CN103922330A - Method for preparing graphene powder by using dry process - Google Patents
Method for preparing graphene powder by using dry process Download PDFInfo
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- CN103922330A CN103922330A CN201410173737.3A CN201410173737A CN103922330A CN 103922330 A CN103922330 A CN 103922330A CN 201410173737 A CN201410173737 A CN 201410173737A CN 103922330 A CN103922330 A CN 103922330A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention belongs to the technical field of nanometer material preparation and particularly relates to a method for preparing graphene powder by using a dry process. The method comprises the steps of firstly, carrying out microwave heat treatment on graphite to form pre-expanded graphite; placing pre-expanded graphite into a high-pressure-resistant peeling reactor, and adding dry ice or liquid nitrogen to peel at high pressure and high speed to obtain graphene. The method for preparing the graphene powder is simple in production equipment, few in process flow, free of oxidation reduction and subsequent acid treatment processes, environment-friendly and suitable for large-scale production; the prepared graphene powder is few in defect, good in conductivity and suitable for the application fields such as supercapacitors, sensors, sea water desalination and the like.
Description
Technical field
The invention belongs to the preparing technical field of nano material, be specifically related to a kind of method of dry process graphene powder.
Technical background
Found that from 2004 many scientists are devoted to the research of graphene preparation method since Graphene, especially to prepare high quality, productive rate is high, cost is low, the method for constitutionally stable Graphene this just seem particularly important.The method of preparing at present Graphene mainly contains following several: stripping method, comprises the method such as micromechanics stripping method and solvent stripping method; Growth method, comprises that crystal is to methods such as epitaxy, epitaxy method, chemical vapour depositions; Redox graphite method, comprises conventional Hummers method, Standenmaier method, Brodie method etc.; In addition, also have arc discharge method, graphite layers chemicals approach method, carbon nanotube strip off method etc.Redox graphite method has the technique of simple and diversification, be a kind of conventional method of preparing Graphene, still, this method is only applicable to laboratory on a small quantity for the preparation of research, and a large amount of preparations easily produce a large amount of spent acid, waste water etc., will cause the pollution of environment.Therefore, be badly in need of development a kind of simple, the graphene preparation method that environmental pollution is little.
summary of the invention:
Based on the deficiencies in the prior art, the object of the present invention is to provide a kind of method of preparing on a large scale graphene powder, its technical scheme comprises the following steps:
(1) graphite is carried out to microwave thermal processing, obtain pre-expanded graphite;
(2) pre-expanded graphite is placed in high pressure resistant stripping reaction device, and adds swelling agent to carry out high pressure to peel off, obtain Graphene.
Wherein, in step (1), the heat treated power of microwave is 200 ~ 1000W, and the microwave time is 5 s ~ 60 min.
Wherein, in step (2), high pressure resistant stripping reaction device is any one in high speed ball mill, high-speed stirring reactor, pair roller mill; The rotating speed of high pressure resistant stripping reaction device is 600-6000 rev/min, and the time of ball milling or stirring is 2 ~ 72h.
Wherein, swelling agent is dry ice, liquid nitrogen, liquid oxygen, supercritical CO
2in any one or multiple mixture, the mass ratio of swelling agent and graphite is 1:10 ~ 100:1, adds swelling agent mainly to utilize volumetric expansion in its gasification or liquefaction process, discharges high pressure, urges the expansion into graphite intercalation compound, and then more effective peeling off.
Beneficial effect of the present invention: production unit is simple, technical process is few, without carrying out redox and follow-up acid treatment process, environmental protection, is applicable to scale operation; Be prepared into that graphene powder defect is few, good conductivity, be applicable to the Application Areass such as ultracapacitor, sensor, sea water desaltination.
Brief description of the drawings
Fig. 1 is the Raman collection of illustrative plates of preparing graphene powder.
Fig. 2 is transmission electron microscope (TEM) figure for preparing graphene powder.
Fig. 3 is atomic force microscope (AFM) figure for preparing graphene powder.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
Take 15g graphite and insert in microwave oven, in the time that power is 500W, microwave 1 min, obtains pre-expanded graphite; Pre-expanded graphite being placed in to (ball grinder volume is 2L) in high-voltage ball miller, and adding 90g dry ice, is under 3500 revs/min of conditions at rotating speed, peels off 16 hours, obtains graphene powder.
The sample of preparation is carried out to TEM, Raman spectrum and AFM and characterize, its result is distinguished as shown in Figure 1, Figure 2 and Figure 3, as can be seen from Figure 1, and at 1351.79cm
-1there is D peak in place, at 1600.98cm
-1there is G peak in place, can show that thus this inventive method can prepare Graphene; Can see clearly that from Fig. 2 and Fig. 3 prepared Graphene is the translucent sheet structure of fine gauze shape, surface is accordion.
Embodiment 2
The graphene powder of the present embodiment and embodiment 1 are in full accord, just dry ice are replaced with to liquid nitrogen, and high-voltage ball miller replaces with high-pressure stirring reactor.
Claims (4)
1. a method of preparing graphene powder, comprises the following steps:
(1) graphite is carried out to microwave thermal processing, obtain pre-expanded graphite;
(2) pre-expanded graphite is placed in high pressure resistant stripping reaction device, and adds swelling agent to carry out high pressure to peel off, obtain graphene powder.
2. a kind of method of preparing graphene powder according to claim 1, is characterized in that: the heat treated power of microwave described in step (1) is 200 ~ 1000W, and the microwave time is 5 s ~ 60 min.
3. a kind of method of preparing graphene powder according to claim 1, is characterized in that: the high pressure resistant stripping reaction device described in step (2) is any one in high speed ball mill, high-speed stirring reactor, pair roller mill; The rotating speed of described high pressure resistant stripping reaction device is 600-6000 rev/min, and the time of ball milling or stirring is 2 ~ 72h.
4. a kind of method of preparing graphene powder according to claim 1, is characterized in that: described swelling agent is dry ice, liquid nitrogen, liquid oxygen, supercritical CO
2in any one or multiple mixture, the mass ratio of swelling agent and graphite is 1:10 ~ 100:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410173737.3A CN103922330A (en) | 2014-04-28 | 2014-04-28 | Method for preparing graphene powder by using dry process |
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| CN201410173737.3A CN103922330A (en) | 2014-04-28 | 2014-04-28 | Method for preparing graphene powder by using dry process |
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| CN103922330A true CN103922330A (en) | 2014-07-16 |
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| CN201410173737.3A Pending CN103922330A (en) | 2014-04-28 | 2014-04-28 | Method for preparing graphene powder by using dry process |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291330A (en) * | 2014-09-28 | 2015-01-21 | 上海第二工业大学 | Preparation method of modified functionalized graphene nanometer material |
| CN104505512A (en) * | 2014-11-25 | 2015-04-08 | 北京理工大学 | Method for preparing microcrystalline graphene through ball milling |
| CN104909348A (en) * | 2015-05-12 | 2015-09-16 | 浙江理工大学 | Method for preparing oxidized graphene with high dispersibility based on microwave pretreatment |
| CN104910378A (en) * | 2015-05-26 | 2015-09-16 | 浙江理工大学 | Preparation method for polyaniline/graphene oxide nanocomposite |
| CN106082195A (en) * | 2016-06-17 | 2016-11-09 | 青岛大学 | A kind of ball milling formula preparation method of Graphene |
| CN106477568A (en) * | 2016-09-30 | 2017-03-08 | 江苏大学 | A kind of method preparing Graphene using liquid nitrogen gas phase stripping |
| CN106753268A (en) * | 2016-11-25 | 2017-05-31 | 青岛华高墨烯科技股份有限公司 | Compound catalyst carrier of a kind of Graphene and preparation method thereof |
| CN107128905A (en) * | 2017-05-17 | 2017-09-05 | 宁波诺丁汉新材料研究院有限公司 | A kind of method for preparing graphene with biomass derivatives based on mechanochemical reaction |
| CN107541709A (en) * | 2017-08-20 | 2018-01-05 | 长沙小新新能源科技有限公司 | The preparation method and graphene film of a kind of graphene film |
| CN108083265A (en) * | 2017-02-27 | 2018-05-29 | 苏州鼎烯聚材纳米科技有限公司 | A kind of dry type of graphene nano powder removes production technology |
| CN108622886A (en) * | 2017-03-17 | 2018-10-09 | 国家纳米科学中心 | A kind of liquid nitrogen auxiliary prepares the method for high-quality graphene and high-quality graphene obtained |
| CN109065219A (en) * | 2018-08-14 | 2018-12-21 | 南通百川新材料有限公司 | A kind of efficient, high dispersive graphene conductive slurry preparation method |
| CN110498407A (en) * | 2019-08-22 | 2019-11-26 | 董恬纲 | Liquid CO2Graphene fragment film build method is integrated in sedimentation |
| CN110734057A (en) * | 2018-07-19 | 2020-01-31 | 矿物股份有限公司 | Synthesis method of graphene oxide |
| CN110817853A (en) * | 2018-08-07 | 2020-02-21 | 中国石油化工股份有限公司 | Preparation method of edge carboxylated graphene |
| CN111559743A (en) * | 2020-05-25 | 2020-08-21 | 西安稀有金属材料研究院有限公司 | Preparation method and application of graphene powder |
-
2014
- 2014-04-28 CN CN201410173737.3A patent/CN103922330A/en active Pending
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291330B (en) * | 2014-09-28 | 2017-02-08 | 上海第二工业大学 | Preparation method of modified functionalized graphene nanometer material |
| CN104291330A (en) * | 2014-09-28 | 2015-01-21 | 上海第二工业大学 | Preparation method of modified functionalized graphene nanometer material |
| CN104505512A (en) * | 2014-11-25 | 2015-04-08 | 北京理工大学 | Method for preparing microcrystalline graphene through ball milling |
| CN104909348A (en) * | 2015-05-12 | 2015-09-16 | 浙江理工大学 | Method for preparing oxidized graphene with high dispersibility based on microwave pretreatment |
| CN104909348B (en) * | 2015-05-12 | 2017-05-03 | 浙江理工大学 | Method for preparing oxidized graphene with high dispersibility based on microwave pretreatment |
| CN104910378A (en) * | 2015-05-26 | 2015-09-16 | 浙江理工大学 | Preparation method for polyaniline/graphene oxide nanocomposite |
| CN104910378B (en) * | 2015-05-26 | 2017-06-06 | 浙江理工大学 | A kind of polyaniline/graphene oxide nano composite material preparation method |
| CN106082195A (en) * | 2016-06-17 | 2016-11-09 | 青岛大学 | A kind of ball milling formula preparation method of Graphene |
| CN106477568A (en) * | 2016-09-30 | 2017-03-08 | 江苏大学 | A kind of method preparing Graphene using liquid nitrogen gas phase stripping |
| CN106753268A (en) * | 2016-11-25 | 2017-05-31 | 青岛华高墨烯科技股份有限公司 | Compound catalyst carrier of a kind of Graphene and preparation method thereof |
| CN108083265A (en) * | 2017-02-27 | 2018-05-29 | 苏州鼎烯聚材纳米科技有限公司 | A kind of dry type of graphene nano powder removes production technology |
| CN108622886A (en) * | 2017-03-17 | 2018-10-09 | 国家纳米科学中心 | A kind of liquid nitrogen auxiliary prepares the method for high-quality graphene and high-quality graphene obtained |
| CN107128905A (en) * | 2017-05-17 | 2017-09-05 | 宁波诺丁汉新材料研究院有限公司 | A kind of method for preparing graphene with biomass derivatives based on mechanochemical reaction |
| CN107128905B (en) * | 2017-05-17 | 2020-07-31 | 宁波诺丁汉新材料研究院有限公司 | Method for preparing graphene from biomass derivative based on mechanochemical method |
| CN107541709A (en) * | 2017-08-20 | 2018-01-05 | 长沙小新新能源科技有限公司 | The preparation method and graphene film of a kind of graphene film |
| CN110734057A (en) * | 2018-07-19 | 2020-01-31 | 矿物股份有限公司 | Synthesis method of graphene oxide |
| CN110734057B (en) * | 2018-07-19 | 2023-01-10 | 矿物股份有限公司 | Synthesis method of graphene oxide |
| CN110817853A (en) * | 2018-08-07 | 2020-02-21 | 中国石油化工股份有限公司 | Preparation method of edge carboxylated graphene |
| CN109065219A (en) * | 2018-08-14 | 2018-12-21 | 南通百川新材料有限公司 | A kind of efficient, high dispersive graphene conductive slurry preparation method |
| CN110498407A (en) * | 2019-08-22 | 2019-11-26 | 董恬纲 | Liquid CO2Graphene fragment film build method is integrated in sedimentation |
| CN111559743A (en) * | 2020-05-25 | 2020-08-21 | 西安稀有金属材料研究院有限公司 | Preparation method and application of graphene powder |
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Application publication date: 20140716 |