CN107311151A - The method of purification of CNT - Google Patents
The method of purification of CNT Download PDFInfo
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- CN107311151A CN107311151A CN201710536664.3A CN201710536664A CN107311151A CN 107311151 A CN107311151 A CN 107311151A CN 201710536664 A CN201710536664 A CN 201710536664A CN 107311151 A CN107311151 A CN 107311151A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/30—Purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention provides a kind of method of purification of CNT, comprise the following steps：CNT is placed in electromagnetic wave device, it is passed through inert gas, it is that 100 2000T, electromagnetic frequency are the 60min of electromagnetic action 15 under conditions of 50 1500Hz in magnetic field intensity, metal impurities physics from the CNT is come off, obtain pre-treatment CNT；The pre-treatment CNT is subjected to centrifuge washing, CNT after purification is obtained.
Description
Technical field
The invention belongs to carbon nanotube technology field, more particularly to a kind of method of purification of CNT.
Background technology
CNT have the specific surface area of super large, lighter quality, superpower mechanical strength, excellent electric conductivity, compared with
Good physics and chemical stability, are a kind of new materials received much concern, are with a wide range of applications in multiple fields.Mesh
Preceding CNT can be prepared by chemical vapor deposition (CVD) method.However, during CVD method prepares CNT,
Need to use metallic catalyst.After preparation terminates, metallic catalyst is easily remained, and is entered with CNT in product.This is tight
CNT is hindered again in some applications to metal impurities requirement higher row industry, and such as in lithium ion battery, (kish is urged
The CNT of agent is applied in lithium ion battery, and the metallic catalyst of residual can enter in electrolyte, cause battery short circuit
Deng), delicate electronic device, field of aerospace application, particularly can not meet boat material Material Field requirement.
In order to reduce the influence of kish catalyst, it will usually which CNT is purified.Existing CNT
Purification mode mainly has two kinds：One kind is pickling method of purification, is mainly catalyzed kish using the strong acid with oxidisability
Agent dissolving oxidation, is then separated by filtration.Although this method can purify CNT to a certain extent, however, it is very difficult to completely
Remove carbon-coating and coat thicker metallic catalyst, while this method complex process, can produce substantial amounts of spent acid and waste water, cause
Environmental pollution, and be possible to introduce new oxidized metal compound impurities.Another method is high-temperature heat treatment method of purification, is adopted
CNT is heat-treated with the temperature higher than 2800 DEG C, kish catalyst is gasified, so as to reach that purification carbon is received
The purpose of mitron.Although the CNT purity that this method is obtained is very high, energy consumption is also very high, while too high heat treatment temperature
Degree can cause the carbon atom in CNT to be reset, and cause some not expected change of properties.
The content of the invention
It is an object of the invention to provide a kind of method of purification of CNT, it is intended to solves existing purification CNT
Pickling purification procedures are complicated, and are difficult to effectively remove metallic catalyst impurity；And high-temperature heat treatment method of purification heat treatment temperature
It is too high, cause the problem of carbon atom in CNT is reset.
The present invention is achieved in that a kind of method of purification of CNT, comprises the following steps：
CNT is placed in electromagnetic wave device, inert gas is passed through, is 100-1500T, electromagnetism frequency in magnetic field intensity
Rate is electromagnetic action 15-60min under conditions of 50-1500Hz, metal impurities physics from the CNT is come off, and is obtained
Pre-treatment CNT；
The pre-treatment CNT is subjected to centrifuge washing, CNT after purification is obtained.
The method of purification for the CNT that the present invention is provided, using the effect of magnetic field and electric field, by pending carbon nanometer
Remaining organo-metallic catalyst is removed in pipe, can each position of thorough cleaning CNT metal impurities, with excellent
Different purification effect.CNT after being purified through the inventive method, purity can meet aeronautical material carbon more than 99.99%
The high request of nano-tube material.
Brief description of the drawings
Fig. 1 is the structural representation of electromagnetic wave device provided in an embodiment of the present invention；
Fig. 2 is the electron-microscope scanning figure of the carbon nanotube-sample before purification provided in an embodiment of the present invention；
Fig. 3 is the electron-microscope scanning figure of the carbon nanotube-sample after purification provided in an embodiment of the present invention；
Fig. 4 is the thermogravimetric analysis figure of the carbon nanotube-sample after the purification that the embodiment of the present invention 8 is provided.
Embodiment
In order that technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only to explain
The present invention, is not intended to limit the present invention.
The embodiments of the invention provide a kind of method of purification of CNT, comprise the following steps：
S01. CNT is placed in electromagnetic wave device, is passed through inert gas, be 100-2000T, electricity in magnetic field intensity
Magnet rate is electromagnetic action 15-60min under conditions of 50-1500Hz, metal impurities physics from the CNT is come off,
Obtain pre-treatment CNT；
S02. the pre-treatment CNT is subjected to centrifuge washing, obtains CNT after purification.
Specifically, in above-mentioned steps S01, CNT is placed in electromagnetic wave device, inert gas is passed through, electromagnetism is prevented
In mechanism, the CNT chemically reacts, it is to avoid introduce new impurity.It is 100-2000T, electromagnetism in magnetic field intensity
Frequency is remaining under conditions of 100-1000Hz, the CNT and metal impurities are larger to electro-magnetic wave absorption capacity variance
Metallic catalyst impurity in the CNT can be offset along the direction of vibration of electromagnetic wave, be filled with the CNT
Separation.In addition, specific electromagnetic wave condition causes the CNT to be straightened, i.e., described CNT is arranged in array
Mode (orientation), in favor of making metal impurities Automatic-falling in the presence of electromagnetic wave.In this special case, even if being wound around
Metal impurities inside the CNT, can also be sufficiently removed, so as to effectively improve the purifying rate of the CNT.
The embodiment of the present invention will be remained in the CNT by setting specific electromagnetic parameter by physical method
Metallic catalyst impurity carries out physical removal, so as to fundamentally ensure carbon nanotube mass (such as carbon nano tube structure) not by shadow
Ring and do not introduce new impurity.
As a kind of preferred situation, while the electromagnetic action, and/or after the electromagnetic action, to the carbon
Nanotube applies centrifugal force.Specific preferred, while the electromagnetic action, the rotating speed for adjusting the electromagnetic wave device is
100-1000r/min, the centrifugal force for forming suitable size takes away the metal impurities on the CNT of pre-treatment, so as to more have
Come off beneficial to the metal impurities being clipped in the CNT from CNT, and then high-purity carbon is obtained by follow-up centrifugal treating
Nanotube.
As another preferred situation, while the electromagnetic action, the windstream that speed is 0.5-5m/s is passed through
The CNT is rinsed, the windstream is inert gas.In the embodiment of the present invention, because the CNT is by electricity
Meeting array arrangement, is passed through after windstream after magnetic wave effect, because metal impurities and CNT have density variation, suitable speed
The windstream of degree can be screened metal impurities with CNT.
On the basis of above-described embodiment, the present invention can utilize the magnetic field difference of CNT and metal impurities, pass through
The magnetic field intensity is adjusted to obtain preferable purification effect.
As a specific embodiment, a kind of method of purification of CNT comprises the following steps：
CNT is placed in electromagnetic wave device, inert gas is passed through, in the condition that magnetic field intensity is 1200-1300T
Lower electromagnetic action 15-60min, obtains pre-treatment CNT；
The pre-treatment CNT is subjected to centrifuge washing, CNT after purification is obtained.
In above-described embodiment, by finely screening, the purifying of CNT disposably can be efficiently realized, and obtain carbon nanometer
Pipe purity reaches more than 99.5% purification effect.
As another specific embodiment, a kind of method of purification of CNT comprises the following steps：
CNT is placed in electromagnetic wave device, inert gas is passed through, is in magnetic field intensity by the CNT
Acted under conditions of 1000-1200T after 10-30min, 10-30min acted under conditions of magnetic field intensity is 1200-1300T,
Obtain pre-treatment CNT；
The pre-treatment CNT is subjected to centrifuge washing, CNT after purification is obtained.
In above-described embodiment, by the purifying flow for fine screening-finely screen, the high-quality purifying of CNT can be achieved,
And obtain the purification effect that carbon nano pipe purity reaches more than 99.7%.
As another specific embodiment, a kind of method of purification of CNT comprises the following steps：
CNT is placed in electromagnetic wave device, inert gas is passed through, is in magnetic field intensity by the CNT
Acted under conditions of 800-1000T after 10-30min；10-30min is acted under conditions of magnetic field intensity is 1200-1300T, is obtained
Obtain pre-treatment CNT；
The pre-treatment CNT is subjected to centrifuge washing, CNT after purification is obtained.
In above-described embodiment, by the purifying flow for coarse sizing-finely screen, the high-quality purifying of CNT can be achieved,
And obtain the purification effect that carbon nano pipe purity reaches more than 99.6%.
As optimal specific embodiment, a kind of method of purification of CNT comprises the following steps：
CNT is placed in electromagnetic wave device, inert gas is passed through, is in magnetic field intensity by the CNT
5-20min is acted under conditions of 800-1000T；Then 5-20min is acted under conditions of magnetic field intensity is 1000-1200T；Most
5-20min is acted under conditions of magnetic field intensity is 1200-1300T afterwards, pre-treatment CNT is obtained；
The pre-treatment CNT is subjected to centrifuge washing, CNT after purification is obtained.
In above-described embodiment, the excellent of CNT can be achieved in the purifying flow that-fine screening-is finely screened by coarse sizing
Matter is purified, and obtains the purification effect that carbon nano pipe purity reaches more than 99.99%.
Of course it is to be understood that the embodiment of the present invention can also realize CNT separately through coarse sizing and/or fine screening
Purifying, simply purification effect is slightly worse compared with the effect of above preferred embodiment.
In above-described embodiment, the CNT can be carbon nanotube dust, or carbon nano-tube solution, preferably
For carbon nano-tube solution.When the CNT can be carbon nano-tube solution, the carbon nano-tube solution is being subjected to electromagnetism
, can be further beneficial to CNT point before effect, in addition to by carbon nano-tube solution progress ultrasonic disperse 10-30min
Dissipate in order and uniform, so that beneficial to the separation of CNT and metal impurities.It is further preferred that the carbon nano-tube solution
Mass percentage concentration is 10-40%, so as under the specific magnetic field intensity of the embodiment of the present invention, be conducive to metal impurities to be received from carbon
Fully come off in mitron.
In the embodiment of the present invention, it is illustrated in fig. 1 shown below, the electromagnetic wave device includes being provided with purifying cavity, and described pure
Change charging aperture, tail gas mouthful, discharging opening and vacuum port that cavity is communicated, wherein, the purifying cavity includes being provided with magnet coil
Roller and both ends of the surface for sealing roller, and the charging aperture and tail gas mouth are separately positioned on both ends of the surface, it is described go out
Material mouth is arranged on the roller and one end away from the charging aperture.
Specifically, the CNT enters from the charging aperture, electromagnetic field space, chain of command are produced using AC coil
Plate can control the open and close in magnetic field, the open and close of control valve, the open and close of discharging opening, the size of alternating current.By institute
State CNT to be passed through from the charging aperture, adjust alternating current, when producing the magnetic field of suitable size, metal impurities are received from the carbon
Come off in mitron.Magnetic field is closed, passes through the CNT of discharging opening collection after purification.Wherein, the vacuum port can be used for taking out true
It is empty, be passed through inert gas；The tail gas mouthful can be used for the discharge for being passed through gas (such as orientation gas).
In the embodiment of the present invention, the end end of the CNT can be made by adjusting the temperature of the CNT
Cap is aoxidized, and forms tubular conduit.In the presence of electromagnetic wave, be conducive to the metal impurities inside CNT more preferable from terminal part
Come off, so as to improve purification effect.
As specific embodiment, with reference to Fig. 1, the CNT is entered by charging aperture, and electromagnetism is produced using AC coil
Field space, control panel can adjust alternating current size.It is that 100-2000T, electromagnetic frequency are 50-1500Hz's in magnetic field intensity
Under the conditions of, adjust magnetic field intensity and make to rise to 300-500 DEG C in the purifying cavity.At such a temperature, oxidizing gas is passed through,
The terminal part of the CNT closing is oxidized to form the tubular passageway of end opening, in the presence of electromagnetic wave, the carbon
Metal impurities inside nanotube preferably can preferably come off from terminal part.In the embodiment of the present invention, the purifying cavity
Interior temperature is unsuitable too high or too low to realize that CNT is adjusted for the purpose of terminal oxidized., can not if temperature is too low
By CNT close it is terminal oxidized fall, be unfavorable for the metal impurities inside CNT and come off from the end, hinder carbon receive
The removal of mitron interior metal impurity；If temperature is too high, the oxidation at other positions can be caused, the structure of CNT is influenceed.
In the embodiment, the CNT is carbon nanotube dust.The embodiment of the present invention is under given conditions by oxide/carbon nanometer tube
Terminal end cap oxidation, it is not necessary to introduce catalyst, the introducing of new impurity can be avoided, and under specific magnetic field intensity, can
To realize excellent purification effect on the premise of carbon nanotube mass is ensured.
In above-mentioned steps S02, because metal impurities have come off in step S01 inside the CNT, or
By the outer surface of vibration to CNT, therefore, by centrifuge washing, CNT after purification can be obtained.Specifically
, it is possible to use the method for centrifugation removes and the metal impurities after carbon nanotube separation or utilizes centrifugal filtration
Mode remove metal impurities.
Specifically, the collection of purified nanotubes can be realized by way of centrifugal filtration or centrifugation.
The method of purification of CNT provided in an embodiment of the present invention, will be pending using the effect of magnetic field and electric field
Remaining organo-metallic catalyst is removed in CNT, can each position of thorough cleaning CNT metal impurities,
With excellent purification effect.CNT after being purified through the inventive method, purity can meet aviation more than 99.99%
The high request of material carbon nanotube material.
Illustrated with reference to specific embodiment.
Embodiment 1
S11. CNT is placed in electromagnetic wave device, is passed through inert gas, under conditions of magnetic field intensity is 1200T
Electromagnetic action 50min, obtains pre-treatment CNT；
S12. the pre-treatment CNT is subjected to centrifuge washing, obtains CNT after purification.
By thermogravimetric analysis, the purity of CNT described in the embodiment of the present invention 1 is 99.56%.
Embodiment 2
S21. CNT is placed in electromagnetic wave device, is passed through inert gas, under conditions of magnetic field intensity is 1250T
Electromagnetic action, meanwhile, the CNT is rinsed by windstream with 2m/s speed, 30min is handled, pre-treatment carbon is obtained
Nanotube；
S22. the pre-treatment CNT is subjected to centrifuge washing, obtains CNT after purification.
By thermogravimetric analysis, the purity of CNT described in the embodiment of the present invention 2 is 99.63%.
Embodiment 3
S31. CNT is placed in electromagnetic wave device, is passed through inert gas, by the CNT in magnetic field intensity
To be acted under conditions of 1100T after 20min, 15min is acted under conditions of magnetic field intensity is 1250T, pre-treatment carbon is obtained and receives
Mitron；
S32. the pre-treatment CNT is subjected to centrifuge washing, obtains CNT after purification.
By thermogravimetric analysis, the purity of CNT described in the embodiment of the present invention 3 is 99.82%.
Embodiment 4
S41. CNT is placed in electromagnetic wave device, is passed through inert gas, by the CNT in magnetic field intensity
To be acted under conditions of 900T after 15min；30min is acted under conditions of magnetic field intensity is 1200T, pre-treatment carbon nanometer is obtained
Pipe；
S42. the pre-treatment CNT is subjected to centrifuge washing, obtains CNT after purification.
By thermogravimetric analysis, the purity of CNT described in the embodiment of the present invention 4 is 99.75%.
Embodiment 5
S51. CNT is placed in electromagnetic wave device, is passed through inert gas, by the CNT in magnetic field intensity
To be acted under conditions of 1000T after 15min；30min is acted under conditions of magnetic field intensity is 1200T；While electromagnetic action,
The CNT is rinsed by windstream with 3m/s speed, pre-treatment CNT is obtained；
S52. the pre-treatment CNT is subjected to centrifuge washing, obtains CNT after purification.
By thermogravimetric analysis, the purity of CNT described in the embodiment of the present invention 5 is 99.81%.
Embodiment 6
S61. CNT is placed in electromagnetic wave device, is passed through inert gas, by the CNT in magnetic field intensity
To act on 20min under conditions of 850T；Then 10min is acted under conditions of magnetic field intensity is 1150T；Finally in magnetic field intensity
To act on 15min under conditions of 1250T, pre-treatment CNT is obtained；
S62. the pre-treatment CNT is subjected to centrifuge washing, obtains CNT after purification.
By thermogravimetric analysis, the purity of CNT described in the embodiment of the present invention 6 is 99.99%.
Embodiment 7
S71. CNT is placed in electromagnetic wave device, is passed through inert gas, by the CNT in magnetic field intensity
To act on 20min under conditions of 850T；Then 10min is acted under conditions of magnetic field intensity is 1150T；Finally in magnetic field intensity
To act on 15min under conditions of 1250T, while electromagnetic action, the carbon is rinsed by windstream with 4m/s speed and received
Mitron, obtains pre-treatment CNT；
S72. the pre-treatment CNT is subjected to centrifuge washing, obtains CNT after purification.
By thermogravimetric analysis, the purity of CNT described in the embodiment of the present invention 7 is 99.995%.
Embodiment 8
S81. CNT is placed in electromagnetic wave device, is passed through inert gas, by the CNT by the charging
Mouthful enter, be that regulation magnetic field intensity makes described pure under conditions of 100-2000T, electromagnetic frequency are 50-1500Hz in magnetic field intensity
Change in cavity and rise to 300-500 DEG C, by the CNT of discharging opening collection after purification, obtain pre-treatment CNT；
S82. the pre-treatment CNT is subjected to centrifuge washing, obtains CNT after purification.
In the embodiment of the present invention there is provided undressed CNT electron-microscope scanning figure as shown in Fig. 2 from figure on can
To find out, carbon nano tube surface is distributed more metal impurities.After present invention method purification processes, CNT sample
The electron-microscope scanning figure of product is not as shown in figure 3, observed the presence of metal impurities.The purifying that the embodiment of the present invention 8 is obtained
CNT carries out thermogravimetric analysis (TG), as a result as shown in figure 4, as seen from the figure, after about 750 DEG C, only residue 0.002% is residual
Stay, that is, almost exist in the CNT after purifying without impurity, the purity of CNT is described in the embodiment of the present invention
99.998%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (10)
1. a kind of method of purification of CNT, it is characterised in that comprise the following steps：
CNT is placed in electromagnetic wave device, inert gas is passed through, is that 100-2000T, electromagnetic frequency are in magnetic field intensity
Electromagnetic action 15-60min under conditions of 50-1500Hz, makes metal impurities physics from the CNT come off, and locates before obtaining
Manage CNT；
The pre-treatment CNT is subjected to centrifuge washing, CNT after purification is obtained.
2. the method for purification of CNT as claimed in claim 1, it is characterised in that while the electromagnetic action and/
Or after the electromagnetic action, the rotating speed for adjusting the electromagnetic wave device is 100-1000r/min.
3. the method for purification of CNT as claimed in claim 1, it is characterised in that while the electromagnetic action, leads to
Enter the windstream that speed is 0.5-5m/s and rinse the CNT, the windstream is inert gas.
4. the method for purification of CNT as claimed in claim 1, it is characterised in that the magnetic field intensity is 1200-
1300T。
5. the method for purification of CNT as claimed in claim 1, it is characterised in that by the CNT in magnetic field intensity
To be acted under conditions of 1000-1200T after 10-30min, 10- is acted under conditions of magnetic field intensity is 1200-1300T
30min。
6. the method for purification of CNT as claimed in claim 1, it is characterised in that by the CNT in magnetic field intensity
To be acted under conditions of 800-1000T after 10-30min；10-30min is acted under conditions of magnetic field intensity is 1200-1300T.
7. the method for purification of CNT as claimed in claim 1, it is characterised in that by the CNT in magnetic field intensity
To act on 5-20min under conditions of 800-1000T；Then 5-20min is acted under conditions of magnetic field intensity is 1000-1200T；
It is last to act on 5-20min under conditions of magnetic field intensity is 1200-1300T.
8. the method for purification of the CNT as described in claim 1-7 is any, it is characterised in that the electromagnetic wave device includes
Purifying cavity is provided with, charging aperture, tail gas mouthful, discharging opening and the vacuum port communicated with the purifying cavity, wherein, the purifying
Cavity includes being provided with the roller of magnet coil and the both ends of the surface for sealing roller, and the charging aperture and the tail gas mouthful point
Both ends of the surface are not arranged on, and the discharging opening is arranged on the roller and one end away from the charging aperture；
The CNT is entered by the charging aperture, is that 100-2000T, electromagnetic frequency are 50-1500Hz in magnetic field intensity
Under conditions of, regulation magnetic field intensity makes to rise to 300-500 DEG C in the purifying cavity, and the carbon collected after purification by discharging opening is received
Mitron.
9. the method for purification of the CNT as described in claim 1-7 is any, it is characterised in that the CNT is received for carbon
Mitron solution, and carried out before the carbon nano-tube solution is carried out into electromagnetic action, in addition to by the carbon nano-tube solution
Ultrasonic disperse 10-30min.
10. the method for purification of CNT as claimed in claim 8, it is characterised in that the CNT is CNT
Powder.
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| CN101254895A (en) * | 2007-07-02 | 2008-09-03 | 兰州理工大学 | Orientation arrangement method for carbon-nano tube and preparation device |
| CN102320592A (en) * | 2011-08-26 | 2012-01-18 | 复旦大学 | Method for separating carbon nanotubes with different conductive performances |
| US8216542B2 (en) * | 2005-08-10 | 2012-07-10 | Korea Institute Of Machinery And Materials | Method for separating nanotubes using microwave radiation |
| CN103030133A (en) * | 2012-12-30 | 2013-04-10 | 深圳市纳米港有限公司 | Carbon nanotube paper and making method thereof |
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2017
- 2017-07-04 CN CN201710536664.3A patent/CN107311151B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8216542B2 (en) * | 2005-08-10 | 2012-07-10 | Korea Institute Of Machinery And Materials | Method for separating nanotubes using microwave radiation |
| CN101254895A (en) * | 2007-07-02 | 2008-09-03 | 兰州理工大学 | Orientation arrangement method for carbon-nano tube and preparation device |
| CN102320592A (en) * | 2011-08-26 | 2012-01-18 | 复旦大学 | Method for separating carbon nanotubes with different conductive performances |
| CN103030133A (en) * | 2012-12-30 | 2013-04-10 | 深圳市纳米港有限公司 | Carbon nanotube paper and making method thereof |
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Effective date of registration: 20210518 Address after: 655000 No.1 Xishan Road, Qujing Development Zone, Yunnan Province Patentee after: Qujing FeiMo Technology Co.,Ltd. Address before: 223-224, kanghesheng building, No.1 ChuangSheng Road, Nanshan District, Shenzhen, Guangdong 518000 Patentee before: SHENZHEN DYNANONIC Co.,Ltd. |