CN110182794A - A kind of equipment and preparation method thereof of batch making graphene quantum dot - Google Patents
A kind of equipment and preparation method thereof of batch making graphene quantum dot Download PDFInfo
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- CN110182794A CN110182794A CN201910605358.XA CN201910605358A CN110182794A CN 110182794 A CN110182794 A CN 110182794A CN 201910605358 A CN201910605358 A CN 201910605358A CN 110182794 A CN110182794 A CN 110182794A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 46
- 239000002096 quantum dot Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 40
- 238000002604 ultrasonography Methods 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 230000000694 effects Effects 0.000 claims abstract description 8
- 238000001802 infusion Methods 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 96
- 229910002804 graphite Inorganic materials 0.000 claims description 84
- 239000010439 graphite Substances 0.000 claims description 84
- 239000007788 liquid Substances 0.000 claims description 59
- 238000012545 processing Methods 0.000 claims description 15
- 238000011084 recovery Methods 0.000 claims description 10
- 230000004913 activation Effects 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000010410 layer Substances 0.000 description 44
- 238000001994 activation Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010044565 Tremor Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000004018 waxing Methods 0.000 description 1
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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Abstract
The invention discloses a kind of equipment and preparation method thereof of batch making graphene quantum dot, the dispersion machine for circulating system it includes the tank liquor formed that connected with each other by N number of work nest and being arranged in work nest, and and ultrasonic equipment；Ultrasound wave vibrating bar in the ultrasonic equipment is arranged in work nest；The tank liquor circulates in system: setting an overflow port in preceding work nest upper end, the front end after terminal part top layer tank liquor flows into an overflow manner in work nest before making in work nest；Between most end work nest and the first work nest, an infusion pump and a cooling device are also set up, is connected in series by pipeline, tank liquor is sent into the first work nest from most end work nest.The equipment and preparation method thereof of batch making graphene quantum dot of the invention has graphene quantum dot size tunable, uniformity good, pollution-free preparation, yield be high, can volume production high-quality graphene quantum dot the advantages of effect.
Description
Technical field
The present invention relates to the technical fields of production graphene equipment to be particularly related to a kind of batch making graphene quantum
The equipment and preparation method thereof of point.
Background technique
Graphene quantum dot (GQDs) is a kind of nano material of quasi-zero dimension, due to the movement of its electronics in each direction
It is all restricted, so the local effect of quantum is particularly significant, there is unique physics, chemical property, for example partly lead with tradition
Body quantum dot is compared, and it is the quanta point material of environment-friendly type that there is graphene quantum dot (1), which to be free of high toxicity metallic element,；(2) it ties
Structure is stablized, resistance to strong acid, highly basic and photoetch；(3) band gap width range is adjustable；(4) surface-functionalized realize is easy;(5) thickness
It can be thin to characteristics such as a monatomic, chemical stabilities.
Currently, waxing development trend is totally presented in Chinese graphene quantum dot technology of preparing, main preparation methods are to reduce
Based on method.Graphene quantum dot reduces method technology of preparing and has that raw material is easy to get, simple production process, to be suitable for prepare with scale etc. excellent
Point, but exist control hardly possible, low yield, product size shakiness the disadvantages of；Enlargement method preparation process controllability is strong, but opposite operation
It is cumbersome, and the deficiencies of product purification difficult.
According to current graphene quantum dot technology of preparing feature and deficiency, preparation key technology, research and development preparation how are broken through
It is good with single layer size tunable, uniformity, pollution-free preparation, yield be high, can volume production high-quality graphene quantum dot, have become stone
The research topic of black alkene quantum dot production and R&D institution.
Summary of the invention
The object of the present invention is to provide a kind of equipment and preparation method thereof of batch making graphene quantum dot, in graphite powder
It prepares in the production process of graphene quantum dot, has controllable, pollution-free preparation, yield be high, can volume production high-quality graphene amount
The advantages of son point.
Above-mentioned purpose of the invention has the technical scheme that
What above-mentioned purpose was achieved through the following technical solutions: a kind of equipment of batch making graphene quantum dot, includes N number of
Work nest connect with each other composition a tank liquor circulate system, with the dispersion machine that is arranged in work nest, He Yuchao
Acoustic wave device；Ultrasound wave vibrating bar in the ultrasonic equipment is arranged in work nest.In order to make in work nest in liquid
Multi-layer graphite particle removed by " cavitation " of omnidirectional ultrasonic, further include having ultrasonic wave vibration in the ultrasonic equipment
Dynamic box, is arranged on the outer wall of work nest surrounding and bottom.
Further, since Multi-layer graphite particle is easy to happen aggregation, in order to make the Multi-layer graphite in each working tank solution
Grain is not assembled, and most effectively can carry out " cavitation " removing by ultrasonic wave, and the tank liquor circulates work in system
Make in slot, dispersion machine and ultrasound wave vibrating bar equipped with several adjacent spaces arrangement, the center spacing of the two is L, the L
=n(V/f), n is that 0 natural number, V are the spread speed of ultrasonic wave in a liquid, and f is the frequency of ultrasonic wave.
Further, since the Multi-layer graphite sheet of particles number of plies in each groove body is not of uniform size, in order to make ultrasound wave vibrating bar and
Disperse function and carries out " cavitation " removing more effective for Multi-layer graphite particle splat, the ultrasonic activation in adjacent work nest
Stick uses different ultrasonic power and frequency, and the tank liquor circulates in system in each work nest, the ultrasonic wave of setting
Vibrating head and dispersion machine center spacing L are different.
Further, it is optimized to run each groove ultrasonic equipment and dispersion machine, the ultrasonic equipment frequency is set
It is set to: 15KHz-60KHz;The dispersing speed setting are as follows: 1-2200r/min.
Further, in order to make the tank liquor in work nest stop the longer time in slot, and make top layer lightweight in end in slot
Multi-layer graphite particle can isolate groove body, and heavy Multi-layer graphite particle, which is kept, continues " cavitation " removing in cell operation slot, described
Tank liquor circulate in system operated adjacent slot perforation connection structure and be: set an overflow port in preceding work nest upper end, make
Front end after terminal part top layer tank liquor flows into an overflow manner in preceding work nest in work nest；In order to keep Multi-layer graphite particle big
Small difference value is more uniform, more stable, and working region is arranged where dispersion machine in the overflow outlet；In order to make to flow out in tank liquor
Multi-layer graphite granular size disparity range minimize, Multi-layer graphite particle is more uniform, and the overflow port is designed as greatly
Width spill mouth, the liquid level for overflowing overflow port are smaller.
Since ultrasound wave vibrating bar, ultrasonic activation box and dispersion machine can generate amount of heat during the work time, in order to
It ensures that temperature of the tank liquor in the work nest circulatory system can control in a certain range, tank liquor circulation system is enable to be normally carried out list
To reciprocal circular flow, the tank liquor circulates most end work nest and first unit work nest in system and penetrates through connection structure
It is: between most end work nest and first unit work nest, also sets up an infusion pump and a cooling device, connected by placed in series
It connects, tank liquor is sent into the first work nest from most end work nest.
Further, in order to enable equipment provided by the invention successfully to feed, for launching the materials such as graphite powder, liquid,
The tank liquor circulates in system and is additionally provided with a feed inlet above the first work front of the slot, in order to enable feed inlet simultaneously
Multinomial charging operation is carried out, the feed inlet can design multiple feeding ports, for launching the materials such as graphite powder, solution；In order to
Liquid level and fluid temperature in slot are observed, the tank liquor circulates in system and is additionally provided with liquid level on the first work nest outer wall
Controller and temp probe.
Further, in order to make finished product graphene quantum dot obtain acquisition recycling, the tank liquor circulates each in system
The tank liquor recovery pipe that work trench bottom is additionally provided with control valve and connects with each other, tank liquor recovery pipe are equipped with liquids recovery
Outlet.
Further, due in cell operation slot ultrasonic equipment and dispersion machine generate heat at work, in order to make work nest
In fluid temperature controlled, the tank liquor, which circulates work nest in system, may be designed as cooling bath.
Further, in order to make ultrasound wave vibrating bar and dispersion machine the center-adjustable spacing L in work nest, and laborsaving province
When, it is efficient and convenient, the tank liquor circulate in system be additionally provided with above work nest for installing, adjusting, mounting ultrasonic
The shifting sledge of equipment and dispersion machine.
A kind of preparation method using above equipment batch making graphene quantum dot:
Step 1: graphite powder, solution being mixed into mixed liquor in proportion and put into the first work nest from feed inlet, mixed liquor exists
It is successively flowed into each work nest from front to back in first work nest, after N number of work nest fills it up with mixed liquor, stops charging；
Step 2: starting tank liquor circulates system, ultrasonic equipment and dispersion machine operation, makes mixed liquor the past in work nest
It flows through, under the action of ultrasonic equipment and dispersion machine, the graphite powder in tank liquor is orderly dispersed, " cavitation " backward
Lift-off processing, making in tank liquor graphite particle size variation, in front end particle, big, rear end particle becomes smaller in slot, under heavies
In the state that heavy, light granules float, and the graphite particle size in tank liquor is controlled in a certain range in an orderly manner；
Step 3: in the first work tank liquid into the flowing of the second work nest: the graphite powder of most light granules is in preceding work nest
In first work nest end top layer liquid level, as top layer liquid flows into the second work nest from terminal part overflow port, the first work
Graphite particle in tank liquid completes a lift-off processing, and the graphite particle entered in the second work tank liquid is made to become smaller；
Step 4: in the second work nest, graphite particle in liquid, in the ultrasonic equipment and dispersion machine for newly setting running parameter
Under effect, to the graphite particle flowed into tank liquor again in groove body, dispersed from front to back, " cavitation " lift-off processing,
Graphite particle in groove body is set to become smaller, graphite particle size is big still in front end particle, rear end particle is small, and heavies sink, is light
In the state that matter particle floats；
Step 5: liquid into third work nest overflow, complete again by the graphite particle in the second work tank liquid in the second work nest
Secondary lift-off processing makes the graphite particle size entered in third work tank liquid become smaller；
Step 6: tank liquor of the invention circulates system, is equipped with N number of work nest, the ultrasonic equipment of each work nest setting
Running parameter is different, and tank liquor circulates the graphite particle in system liquid successively from the first work nest to N work nest
Operation circulates in tank liquor until terminating and completes a wheel circulation in system；Graphite particle in a wheel circulation, in liquid
In N number of work nest, n times lift-off processing is completed, the graphite particle number of plies is fewer and fewer, and graphite particle diameter becomes increasingly
It is small, it is intended to graphene quantum dot；
Step 7: tank liquor is inputted the first work nest after completing first time circular flow, with infusion pump by the graphite particle in liquid
In, carry out the second wheel circular flow；
Step 8: pressing step 2-7 program, so unidirectional reciprocation cycle continuous service, graphite powder first removes into Multi-layer graphite in tank liquor
Particle, Multi-layer graphite particle are stripped again, so that the Multi-layer graphite sheet of particles number of plies becomes fewer and fewer, diameter is smaller and smaller, the phase
Between tank liquor circulate the cooling device in system and opened simultaneously with ultrasonic equipment and dispersion machine, to control on tank liquor temperature
It rises, the Multi-layer graphite particle in tank liquor is increasingly becoming carbon quantum dot；
Step 9: with the increase of working time, carbon quantum dot is circulated in system in tank liquor and is further peeled, and the number of plies becomes
Fewer and fewer, diameter is smaller and smaller, eventually becomes graphene quantum dot；
Step 10: after the Multi-layer graphite particle in tank liquor is removed into graphene quantum dot, control valve is opened, from tank liquor recovery port
Acquire finished product graphene quantum dot.
1. beneficial effects of the present invention: 1, installing several ultrasonic activations regularly due to inside and outside in each work nest
Stick, ultrasonic activation box and dispersion machine, so that being shelled including Multi-layer graphite particle, under the effect of outer ultrasonic wave by " cavitation " in each groove body
From becoming smaller.2, due to setting an overflow port in preceding work nest upper end, so that top layer light-weight multi-layer graphite in end in work nest
Grain can isolate groove body, and heavy Multi-layer graphite particle, which is kept, continues " cavitation " removing in cell operation slot, flow into lower road work nest
In Multi-layer graphite granular size tend to be uniform.3, a tank liquor circulation system is formed since N number of work nest connects with each other,
So that the tank liquor in each groove body is able to maintain normal unidirectional reciprocation cycle operation, in ultrasound wave vibrating bar, ultrasonic activation box and divide
It dissipates under machine effect, the Multi-layer graphite sheet of particles number of plies is removed fewer and fewer by ultrasonic wave " cavitation ", and Multi-layer graphite particle splat becomes
To graphene quantum dot grade.4, since work nest can be cooling bath, so that fluid temperature is controllable in slot, liquid will not be added
Heat.
Detailed description of the invention
Fig. 1 is the horizontal layout schematic illustration in the present invention；
Fig. 2 is the mounting structure schematic diagram of the first work nest in Fig. 1, ultrasound wave vibrating bar, ultrasonic activation box and dispersion machine；
Fig. 3 is between operated adjacent slot in Fig. 1 using the structural schematic diagram of overflow manner perforation connection.
In figure, 1, work nest；2, dispersion machine；3, ultrasound wave vibrating bar；4, vibration of ultrasonic wave box；5, overflow port；6, it is infused
Pump；7, cooling device；8, feed inlet；9, liquid-level controller；10, control valve；11, recovery port；12, shifting sledge.
Specific embodiment
Presently in connection with attached drawing, the present invention is described in detail.This figure is simplified schematic diagram, is only illustrated in a schematic way
Basic structure of the invention, therefore it only shows the composition relevant to the invention.
As shown in Figure 1 and Figure 2, a kind of equipment of batch making graphene quantum dot, comprising there are four work nests 1 mutually to pass through
Lead to and connect two dispersion machines 2 that a tank liquor of composition circulates system and is arranged in work nest 1, and is set with ultrasonic wave
It is standby；Two ultrasound wave vibrating bars 3 in the ultrasonic equipment are arranged in work nest 1.In order to make in work nest 1 in liquid
Multi-layer graphite particle removed by " cavitation " of omnidirectional ultrasonic, further include having ultrasonic wave in the ultrasonic equipment
Vibration box 4 is arranged on the outer wall of 1 surrounding of work nest and bottom.
In order to assemble the Multi-layer graphite particle in each 1 solution of work nest not, and can be most effectively by ultrasonic wave
" cavitation " removing is carried out, in the work nest 1, two dispersion machines 2 and two 3 adjacent spaces of ultrasound wave vibrating bar arrangements,
The center spacing of the two is L, the L=n(V/f), n is that 0 natural number, V are the propagation of ultrasonic wave in a liquid
Speed, f are the frequency of ultrasonic wave.
Since the Multi-layer graphite particle splat in each groove body is not of uniform size, in order to enable ultrasonic equipment and dispersion machine 2 more
" cavitation " removing effectively is carried out for Multi-layer graphite particle, tank liquor circulates the ultrasound in system in adjacent work nest 1
Wave device uses different ultrasonic power and frequency, in 1 circulatory system of work nest, the ultrasound that is arranged in each work nest 1
Wave device and 2 center spacing L of dispersion machine be not identical.In first order work nest 1, n=1；In second level work nest 1, n=2；The
In three-level work nest 1, n=3；In fourth stage work nest 1, n=4；In n-th level work slot 1, n=n.
It is optimized to run each groove ultrasonic equipment and dispersion machine, the ultrasonic equipment set of frequency are as follows:
15KHz-60KHz;The dispersing speed setting are as follows: 1-22000r/min.
In order to make the tank liquor in work nest 1 stop the longer time in slot, and make top layer light-weight multi-layer stone in end in slot
Black particle splat can isolate groove body, and heavy Multi-layer graphite particle splat, which is kept, continues " cavitation " removing in work nest 1, described
Tank liquor circulates the perforation of operated adjacent slot 1 connection structure in system: setting an overflow port 5 in preceding 1 upper end of work nest, makes
Front end after terminal part top layer tank liquor flows into an overflow manner in preceding work nest 1 in work nest 1, sees Fig. 3；In order to make multilayer stone
Black sheet of particles number of plies difference in size value is more uniform, more stable, and the overflow port 5 is arranged in 2 place working region of dispersion machine；For
Make to flow out the Multi-layer graphite sheet of particles number of plies difference in size value range in tank liquor to minimize, the Multi-layer graphite sheet of particles number of plies is more
Uniformly, the overflow port 5 is designed as big width concave exit, and the liquid level for overflowing overflow port 5 is smaller.
Since ultrasonic equipment and dispersion machine 2 can generate amount of heat during the work time, in order to ensure tank liquor unidirectional
Temperature in the circulatory system can control makes the Multi-layer graphite sheet of particles number of plies in tank liquor in this circulatory system in a certain range
It is removed to continuous reciprocation cycle, tank liquor circulates the knot of the 4th work nest 1 and the perforation connection of the first work nest 1 in system
Structure is: between the 4th work nest 11 and the first work nest 1, an infusion pump 6 and a cooling device 7 is arranged, passes through placed in series
Tank liquor is inputted the first work nest 1 from the 4th work nest 1 by connection.Cooling device can be set to cooler or other refrigeration are set
It is standby.
The feed inlet 8 of 1 circulatory system of this work nest is arranged above 1 front end of the first work nest, and feed inlet 8 can design multiple
Feeding port, launching materials, the solution such as graphite powder, solution respectively includes but is not limited to pure water, various dispersing agents (ethyl alcohol, DMF, NMP
Deng), in work nest 1, being adapted to property selects the one or more of pure water or dispersing agent.
In order to observe liquid level and fluid temperature in slot, 9 He of liquid-level controller is additionally provided on 1 outer wall of the first work nest
Liquid probe.
Further, in order to make finished product graphene quantum dot obtain acquisition recycling, the tank liquor circulates each in system
The tank liquor recovery pipe that work trench bottom is additionally provided with control valve 10 and connects with each other, tank liquor recovery pipe are returned equipped with liquid
Receive outlet 11.
Further, due in work nest 1 ultrasonic equipment and dispersion machine 2 generate heat at work, in order to make in work nest 1
Fluid temperature controlled, the tank liquor, which circulates work nest 1 in system, may be designed as cooling bath.In work nest outer wall
Cooling coil is arranged in setting cooler in work nest, to realize the cooling effect to work nest internal liquid.
Further, in order to make dispersion machine 2 and the center-adjustable spacing in work nest 1 of ultrasound wave vibrating bar 3, and it is laborsaving
It is time saving, it is efficient and convenient, the tank liquor circulate be additionally provided with above each work nest 1 in system it is super for installing, adjusting, fix
The shifting sledge 12 of acoustic wave device and dispersion machine 2.
A kind of preparation method using above equipment batch making graphene quantum dot:
Step 1: graphite powder, pure water are mixed into mixed liquor in proportion and put into the first work nest 1 from feed inlet 8, mixed liquor
It is successively flowed into from front to back in each work nest 1 in the first work nest 1, after N number of work nest 1 fills it up with mixed liquor, stops adding
Material；
Step 2: starting tank liquor circulates system, ultrasonic equipment and dispersion machine 2 are run, make mixed liquor in work nest 1 from
It is flowed through after going to, under the action of ultrasonic equipment and dispersion machine, the graphite powder in tank liquor is orderly dispersed, is " empty
Change " lift-off processing, making in tank liquor graphite particle size variation, in front end particle, big, rear end particle becomes smaller in work nest 1, weight
In the state that matter particles sink, light granules float, and the graphite particle size in tank liquor is controlled in an orderly manner in certain model
In enclosing；
Step 3: in 1 liquid of the first work nest into the flowing of the second work nest 1: the graphite powder of most light granules in preceding work nest 1
It is in 1 end top layer liquid level of the first work nest, as top layer liquid flows into the second work nest 1 from terminal part overflow port 5, the
Graphite particle in one work nest, 1 liquid completes a lift-off processing, makes the graphite particle entered in 1 liquid of the second work nest
Become smaller；
Step 4: in the second work nest 1, graphite particle in liquid, in the ultrasonic equipment and dispersion machine for newly setting running parameter
Under effect, to the graphite particle flowed into tank liquor again in groove body, dispersed from front to back, " cavitation " lift-off processing,
Graphite particle in groove body is set to become smaller, graphite particle size is big still in front end particle, rear end particle is small, and heavies sink, is light
In the state that matter particle floats；
Step 5: liquid is into 1 overflow of third work nest in the second work nest 1, and the graphite particle in 1 liquid of the second work nest is again
A lift-off processing is completed, the graphite particle size entered in 1 liquid of third work nest is made to become smaller；
Step 6: tank liquor of the invention circulates system, is equipped with N number of work nest 1, the ultrasonic equipment that each work nest 1 is arranged
Running parameter is different, and tank liquor circulates the graphite particle in system liquid successively from the first work nest 1 to N work nest
1 operation circulates in tank liquor until terminating and completes a wheel circulation in system；Graphite particle in a wheel circulation, in liquid
In N number of work nest 1, n times lift-off processing is completed, the graphite particle number of plies is fewer and fewer, and graphite particle diameter becomes increasingly
It is small, it is intended to graphene quantum dot；
Step 7: the graphite particle in liquid works tank liquor input first after completing first time circular flow, with infusion pump 6
In slot 1, the second wheel circular flow is carried out；
Step 8: pressing step 2-7 program, so toward unidirectionally circulation continuous operation again, circulated in system in tank liquor, in tank liquor
Graphite powder first removes into Multi-layer graphite particle, and Multi-layer graphite particle is stripped again, so that the Multi-layer graphite sheet of particles number of plies becomes to get over
Come fewer, diameter is smaller and smaller, and during which tank liquor circulates cooling device 7 in system and ultrasonic equipment and dispersion machine 2 is same
Shi Kaiqi, control tank liquor temperature rise, and the Multi-layer graphite particle in tank liquor is increasingly becoming carbon quantum dot；
Step 9: with the increase of working time, carbon quantum dot is circulated in system in tank liquor and is further peeled, and the number of plies becomes
Fewer and fewer, diameter is smaller and smaller, eventually becomes graphene quantum dot；
Step 10: when the Multi-layer graphite particle in tank liquor is removed into graphene quantum dot, opening control valve 10, recycled from tank liquor
Mouth 11 acquires finished product graphene quantum dots.
Basic principles and main features and the features of the present invention of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe hairs
Bright principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement is both fallen in the range of claimed invention.The scope of protection of present invention is by appended claims
And its equivalent thereof.
Claims (12)
- It include that N number of work nest connects with each other a slot of composition 1. a kind of equipment of batch making graphene quantum dot The dispersion machine that liquid recycle stream moves system and is arranged in work nest, and and ultrasonic equipment；It is super in the ultrasonic equipment Acoustic vibration stick is arranged in work nest.
- 2. a kind of equipment of batch making graphene quantum dot according to requiring 1, it is characterised in that: the ultrasonic wave is set Further include having ultrasonic activation box in standby, is arranged on the outer wall of work nest surrounding and bottom.
- 3. a kind of equipment of batch making graphene quantum dot according to requiring 1, it is characterised in that: the tank liquor circulation In running system in work nest, dispersion machine and ultrasound wave vibrating bar equipped with several adjacent spaces arrangement, between the center of the two Away from for L；L=the n(V/f), n is that 0 natural number, V are the spread speed of ultrasonic wave in a liquid, and f is ultrasonic wave Frequency.
- 4. a kind of equipment of batch making graphene quantum dot according to requiring 1, it is characterised in that: the tank liquor circulation In running system in each work nest, the ultrasound wave vibrating bar and dispersion machine center spacing L of setting are different.
- 5. a kind of equipment of batch making graphene quantum dot according to requiring 1, it is characterised in that: the ultrasonic wave is set Standby set of frequency are as follows: 15KHz-60KHz;The dispersing speed setting are as follows: 1-22000r/min.
- 6. a kind of equipment of batch making graphene quantum dot according to requiring 1, it is characterised in that: the tank liquor circulation Operated adjacent slot perforation connection structure is in running system: an overflow port is set in preceding work nest upper end, before making in work nest Front end after terminal part top layer tank liquor flows into an overflow manner in work nest.
- 7. a kind of equipment of batch making graphene quantum dot according to requiring 5, it is characterised in that: the overflow outlet Working region is set where dispersion machine；The overflow port is designed as the spill mouth of big width.
- 8. a kind of equipment of batch making graphene quantum dot according to requiring 1, it is characterised in that: the tank liquor circulation Most end work nest and the first work nest perforation connection structure are in running system: between most end work nest and the first work nest, An infusion pump and a cooling device are also set up, is connected in series by pipeline, tank liquor is sent into the first work nest from most end work nest In.
- 9. a kind of equipment of batch making graphene quantum dot according to requiring 1, it is characterised in that: the tank liquor circulation It is additionally provided with a feed inlet above the first work front of the slot in running system, the feed inlet may be designed as multiple feeding ports；The tank liquor circulates the tank liquor recycling that the trench bottom that respectively works in system is additionally provided with control valve and connects with each other Pipeline, tank liquor recovery pipe are exported equipped with liquids recovery；Liquid-level controller is additionally provided on the first work nest outer wall.
- 10. a kind of equipment of batch making graphene quantum dot according to requiring 1, it is characterised in that: the tank liquor follows It is additionally provided with above work nest for installing, adjusting in ring running system, the shifting sledge of mounting ultrasonic vibrating head and dispersion machine.
- 11. a kind of equipment of batch making graphene quantum dot according to requiring 1, it is characterised in that: the tank liquor follows Work nest may be designed as cooling bath in ring running system.
- 12. a kind of preparation method using any one of the claims 1-11 equipment batch making graphene quantum dot, special Sign is:Step 1: graphite powder, solution being mixed into mixed liquor in proportion and put into the first work nest from feed inlet, mixed liquor exists It is successively flowed into each work nest from front to back in first work nest, after N number of work nest fills it up with mixed liquor, stops charging；Step 2: starting tank liquor circulates system, ultrasonic equipment and dispersion machine operation, makes mixed liquor the past in work nest It flows through, under the action of ultrasonic equipment and dispersion machine, the graphite powder in tank liquor is orderly dispersed, " cavitation " backward Lift-off processing, making in tank liquor graphite particle size variation, in front end particle, big, rear end particle becomes smaller in slot, under heavies In the state that heavy, light granules float, and the graphite particle size in tank liquor is controlled in a certain range in an orderly manner；Step 3: in the first work tank liquid into the flowing of the second work nest: the graphite powder of most light granules is in preceding work nest In first work nest end top layer liquid level, as top layer liquid flows into the second work nest from terminal part overflow port, the first work Graphite particle in tank liquid completes a lift-off processing, and the graphite particle entered in the second work tank liquid is made to become smaller；Step 4: in the second work nest, graphite particle in liquid, in the ultrasonic equipment and dispersion machine for newly setting running parameter Under effect, to the graphite particle flowed into tank liquor again in groove body, dispersed from front to back, " cavitation " lift-off processing, Graphite particle in groove body is set to become smaller, graphite particle size is big still in front end particle, rear end particle is small, under heavies In the state that heavy, light granules float；Step 5: for liquid into third work nest overflow, the graphite particle in the second work tank liquid is again complete in the second work nest At secondary lift-off processing, the graphite particle size entered in third work tank liquid is made to become smaller；Step 6: tank liquor of the invention circulates system, is equipped with N number of work nest, the ultrasonic equipment of each work nest setting Running parameter is different, and tank liquor circulates in system, and the graphite particle in liquid successively works from the first work nest to N Slot operation circulates in tank liquor until terminating and completes a wheel circulation in system；Graphite in a wheel circulation, in liquid Grain completes n times lift-off processing, the graphite particle number of plies is fewer and fewer, and graphite particle diameter becomes increasingly in N number of work nest It is small；Step 7: the graphite particle in liquid is after completing first time circular flow, with infusion pump by the slot in last liquid bath Liquid inputs in the first work nest, carries out the second wheel circular flow；Step 8: pressing step 2-7 program, so unidirectional reciprocation cycle continuous service, graphite powder first removes into Multi-layer graphite in tank liquor Particle, Multi-layer graphite particle are stripped again, so that the Multi-layer graphite sheet of particles number of plies becomes fewer and fewer, diameter is smaller and smaller, the phase Between tank liquor circulate cooling device in system and ultrasonic equipment and dispersion machine opens operation simultaneously, to control tank liquor temperature Rise；Multi-layer graphite particle in tank liquor is increasingly becoming carbon quantum dot；Step 9: with the increase of working time, carbon quantum dot is circulated in system in tank liquor and is further peeled, and the number of plies becomes Fewer and fewer, diameter is smaller and smaller, eventually becomes graphene quantum dot；Step 10: after the Multi-layer graphite particle in tank liquor is removed into graphene quantum dot, control valve is opened, from tank liquor recovery port Acquire finished product graphene quantum dot.
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