CN107572512A - A kind of new way that graphene is prepared using glycerine as liquid phase planetary ball mill wet method - Google Patents
A kind of new way that graphene is prepared using glycerine as liquid phase planetary ball mill wet method Download PDFInfo
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- CN107572512A CN107572512A CN201711003384.2A CN201711003384A CN107572512A CN 107572512 A CN107572512 A CN 107572512A CN 201711003384 A CN201711003384 A CN 201711003384A CN 107572512 A CN107572512 A CN 107572512A
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Abstract
The invention provides a kind of new way that graphene is prepared using glycerine 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 glycerine 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 glycerine as liquid phase planetary ball mill wet method, belong to advanced
Technical field of nano-composite material preparation technology.
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 find that it is organic solution to think glycerine, is using the wet ball-milling environment with certain viscosity
Graphite provides sufficiently scattered, buffering and package action, impact of the reduction mechanical milling process to graphite in ball mill mechanical milling process
Power, and well by graphene dispersion in viscosity solution so that the graphene size being prepared is larger, and defect is less, compared with
It is good the drawbacks of 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 glycerine as liquid phase planet
Ball mill wet method prepares the new way of graphene.With simple production process, yield is high, graphene defect is less and crystal
The more complete feature of size.The nano material of gained graphene can be used for improving the new of 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.It is special
Sign is：Weigh a certain amount of graphite to be placed in ceramic pot, after calcining certain time in the Muffle furnace of certain temperature, will calcine
Expanded graphite afterwards is positioned over stand-by in brown glass vessel；Then a certain amount of expanded graphite is weighed, is placed in 100ml beaker
In, then the glycerine organic solution for being incubated dog at a certain temperature is poured into beaker, at a certain temperature stirring ultrasound one
It is stand-by after fixing time；Aforesaid liquid is poured under certain temperature in the agate pot after being incubated, rocked to uniform state, then by agate
Nao tanks are placed on planetary ball mill, by certain rotating speed and after certain time, the liquid in agate pot are poured out, uses deionized water
Graphene is can obtain after certain time is freeze-dried after centrifugation.This method simple production process, gained graphene sheet layer are completeer
Whole and crystal grain size is larger, and more excellent performance is provided for the application of graphene.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 by the glycerine organic solution under 10-50ml certain temperatures
Pour into 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
For 100-500W, glycerine organic solution is stand-by after 25-55 DEG C of insulation 30-60min, and whipping temp is controlled at 25-55 DEG C；
3rd, aforesaid liquid is poured into the agate pot after insulation, rocks to uniform state, agate pot is then placed in planetary ball mill
On machine, after 300-800 rpm/min and 2-8h, the liquid in agate pot is poured out, supernatant is taken after being centrifuged with deionized water
Graphene is can obtain after liquid freeze-drying 24h.It is 1 to control pellet mass ratio：8-15；Agate pot is incubated 30- at 25-55 DEG C
It is stand-by after 60min.
Brief description of the drawings
Fig. 1 is that the SEM of sticky wet type graphene schemes；
Fig. 2 is that the FESEM of sticky 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, weigh 2g graphite be placed in ceramic pot and control graphite in ceramic pot shared volume ratio be 1:1.5, then 300
In Muffle furnace at DEG C after calcining 2h, the expanded graphite after calcining is positioned over stand-by in brown glass vessel；
2nd, 1g expanded graphite is weighed, is placed in beaker, the glycerine organic solution under 20ml certain temperatures is then poured into burning
It is stand-by after ultrasonic agitation 60min in cup；It is 1 to control the mol ratio of graphite and ethanol:4, ultrasonic power scope is 200W, the third three
Alcohol organic solution is stand-by after 35 DEG C of insulation 300min, and whipping temp is controlled at 35 DEG C；
3rd, aforesaid liquid is poured into the agate pot after insulation, rocks to uniform state, agate pot is then placed in planetary ball mill
On machine, after 500 rpm/min and 3h, the liquid in agate pot is poured out, takes supernatant to freeze after being centrifuged with deionized water
Graphene is can obtain after drying 24h.It is 1 to control pellet mass ratio：11；Agate pot is stand-by after 35 DEG C of insulation 30min；
Embodiment 2
1st, weigh 3g graphite be placed in ceramic pot and control graphite in ceramic pot shared volume ratio be 1:2, then at 280 DEG C
Under Muffle furnace in calcining 3h after, the expanded graphite after calcining is positioned over stand-by in brown glass vessel；
2nd, 0.5g expanded graphite is weighed, is placed in beaker, then pours into the glycerine organic solution under 15ml certain temperatures
It is stand-by after ultrasonic agitation 80min in beaker；It is 1 to control the mol ratio of graphite and ethanol:3.5, ultrasonic power scope is 300W,
Glycerine organic solution is stand-by after 30 DEG C of insulation 40min, and whipping temp is controlled at 30 DEG C；
3rd, aforesaid liquid is poured into the agate pot after insulation, rocks to uniform state, agate pot is then placed in planetary ball mill
On machine, after 400 rpm/min and 4h, the liquid in agate pot is poured out, takes supernatant to freeze after being centrifuged with deionized water
Graphene is can obtain after drying 24h.It is 1 to control pellet mass ratio：10；Agate pot is stand-by after 30 DEG C of insulation 40min.
Claims (1)
- A kind of 1. new way that graphene is prepared using glycerine 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 by the glycerine after being incubated under certain temperature Organic solution is poured into beaker, is stirred ultrasonic certain time offspring at a certain temperature and is used；（3）Aforesaid liquid is poured into the agate pot being incubated at a certain temperature, rock to uniform state, then put agate pot In on planetary ball mill, by certain rotating speed and after certain time, the liquid in agate pot is poured out, centrifuged with deionized water After take supernatant freeze-drying certain time after can obtain graphene, the wherein quality of graphite is 0.5-5g, and control graphite Mol ratio with glycerine is 1:2-7.
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| CN201711003384.2A CN107572512A (en) | 2017-10-24 | 2017-10-24 | A kind of new way that graphene is prepared using glycerine as liquid phase planetary ball mill wet method |
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Cited By (1)
| 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 |
Citations (3)
| 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 |
| CN102225758A (en) * | 2011-04-13 | 2011-10-26 | 昆明物理研究所 | Supersonic chemical preparation method for grapheme quantum dots |
| CN103058181A (en) * | 2013-01-25 | 2013-04-24 | 哈尔滨工业大学 | Preparation method for nano multilayer graphene emulsion |
-
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- 2017-10-24 CN CN201711003384.2A patent/CN107572512A/en active Pending
Patent Citations (3)
| 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 |
| CN102225758A (en) * | 2011-04-13 | 2011-10-26 | 昆明物理研究所 | Supersonic chemical preparation method for grapheme quantum dots |
| CN103058181A (en) * | 2013-01-25 | 2013-04-24 | 哈尔滨工业大学 | Preparation method for nano multilayer graphene emulsion |
Cited By (1)
| 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 |
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Application publication date: 20180112 |