CN107758648A - A kind of new way that graphene is prepared using ethanol as liquid phase planetary ball mill wet method - Google Patents
A kind of new way that graphene is prepared using ethanol as liquid phase planetary ball mill wet method Download PDFInfo
- Publication number
- CN107758648A CN107758648A CN201711003385.7A CN201711003385A CN107758648A CN 107758648 A CN107758648 A CN 107758648A CN 201711003385 A CN201711003385 A CN 201711003385A CN 107758648 A CN107758648 A CN 107758648A
- Authority
- CN
- China
- Prior art keywords
- graphene
- ethanol
- graphite
- ball mill
- planetary ball
- 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 provides a kind of new way that graphene is prepared using ethanol as liquid phase planetary ball mill wet method.The preparation method specifically includes：Using the expanded graphite after high-temperature calcination as raw material, using ethanol as organic solution, peel off expanded graphite by planetary ball mill wet lapping machinery and obtain lamella than more complete, the larger graphene of crystalline size.This method simple production process, cost is low, and the graphene being prepared is less than dry type graphene defect, and lamella is more complete, and the application to later graphene provides broader prospect.
Description
Technical field
The present invention relates to a kind of new way that graphene is prepared using ethanol as liquid phase planetary ball mill wet method, belong to advanced and receive
Rice material preparation process technical field.
Background technology
A kind of carbon material with bi-dimensional cellular shape structure of the graphene as monoatomic layer thickness, possesses huge ratio table
Area and superior electron mobility and property stabilization, are widely used in the fields such as electronics, sensor, medicine and catalysis, are
The wider research of nano composite material provides new thinking and direction.Various countries expert is become since graphene is found
The focus of scholar's research, while it is also considered as improving the new material in the fields such as sensor, medicine and catalysis.China is graphite
The most abundant country of resource, and big producer, but the deep processing to its high-tech is probed into and is still in the junior stage.Graphene
Research is concentrated mainly on last decade, and also many problems need to study.Therefore, the preparation method for exploring grapheme material is one
It is individual to still need to solve the problems, such as.It should be noted that preparation and its difficulty of single-layer graphene, therefore will lack with its similar nature
Layer graphene is also classified as the category of graphene.
The preparation method of graphene is concentrated mainly on chemical stripping method, CVD growth method and physics stripping method at present, wherein changing
The defects of learning the redox graphene that stripping method is prepared is more, and experimental period is grown, and the cost of CVD growth method is higher, therefore
Short preparation period using graphite as raw material, cost is low, and experiment is simple and less physics stripping method the defects of graphene enjoys pass
Note.What is commonly used in currently used physics stripping method is adhesive tape tear, mortar formula grinding, the methods of agitation grinding and ball milling.Wherein
Adhesive tape method of Tearing efficiency is too low and the graphene quality of preparation is uneven, and the grinding of mortar formula and stirring ball-milling are because equipment carries in itself
The crystalline size that the energy of confession is relatively low can not to be peeled off graphite well and prepare is smaller, although ball mill can provide higher grinding
Energy, but the graphene edge defect that the impulsive force in grinding can make the graphene size of preparation smaller and prepare is more.It is existing
The common disadvantages of physical separation methods be that obtained graphene general size is all smaller, and poor controllability.This will be very big
Ground hinders application of the graphene in practical devices.
Therefore, in order to preferably using ball mill provide higher grinding energy and overcome impulsive force pair in mechanical milling process
The destruction of graphite, research finds to use wet ball-milling environment, using ethanol as organic solution, be graphite in ball mill ball milling mistake
Sufficient peptizaiton is provided in journey, reduces impulsive force of the mechanical milling process to graphite so that the graphene size being prepared compared with
Greatly, defect is less, the drawbacks of preferably improving original dry type ball milling.
The content of the invention
It is an object of the invention to overcome the shortcomings of existing physics stripping method, there is provided using one kind using ethanol as liquid phase planet ball
Grinding machine wet method prepares the new way of graphene.With simple production process, yield is high, graphene defect is less and crystal chi
Very little more complete feature.The nano material of gained graphene can be used for the novel-section for improving the fields such as sensor, medicine and catalysis
The prospect of material.Realizing the object of the invention technical scheme is：A kind of wet type mechanical milling method prepares the new way of graphene.Its feature
It is：Weigh a certain amount of graphite to be placed in ceramic pot, after calcining certain time in the Muffle furnace of certain temperature, after calcining
Expanded graphite be positioned over it is stand-by in brown glass vessel；Then a certain amount of expanded graphite is weighed, is placed in 100ml beaker
In, then a certain amount of ethanol organic solution is poured into beaker, it is stand-by after ultrasonic agitation certain time；Aforesaid liquid is poured into
In agate pot, rock to uniform state, then agate pot is placed on planetary ball mill, by certain rotating speed and certain time
Afterwards, the liquid in agate pot is poured out, graphene is can obtain with after being freeze-dried certain time after being centrifuged with deionized water.This
Method simple production process, gained graphene sheet layer is more complete and crystal grain size is larger, is provided for the application of graphene
More excellent performance.Specific synthesis step is as follows：
1st, weigh 0.5-5g graphite be placed in ceramic pot and control graphite in ceramic pot shared volume ratio be 1:1.5-3, so
After calcining 2-5h in the Muffle furnace at 250-400 DEG C afterwards, the expanded graphite after calcining is positioned in brown glass vessel and treated
With；
2nd, 0.5-2g expanded graphite is weighed, is placed in beaker, then pours into 10-50ml ethanol organic solution in beaker,
It is stand-by after ultrasonic agitation 30-90min；It is 1 to control the mol ratio of graphite and ethanol:2-7, ultrasonic power scope are 100-500W;
3rd, aforesaid liquid is poured into agate pot, rocks to uniform state, then agate pot is placed on planetary ball mill, passed through
After 300-800 rpm/min and 2-8h, the liquid in agate pot is poured out, takes supernatant to be freeze-dried after being centrifuged with deionized water
Graphene is can obtain after 24h.It is 1 to control pellet mass ratio：8-15.
Brief description of the drawings
Fig. 1 is that the SEM of wet type graphene schemes；
Fig. 2 is that the FESEM of wet type graphene schemes.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
1st, the graphite for weighing 5g is placed in ceramic pot, after calcining 2h in the Muffle furnace at 300 DEG C, by the expanded graphite after calcining
It is positioned over alternative in brown glass vessel；
2nd, 0.5g expanded graphite is weighed, is placed in beaker, is then poured into 20ml ethanol organic solution in beaker, ultrasound is stirred
Mix stand-by after 60min；It is 1 to control the mol ratio of graphite and ethanol:4；
3rd, aforesaid liquid is poured into agate pot, rocks to uniform state, then agate pot is placed on planetary ball mill, passed through
After 500 rpm/min and 3h, the liquid in agate pot is poured out, after supernatant freeze-drying 24h is taken after being centrifuged with deionized water
It can obtain graphene.
Embodiment 2
1st, the graphite for weighing 3g is placed in ceramic pot, after calcining 2.5h in the Muffle furnace at 290 DEG C, by the expansion stone after calcining
Ink is positioned over alternative in brown glass vessel；
2nd, 0.6g expanded graphite is weighed, is placed in beaker, is then poured into 25ml ethanol organic solution in beaker, ultrasound is stirred
Mix stand-by after 50min；It is 1 to control the mol ratio of graphite and ethanol:4；
3rd, aforesaid liquid is poured into agate pot, rocks to uniform state, then agate pot is placed on planetary ball mill, passed through
After 600 rpm/min and 2.5h, the liquid in agate pot is poured out, takes supernatant to be freeze-dried 24h after being centrifuged with deionized water
It can obtain graphene afterwards.
Embodiment 3
1st, the graphite for weighing 3.5g is placed in ceramic pot, after calcining 1.5h in the Muffle furnace at 310 DEG C, by the expansion after calcining
Graphite is positioned over alternative in brown glass vessel；
2nd, 0.35g expanded graphite is weighed, is placed in beaker, then pours into 18ml ethanol organic solution in beaker, ultrasound
It is stand-by after stirring 40min；It is 1 to control the mol ratio of graphite and ethanol:4；
3rd, aforesaid liquid is poured into agate pot, rocks to uniform state, then agate pot is placed on planetary ball mill, passed through
After 450 rpm/min and 3.5h, the liquid in agate pot is poured out, takes supernatant to be freeze-dried 24h after being centrifuged with deionized water
It can obtain graphene afterwards.
Claims (1)
- A kind of 1. new way that graphene is prepared using ethanol as liquid phase planetary ball mill wet method：Specific preparation method：（1）Weigh a certain amount of graphite to be placed in ceramic pot, in Muffle furnace at a certain temperature after calcining certain time, will forge Expanded graphite after burning is positioned over alternative in brown glass vessel；（2）A certain amount of expanded graphite is weighed, is placed in 100ml beaker, then pours into a certain amount of ethanol organic solution In beaker, ultrasonic agitation certain time, offspring used；（3）Aforesaid liquid is poured into agate pot, rocks to uniform state, then agate pot is placed on planetary ball mill, is passed through Cross certain rotating speed and after certain time, the liquid in agate pot is poured out, supernatant freezing is dry with taking after being centrifuged with deionized water Graphene is can obtain after dry certain time, the wherein quality of graphite is 0.5-5g, and controls the mol ratio of graphite and ethanol to be 1:2-7。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711003385.7A CN107758648A (en) | 2017-10-24 | 2017-10-24 | A kind of new way that graphene is prepared using ethanol as liquid phase planetary ball mill wet method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711003385.7A CN107758648A (en) | 2017-10-24 | 2017-10-24 | A kind of new way that graphene is prepared using ethanol as liquid phase planetary ball mill wet method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107758648A true CN107758648A (en) | 2018-03-06 |
Family
ID=61270242
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711003385.7A Pending CN107758648A (en) | 2017-10-24 | 2017-10-24 | A kind of new way that graphene is prepared using ethanol as liquid phase planetary ball mill wet method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107758648A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761226A (en) * | 2019-02-16 | 2019-05-17 | 江苏大学 | A kind of method that liquid phase ball milling prepares two-dimensional nano graphite flake |
| CN111393823A (en) * | 2020-04-22 | 2020-07-10 | 福州大学 | Gn-PET/PC alloy with excellent mechanical property and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN103420362A (en) * | 2012-05-22 | 2013-12-04 | 海洋王照明科技股份有限公司 | Preparation method for graphene |
| CN103803539A (en) * | 2014-02-17 | 2014-05-21 | 上海交通大学 | Nitrogen-doped graphene oxide material and preparation method thereof |
| CN105883757A (en) * | 2014-12-09 | 2016-08-24 | 戴加龙 | Method for producing graphene |
| CN106587034A (en) * | 2017-02-24 | 2017-04-26 | 安徽桑瑞斯环保新材料有限公司 | Lamina graphene production method |
-
2017
- 2017-10-24 CN CN201711003385.7A patent/CN107758648A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN103420362A (en) * | 2012-05-22 | 2013-12-04 | 海洋王照明科技股份有限公司 | Preparation method for graphene |
| CN103803539A (en) * | 2014-02-17 | 2014-05-21 | 上海交通大学 | Nitrogen-doped graphene oxide material and preparation method thereof |
| CN105883757A (en) * | 2014-12-09 | 2016-08-24 | 戴加龙 | Method for producing graphene |
| CN106587034A (en) * | 2017-02-24 | 2017-04-26 | 安徽桑瑞斯环保新材料有限公司 | Lamina graphene production method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761226A (en) * | 2019-02-16 | 2019-05-17 | 江苏大学 | A kind of method that liquid phase ball milling prepares two-dimensional nano graphite flake |
| CN111393823A (en) * | 2020-04-22 | 2020-07-10 | 福州大学 | Gn-PET/PC alloy with excellent mechanical property and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105293476B (en) | A kind of preparation method of large scale graphene oxide or graphene | |
| CN104556022A (en) | Method for preparing expanded microcrystal graphite material from microcrystal graphite | |
| CN107758648A (en) | A kind of new way that graphene is prepared using ethanol as liquid phase planetary ball mill wet method | |
| CN104003375A (en) | Preparation method for small-size graphene | |
| CN104386676B (en) | A kind of preparation method of graphene | |
| CN103667046B (en) | PCR (polymerase chain reaction) instrument with partitions | |
| CN105347332A (en) | Preparation method for graphene | |
| CN103553030A (en) | Preparation method of few-layer graphene | |
| CN106564893A (en) | Hundred micron-order graphene oxide and preparation method thereof | |
| CN103253672A (en) | Preparation method of silicon carbide nanowire thin film based on hydrogen production by photoelectric catalytic decomposition of water | |
| CN104071777A (en) | Preparation method of graphene | |
| CN107934947B (en) | Graphene preparation method based on efficient surfactant | |
| CN107161989A (en) | A kind of preparation method of cellular three-dimensional grapheme | |
| CN114933327B (en) | Hydrogen production material and preparation method and application thereof | |
| CN106517224B (en) | A kind of preparation method of kaolinite nanometer sheet | |
| CN107572512A (en) | A kind of new way that graphene is prepared using glycerine as liquid phase planetary ball mill wet method | |
| CN104692371B (en) | A kind of pressure-fired produces the method and device of graphene film continuously | |
| CN109279605A (en) | A kind of hafnium carbide preparation method | |
| CN104860327B (en) | A kind of ZrB with columnar grain2Raw powder's production technology | |
| CN109264785A (en) | A kind of Lacking oxygen WO3-XThe fast preparation method of powder body material | |
| CN108862259B (en) | Graphene production method and device | |
| CN107352531A (en) | A kind of method that micro crystal graphite prepares graphene | |
| CN103848419B (en) | The washing of a kind of membrane process separates the method preparing ultra-fine graphite oxide | |
| CN106829939B (en) | Method and device for preparing graphene | |
| CN108975315A (en) | The preparation method of the grapheme material of three-dimensional manometer lamellar structure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180306 |