CN107381552A - A kind of quick apparatus and method for preparing graphene - Google Patents
A kind of quick apparatus and method for preparing graphene Download PDFInfo
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- CN107381552A CN107381552A CN201710791479.9A CN201710791479A CN107381552A CN 107381552 A CN107381552 A CN 107381552A CN 201710791479 A CN201710791479 A CN 201710791479A CN 107381552 A CN107381552 A CN 107381552A
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Abstract
The invention discloses a kind of quick apparatus and method for preparing graphene, the quick device for preparing graphene includes retort, the top of retort is provided with feed pipe and gas outlet, gas outlet is communicated with waste heat box by flue gas leading, the bottom of retort fixes connection and is provided with discharge nozzle, the top inner wall of retort is fixed with circular slide rail, circular slide rail is connected with electric rotating machine by connecting rod, the output shaft of electric rotating machine is connected with the first electric pushrod by shaft coupling, and the lever arm of the first electric pushrod is provided with multiple stirring sheets.The present invention proposes a kind of quick apparatus and method for preparing graphene, its structure design advantages of simple, it is easy to operate,, raising reaction rate, more effectively to retort progress constant temperature, insulation or heating uniform to the sufficient mix of material progress in retort can be realized, preferably control temperature change, the movement of device is facilitated, the burden of staff is alleviated, meets the needs of people.
Description
Technical field
The present invention relates to technical field of graphene preparation, more particularly to a kind of quick apparatus and method for preparing graphene.
Background technology
Graphene be one kind by carbon atom with SP2The cellular flat film that hybrid form is formed, it is a kind of only one
The quasi- two-dimensional material of atomic layer level thickness, monoatomic layer graphite is done so being called, the method for the common power production of graphene is machine
Tool stripping method, oxidation-reduction method, SIC epitaxial growth methods, film production method are chemical vapour deposition technique, because it is very good
Intensity well, flexible, conductive, heat conduction, optical characteristics, led in physics, materialogy, electronic information, computer, Aero-Space etc.
Domain is obtained for significant progress.
A kind of novel nano-material most strong as the most thin, maximum intensity, electrical and thermal conductivity that have now been found that, graphene quilt
Referred to as " dark fund ", it is " king of new material " that scientist even foretells that graphene " will thoroughly change 21 century ".Very likely start
One subversiveness new technology new industrial revolution have swept the globe.
Graphene is made by micromechanics stripping method first, and micromechanics stripping method is by highly oriented pyrolytic graphite with adhesive tape
Piece is pressed on other surfaces and repeatedly peeled off, and finally gives individual layer or several layers of graphene, micromechanics stripping method operation letter
Single, makes sample quality height, but obtained graphene size is smaller and very big uncertainty be present, while efficiency is low, cost
Height, be not suitable for large-scale production.
Chemical vapor infiltration is metal base Cu, Ni that hydrocarbon methane, ethanol etc. are passed into high-temperature heating
Surface, react certain time after cooled down, will form several layers or mono-layer graphite in substrate surface in cooling procedure
Alkene, growth two parts are dissolved and spread in substrate comprising carbon atom during this.
Oxidation-reduction method is also considered as preparing one of best approach of graphene at present, and this method is simple to operate, prepares
Cost is low, can prepare graphene on a large scale, but the graphene quality that this method is prepared is not relatively high.
Existing oxidation-reduction method, which prepares graphene, very big requirement to stirring and temperature control, and stirring and temperature are very
The influence of big degree prepares the speed of graphene, and prior art stirs not uniform enough during graphene is prepared, temperature
Can not well control, influence to prepare the throughput rate of graphene, the existing device movement inconvenience for preparing graphene, it is necessary to
Very big trouble is brought to staff when mobile.
The content of the invention
The invention aims to solve shortcoming present in prior art, and the one kind proposed quickly prepares graphene
Apparatus and method.
To achieve these goals, present invention employs following technical scheme：
A kind of quick device for preparing graphene, including retort, the surrounded surface of the retort, which is fixed with, to be added
Thermosphere, the outer surface of the zone of heating are provided with constant temperature import and constant temperature outlet, the constant temperature import and constant temperature outlet and zone of heating
Connection, the constant temperature import, which is fixed, is communicated with the first constant warm tube, and the one end of first constant warm tube away from constant temperature import, which is fixed, to be connected
Thermostat is connected with, the one end of the thermostat away from the first constant warm tube, which is fixed, is communicated with the second constant warm tube, second constant warm tube
One end away from thermostat connects with constant temperature outlet, and the top of the retort is provided with feed pipe, and the feed pipe is away from reaction
One end of tank is fixed and is communicated with loading hopper, and the surface of the feed pipe is provided with the first valve, and the top of the retort is fixed
Provided with gas outlet, the one end of the gas outlet away from retort is communicated with flue gas leading, the one end of the flue gas leading away from gas outlet
Fixed to be communicated with waste heat box, the bottom of the retort fixes connection and is provided with discharge nozzle, and the surface of the discharge nozzle is provided with second
Valve.
The top inner wall of the retort is fixed with circular slide rail, and vertically fixation is connected with connection to the circular slide rail
Bar, the one end of the connecting rod away from circular slide rail are vertically fixedly connected with electric rotating machine, and the output shaft of the electric rotating machine leads to
Cross shaft coupling and be connected with the first electric pushrod, multiple stirring sheets are uniformly provided with the lever arm of first electric pushrod.
Preferably, support tube is fixed with the corner of the reaction pot bottom, the bottom of the retort is vertically solid
Fixed to be provided with the second electric pushrod corresponding with support tube, the described one end of second electric pushrod away from retort is fixed with universal
Wheel.
Preferably, the bottom of the retort is fixed with heating rod.
Preferably, the top of the retort is provided with observation window.
Preferably, the side wall of the zone of heating is fixed with controller, and the controller is 80C51 programmable single chip computers,
The output end of the controller respectively with the circular slide rail, electric rotating machine, the first electric pushrod, the second electric pushrod and heating
The input of rod is electrically connected with.
Preferably, the circular slide rail, electric rotating machine, the first electric pushrod, the second electric pushrod, heating rod and controller
It is electrically connected with respectively with external power source.
Preferably, the one end of the support tube away from retort is provided with the anti-skid wearable pad of a circle.
Preferably, the side wall of the zone of heating is fixed with temperature indicator, and the output end of the temperature indicator is with adding
Thermosphere sealing connection.
Preferably, the thermostatic medium in the thermostat is vapor or oil.
Preferably, a kind of quick method for preparing graphene, comprises the following steps：
S1, in retort, a large amount of 98% concentrated sulfuric acids are put into, add graphite block or graphite flake, stirring, heating, control
Temperature reacts 3-6h, obtains graphite oxide at 40-80 DEG C；
S2, by graphite oxide and its reaction solution, 1-5h is handled by ultrasonic machine, obtains graphene oxide solution；
S3, graphene oxide solution is neutralized slightly with ammoniacal liquor, it is 4-6 to control pH, strong reductant is added, by graphite oxide
Alkene reduces, and obtains finished product graphene.
Preferably, in the S3, strong reductant is specially one kind in hydrazine hydrate, sodium borohydride.
Compared with prior art, the beneficial effects of the invention are as follows：
1. the circular slide rail being fixed with by the inwall at the top of retort, circular slide rail is driven by connecting rod to be rotated
Motor moves in a circle, and the output end of electric rotating machine is fixedly connected with the first electric pushrod, and electric rotating machine drive first is electronic to be pushed away
Bar is rotated, and the first electric pushrod drives stirring sheet to be rotated and moved up and down, and can realize to the material in retort
Sufficient mix is carried out, is made to stir in its course of reaction evenly, stirring scope is more comprehensive, improves reaction rate.
2. by the zone of heating set in reaction tank wall, zone of heating is by the constant warm tube of constant temperature inlet communication first, first
Constant warm tube connects thermostat, and thermostat connects constant temperature outlet, and the heating rod that reaction pot bottom is provided with by the second constant warm tube,
Thermostat conveys thermostatic medium into the first constant warm tube, by zone of heating, is discharged, is circulated by the second constant warm tube, can
Constant temperature, insulation or heating effectively more are carried out to retort, temperature change is preferably controlled, improves reaction rate.
3. fixed by reacting support tube that pot bottom is provided with and one end of the second electric pushrod and the second electric pushrod
The universal wheel of connection, universal wheel is released by support tube by the second electric pushrod when needing to move, move, it is necessary to
Retracted during fixed position the second electric pushrod, ground is contacted using support tube, carried out the stable placement of device, device can be facilitated
Movement, mitigate the burden of staff.
The structure design advantages of simple of the present invention, it is easy to operate, it can realize and the material in retort is carried out sufficiently
Mix is uniform, improves reaction rate, more effectively carries out constant temperature, insulation or heating to retort, preferably controls temperature
Change, facilitates the movement of device, alleviates the burden of staff, meet the needs of people.
Brief description of the drawings
Fig. 1 is a kind of structural representation of quick apparatus and method for preparing graphene proposed by the present invention；
Fig. 2 is the second electric pushrod and universal wheel of a kind of quick apparatus and method for preparing graphene proposed by the present invention
The structural representation of connection；
Fig. 3 is a kind of structural representation of the heating rod of quick apparatus and method for preparing graphene proposed by the present invention；
Fig. 4 is that a kind of circular slide rail of quick apparatus and method for preparing graphene proposed by the present invention connects with electric rotating machine
The structural representation connect；
Fig. 5 is a kind of part A structural representation of quick apparatus and method for preparing graphene proposed by the present invention.
In figure：1 retort, 2 zones of heating, 3 constant temperature imports, 4 constant temperature outlets, 5 first constant warm tubes, 6 thermostats, 7 second perseverances
Wen Guan, 8 feed pipes, 9 loading hoppers, 10 first valves, 11 gas outlets, 12 flue gas leadings, 13 waste heat boxes, 14 discharge nozzles, 15 second
Valve, 16 circular slide rails, 17 connecting rods, 18 electric rotating machines, 19 first electric pushrods, 20 stirring sheets, 21 support tubes, 22 second electricity
Dynamic push rod, 23 universal wheels, 24 heating rods, 25 controllers, 26 temperature indicators.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.
In the description of the invention, it is to be understood that term " on ", " under ", "front", "rear", "left", "right", " top ",
The orientation or position relationship of the instruction such as " bottom ", " interior ", " outer " are based on orientation shown in the drawings or position relationship, merely to just
In description the utility model and simplified description, rather than indicate or imply that signified device or element must be with specifically square
Position, with specific azimuth configuration and operation, therefore be not considered as limiting the invention.
Reference picture 1-5, a kind of quick apparatus and method for preparing graphene, including retort 1, the surrounding of retort 1
Surface is fixed with zone of heating 2, and the outer surface of zone of heating 2 is provided with constant temperature import 3 and constant temperature outlet 4, and constant temperature import 3 and constant temperature go out
Mouthfuls 4 connect with zone of heating 2, and the fixation of constant temperature import 3 is communicated with the first constant warm tube 5, the first constant warm tube 5 away from constant temperature import 3 one
End is fixed to be communicated with thermostat 6, and the one end of thermostat 6 away from the first constant warm tube 5, which is fixed, is communicated with the second constant warm tube 7, and second is permanent
The one end of warm pipe 7 away from thermostat 6 connects with constant temperature outlet 3, can more effectively to retort carry out constant temperature, insulation or
Heating, preferably controls temperature change, the top of retort 1 is provided with feed pipe 8, the one end of feed pipe 8 away from retort 1
Fixation is communicated with loading hopper 9, and the surface of feed pipe 8 is provided with the first valve 10, the first valve is opened when blowing is needed,
Material is put into, the top of retort 1 is fixed with gas outlet 11, and the one end of gas outlet 11 away from retort 1 is communicated with flue gas leading
12, the one end of flue gas leading 12 away from gas outlet 11, which is fixed, is communicated with waste heat box 13, will can be received in the exhaust gas centralized in course of reaction
Collection processing, avoid polluting environment, the bottom of retort 1 fixes connection and is provided with discharge nozzle 14, and the surface of discharge nozzle 14 is provided with second
Valve 15, after the completion of preparation, the second valve 15 is opened, taken out the material of needs by discharge nozzle 14.
The top inner wall of retort 1 is fixed with circular slide rail 16, and vertically fixation is connected with connecting rod 17 to circular slide rail 16,
The one end of connecting rod 17 away from circular slide rail 16 is vertically fixedly connected with electric rotating machine 18, and the output shaft of electric rotating machine 18 passes through connection
Axle device is connected with the first electric pushrod 19, and multiple stirring sheets 20, Neng Goushi are uniformly provided with the lever arm of the first electric pushrod 19
It is uniform that sufficient mix is now carried out to the material in retort 1, improves reaction rate.
Support tube 21 is fixed with the corner of the bottom of retort 1, the bottom of retort 1 is vertically fixed with and supported
Second electric pushrod 22 corresponding to cylinder 21, second one end of electric pushrod 22 away from retort 1 is fixed with universal wheel 23, energy
Enough it is easy to the movement of device, device is moved to suitable position.
The bottom of retort 1 is fixed with heating rod 24, constant temperature, insulation more can be effectively carried out to retort or added
Heat, preferably control temperature change.
The top of retort 1 is provided with observation window, can be easy to situation of the personal observations in reaction in retort, to do
Go out adjustment.
The side wall of zone of heating 2 is fixed with controller 25, and controller 25 is 80C51 programmable single chip computers, controller 25
Output end is defeated with circular slide rail 16, electric rotating machine 18, the first electric pushrod 19, the second electric pushrod 22 and heating rod 24 respectively
Enter end to be electrically connected with, circular slide rail 16, electric rotating machine 18, the first electric pushrod 19, the second electric pushrod can be accurately controlled
22 and the power output of heating rod 24, meet different stirrings and heating requirements.
Circular slide rail 16, electric rotating machine 18, the first electric pushrod 19, the second electric pushrod 22, heating rod 24 and controller
25 are electrically connected with external power source respectively, can ensure device in normal work, and the electricity for obtaining abundance ensures.
The one end of support tube 21 away from retort 1 is provided with the anti-skid wearable pad of a circle, preferably can fix device, subtract
Lack the friction between support tube 21 and ground and cause the abrasion of support tube 21, so as to influence the service life of support tube 21.
The side wall of zone of heating 2 is fixed with temperature indicator 26, and the output end and zone of heating 2 of the temperature indicator 26 are close
Envelope connection, temperature during staff's reaction can be accurately informed, be easy to record data and the whole reaction temperature of regulation and control
Degree, makes more convenient operation.
Thermostatic medium in thermostat 6 is vapor or oil, regulation and control for entering trip temperature that can be relatively stable, can be followed
Ring utilizes, energy-conserving and environment-protective.
Present invention also offers a kind of quick method for preparing graphene, comprise the following steps：
S1, in retort 1, a large amount of 98% concentrated sulfuric acids are put into, add graphite block or graphite flake, stirring, heating, control
Temperature reacts 3-6h, obtains graphite oxide at 40-80 DEG C；
S2, by graphite oxide and its reaction solution, 1-5h is handled by ultrasonic machine, obtains graphene oxide solution；
S3, graphene oxide solution is neutralized slightly with ammoniacal liquor, it is 4-6 to control pH, strong reductant is added, by graphite oxide
Alkene reduces, and obtains finished product graphene.
In the S3, strong reductant is specially one kind in hydrazine hydrate, sodium borohydride.
The course of work of the present invention：In use, manipulating the second electric pushrod 22 by controller 25, second is set electronic to push away
Bar 22 promotes universal 23 wheel to stretch out outside support tube 21, can be easy to the movement of device, device is moved into suitable position, then lead to
Cross controller 25 second electric pushrod 22 is retracted in support tube 21, be easy to the fixation of device, the first valve 10 is opened, by stone
Ink, strong oxidizer and strong reductant enter in retort 1 with time sequencing after loading hopper 9 falls into feed pipe 8 as desired,
The circular slide rail 16 being fixed with by the top inner wall of retort 1, circular slide rail 16 are fixedly connected with electric rotating by connecting rod 17
Machine 18, electric rotating machine 18 is driven to move in a circle, electric rotating machine 18 drives the first electric pushrod 19 to rotate, the first electric pushrod 19
Drive stirring sheet 20 to carry out stretching motion up and down, can realize that sufficient mix is carried out to the material in retort 1 is uniform, carry
High reaction rate, by the zone of heating 2 set in the outer wall of retort 1, zone of heating 2 connects the first constant warm tube by constant temperature import 3
5, the first constant warm tube 5 connection thermostat 6, thermostat 6 connects constant temperature outlet 4, and the bottom of retort 1 by the second constant warm tube 7
The heating rod 24 being provided with, constant temperature, insulation or heating effectively more can be carried out to retort 1, preferably control temperature change
Change, during reaction generates graphene, by the gas outlet 11 being provided with the top of retort 1, gas outlet 11 passes through flue gas leading
12 are communicated with waste heat box 13, can handle the waste gas centralized collection in course of reaction, avoid polluting environment, after the completion of preparation,
The second valve 15 is opened, is taken out the material of needs by discharge nozzle 14.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (10)
1. a kind of quick device for preparing graphene, including retort (1), it is characterised in that the surrounding of the retort (1)
Surface is fixed with zone of heating (2), and the outer surface of the zone of heating (2) is provided with constant temperature import (3) and constant temperature outlet (4), described
Constant temperature import (3) and constant temperature outlet (4) connect with zone of heating (2), and constant temperature import (3) fixation is communicated with the first constant warm tube
(5), the one end of first constant warm tube (5) away from constant temperature import (3), which is fixed, is communicated with thermostat (6), and the thermostat (6) is remote
One end fixation from the first constant warm tube (5) is communicated with the second constant warm tube (7), the remote thermostat (6) of second constant warm tube (7)
One end connects with constant temperature outlet (3), and the top of the retort (1) is provided with feed pipe (8), and the feed pipe (8) is away from reaction
One end of tank (1) is fixed and is communicated with loading hopper (9), and the surface of the feed pipe (8) is provided with the first valve (10), the reaction
Gas outlet (11) is fixed with the top of tank (1), the one end of the gas outlet (11) away from retort (1) is communicated with flue gas leading
(12), the one end of the flue gas leading (12) away from gas outlet (11), which is fixed, is communicated with waste heat box (13), the bottom of the retort (1)
Portion fixes connection and is provided with discharge nozzle (14), and the surface of the discharge nozzle (14) is provided with the second valve (15).
The top inner wall of the retort (1) is fixed with circular slide rail (16), and the circular slide rail (16) vertically fixes clamping
There is connecting rod (17), the one end of the connecting rod (17) away from circular slide rail (16) is vertically fixedly connected with electric rotating machine (18),
The output shaft of the electric rotating machine (18) is connected with the first electric pushrod (19), first electric pushrod (19) by shaft coupling
Lever arm on be uniformly provided with multiple stirring sheets (20).
A kind of 2. quick device for preparing graphene according to claim 1, it is characterised in that retort (1) bottom
It is fixed with support tube (21) at the corner in portion, it is right with support tube (21) that the bottom of the retort (1) is vertically fixed with
The second electric pushrod (22) answered, the one end of second electric pushrod (22) away from retort (1) are fixed with universal wheel
(23)。
3. a kind of quick device for preparing graphene according to claim 1, it is characterised in that the retort (1)
Bottom is fixed with heating rod (24)；The top of the retort (1) is provided with observation window.
4. a kind of quick device for preparing graphene according to claim 1, it is characterised in that the zone of heating (2)
Side wall is fixed with controller (25), and the controller (25) is 80C51 programmable single chip computers, the output of the controller (25)
End respectively with the circular slide rail (16), electric rotating machine (18), the first electric pushrod (19), the second electric pushrod (22) and heating
The input of rod (24) is electrically connected with.
A kind of 5. quick device for preparing graphene according to claim 1, it is characterised in that the circular slide rail
(16), electric rotating machine (18), the first electric pushrod (19), the second electric pushrod (22), heating rod (24) and controller (25) point
It is not electrically connected with external power source.
6. a kind of quick device for preparing graphene according to claim 1, it is characterised in that the support tube (21) is remote
One end from retort (1) is provided with the anti-skid wearable pad of a circle.
7. a kind of quick device for preparing graphene according to claim 1, it is characterised in that the zone of heating (2)
Side wall is fixed with temperature indicator (26), and the output end of the temperature indicator (26) connects with zone of heating (2) sealing.
8. a kind of quick device for preparing graphene according to claim 1, it is characterised in that in the thermostat (6)
Thermostatic medium be vapor or oil.
9. a kind of quick method for preparing graphene according to claim 1, it is characterised in that comprise the following steps：
S1, in retort (1), a large amount of 98% concentrated sulfuric acids are put into, add graphite block or graphite flake, stirring, heating, control temperature
Degree reacts 3-6h, obtains graphite oxide at 40-80 DEG C；
S2, by graphite oxide and its reaction solution, 1-5h is handled by ultrasonic machine, obtains graphene oxide solution；
S3, graphene oxide solution is neutralized slightly with ammoniacal liquor, it is 4-6 to control pH, adds strong reductant, by graphene oxide also
Original, obtain finished product graphene.
10. a kind of quick method for preparing graphene according to claim 10, it is characterised in that strong also in the S3
Former agent is specially one kind in hydrazine hydrate, sodium borohydride.
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| CN201710791479.9A CN107381552A (en) | 2017-09-05 | 2017-09-05 | A kind of quick apparatus and method for preparing graphene |
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| CN201710791479.9A CN107381552A (en) | 2017-09-05 | 2017-09-05 | A kind of quick apparatus and method for preparing graphene |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059153A (en) * | 2018-02-05 | 2018-05-22 | 苏州第元素纳米技术有限公司 | A kind of synthesizer and its method for preparing graphene |
| CN108483436A (en) * | 2018-06-12 | 2018-09-04 | 杨柳 | A kind of technical grade graphene oxide process units |
| CN108726512A (en) * | 2018-06-05 | 2018-11-02 | 刘强 | A kind of Large-scale graphene production equipment |
| CN108793132A (en) * | 2018-07-28 | 2018-11-13 | 赣州市兴顺辉科技有限公司 | It is a kind of can be to graphene preparation oxidation pond that irritant gas is handled |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205133157U (en) * | 2015-12-02 | 2016-04-06 | 安徽易能新材料科技有限公司 | Device of integration production oxidation graphite alkene or reduction -oxidation graphite alkene |
-
2017
- 2017-09-05 CN CN201710791479.9A patent/CN107381552A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205133157U (en) * | 2015-12-02 | 2016-04-06 | 安徽易能新材料科技有限公司 | Device of integration production oxidation graphite alkene or reduction -oxidation graphite alkene |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059153A (en) * | 2018-02-05 | 2018-05-22 | 苏州第元素纳米技术有限公司 | A kind of synthesizer and its method for preparing graphene |
| CN108059153B (en) * | 2018-02-05 | 2021-02-09 | 苏州第一元素纳米技术有限公司 | Synthesizer and method for preparing graphene by synthesizer |
| CN108726512A (en) * | 2018-06-05 | 2018-11-02 | 刘强 | A kind of Large-scale graphene production equipment |
| CN108483436A (en) * | 2018-06-12 | 2018-09-04 | 杨柳 | A kind of technical grade graphene oxide process units |
| CN108793132A (en) * | 2018-07-28 | 2018-11-13 | 赣州市兴顺辉科技有限公司 | It is a kind of can be to graphene preparation oxidation pond that irritant gas is handled |
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Application publication date: 20171124 |
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