CN103935991A - Method for large-scale continuous preparation of high-quality graphene - Google Patents
Method for large-scale continuous preparation of high-quality graphene Download PDFInfo
- Publication number
- CN103935991A CN103935991A CN201410165358.XA CN201410165358A CN103935991A CN 103935991 A CN103935991 A CN 103935991A CN 201410165358 A CN201410165358 A CN 201410165358A CN 103935991 A CN103935991 A CN 103935991A
- Authority
- CN
- China
- Prior art keywords
- graphene
- vacuum system
- powder
- graphite oxide
- graphene powder
- 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.)
- Pending
Links
Abstract
The invention discloses a method for large-scale continuous preparation of high-quality graphene. The method comprises the following steps: pumping an overall feeding, puffing and collecting system to a pressure of 0-1000 Pa; heating a puffing furnace to a temperature of 150-1000 DEG C and keeping the temperature; enabling graphite oxide powder to pass through a heating area of a furnace body by the effects of the own gravity and pumping of a vacuum system and stay in the heating area for 30-1000 seconds to obtain graphene powder; enabling the graphene powder to enter a cyclone separator by driving of an air flow formed by pumping of the vacuum system, be separated from air and fall into a collector. The method disclosed by the invention has the advantages of being simple in equipment, convenient to operate, also low in energy consumption and suitable for large-scale production.
Description
Technical field
The invention belongs to a kind of preparation method of Graphene, relate in particular to a kind of method of mass-producing continuous production high-quality Graphene.
Background technology
Graphene (Graphene) is that carbon atom is arranged the two dimensional crystal forming according to hexagonal.After being found by the scientist of University of Manchester from 2004, Graphene just becomes the focus of scientific circles and industry member concern.The thickness of Graphene only has 0.335 nm, is not only one the thinnest in known materials, also very firmly hard; As simple substance, it is all faster than known all conductors and semi-conductor that it at room temperature transmits the speed of electronics.Meanwhile, as monolayer carbon atomic structure, the theoretical specific surface area of Graphene is up to 2630m
2/ g.Therefore, Graphene has a wide range of applications in fields such as storage hydrogen, new type lithium ion battery, ultracapacitor and fuel cells.
The main preparation method of Graphene is Physical and chemical method at present, the main micromechanics stripping method of Physical, and epitaxial growth methods etc., though Graphene defect prepared by Physical is less, are limited to equipment and process, and cost is higher, is difficult for mass-producing preparation; Chemical method generally includes thermal reduction graphite oxide method, reductive agent reduction-oxidation graphite method etc.And can prepare on a large scale functionalization graphene by graphite oxide dilatometry, and there is good application prospect in energy storage field.Therefore, be it is believed that it is the strategic starting point of preparing on a large scale Graphene from graphite-made for graphite oxide.
Publication number is the ultra-low temperature thermal expansion preparation method that the Chinese invention patent of CN101935035B discloses graphene with high specific surface, and the method has realized peeling off of Graphene under low temperature again.But the method is intermittently preparation, and the reaction times reaches 24 h, cannot realize serialization and produce, production efficiency is too low.
CN102139873A discloses a kind of material method of preparing Graphene in vacuum or inert gas environment with micro-irradiation, and the method is comparatively strict to equipment requirements, complex operation, and preparation process is discontinuous, is not suitable for extensive preparation in batches.
Summary of the invention
A kind of method that the object of the present invention is to provide mass-producing continuous production high-quality Graphene, the method equipment is simple, easy to operate, and energy consumption is lower, suitable for mass production.
The present invention realizes the technical scheme that above-mentioned purpose adopts: a kind of method of mass-producing continuous production high-quality Graphene, comprises the following steps:
(1) open vacuum system, whole feed, expanded and material-receiving system are evacuated to 0-1000Pa;
(2) puffing furnace is heated to 150-1000 DEG C and keep constant temperature;
(3) open feeding system, under the effect that graphite oxide powder is bled in self gravitation and vacuum system, by body of heater heating zone, be 30-1000s in the residence time of heating zone, after graphite oxide is heated, occur sharply to expand, in peeling off, be reduced, obtain graphene powder;
(4) graphene powder is bled under the drive of air-flow forming in vacuum system, enters cyclonic separator, and graphene powder is separated from the gas, falls into collector.
The made Graphene quality of the present invention is high, and specific surface area is 600-2000 m
2/ g, is with a wide range of applications.
The present invention compared with prior art, has adopted large rate of air sucked in required vacuum pump in the present invention, peel off the vacuum tightness that provides higher on the one hand for the expansion of graphite oxide, makes it realize expansion in lower temperature and peels off and reduce; On the other hand, rely on the air-flow of bleeding fast and forming of vacuum pump, the Graphene of peeling away is brought to and in cyclonic separator, carries out gas solid separation and collection.Realized graphite oxide charging, peeled off and reduction, Graphene are collected carries out continuously, production efficiency is high, and made Graphene quality is high, and specific surface area is 600-2000 m
2/ g, is with a wide range of applications.In addition, the method equipment is simple, easy to operate, and energy consumption is lower, suitable for mass production.
Brief description of the drawings
Fig. 1 is process flow sheet;
Fig. 2 is Graphene product scanning electron microscope (SEM) photograph in embodiment 1.
Concrete embodiment
Embodiment 1
(1) open vacuum system, whole feed, expanded and material-receiving system are evacuated to 10 Pa;
(2) puffing furnace is heated to 800 DEG C and keep constant temperature;
(3) opening feeding system, under the effect that graphite oxide powder is bled in self gravitation and vacuum system, by body of heater heating zone, is 300 s in the residence time of heating zone.After graphite oxide is heated, occur sharply to expand, in peeling off, be reduced, obtain graphene powder;
(4) graphene powder is bled under the drive of air-flow forming in vacuum system, enters cyclonic separator, and graphene powder is separated from the gas, falls into collector.Made Graphene specific surface area is 1500 m
2/ g;
Embodiment 2
(1) open vacuum system, whole feed, expanded and material-receiving system are evacuated to 300 Pa;
(2) puffing furnace is heated to 150 DEG C and keep constant temperature;
(3) opening feeding system, under the effect that graphite oxide powder is bled in self gravitation and vacuum system, by body of heater heating zone, is 30 s in the residence time of heating zone.After graphite oxide is heated, occur sharply to expand, in peeling off, be reduced, obtain graphene powder;
(4) graphene powder is bled under the drive of air-flow forming in vacuum system, enters cyclonic separator, and graphene powder is separated from the gas, falls into collector.Made Graphene specific surface area is 600 m
2/ g;
Embodiment 3
(1) open vacuum system, whole feed, expanded and material-receiving system are evacuated to 1000 Pa;
(2) puffing furnace is heated to 800 DEG C and keep constant temperature;
(3) opening feeding system, under the effect that graphite oxide powder is bled in self gravitation and vacuum system, by body of heater heating zone, is 100 s in the residence time of heating zone.After graphite oxide is heated, occur sharply to expand, in peeling off, be reduced, obtain graphene powder;
(4) graphene powder is bled under the drive of air-flow forming in vacuum system, enters cyclonic separator, and graphene powder is separated from the gas, falls into collector.Made Graphene specific surface area is 750 m
2/ g;
Embodiment 4
(1) open vacuum system, whole feed, expanded and material-receiving system are evacuated to 500 Pa;
(2) puffing furnace is heated to 1000 DEG C and keep constant temperature;
(3) opening feeding system, under the effect that graphite oxide powder is bled in self gravitation and vacuum system, by body of heater heating zone, is 1000 s in the residence time of heating zone.After graphite oxide is heated, occur sharply to expand, in peeling off, be reduced, obtain graphene powder;
(4) graphene powder is bled under the drive of air-flow forming in vacuum system, enters cyclonic separator, and graphene powder is separated from the gas, falls into collector.Made Graphene specific surface area is 1000 m
2/ g;
Embodiment 5
(1) open vacuum system, whole feed, expanded and material-receiving system are evacuated to 1 Pa;
(2) puffing furnace is heated to 1000 DEG C and keep constant temperature;
(3) opening feeding system, under the effect that graphite oxide powder is bled in self gravitation and vacuum system, by body of heater heating zone, is 1500 s in the residence time of heating zone.After graphite oxide is heated, occur sharply to expand, in peeling off, be reduced, obtain graphene powder;
(4) graphene powder is bled under the drive of air-flow forming in vacuum system, enters cyclonic separator, and graphene powder is separated from the gas, falls into collector.Made Graphene specific surface area is 2000 m
2/ g.
Claims (2)
1. a method for mass-producing continuous production high-quality Graphene, is characterized in that comprising the steps:
(1) open vacuum system, whole feed, expanded and material-receiving system are evacuated to 0-1000Pa;
(2) puffing furnace is heated to 150-1000 DEG C and keep constant temperature;
(3) open feeding system, under the effect that graphite oxide powder is bled in self gravitation and vacuum system, by body of heater heating zone, be 30-1000s in the residence time of heating zone, after graphite oxide is heated, occur sharply to expand, in peeling off, be reduced, obtain graphene powder;
(4) graphene powder is bled under the drive of air-flow forming in vacuum system, enters cyclonic separator, and graphene powder is separated from the gas, falls into collector.
2. the product of the method for a kind of mass-producing continuous production high-quality Graphene as claimed in claim 1, the specific surface area that it is characterized in that made Graphene is 600-2000 m
2/ g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410165358.XA CN103935991A (en) | 2014-04-23 | 2014-04-23 | Method for large-scale continuous preparation of high-quality graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410165358.XA CN103935991A (en) | 2014-04-23 | 2014-04-23 | Method for large-scale continuous preparation of high-quality graphene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103935991A true CN103935991A (en) | 2014-07-23 |
Family
ID=51183920
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410165358.XA Pending CN103935991A (en) | 2014-04-23 | 2014-04-23 | Method for large-scale continuous preparation of high-quality graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103935991A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556006A (en) * | 2014-12-31 | 2015-04-29 | 江苏江大环保科技开发有限公司 | Equipment and process for industrially producing graphene by microwaves |
| CN106582994A (en) * | 2016-11-04 | 2017-04-26 | 成都新柯力化工科技有限公司 | Device for continuously preparing graphene slurry and production method |
| CN106744891A (en) * | 2016-11-23 | 2017-05-31 | 山东希诚新材料科技有限公司 | A kind of method that expanded stripping of light wave prepares graphene powder |
| CN106829940A (en) * | 2017-03-31 | 2017-06-13 | 长沙蓝态尔电子科技有限公司 | The production equipment and its production technology of a kind of grapheme material |
| CN107253717A (en) * | 2017-07-24 | 2017-10-17 | 郴州国盛新材科技有限公司 | A kind of graphene production system |
| CN107500282A (en) * | 2017-09-15 | 2017-12-22 | 兰州大学 | A kind of preparation method of scale Low Temperature Thermal reduced graphene |
| CN109292755A (en) * | 2018-09-07 | 2019-02-01 | 合肥日新高温技术有限公司 | Graphene puffing furnace production line |
| CN109455703A (en) * | 2018-12-07 | 2019-03-12 | 四川聚创石墨烯科技有限公司 | A kind of graphene and its continuous preparation method |
| CN111908461A (en) * | 2020-07-16 | 2020-11-10 | 深圳石墨烯创新中心有限公司 | Graphite oxide high-temperature heat treatment reduction device and method capable of realizing continuous production |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935035A (en) * | 2010-09-02 | 2011-01-05 | 中国科学院宁波材料技术与工程研究所 | Ultra-low temperature thermal expansion preparation method of high specific area graphene |
| CN102471068A (en) * | 2009-08-10 | 2012-05-23 | 新正直技术株式会社 | A method of producing nano-size graphene-based material and an equipment for producing the same |
-
2014
- 2014-04-23 CN CN201410165358.XA patent/CN103935991A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102471068A (en) * | 2009-08-10 | 2012-05-23 | 新正直技术株式会社 | A method of producing nano-size graphene-based material and an equipment for producing the same |
| CN101935035A (en) * | 2010-09-02 | 2011-01-05 | 中国科学院宁波材料技术与工程研究所 | Ultra-low temperature thermal expansion preparation method of high specific area graphene |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556006A (en) * | 2014-12-31 | 2015-04-29 | 江苏江大环保科技开发有限公司 | Equipment and process for industrially producing graphene by microwaves |
| CN106582994A (en) * | 2016-11-04 | 2017-04-26 | 成都新柯力化工科技有限公司 | Device for continuously preparing graphene slurry and production method |
| CN106582994B (en) * | 2016-11-04 | 2019-03-29 | 成都新柯力化工科技有限公司 | A kind of device and production method continuously preparing graphene slurry |
| CN106744891A (en) * | 2016-11-23 | 2017-05-31 | 山东希诚新材料科技有限公司 | A kind of method that expanded stripping of light wave prepares graphene powder |
| CN106744891B (en) * | 2016-11-23 | 2018-10-16 | 山东希诚新材料科技有限公司 | A kind of method that the puffing stripping of light wave prepares graphene powder |
| CN106829940A (en) * | 2017-03-31 | 2017-06-13 | 长沙蓝态尔电子科技有限公司 | The production equipment and its production technology of a kind of grapheme material |
| CN107253717A (en) * | 2017-07-24 | 2017-10-17 | 郴州国盛新材科技有限公司 | A kind of graphene production system |
| CN107500282A (en) * | 2017-09-15 | 2017-12-22 | 兰州大学 | A kind of preparation method of scale Low Temperature Thermal reduced graphene |
| CN109292755A (en) * | 2018-09-07 | 2019-02-01 | 合肥日新高温技术有限公司 | Graphene puffing furnace production line |
| CN109455703A (en) * | 2018-12-07 | 2019-03-12 | 四川聚创石墨烯科技有限公司 | A kind of graphene and its continuous preparation method |
| CN111908461A (en) * | 2020-07-16 | 2020-11-10 | 深圳石墨烯创新中心有限公司 | Graphite oxide high-temperature heat treatment reduction device and method capable of realizing continuous production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103935991A (en) | Method for large-scale continuous preparation of high-quality graphene | |
| CN106784692B (en) | Graphene array loads lithium titanate/carbon/carbon nano tube composite array electrode material and its preparation method and application | |
| CN104386678B (en) | A kind of preparation method of Graphene | |
| CN104659358A (en) | Preparation method of hollow nickel cobaltate nano polyhedron | |
| CN103991899B (en) | The preparation method of the flower-shaped tin oxide micro-nano structure of a kind of porous | |
| CN102139873A (en) | Method for preparing graphene material by microwave irradiation in vacuum or inert gas environment | |
| CN102180462A (en) | Method for preparing modified graphene material in controlled atmosphere environment by microwave irradiation | |
| CN102557023A (en) | Method for preparing graphene | |
| CN104150465A (en) | Method for preparing hollow carbon ball | |
| CN104108705B (en) | A kind of preparation method of nitrogen doping oriented graphite alkene | |
| CN103553030A (en) | Preparation method of few-layer graphene | |
| CN103811768B (en) | Pit affluxion body in lithium ion batteries and preparation method thereof and equipment | |
| CN102745678A (en) | Method for preparing nitrogen-doped graphene by utilizing plasma sputtering | |
| CN108264037A (en) | Three-dimensional porous nitrogen-doped graphene answers the preparation method of material and nitrogen-doped graphene | |
| CN103910341B (en) | A kind of manufacture method of nanoscale hexagonal plate bismuth telluride thermoelectric material | |
| CN106981631A (en) | A kind of nitrogen-doped carbon micro Nano material and its preparation method and application | |
| CN103880003A (en) | Graphene material prepared from biological calcium carbonate source and application thereof | |
| CN103482614A (en) | Preparation method of graphene-ZnO nanoparticle composite material | |
| CN107161989A (en) | A kind of preparation method of cellular three-dimensional grapheme | |
| CN105839189B (en) | A kind of tow -dimensions atom layer thickness TiO2 monocrystal nano piece and preparation method thereof | |
| JP5789002B2 (en) | Method for producing molybdenum sputtering target for back electrode of CIGS solar cell | |
| CN103022468A (en) | Environment-friendly preparation method for high-specific-capacitance Mn3O4/graphene composite material for poles | |
| CN104167552A (en) | Graphene cage with hierarchy structure and preparation method thereof | |
| CN102602921A (en) | Method for conveniently and efficiently improving graphite oxide layer interval | |
| CN107720740A (en) | A kind of preparation method that graphene nanometer sheet is prepared based on crystalline flake graphite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140723 |