based on microwave reduction | |
| CN103288069A (en) | Method for preparing fluorinated graphene through microwave hydrothermal method | |
| CN104617275A (en) | Method for preparing silicon-carbon compound from silicon-containing biomass as raw material as well as prepared silicon-carbon compound and application thereof | |
| CN106744951A (en) | A kind of quick method for preparing activated carbon | |
| CN102616778A (en) | Method for preparing mesoporous activated carbon by regenerating waste coal-based activated carbon through microwave heating | |
| CN103436904A (en) | Method for preparing carbide derived carbon by fused salt electrolysis method | |
| CN103112844B (en) | Macro preparation method for mesoporous ordered graphene | |
| CN103030128A (en) | Industrial production method for preparing nanometer lithium iron phosphate by adopting solvent thermal method | |
| CN104891479A (en) | Plant-based graphene and preparation method thereof | |
| CN103407991A (en) | Preparation method of nickel/nickel oxide-decorated nitrogen-doped graphene material | |
| CN102718209B (en) | Method for preparing graphene based on reduction of divalent iron ion | |
| CN101525135B (en) | Method for inducing and synthesizing carborundum or carborundum nano tube by low-temperature auxiliary reaction | |
| CN103818894A (en) | Method for preparing multilayer graphene by using tar residue | |
| CN104129781A (en) | In-situ nitrogen-doped porous graphene and preparation method thereof | |
| CN106115785A (en) | A kind of pure phase MoO2anode material of lithium-ion battery and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190129 Termination date: 20200109 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |