CN103771403B - A method of preparing multi-layer graphene with lignite slag - Google Patents
A method of preparing multi-layer graphene with lignite slag Download PDFInfo
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- CN103771403B CN103771403B CN201410009752.4A CN201410009752A CN103771403B CN 103771403 B CN103771403 B CN 103771403B CN 201410009752 A CN201410009752 A CN 201410009752A CN 103771403 B CN103771403 B CN 103771403B
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- layer graphene
- lignite
- highly basic
- slag
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Abstract
The invention discloses a kind of methods directly preparing multi-layer graphene powder by microwave heating for raw material using lignite slag.The preparation method mixes lignite slag with highly basic, it is a large amount of by the way of microwave fast heating, quickly prepare multi-layer graphene, lignite slag is obtained by multi-layer graphene under the action of highly basic by high temperature pyrolysis in preparation process, it is follow-up to remove impurity using washing, pickling.The effect and advantage of the present 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, sorbing material and catalyst carriers；The features such as raw material is cheap and easy to get, simple for process, properties of product are excellent simultaneously is suitable for the large-scale production of multi-layer graphene.
Description
Technical field
The invention belongs to carbon material preparing technical fields, are related to a kind of method preparing multi-layer graphene with lignite.
Background technology
Graphene（Graphene）It 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
The methods of have micromechanics stripping method, thermally expand graphite method, graphite oxide reduction method and gas phase chemical deposition.Wherein, micromechanics
Stripping method is low with graphite method efficiency is thermally expanded, yield is 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.
China's lignite resource is abundant, cheap, but since the degree of coalification of lignite is low, water content is high, and it is big to limit it
Scale development utilizes.The high added value research for developing lignite has significant Social benefit and economic benefit.And at present with lignite
The domestic and international open report of graphene is prepared for raw material and document is not found still.
Invention content
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 lignite raw material and highly basic hybrid microwave heating directly system
Standby multi-layer graphene powder, includes the following steps：
（1）By lignite raw material and highly basic according to mass flow ratio 1：0.1 to 1：10 ground and mixeds are uniform；
（2）The hydroxide such as potassium hydroxide, sodium hydroxide, calcium hydroxide may be selected in highly basic；
（3）After mixing by lignite and highly basic, it is put into and absorbs in container prepared by microwave material；
（4）Container equipped with raw material is put into microwave reactor, microwave heating obtains multi-layer graphene production for 5-50 minutes
Object；
（5）By product using washing, pickling, the inorganic impurity in product is removed, the Multi-layer graphite of high-purity is finally obtained
Ene product.
The present invention prepares multi-layer graphene using lignite raw material, by analysis methods such as Raman, XRD, is carried 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 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.
Description of the drawings
Fig. 1 is the microwave reactor schematic diagram of multi-layer graphene prepared by the embodiment of the present invention.
Fig. 2 is the Raman spectrogram of Multi-layer graphite ene product prepared by the embodiment of the present invention.
Fig. 3 is the XRD spectra of Multi-layer graphite ene product prepared by the embodiment of the present invention.
Specific implementation mode
Below by specific embodiment, the present invention will be further described.
By 1.0 grams of lignite 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 heats, absorbing microwave by graphite powder quickly heats crucible and raw material,
It is naturally cooling to room temperature after reaction, product is collected in crucible.
It is washed using multiple deionization and removes soluble inorganic salt in product, then use 1M hydrochloric acid and 0.5M hydrogen fluorine successively
Cleaning removes indissoluble inorganic salt impurities to acid successively.
Under these conditions, the yield of multi-layer graphene is 0.4 gram.Fig. 1 is microwave reactor schematic diagram；Raman spectrogram
（See Fig. 2）Show that the sample has the distinctive peaks G of grapheme material, the peaks D and the peaks 2D；Nitrogen adsorption is analysis shows that its specific surface area
For 1800m2/ 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 (3)
1. a kind of method preparing multi-layer graphene with lignite slag, it is characterised in that lignite slag raw material and highly basic are pressed certain mass
Than after mixing, multi-layer graphene is prepared in 5-50 minutes in microwave heating；
It assists preparing using highly basic, highly basic is potassium hydroxide, sodium hydroxide, calcium hydroxide；The mass ratio of lignite slag and highly basic exists
1：0. 1-1：Between 10.
2. according to the method described in claim 1, it is characterized in that after microwave-heating prepares multi-layer graphene, washing, acid are used
It washes away and removes inorganic impurity, purification obtains Multi-layer graphite ene product.
3. according to the method described in claim 2, it is characterized in that pickling uses nitric acid, hydrochloric acid, sulfuric acid or hydrofluoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410009752.4A CN103771403B (en) | 2014-01-09 | 2014-01-09 | A method of preparing multi-layer graphene with lignite slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410009752.4A CN103771403B (en) | 2014-01-09 | 2014-01-09 | A method of preparing multi-layer graphene with lignite slag |
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| Publication Number | Publication Date |
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| CN103771403A CN103771403A (en) | 2014-05-07 |
| CN103771403B true CN103771403B (en) | 2018-10-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410009752.4A Expired - Fee Related CN103771403B (en) | 2014-01-09 | 2014-01-09 | A method of preparing multi-layer graphene with lignite slag |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016184355A1 (en) * | 2015-05-19 | 2016-11-24 | 张雨虹 | Method for preparing graphene using coal as raw material |
| JP7190735B2 (en) * | 2016-04-13 | 2022-12-16 | グリーン ナノテク ラブズ，エルエルシー | A low-cost and rapid method for mass production of graphene and graphene oxide using carbon-rich natural materials |
| CN106006604B (en) * | 2016-05-31 | 2017-12-08 | 太原理工大学 | The method of catalysis pyrolysis solid carbon materials CNT |
| 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 |
| CN108516534A (en) * | 2018-06-09 | 2018-09-11 | 太原理工大学 | The method of catalyzed conversion solid carbon materials nano-carbon material |
| CN110104634B (en) * | 2019-05-17 | 2021-04-30 | 新奥石墨烯技术有限公司 | Three-dimensional graphene and preparation method and application thereof |
| US20220363547A1 (en) * | 2021-05-17 | 2022-11-17 | University Of Wyoming | Method and system for converting raw coal powder into polycrystalline nano-graphite by metal-assisted microwave treatment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850960A (en) * | 2010-05-26 | 2010-10-06 | 安徽工业大学 | Method for preparing carbon micro-spheres by using coal as raw material |
| CN102612490A (en) * | 2009-04-03 | 2012-07-25 | 沃尔贝克材料有限公司 | Polymer compositions containing graphene sheets and graphite |
| CN102992313A (en) * | 2012-12-12 | 2013-03-27 | 常州第六元素材料科技股份有限公司 | High specific surface area graphene with well-developed mesopores, 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 |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102612490A (en) * | 2009-04-03 | 2012-07-25 | 沃尔贝克材料有限公司 | Polymer compositions containing graphene sheets and graphite |
| CN101850960A (en) * | 2010-05-26 | 2010-10-06 | 安徽工业大学 | Method for preparing carbon micro-spheres by using coal as raw material |
| CN102992313A (en) * | 2012-12-12 | 2013-03-27 | 常州第六元素材料科技股份有限公司 | High specific surface area graphene with well-developed mesopores, 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 |
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Granted publication date: 20181030 Termination date: 20200109 |