CN105217612A - A kind of ultrasonic assistant sand mill peels off the method preparing Graphene and the device peeling off Graphene processed - Google Patents
A kind of ultrasonic assistant sand mill peels off the method preparing Graphene and the device peeling off Graphene processed Download PDFInfo
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Abstract
The invention discloses a kind of ultrasonic assistant sand mill and peel off the method preparing Graphene and the device peeling off Graphene processed, the method is loaded with ultrasonic stripping by the graphite dispersing solution mixed with the water containing tensio-active agent by crystalline flake graphite in the process of grinding, under grinding rotating speed 1000 ~ 3000r/min, ultrasonic power 100 ~ 750KW condition, ultrasonic stripping is ground to graphite dispersing solution, obtain graphene dispersing solution by centrifugation.The method utilizes the shearing action in sand mill process of lapping, and in conjunction with the ultrasonic cavitation in ultrasonic grinder, preparation is peeled off in the pure physics fragmentation realizing crystalline flake graphite, technological process is simple, mild condition, and with low cost, be applicable to large-scale industrial production.
Description
Technical field
The present invention relates to a kind of method preparing Graphene, more particularly, refer to that the method preparing Graphene peeled off by a kind of ultrasonic assistant sand mill that adopts.
Background technology
First Graphene obtains in professor Geim etc. by Univ Manchester UK in 2004, and it is by the former molecular bi-dimensional cellular shape structure of monolayer carbon.Since being found, Graphene becomes one of focus of investigation of materials in recent years due to the character of its uniqueness, expose huge application prospect in field exhibitions such as novel material, new forms of energy, electronics, but its output and price are the bottlenecks limiting its commercial application always.
The preparation method of current Graphene is divided into chemical method and the large class of Physical two.Wherein chemical method mainly adopts oxidation-reduction method, and it is, by oxygenant, graphite oxidation is become graphite oxide, then by obtaining graphene oxide after ultrasonic stripping, finally by reductive agent, graphene oxide reduction is obtained Graphene.But the method needs to use strong oxidizer and severe corrosive acid, completely the oxygen-containing functional group of surface of graphene oxide can not be reduced in reduction process simultaneously, also there is oxygen-containing functional group defect in the reduced graphene surface obtained, and preparation process is loaded down with trivial details, and the time is longer.
And physical method is mainly a kind of in the mode overcoming graphite carbon interlayer Van der Waals force, realizes the top-down stripping of graphite and prepare the method for Graphene, as tape stripping method, ultrasonic stripping method, ball milled etc.Geim etc. adopt tape stripping method to prepare first Graphene in the world, but the method to prepare Graphene uncontrollable, yield poorly, graphene film size be little, transfer difficulty etc.Be developed ultrasonic wave for this reason and directly peel off powdered graphite to prepare the method for Graphene, the method mainly utilizes ultrasonic cavitation to realize the stripping of graphite layers, there is technique simple, with low cost, prepared Graphene defect is less, but the biggest obstacle adopting the method to realize suitability for industrialized production Graphene is at present that the capacity usage ratio of ultrasonic stripping is lower, ultrasonic cavitation region is little.People develop again ball milled to prepare the method for Graphene for this reason, the method mainly utilizes the shearing action of grinding medium to realize the stripping of graphite layers, there is technique simple, with low cost, prepared Graphene defect is less, but preparation time is longer, the productive rate of prepared Graphene is lower.
Summary of the invention
The object of the inventive method is intended to overcome the deficiencies in the prior art part and provides a kind of ultrasonic assistant sand mill that adopts to peel off the method preparing Graphene.The inventive method adopt relative to ball mill have more intensive grinding energy, higher mill efficiency and material can the sand mill of Continuous maching to prepare Graphene, the ultrasound probe of ultrasonic grinder is put into sand mill hopper simultaneously, while graphite grinding, carry out ultrasonic stripping, realize ultrasonic stripping method and prepare the combination that Graphene and ball milled prepare both Graphenes.Ultrasonic cavitation Graphene being prepared by ultrasonic stripping method combines with both grinding medium shearing actions that ball milled prepares Graphene, peels off graphite and obtain Graphene by the acting in conjunction of both shearing action and ultrasonic cavitation.
Another object of the present invention is to provide a kind ofly assists the stripping Graphene device on sand mill by ultrasonic grinding, this stripping Graphene device improves on existing sand mill, ultrasonic grinding is adopted to substitute mechanical stirring, thus realize carrying out ultrasonic stripping while graphite grinding, realize ultrasonic stripping method and prepare the combination that Graphene and ball milled prepare both Graphenes.
The present invention is that the method preparing Graphene peeled off by a kind of ultrasonic assistant sand mill, and it includes the following step:
Steps A, graphite dispersing solution processed;
Crystalline flake graphite is mixed in raw material mixing system with water phase surfactant mixture, obtained graphite dispersing solution.
Described crystalline flake graphite size is less than 325 orders, and the concentration of crystalline flake graphite is 1 ~ 50mg/ml, and the concentration of water phase surfactant mixture is 0.05 ~ 10mg/ml;
Step B, ultrasonic assistant grinding graphite stripping liquid processed;
The graphite dispersing solution obtained through steps A is added in the loading hopper of sand mill system, graphite dispersing solution can be circulated in the grinding chamber and hopper of sand mill;
After milled processed 3 ~ 30min being carried out to graphite dispersing solution under grinding rotating speed is 1550 ~ 3000r/min condition, the ultrasound probe of ultrasonic grinder system is placed in loading hopper;
Grinding rotating speed be 1550 ~ 3000r/min, ultrasonic power be the condition of 100 ~ 750KW under to circulation graphite dispersing solution carry out process 0.5 ~ 6h after, stop ultrasonication;
After milled processed 3 ~ 30min being carried out to graphite dispersing solution under grinding rotating speed is 1000 ~ 1500r/min condition, the ultrasound probe of ultrasonic grinder is placed in loading hopper;
Grinding rotating speed be 1000 ~ 1500r/min, after ultrasonic power carries out process 0.5 ~ 6h to the graphite dispersing solution of circulation under being the condition of 100 ~ 750KW, obtained graphite stripping liquid;
Step C, centrifugation graphene dispersing solution;
The graphite stripping liquid obtained by step B centrifugation 1 ~ 4h in centrifugal separation system 4 under 1000 ~ 6000r/min condition, gets supernatant liquid, is graphene dispersing solution.
Through the obtained Graphene lateral dimension of the inventive method at 0.4 ~ 1.8 microns, lateral dimension is evenly distributed.
Through the obtained graphene solution concentration of the inventive method 0.7% ~ 1.5%.
The present invention adopts ultrasonic assistant sand mill to peel off the advantage preparing the method for Graphene and is:
1. can realize the production Graphene of industrialization, and productive rate is high, quality is good.
2. applying the inventive method, to prepare Graphene technique simply controlled, with low cost, and prepared Graphene defect is little.
3. the method utilizes the shearing action in sand mill process of lapping, and in conjunction with the ultrasonic cavitation in ultrasonic grinder, preparation is peeled off in the pure physics fragmentation realizing crystalline flake graphite, and technological process is simple, mild condition, and with low cost, be applicable to scale operation.
Accompanying drawing explanation
Fig. 1 is that the present invention adopts ultrasonic assistant sand mill to peel off the system architecture schematic diagram preparing Graphene.
Figure 1A is the combination schematic diagram between the probe of ultrasonic grinder system in the present invention and the loading hopper of sand mill system.
Fig. 2 is the equipment photo of existing laboratory horizontal sand mill.
Fig. 3 is the atomic force microscopy of the Graphene that embodiment 1 adopts the inventive method to obtain.
Fig. 4 is the atomic force microscopy of the Graphene that comparative example 1 obtains.
Fig. 5 is the atomic force microscopy of the Graphene that comparative example 2 obtains.
1. raw material mixing system | 2. ultrasonic grinding system | 21. ultrasonic probes |
3. sand mill system | 31. grinding main frames | 32. loading hoppers |
33.A pipeline | 34.B pipeline | 4. centrifugal separation system |
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Shown in Figure 2, be at least provided with grinding main frame, grinding container, loading hopper, stirrer in the horizontal sand mill system of laboratory.Because stirrer is merely able to play the effect preventing graphite from precipitating in hopper, in order to strengthen the peeling effect of graphite, therefore stirrer is replaced with ultrasonic grinder system, the cavatition that using ultrasound is peeled off in grinding stripping process combines with strong grinding medium shearing force, and the acting in conjunction reaching both shearing action and ultrasonic cavitation obtains low defect, Graphene that productive rate is high to peel off graphite.
In the present invention, the device preparing the stripping Graphene of Graphene peeled off by ultrasonic assistant sand mill, be the loading hopper 32 ultrasonic probe 21 of ultrasonic grinder system 2 being placed in sand mill system 3, and remove the stirrer of sand mill system 3, as shown in Figure 1A.Graphite dispersing solution adds in the loading hopper 32 of sand mill system 3, and under the negative pressure that sand mill system 3 produces, graphite dispersing solution enters into grinding main frame 31 through A pipeline 33, again enters the circulation realizing material in hopper 32 by B pipeline 34.
Shown in Fig. 1, Figure 1A, the present invention adopts the stripping of ultrasonic assistant sand mill to prepare Graphene and includes the following step:
Steps A, graphite dispersing solution processed;
Crystalline flake graphite is mixed in raw material mixing system 1 with water phase surfactant mixture, obtained graphite dispersing solution.
Described crystalline flake graphite size is less than 325 orders, and the concentration of crystalline flake graphite is 1 ~ 50mg/ml.
Described tensio-active agent is the combination of a kind of in Sodium dodecylbenzene sulfonate, Xylo-Mucine, stearoyl aminoethyl trimethylammonium ammonium sulfate, mnyristoyl aminopropyl dimethyl benzyl ammonium chloride, Sodium cholic acid, sodium taurodeoxycholate, polyoxyethylenes (40) nonylplenyl ether and sorbitan monooleate Soxylat A 25-7 or two kinds.The concentration of water phase surfactant mixture is 0.05 ~ 10mg/ml.
Described raw material mixing system 1 can be beaker, glass measure, grinding container, common plastics, glass or container made of iron.
Step B, ultrasonic assistant grinding graphite stripping liquid processed;
The graphite dispersing solution obtained through steps A is added in the loading hopper of sand mill system 3, graphite dispersing solution can be circulated in the grinding chamber and hopper of sand mill;
After milled processed 3 ~ 30min being carried out to graphite dispersing solution under grinding rotating speed is 1550 ~ 3000r/min condition, the ultrasound probe of ultrasonic grinder system 2 is placed in loading hopper;
Grinding rotating speed be 1550 ~ 3000r/min, ultrasonic power be the condition of 100 ~ 750KW under to circulation graphite dispersing solution carry out process 0.5 ~ 6h after, stop ultrasonication;
After milled processed 3 ~ 30min being carried out to graphite dispersing solution under grinding rotating speed is 1000 ~ 1500r/min condition, the ultrasound probe of ultrasonic grinder is placed in loading hopper;
Grinding rotating speed be 1000 ~ 1500r/min, after ultrasonic power carries out process 0.5 ~ 6h to the graphite dispersing solution of circulation under being the condition of 100 ~ 750KW, obtained graphite stripping liquid;
In the present invention, ultrasonic wave can synchronously be carried out with grinding, also can carry out at interval.
Step C, centrifugation graphene dispersing solution;
The graphite stripping liquid obtained by step B centrifugation 1 ~ 4h in centrifugal separation system 4 under 1000 ~ 6000r/min condition, gets supernatant liquid, is graphene dispersing solution.
embodiment 1
The MSG-LNO.3 laboratory horizontal sand mill that sand mill selects Shanghai Ming Shi mechanical & electronic equipment corporation, Ltd to produce.
The Scientz-IID type ultrasonic cell disruptor that ultrasonic grinder selects NingBo XinZhi Biology Science Co., Ltd to produce.
Shown in Fig. 1, Figure 1A, Fig. 2, adopt the stripping of ultrasonic assistant sand mill to prepare Graphene and include the following step:
Steps A, graphite dispersing solution processed;
Crystalline flake graphite is mixed in beaker with water phase surfactant mixture, the graphite dispersing solution of obtained 400mL.
Described crystalline flake graphite mean sizes is 325 orders, and the concentration of crystalline flake graphite is 30mg/ml.
Described tensio-active agent is sodium taurodeoxycholate, and the concentration of its sodium taurodeoxycholate aqueous solution is 3mg/ml.
Step B, ultrasonic assistant grinding graphite stripping liquid processed;
The graphite dispersing solution obtained through steps A is added in the loading hopper of sand mill, graphite dispersing solution can be circulated in the grinding chamber and hopper of sand mill;
After milled processed 10min being carried out to graphite dispersing solution under grinding rotating speed is 2600r/min condition, the ultrasound probe of ultrasonic grinder is placed in loading hopper;
Grinding rotating speed be 2600r/min, ultrasonic power be the condition of 550KW under to circulation graphite dispersing solution carry out process 0.5h after, stopping ultrasonication;
After milled processed 10min being carried out to graphite dispersing solution under grinding rotating speed is 1000r/min condition, the ultrasound probe of ultrasonic grinder is placed in loading hopper;
Grinding rotating speed be 1000r/min, ultrasonic power be the condition of 550KW under to circulation graphite dispersing solution carry out process 0.5h after, obtain graphite stripping liquid;
Step C, centrifugation graphene dispersing solution;
The graphite stripping liquid obtained by step B centrifugation 1h under 4000r/min condition, gets supernatant liquid, is graphene dispersing solution.
The graphene dispersing solution adopting atomic force microscope obtained to embodiment 1 carries out dimensional characteristic analysis.The Graphene lateral dimension that in figure, known embodiment 1 is obtained is at 0.8 ~ 1.2 microns, and lateral dimension is evenly distributed.
embodiment 2
The MSG-LNO.3 laboratory horizontal sand mill that sand mill selects Shanghai Ming Shi mechanical & electronic equipment corporation, Ltd to produce.
The Scientz-IID type ultrasonic cell disruptor that ultrasonic grinder selects NingBo XinZhi Biology Science Co., Ltd to produce.
Shown in Fig. 1, Figure 1A, Fig. 2, adopt the stripping of ultrasonic assistant sand mill to prepare Graphene and include the following step:
Steps A, graphite dispersing solution processed;
Crystalline flake graphite is mixed in glass measure with water phase surfactant mixture, the graphite dispersing solution of obtained 400mL.
Described crystalline flake graphite mean sizes is 1250 orders, and the concentration of crystalline flake graphite is 15mg/ml.
Described tensio-active agent is that sodium taurodeoxycholate and Sodium dodecylbenzene sulfonate are configured by 1:1.The concentration of water phase surfactant mixture is 8mg/ml.
Step B, ultrasonic assistant grinding graphite stripping liquid processed;
The graphite dispersing solution obtained through steps A is added in the loading hopper of sand mill, graphite dispersing solution can be circulated in the grinding chamber and hopper of sand mill;
Grinding rotating speed be 2600r/min, ultrasonic power be the condition of 550KW under to circulation graphite dispersing solution carry out process 2.5h after, obtain graphite stripping liquid;
Step C, centrifugation graphene dispersing solution;
The graphite stripping liquid obtained by step B centrifugation 1h under 4000r/min condition, gets supernatant liquid, is graphene dispersing solution.
The graphene dispersing solution adopting atomic force microscope obtained to embodiment 2 carries out dimensional characteristic analysis, and Graphene lateral dimension is at 0.6 ~ 1.0 microns, and lateral dimension is evenly distributed.
embodiment 3
The MSG-LNO.3 laboratory horizontal sand mill that sand mill selects Shanghai Ming Shi mechanical & electronic equipment corporation, Ltd to produce.
The Scientz-IID type ultrasonic cell disruptor that ultrasonic grinder selects NingBo XinZhi Biology Science Co., Ltd to produce.
Shown in Fig. 1, Figure 1A, Fig. 2, adopt the stripping of ultrasonic assistant sand mill to prepare Graphene and include the following step:
Steps A, graphite dispersing solution processed;
Crystalline flake graphite is mixed in glass measure with water phase surfactant mixture, the graphite dispersing solution of obtained 400mL.
Described crystalline flake graphite mean sizes is 325 orders, and the concentration of crystalline flake graphite is 50mg/ml.
Described tensio-active agent is sodium taurodeoxycholate.The concentration of water phase surfactant mixture is 1.5mg/ml.
Step B, ultrasonic assistant grinding graphite stripping liquid processed;
The graphite dispersing solution obtained through steps A is added in the loading hopper of sand mill, graphite dispersing solution can be circulated in the grinding chamber and hopper of sand mill;
After milled processed 5min being carried out to graphite dispersing solution under grinding rotating speed is 2200r/min condition, the ultrasound probe of ultrasonic grinder is placed in loading hopper;
Grinding rotating speed be 2200r/min, ultrasonic power be the condition of 400KW under to circulation graphite dispersing solution carry out process 1h after, stopping ultrasonication;
After milled processed 5min being carried out to graphite dispersing solution under grinding rotating speed is 1500r/min condition, the ultrasound probe of ultrasonic grinder is placed in loading hopper;
Grinding rotating speed be 1500r/min, ultrasonic power be the condition of 750KW under to circulation graphite dispersing solution carry out process 0.5h after, obtain graphite stripping liquid;
Step C, centrifugation graphene dispersing solution;
The graphite stripping liquid obtained by step B centrifugation 1h under 4000r/min condition, gets supernatant liquid, is graphene dispersing solution.
The graphene dispersing solution adopting atomic force microscope obtained to embodiment 3 carries out dimensional characteristic analysis, and Graphene lateral dimension is at 1.0 ~ 1.2 microns, and lateral dimension is evenly distributed.
simple sand mill obtains the comparison example 1 of Graphene
The MSG-LNO.3 laboratory horizontal sand mill that sand mill selects Shanghai Ming Shi mechanical & electronic equipment corporation, Ltd to produce.
By the step that Graphene prepared by sand mill be only:
Steps A, graphite dispersing solution processed;
Crystalline flake graphite is mixed in beaker with water phase surfactant mixture, the graphite dispersing solution of obtained 400mL.
Described crystalline flake graphite mean sizes is 325 orders, and the concentration of crystalline flake graphite is 30mg/ml.
Described tensio-active agent is sodium taurodeoxycholate.The concentration of water phase surfactant mixture is 3mg/ml.
Step B, grinds graphite stripping liquid processed;
The graphite dispersing solution obtained through steps A is added in the loading hopper of sand mill, graphite dispersing solution can be circulated in the grinding chamber and hopper of sand mill; After milled processed 1h being carried out to graphite dispersing solution under grinding rotating speed is 2600r/min condition, obtained graphite stripping liquid;
Step C, centrifugation graphene dispersing solution;
The graphite stripping liquid obtained by step B centrifugation 1h under 4000r/min condition, gets supernatant liquid, is graphene dispersing solution.
The Graphene clear liquid adopting atomic force microscope obtained to comparison example 1 carries out dimensional characteristic analysis, in figure the lateral dimension of known Graphene large at 2 ~ 6 microns, there is a small amount of lateral dimension at the Graphene of 0.2 ~ 1 micron, there is the Graphene of two kinds of lateral dimension distributions.
simple ultrasonic grinder obtains the comparison example 2 of Graphene
The Scientz-IID type ultrasonic cell disruptor that ultrasonic grinder selects NingBo XinZhi Biology Science Co., Ltd to produce.
By the step that ultrasonic grinder prepares Graphene be only:
Steps A, graphite dispersing solution processed;
Crystalline flake graphite is mixed in beaker with water phase surfactant mixture, the graphite dispersing solution of obtained 400mL.
Described crystalline flake graphite mean sizes is 325 orders, and the concentration of crystalline flake graphite is 30mg/ml.
Described tensio-active agent is sodium taurodeoxycholate.The concentration of water phase surfactant mixture is 3mg/ml.
Step B, grinds graphite stripping liquid processed;
Adding in the loading hopper of ultrasonic grinder by the graphite dispersing solution obtained through steps A, is after carrying out ultrasonic separation process 1h to graphite dispersing solution under the condition of 550KW at ultrasonic power, obtained graphite stripping liquid;
Step C, centrifugation graphene dispersing solution;
The graphite stripping liquid obtained by step B centrifugation 1h under 4000r/min condition, gets supernatant liquid, is graphene dispersing solution.
The Graphene clear liquid adopting atomic force microscope obtained to comparison example 2 carries out dimensional characteristic analysis, in figure the lateral dimension of known Graphene large at 1 ~ 3 micron, have half lateral dimension at the Graphene of 0.2 ~ 1 micron.
Graphene dispersing solution concentrations versus shows:
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 that the method preparing Graphene peeled off by a kind of ultrasonic assistant sand mill that adopts, to be solved is the technical problem how improving the quality of preparing graphite alkene in process of lapping, ultrasonic cavitation combines with grinding medium shearing action by the method, and the technique means that graphite obtains Graphene is peeled off in acting in conjunction.The method utilizes the shearing action in sand mill process of lapping, in conjunction with the ultrasonic cavitation in ultrasonic grinder, preparation is peeled off in the pure physics fragmentation realizing crystalline flake graphite, and technological process is simple, mild condition, and with low cost, be applicable to large-scale industrialization produce.
Claims (7)
1. the method preparing Graphene peeled off by ultrasonic assistant sand mill, it is characterized in that including the following step:
Steps A, graphite dispersing solution processed;
Crystalline flake graphite is mixed in raw material mixing system with water phase surfactant mixture, obtained graphite dispersing solution.
Described crystalline flake graphite size is less than 325 orders, and the concentration of crystalline flake graphite is 1 ~ 50mg/ml, and the concentration of water phase surfactant mixture is 0.05 ~ 10mg/ml;
Step B, ultrasonic assistant grinding graphite stripping liquid processed;
The graphite dispersing solution obtained through steps A is added in the loading hopper of sand mill system, graphite dispersing solution can be circulated in the grinding chamber and hopper of sand mill;
After milled processed 3 ~ 30min being carried out to graphite dispersing solution under grinding rotating speed is 1550 ~ 3000r/min condition, the ultrasound probe of ultrasonic grinder system is placed in loading hopper;
Grinding rotating speed be 1550 ~ 3000r/min, ultrasonic power be the condition of 100 ~ 750KW under to circulation graphite dispersing solution carry out process 0.5 ~ 6h after, stop ultrasonication;
After milled processed 3 ~ 30min being carried out to graphite dispersing solution under grinding rotating speed is 1000 ~ 1500r/min condition, the ultrasound probe of ultrasonic grinder is placed in loading hopper;
Grinding rotating speed be 1000 ~ 1500r/min, after ultrasonic power carries out process 0.5 ~ 6h to the graphite dispersing solution of circulation under being the condition of 100 ~ 750KW, obtained graphite stripping liquid;
Step C, centrifugation graphene dispersing solution;
The graphite stripping liquid obtained by step B centrifugation 1 ~ 4h in centrifugal separation system 4 under 1000 ~ 6000r/min condition, gets supernatant liquid, is graphene dispersing solution.
2. the method preparing Graphene peeled off by a kind of ultrasonic assistant sand mill according to claim 1, it is characterized in that: described tensio-active agent is the combination of a kind of in Sodium dodecylbenzene sulfonate, Xylo-Mucine, stearoyl aminoethyl trimethylammonium ammonium sulfate, mnyristoyl aminopropyl dimethyl benzyl ammonium chloride, Sodium cholic acid, sodium taurodeoxycholate, polyoxyethylenes (40) nonylplenyl ether and sorbitan monooleate Soxylat A 25-7 or three kinds.
3. the method preparing Graphene peeled off by a kind of ultrasonic assistant sand mill according to claim 1, it is characterized in that: sand mill system selects horizontal sand mill.
4. the method preparing Graphene peeled off by a kind of ultrasonic assistant sand mill according to claim 1, it is characterized in that: ultrasonic grinder selects ultrasonic cell disruptor.
5. the method preparing Graphene peeled off by a kind of ultrasonic assistant sand mill according to claim 1, it is characterized in that: obtained Graphene lateral dimension is at 0.4 ~ 1.8 microns, and lateral dimension is evenly distributed.
6. the method preparing Graphene peeled off by a kind of ultrasonic assistant sand mill according to claim 1, it is characterized in that: obtained graphene solution concentration is 0.7% ~ 1.5%.
7. peel off a Graphene device processed, include raw material mixing system (1), ultrasonic grinding system (2), sand mill system (3) and centrifugal separation system (4); It is characterized in that: the probe (21) of ultrasonic grinder system (2) is placed in the loading hopper (32) of sand mill system (3); The ultrasonic power that ultrasonic grinder system (2) is arranged is 100 ~ 750KW; The grinding rotating speed that sand mill system (3) is arranged is 1000 ~ 3000r/min.
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