CN105217612B - A kind of ultrasonic assistant sand mill stripping prepares the method for graphene and peels off the device of graphene processed - Google Patents
A kind of ultrasonic assistant sand mill stripping prepares the method for graphene and peels off the device of graphene processed Download PDFInfo
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- CN105217612B CN105217612B CN201510634802.2A CN201510634802A CN105217612B CN 105217612 B CN105217612 B CN 105217612B CN 201510634802 A CN201510634802 A CN 201510634802A CN 105217612 B CN105217612 B CN 105217612B
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Abstract
The method of graphene is prepared the invention discloses a kind of ultrasonic assistant sand mill stripping and peels off the device of graphene processed, this method is loaded with ultrasonic stripping by the graphite dispersing solution that mixes crystalline flake graphite with the water containing surfactant in the process of grinding, in grinding 1000~3000r/min of rotating speed, ultrasonic stripping is ground to graphite dispersing solution under the conditions of 100~750KW of ultrasonic power, by being centrifugally separating to obtain graphene dispersing solution.This method utilizes the shear action in sand mill process of lapping, with reference to the ultrasonic cavitation in ultrasonic grinder, realizes prepared by broken peel off of the pure physics of crystalline flake graphite, technical process is simple, mild condition, and it is with low cost, it is adaptable to large-scale industrial production.
Description
Technical field
The present invention relates to a kind of method for preparing graphene, more particularly, refer to a kind of using ultrasonic assistant sand milling
The method that machine stripping prepares graphene.
Background technology
Graphene is waited in professor Geim by Univ Manchester UK in 2004 and obtained first, and it is by single layer of carbon atom
The bi-dimensional cellular shape structure of composition.Since being found, graphene becomes investigation of materials in recent years due to its unique property
One of focus, in fields such as new material, new energy, electronics, exhibition exposes huge application prospect, but its yield and valency
Lattice are always the bottleneck for limiting its commercial application.
The preparation method of current graphene is divided into chemical method and the major class of Physical two.Wherein chemical method mainly using oxidation-
Reducing process, it is, as graphite oxide, graphene oxide to be obtained after then being peeled off by ultrasound by oxidant by graphite oxidation,
Graphene oxide reduction is obtained into graphene finally by reducing agent.But this method needs to use strong oxidizer and severe corrosive
Acid, while completely can not be reduced the oxygen-containing functional group of surface of graphene oxide in reduction process, resulting reduction graphite
Also there is oxygen-containing functional group defect in alkene surface, and preparation process is cumbersome, and the time is longer.
And physical method is mainly a kind of in the way of overcoming graphitic carbon interlayer Van der Waals force, realize that graphite is top-down
The method peeled off and prepare graphene, such as adhesive tape stripping method, ultrasonic stripping method, ball-milling method.Geim etc. uses adhesive tape stripping method
Prepare piece of graphite alkene in the world, but to prepare graphene uncontrollable for this method, yields poorly, graphene film size is small, turn
Move difficulty etc..The method that ultrasonic wave directly peels off powdered graphite to prepare graphene is developed for this, this method is mainly sharp
The stripping of graphite layers is realized with ultrasonic cavitation, it is simple with technique, it is with low cost, prepared graphene defect compared with
It is small etc., but at present using this method realize the biggest obstacle of industrialized production graphene be ultrasound stripping capacity usage ratio compared with
Low, ultrasonic cavitation region is small etc..The method for developing ball-milling method again for this people to prepare graphene, this method is mainly using grinding
The shear action of grinding media realizes the stripping of graphite layers, graphene defect simple with technique, with low cost, prepared
It is smaller etc., but preparation time is longer, and the yield of prepared graphene is relatively low.
The content of the invention
The purpose of the inventive method is intended to overcome the deficiencies in the prior art part and provide a kind of using ultrasonic assistant sand
The method that grinding machine stripping prepares graphene.The inventive method is used has more dense grinding energy, more Gao Yan relative to ball mill
Mill efficiency and material can the sand mill of Continuous maching prepare graphene, while the ultrasonic probe of ultrasonic grinder is put into sand
In grinding machine hopper, ultrasonic stripping is carried out while graphite is ground, realizes that ultrasonic stripping method prepares graphene and prepared with ball-milling method
The combination of both graphenes.Ultrasonic stripping method is prepared into the ultrasonic cavitation of graphene and ball-milling method prepares the grinding of graphene
Both medium shear actions combine, peel off graphite by the collective effect of shear action and both ultrasonic cavitations and
Obtain graphene.
Ultrasonic grind is aided in the stripping graphene dress on sand mill it is a further object of the present invention to provide a kind of
Put, the stripping graphene device is improved on existing sand mill, mechanical agitation is substituted using ultrasonic grind, from
And realize and ultrasonic stripping is carried out while graphite is ground, realize that ultrasonic stripping method prepares graphene and prepares graphene with ball-milling method
The combination of the two.
The present invention is a kind of method that ultrasonic assistant sand mill stripping prepares graphene, and it includes the following steps：
Step A, graphite dispersing solution processed；
Crystalline flake graphite is mixed in raw material mixing system with aqueous surfactant solution, graphite dispersing solution is made.
The crystalline flake graphite size is less than 325 mesh, and the concentration of crystalline flake graphite is 1~50mg/ml, aqueous surfactant solution
Concentration be 0.05~10mg/ml；
Step B, ultrasonic assistant grinds graphite stripper processed；
It will be added through graphite dispersing solution made from step A in the loading hopper of sand mill system, make graphite dispersing solution in sand milling
It can be circulated in the grinding chamber and hopper of machine；
After 3~30min of processing is ground to graphite dispersing solution under the conditions of grinding rotating speed is 1550~3000r/min,
The ultrasonic probe of ultrasonic grinder system is placed in loading hopper；
It is that 1550~3000r/min, ultrasonic power are the graphite to circulation under conditions of 100~750KW in grinding rotating speed
Dispersion liquid is carried out after 0.5~6h of processing, stops Ultrasonic Pulverization；
After 3~30min of processing is ground to graphite dispersing solution under the conditions of grinding rotating speed is 1000~1500r/min,
The ultrasonic probe of ultrasonic grinder is placed in loading hopper；
It is that 1000~1500r/min, ultrasonic power are the graphite to circulation under conditions of 100~750KW in grinding rotating speed
Dispersion liquid is carried out after 0.5~6h of processing, and graphite stripper is made；
Step C, centrifuges graphene dispersing solution processed；
The graphite stripper that step B is obtained is centrifuged in centrifugal separation system 4 under the conditions of 1000~6000r/min
1~4h, takes supernatant liquor, as graphene dispersing solution.
Through graphene lateral dimension made from the inventive method in 0.4~1.8 microns, lateral dimension is evenly distributed.
Through graphene solution concentration made from the inventive method 0.7%~1.5%.
The advantage for the method that the present invention prepares graphene using ultrasonic assistant sand mill stripping is：
1. the production graphene of industrialization can be realized, and yield is high, quality is good.
2. applying the inventive method to prepare, graphene technique is simply controllable, and with low cost, prepared graphene defect is small.
3. this method utilizes the shear action in sand mill process of lapping, makees with reference to the ultrasonic cavitation in ultrasonic grinder
With, realize prepared by broken peel off of the pure physics of crystalline flake graphite, technical process is simple, mild condition, and it is with low cost, suitable for big
Large-scale production.
Brief description of the drawings
Fig. 1 is the system structure diagram that the present invention prepares graphene using ultrasonic assistant sand mill stripping.
Figure 1A is that the combination between the probe of ultrasonic grinder system in the present invention and the loading hopper of sand mill system is shown
It is intended to.
Fig. 2 is the equipment photo of existing laboratory horizontal sand mill.
Fig. 3 is atomic force microscopy of the embodiment 1 using graphene made from the inventive method.
Fig. 4 is the atomic force microscopy of graphene made from comparative example 1.
Fig. 5 is the atomic force microscopy of graphene made from comparative example 2.
| 1. raw material mixing system | 2. ultrasonic grind system | 21. ultrasonic probe |
| 3. sand mill system | 31. grind main frame | 32. loading hopper |
| 33.A pipelines | 34.B pipelines | 4. centrifugal separation system |
Embodiment
Below in conjunction with drawings and examples, the present invention is described in further detail.
It is shown in Figure 2, in the horizontal sand mill system of laboratory at least provided with grinding main frame, grinding container, loading hopper,
Mixer.Because mixer is merely able to play a part of preventing graphite from precipitating in hopper, in order to strengthen the peeling effect of graphite,
Therefore mixer is replaced with into ultrasonic grinder system, the cavitation peeled off in grinding stripping process using ultrasound with it is strong
Abrasive media shearing force is combined, and is reached shear action with the collective effect of both ultrasonic cavitations and is obtained to peel off graphite
The high graphene of low defect, yield.
In the present invention, the stripping of ultrasonic assistant sand mill prepares the device of the stripping graphene processed of graphene, and being will be super
The ultrasonic probe 21 of sonic disintegrator system 2 is placed in the loading hopper 32 of sand mill system 3, and removes sand mill system 3
Mixer, as shown in Figure 1A.Graphite dispersing solution is added in the loading hopper 32 of sand mill system 3, in bearing that sand mill system 3 is produced
Pressure, graphite dispersing solution is entered in grinding main frame 31 through A pipelines 33, is again introduced into by B pipelines 34 in hopper 32 and is realized thing
The circulation of material.
Referring to shown in Fig. 1, Figure 1A, the present invention prepares graphene using ultrasonic assistant sand mill stripping and includes following step
Suddenly：
Step A, graphite dispersing solution processed；
Crystalline flake graphite is mixed with aqueous surfactant solution in raw material mixing system 1, graphite dispersing solution is made.
The crystalline flake graphite size is less than 325 mesh, and the concentration of crystalline flake graphite is 1~50mg/ml.
The surfactant is neopelex, sodium carboxymethylcellulose, 18 acyl aminoethyl trimethyl sulphur
Sour ammonium, myristoyl aminopropyl dimethyl benzyl ammonium chloride, sodium taurocholate, sodium taurodeoxycholate, polyoxyethylenes (40) nonyl benzene
A kind of in base ether and sorbitan monooleate APEO or two kinds of combination.Aqueous surfactant solution it is dense
Spend for 0.05~10mg/ml.
The raw material mixing system 1 can be beaker, burette, grinding container, common plastics, glass or irony
Container.
Step B, ultrasonic assistant grinds graphite stripper processed；
It will be added through graphite dispersing solution made from step A in the loading hopper of sand mill system 3, make graphite dispersing solution in sand milling
It can be circulated in the grinding chamber and hopper of machine；
After 3~30min of processing is ground to graphite dispersing solution under the conditions of grinding rotating speed is 1550~3000r/min,
The ultrasonic probe of ultrasonic grinder system 2 is placed in loading hopper；
It is that 1550~3000r/min, ultrasonic power are the graphite to circulation under conditions of 100~750KW in grinding rotating speed
Dispersion liquid is carried out after 0.5~6h of processing, stops Ultrasonic Pulverization；
After 3~30min of processing is ground to graphite dispersing solution under the conditions of grinding rotating speed is 1000~1500r/min,
The ultrasonic probe of ultrasonic grinder is placed in loading hopper；
It is that 1000~1500r/min, ultrasonic power are the graphite to circulation under conditions of 100~750KW in grinding rotating speed
Dispersion liquid is carried out after 0.5~6h of processing, and graphite stripper is made；
In the present invention, ultrasonic wave and grinding can synchronously carry out, progress can also be spaced.
Step C, centrifuges graphene dispersing solution processed；
The graphite stripper that step B is obtained is centrifuged in centrifugal separation system 4 under the conditions of 1000~6000r/min
1~4h, takes supernatant liquor, as graphene dispersing solution.
Embodiment 1
Sand mill selects the MSG-LNO.3 laboratories horizontal sand mill that Shanghai Ming Shi mechanical ＆ electronic equipment corporation, Ltds produce.
Ultrasonic grinder selects the Scientz-IID type ultrasonic waves that NingBo XinZhi Biology Science Co., Ltd produces
Cell disruptor.
Referring to shown in Fig. 1, Figure 1A, Fig. 2, graphene is prepared using ultrasonic assistant sand mill stripping and includes following step
Suddenly：
Step A, graphite dispersing solution processed；
Crystalline flake graphite is well mixed in beaker with aqueous surfactant solution, 400mL graphite dispersing solution is made.
The crystalline flake graphite average-size is 325 mesh, and the concentration of crystalline flake graphite is 30mg/ml.
The surfactant is sodium taurodeoxycholate, and the concentration of its sodium taurodeoxycholate aqueous solution is 3mg/ml.
Step B, ultrasonic assistant grinds graphite stripper processed；
It will be added through graphite dispersing solution made from step A in the loading hopper of sand mill, make graphite dispersing solution in sand mill
It can be circulated in grinding chamber and hopper；
After processing 10min is ground to graphite dispersing solution under the conditions of grinding rotating speed is 2600r/min, by ultrasonic wave powder
The ultrasonic probe of broken machine is placed in loading hopper；
It is that 2600r/min, ultrasonic power are at the graphite dispersing solution progress under conditions of 550KW to circulation in grinding rotating speed
Manage after 0.5h, stop Ultrasonic Pulverization；
After processing 10min is ground to graphite dispersing solution under the conditions of grinding rotating speed is 1000r/min, by ultrasonic wave powder
The ultrasonic probe of broken machine is placed in loading hopper；
It is that 1000r/min, ultrasonic power are at the graphite dispersing solution progress under conditions of 550KW to circulation in grinding rotating speed
Manage after 0.5h, graphite stripper is made；
Step C, centrifuges graphene dispersing solution processed；
The obtained graphite strippers of step B are centrifuged into 1h under the conditions of 4000r/min, supernatant liquor, as stone is taken
Black alkene dispersion liquid.
Dimensional characteristic analysis is carried out to graphene dispersing solution made from embodiment 1 using AFM.Understood in figure
Graphene lateral dimension made from embodiment 1 is in 0.8~1.2 microns, and lateral dimension is evenly distributed.
Embodiment 2
Sand mill selects the MSG-LNO.3 laboratories horizontal sand mill that Shanghai Ming Shi mechanical ＆ electronic equipment corporation, Ltds produce.
Ultrasonic grinder selects the Scientz-IID type ultrasonic waves that NingBo XinZhi Biology Science Co., Ltd produces
Cell disruptor.
Referring to shown in Fig. 1, Figure 1A, Fig. 2, graphene is prepared using ultrasonic assistant sand mill stripping and includes following step
Suddenly：
Step A, graphite dispersing solution processed；
Crystalline flake graphite is well mixed in burette with aqueous surfactant solution, 400mL graphite dispersion is made
Liquid.
The crystalline flake graphite average-size is 1250 mesh, and the concentration of crystalline flake graphite is 15mg/ml.
The surfactant is sodium taurodeoxycholate and neopelex by 1:1 is configured.Live on surface
Property the agent aqueous solution concentration be 8mg/ml.
Step B, ultrasonic assistant grinds graphite stripper processed；
It will be added through graphite dispersing solution made from step A in the loading hopper of sand mill, make graphite dispersing solution in sand mill
It can be circulated in grinding chamber and hopper；
It is that 2600r/min, ultrasonic power are at the graphite dispersing solution progress under conditions of 550KW to circulation in grinding rotating speed
Manage after 2.5h, graphite stripper is made；
Step C, centrifuges graphene dispersing solution processed；
The obtained graphite strippers of step B are centrifuged into 1h under the conditions of 4000r/min, supernatant liquor, as stone is taken
Black alkene dispersion liquid.
Dimensional characteristic analysis is carried out to graphene dispersing solution made from embodiment 2 using AFM, graphene is horizontal
To size in 0.6~1.0 microns, lateral dimension is evenly distributed.
Embodiment 3
Sand mill selects the MSG-LNO.3 laboratories horizontal sand mill that Shanghai Ming Shi mechanical ＆ electronic equipment corporation, Ltds produce.
Ultrasonic grinder selects the Scientz-IID type ultrasonic waves that NingBo XinZhi Biology Science Co., Ltd produces
Cell disruptor.
Referring to shown in Fig. 1, Figure 1A, Fig. 2, graphene is prepared using ultrasonic assistant sand mill stripping and includes following step
Suddenly：
Step A, graphite dispersing solution processed；
Crystalline flake graphite is well mixed in burette with aqueous surfactant solution, 400mL graphite dispersion is made
Liquid.
The crystalline flake graphite average-size is 325 mesh, and the concentration of crystalline flake graphite is 50mg/ml.
The surfactant is sodium taurodeoxycholate.The concentration of aqueous surfactant solution is 1.5mg/ml.
Step B, ultrasonic assistant grinds graphite stripper processed；
It will be added through graphite dispersing solution made from step A in the loading hopper of sand mill, make graphite dispersing solution in sand mill
It can be circulated in grinding chamber and hopper；
After processing 5min is ground to graphite dispersing solution under the conditions of grinding rotating speed is 2200r/min, by ultrasonic wave powder
The ultrasonic probe of broken machine is placed in loading hopper；
It is that 2200r/min, ultrasonic power are at the graphite dispersing solution progress under conditions of 400KW to circulation in grinding rotating speed
Manage after 1h, stop Ultrasonic Pulverization；
After processing 5min is ground to graphite dispersing solution under the conditions of grinding rotating speed is 1500r/min, by ultrasonic wave powder
The ultrasonic probe of broken machine is placed in loading hopper；
It is that 1500r/min, ultrasonic power are at the graphite dispersing solution progress under conditions of 750KW to circulation in grinding rotating speed
Manage after 0.5h, graphite stripper is made；
Step C, centrifuges graphene dispersing solution processed；
The obtained graphite strippers of step B are centrifuged into 1h under the conditions of 4000r/min, supernatant liquor, as stone is taken
Black alkene dispersion liquid.
Dimensional characteristic analysis is carried out to graphene dispersing solution made from embodiment 3 using AFM, graphene is horizontal
To size in 1.0~1.2 microns, lateral dimension is evenly distributed.
The comparison example 1 of graphene is made in simple sand mill
Sand mill selects the MSG-LNO.3 laboratories horizontal sand mill that Shanghai Ming Shi mechanical ＆ electronic equipment corporation, Ltds produce.
The step of only preparing graphene with sand mill be：
Step A, graphite dispersing solution processed；
Crystalline flake graphite is well mixed in beaker with aqueous surfactant solution, 400mL graphite dispersing solution is made.
The crystalline flake graphite average-size is 325 mesh, and the concentration of crystalline flake graphite is 30mg/ml.
The surfactant is sodium taurodeoxycholate.The concentration of aqueous surfactant solution is 3mg/ml.
Step B, grinds graphite stripper processed；
It will be added through graphite dispersing solution made from step A in the loading hopper of sand mill, make graphite dispersing solution in sand mill
It can be circulated in grinding chamber and hopper；Processing 1h is ground to graphite dispersing solution under the conditions of grinding rotating speed is 2600r/min
Afterwards, graphite stripper is made；
Step C, centrifuges graphene dispersing solution processed；
The obtained graphite strippers of step B are centrifuged into 1h under the conditions of 4000r/min, supernatant liquor, as stone is taken
Black alkene dispersion liquid.
Graphene clear liquid made from comparison example 1 is carried out using AFM to understand in dimensional characteristic analysis, figure
The lateral dimension of graphene it is big at 2~6 microns, have graphene of a small amount of lateral dimension at 0.2~1 micron, there are two kinds of horizontal strokes
To the graphene of Size Distribution.
The comparison example 2 of graphene is made in simple ultrasonic grinder
Ultrasonic grinder selects the Scientz-IID type ultrasonic waves that NingBo XinZhi Biology Science Co., Ltd produces
Cell disruptor.
The step of only preparing graphene with ultrasonic grinder be：
Step A, graphite dispersing solution processed；
Crystalline flake graphite is well mixed in beaker with aqueous surfactant solution, 400mL graphite dispersing solution is made.
The crystalline flake graphite average-size is 325 mesh, and the concentration of crystalline flake graphite is 30mg/ml.
The surfactant is sodium taurodeoxycholate.The concentration of aqueous surfactant solution is 3mg/ml.
Step B, grinds graphite stripper processed；
It will be added through graphite dispersing solution made from step A in the loading hopper of ultrasonic grinder, be 550KW in ultrasonic power
Under conditions of graphite dispersing solution is carried out after ultrasonic Separation processing 1h, graphite stripper is made；
Step C, centrifuges graphene dispersing solution processed；
The obtained graphite strippers of step B are centrifuged into 1h under the conditions of 4000r/min, supernatant liquor, as stone is taken
Black alkene dispersion liquid.
Graphene clear liquid made from comparison example 2 is carried out using AFM to understand in dimensional characteristic analysis, figure
The lateral dimension of graphene it is big at 1~3 micron, have graphene of the half lateral dimension at 0.2~1 micron.
Graphene dispersing solution concentrations versus's table：
| Graphene dispersing solution concentration | |
| Embodiment 1 | 0.8mg/mL |
| Embodiment 2 | 1.1mg/ml |
| Embodiment 3 | 0.7mg/mL |
| Comparison example 1 | 0.2mg/mL |
| Comparison example 2 | 0.4mg/mL |
The present invention is a kind of method that use ultrasonic assistant sand mill stripping prepares graphene, and how to be solved be
The technical problem of the quality of preparing graphite alkene is improved in process of lapping, this method is by ultrasonic cavitation and abrasive media
Shear action is combined, collective effect come peel off graphite obtain graphene technological means.This method is ground using sand mill
Shear action in journey, with reference to the ultrasonic cavitation in ultrasonic grinder, realizes that the pure physics of crystalline flake graphite is broken and peels off
Prepare, technical process is simple, mild condition, and it is with low cost, suitable for large-scale industrialization production.
Claims (1)
1. a kind of method that ultrasonic assistant sand mill stripping prepares graphene, it is characterised in that include the following steps：
Step A, graphite dispersing solution processed；
Crystalline flake graphite is mixed in raw material mixing system with aqueous surfactant solution, graphite dispersing solution is made；The surface
Activating agent be sodium carboxymethylcellulose, 18 acyl aminoethyl trimethyl ammonium sulfate, myristoyl aminopropyl dimethyl benzyl ammonium chloride,
Sodium taurocholate, sodium taurodeoxycholate, polyoxyethylenes (40) nonylplenyl ether and sorbitan monooleate APEO
In a kind of or three kinds of combination；
The crystalline flake graphite size is less than 325 mesh, and the concentration of crystalline flake graphite is 1~50mg/ml, aqueous surfactant solution it is dense
Spend for 0.05~10mg/ml；
Step B, ultrasonic assistant grinds graphite stripper processed；
It will be added through graphite dispersing solution made from step A in the loading hopper of horizontal sand mill, graphite dispersing solution is sanded horizontal
It can be circulated in the grinding chamber and hopper of machine；Mixer in horizontal sand mill is replaced with into ultrasonic cell disruptor；
, will be super after 3~30min of processing is ground to graphite dispersing solution under the conditions of grinding rotating speed is 1550~3000r/min
The ultrasonic probe of sound wave cell disruptor is placed in loading hopper；
It is that 1550~3000r/min, ultrasonic power are the graphite dispersion to circulation under conditions of 100~750KW in grinding rotating speed
Liquid is carried out after 0.5~6h of processing, stops Ultrasonic Pulverization；
, will be super after 3~30min of processing is ground to graphite dispersing solution under the conditions of grinding rotating speed is 1000~1500r/min
The ultrasonic probe of sound wave cell disruptor is placed in loading hopper；
It is that 1000~1500r/min, ultrasonic power are the graphite dispersion to circulation under conditions of 100~750KW in grinding rotating speed
Liquid is carried out after 0.5~6h of processing, and graphite stripper is made；
Step C, centrifuges graphene dispersing solution processed；
The graphite stripper that step B is obtained centrifuges 1 in centrifugal separation system 4 under the conditions of 1000~6000r/min~
4h, takes supernatant liquor, as graphene dispersing solution；The concentration of the graphene is 0.7%~1.5%；
Graphene lateral dimension after being peeled off in the graphene dispersing solution is at 0.4~1.8 micron.
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Effective date of registration: 20211229 Address after: Nanping Nan'an District of Chongqing City Road 400060 No. 168 Patentee after: CHONGQING JIAN'AN INSTRUMENT Co.,Ltd. Address before: 100191 No. 37, Haidian District, Beijing, Xueyuan Road Patentee before: BEIHANG University |