CN110228799A - Continuously prepare device, the preparation method and application of monodisperse carbosphere - Google Patents
Continuously prepare device, the preparation method and application of monodisperse carbosphere Download PDFInfo
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- CN110228799A CN110228799A CN201910647772.7A CN201910647772A CN110228799A CN 110228799 A CN110228799 A CN 110228799A CN 201910647772 A CN201910647772 A CN 201910647772A CN 110228799 A CN110228799 A CN 110228799A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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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
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
A kind of device, preparation method and application continuously preparing monodisperse carbosphere, which includes: reaction chamber, and top is equipped with feed inlet；Reactor, is arranged inside reaction chamber and its bottom is equipped with centre bore, and reactor is used for fused materials；Piezoelectricity gear unit, is arranged in inside reactor and one end can squeeze out the material in reactor out of centre bore；Micropore unit, centrally disposed hole bottom, for controlling the size for forming particle；Heating unit is used for heating response device；And vacuum unit, to provide pressure difference inside and outside reactor.The carbon material that the present invention melts in crucible is evenly dispersed under the action of stirring blade, it is come out by way of pulse from crucible bottom small hole injection later, carbosphere is formed by no container process of setting, the carbosphere prepared with this method has particle diameter distribution uniform, sphericity is high, the advantages that purity is high, yield and high extraction efficiency.
Description
Technical field
The invention belongs to micron order carbosphere preparation technical fields, and in particular to a kind of continuously to prepare monodisperse carbosphere
Device, preparation method and application.
Background technique
In the 1960s, people have unexpectedly discovered a kind of spherical carbon material in the research of STRENGTH ON COKE developmental process,
Further result of study shows that this spherical carbon material is that intermediate phase transition occurs in high-temperature process by pitch class compound
And generate.
In the 1970s, Yamada and Hond isolate mesophase ball from pitch precursor, and it is referred to as centre
Phase carbosphere.1978, Lewis had found the solvable thermal change feature of interphase on Hot stage microscope, finally assert interphase
It may include the insoluble high molecular weight component of solvent and the soluble lower-molecular-weight component of solvent.Hereafter, Japanese scholars are also further
Carbonaceous mesophase theory is developed, and its structure has been studied, further deep grind is done to carbosphere for numerous scholars
Study carefully and provides stronger theoretical direction.So more and more scholars utilize non-bituminous class raw material to pass through not Tongfang in recent years
Method successfully prepares the more uniform carbosphere of partial size, has greatly enriched carbon material in the extensive use of various fields.
Carbosphere has important development trend and application prospect, can be applicable to the electrode material of lithium ion secondary battery
The neck such as packing material of material, high-ratio surface active-carbon-microball, high density isotropic carbon/graphite material and performance liquid chromatographic column
Domain.
The method for preparing carbosphere at present has thermal polycondensation process, emulsion process, suspension method etc..Thermal polycondensation process have process it is simple,
The advantages that preparation condition is easy to control, Yi Shixian continuous production, but occur during the reaction bead melt and phenomenon so that
The size distribution of bead is wide and partial size is uneven, to limit yield；And emulsion process and suspension method are answered due to complex process
With being restricted.
Summary of the invention
In view of this, one of main object of the present invention be to propose a kind of device for continuously preparing monodisperse carbosphere,
Preparation method and application, at least be partially solved at least one of above-mentioned technical problem.
To achieve the goals above, it as one aspect of the present invention, provides one kind and continuously prepares monodisperse carbosphere
Device, comprising:
Reaction chamber, top are equipped with feed inlet；
Reactor, is arranged inside reaction chamber and its bottom is equipped with centre bore, and reactor is used for fused materials；
Piezoelectricity gear unit, is arranged in inside reactor and one end can squeeze the material in reactor out of centre bore
Out；
Micropore unit, centrally disposed hole bottom, for controlling the size for forming particle；
Heating unit is used for heating response device；And
Vacuum unit, to provide pressure difference inside and outside reactor.
As another aspect of the present invention, additionally provides and a kind of micron size is obtained using device as described above
The preparation method of carbosphere, includes the following steps:
(1) the molten condition carbon material in reactor is mixed with solvent, obtains carbon material one after cooling；
(2) it is sprayed from micropore unit under the action of piezoelectricity gear unit after melting carbon material one and forms drop, liquid
Microballoon is formed after drop is cooling to get the micron size carbosphere is arrived.
As an additional aspect of the present invention, a kind of be prepared using device as described above or using such as is additionally provided
The monodisperse carbosphere that the upper preparation method obtains.
As another aspect of the invention, monodisperse carbosphere as described above is additionally provided in lithium ion secondary battery
Electrode material, isotropism carbon/graphite material and performance liquid chromatographic column packing material field in application.
Based on the above-mentioned technical proposal it is found that the of the invention device for continuously preparing monodisperse carbosphere, preparation method and answering
With one of at least having the advantage that compared with the existing technology:
1, the carbon material that the present invention melts in crucible is evenly dispersed under the action of stirring blade, passes through pulse later
Mode comes out from crucible bottom small hole injection, forms carbosphere by no container process of setting.It prepares with this method
The advantages that carbosphere has particle diameter distribution uniform, and sphericity is high, purity is high, yield and high extraction efficiency.
2, the present invention can continuously produce carbosphere, improve production efficiency.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of device described in the embodiment of the present invention.
In upper figure, appended drawing reference meaning is as follows:
1- piezoelectricity gear unit；2- water outlet；3- feed inlet；4- heat shield；5- drive rod；6- crucible；7- blade；8- ring
Shape heater；9- fire door；10- nanopore device；11- bracket；12- collecting chamber；The upper snorkel of 13-；14- water inlet；15- is cooling
Water；16- vent valve；17- melt；18- cavity；Snorkel under 19-；20- drop；21- landing pipe.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in further detail.
The invention discloses a kind of devices for preparing monodisperse carbosphere, comprising:
Reaction chamber, top are equipped with feed inlet；
Reactor, is arranged inside reaction chamber and its bottom is equipped with centre bore, and reactor is used for fused materials；
Piezoelectricity gear unit, is arranged in inside reactor and one end can squeeze the material in reactor out of centre bore
Out；
Micropore unit, centrally disposed hole bottom, for controlling the size for forming particle；
Heating unit is used for heating response device；And
Vacuum unit, to provide pressure difference inside and outside reactor.
The inside reactor is equipped with the agitating unit for stirring material；
Wherein, the agitating unit includes blade；The blade rotates horizontally；The axle center of the blade and the piezoelectricity pass
The axle center of moving cell is on a vertical line；
Wherein, the reaction chamber side wall is equipped with gas vent；It is equipped in gas vent in the connection reaction chamber to shield
The vent valve in portion and outside atmosphere.
Wherein, the contact angle between the reactor and micropore unit and melt is all larger than 90 degree, and the two does not occur instead
It answers；
Wherein, the reactor includes crucible；
Wherein, the reaction chamber is equipped with the watch window for real-time observing response device.
Wherein, the piezoelectricity gear unit includes piezoelectric ceramics, thermal insulation board and drive rod, and the thermal insulation board setting is being driven
Above bar, the drive rod bottom end can be protruded into the centre bore in reactor；
Wherein, the aperture of the micropore unit is 0.05-0.8mm；
Wherein, the heating unit includes heater；
Wherein, the heater is annular；
Wherein, the heater is resistance heater；
Wherein, the vacuum unit includes:
First snorkel is arranged in reactor head, for adjusting the pressure of inside reactor；
Second snorkel is arranged on reaction chamber side wall, for adjusting the pressure inside reaction chamber；And
Third snorkel is connected to the first snorkel and the second snorkel, and third snorkel is equipped with for adjusting instead
Answer the third breather pipe valve of pressure difference between device and reaction chamber.
Wherein, the device for preparing monodisperse carbosphere further includes the collector unit for collecting product, collector unit
It is arranged below reaction chamber；
Wherein, the collector unit includes landing pipe and collecting chamber, and landing pipe is arranged between reaction chamber and collecting chamber, system
The monodisperse carbosphere got ready enters the collecting chamber from landing pipe；
Wherein, the device for preparing monodisperse carbosphere further includes the water cooling unit for cooling down reaction chamber, the water
Cold unit includes cooling water intake and cooling water outlet；
Wherein, the device for preparing monodisperse carbosphere further includes the branch that reaction chamber bottom is arranged in and plays a supportive role
Frame.
The preparation method of micron size carbosphere is obtained using device as described above the invention also discloses a kind of,
Include the following steps:
(1) the molten condition carbon material in reactor is mixed with solvent, obtains carbon material one after cooling；
(2) it is sprayed from micropore unit under the action of piezoelectricity gear unit after melting carbon material one and forms drop, liquid
Microballoon is formed after drop is cooling to get the micron size carbosphere is arrived.
Wherein, the internal and external pressure difference of reactor described in step (1) is 1-10Kpa；
Wherein, form the process of drop specifically: preset pulse letter is set after melting carbon material described in step (2)
Number, by pumping for the state modulator drive rod of pulse waveform regulated, carbon material is made to spray shape from nanopore device
At drop；
Wherein, pulse signal described in step (2) is trapezoidal wave, and the rising time of the trapezoidal wave is 50-1000 μ
S keeps being 500-5000 μ s along the time, and the failing edge time is 500-5000 μ s；
Wherein, the cooling method of drop described in step (2) includes natural cooling in landing pipe；
Wherein, the sphericity for the micron size carbosphere being prepared in step (2) is distributed S50≥0.94。
Wherein, incubation step is carried out after the fusing of carbon material one described in step (2) step；
Wherein, it is stirred step again after one incubation step of carbon material in step (2)；
Wherein, the whipping step specifically: the piezoelectricity gear unit is before unlatching, the blade elder generation work of agitating unit
Make 10-30min, keeps melt dispersion uniform；
Wherein, the process of the preparation method has continuity, and the continuity is to make to react by continuous adding raw materials
The amount of indoor melt remains unchanged realization.
It is prepared using device as described above or the invention also discloses a kind of using preparation method as described above
Obtained monodisperse carbosphere.
Electrode material, Gao Bibiao the invention also discloses monodisperse carbosphere as described above in lithium ion secondary battery
Application in the packing material field of face active-carbon-microball, high density isotropic carbon/graphite material and performance liquid chromatographic column.
In one embodiment, the present invention is for example, by using following technical solution:
The invention discloses a kind of device and method for continuously preparing micron size carbosphere, including cavity, crucible,
Feed inlet, ring heater, piezoelectricity gear unit, nanopore device, landing pipe, collecting chamber, agitating unit, vacuum unit and water cooling
Unit.The present invention devises a kind of device for preparing monodisperse carbosphere using stirring and impulse action high-efficiency and continuous simultaneously, earthenware
The carbon material melted in crucible is evenly dispersed under the action of stirring blade, is sprayed by way of pulse from crucible bottom aperture later
It shoots out, forms carbosphere by no container process of setting.The carbosphere prepared with this method has particle diameter distribution equal
The advantages that one, sphericity is high, with high purity.
In a preferred embodiment, the present invention is for example, by using following technical solution:
A kind of device continuously preparing micron size carbosphere, including cavity, crucible (reaction chamber), annular-heating
Device, piezoelectricity gear unit, nanopore device, landing pipe, collecting chamber, agitating unit, vacuum unit and water cooling unit；Wherein:
The crucible is located in the cavity, there is the ring heater, the piezoelectricity gear unit around the crucible
Above the crucible, the crucible bottom has centre bore to be connected with the nanopore device, and the landing pipe is by the cavity
It is connected with the collecting chamber, the agitating unit is located inside the crucible.
The ring heater is resistance heater, and the agitating unit includes blade, and the blade rotates horizontally, described
Blade axle center and the drive rod axle center are on a vertical line.
The feed inlet by the crucible melt and raw material to be added connect, guarantee in the crucible that melt amount is protected
It holds constant.
The micropore size range of the nanopore device is between 0.05-0.8mm.
The contact angle of the material of the crucible and the carbon melt being added after solvent is greater than 90 degree, and the two does not react.
The cavity is equipped with the watch window recorded in real time for high-speed camera.
The present invention also provides a kind of methods that micron size carbosphere is continuously prepared using aforementioned device, including such as
Lower step:
(1) it pre-processes: carbon material uniformly being mixed with a certain amount of solvent in the molten state, the standby to cool down
With.
(2) stirring and pulse collective effect: carbon material is heated to certain temperature fusing, keeps the temperature 5-10min, unlatching is stirred
Unit is mixed, wait be uniformly dispersed.Preset pulse signal is set, the upper and lower past of the state modulator drive rod of pulse waveform regulated is passed through
Multiple movement, sprays carbon material from nanopore device and forms drop.
(3) continuity: raw material to be added is continuously added from feed inlet, guarantees that the amount of melt in crucible is constant.
(4) form microballoon: drop solidifies to form microballoon in landing Guan Zhongwu container, then falls in collecting chamber.
(5) after reaction, device is closed, monodisperse carbosphere is taken out.
The piezoelectricity gear unit includes piezoelectric ceramics, thermal insulation board and drive rod, the pulse signal wave of the piezoelectric ceramics
Shape is trapezoidal wave, and the rising time of the trapezoidal wave is 50-500 μ s, keeps along the time being 500-5000 μ s, failing edge time
For 500-5000 μ s.
To a rated differential head inside and outside crucible, control in 1-10Kpa.
Before unlatching, the blade of agitating unit first works 10-30min the piezoelectricity gear unit, keeps melt dispersion equal
It is even.
It fits through the method for the present invention and continuously prepares micron size carbosphere, the micron size carbon being prepared
The sphericity of microballoon is distributed S50≥0.94。
Explanation is further elaborated to technical solution of the present invention below by way of specific embodiment combination attached drawing.It should be noted that
, following specific embodiments are only as example, the scope of protection of the present invention is not limited thereto.
Raw material is fitted into crucible, fire door is closed, then crucible chamber and cavity is vacuumized, then pass through annular-heating
Device heats crucible, and carbon material is fused into melt, then starts agitating unit, and blade horizontal rotation keeps melt mixed equal
Even, then give piezoelectricity gear unit input pulse signal, piezoelectricity gear unit drives drive rod to be pressed down against melt, and melt is from micropore
It ejects to form drop in the micropore of component, drop is frozen into mono-dispersion microballoon in landing Guan Zhongwu container.Meanwhile raw material from
Feed inlet is continuously added, and guarantees that the amount of melt in crucible is constant.
Embodiment 1
The mono-dispersion microballoon of graphite is prepared, graphite raw material is fitted into crucible 6 of the customization with centre bore first, charge weight is big
About the 1/2 of 6 capacity of crucible；Then nanopore device 10 is fixed on to the underface of crucible 6, guarantee the centre bore of crucible 6 with it is micro-
Hole is in same vertical line；Drive rod 5 is fixed on right above 6 centre bore of crucible, thermocouple temperature measuring apparatus is loaded onto, closes fire door
9；First low vacuum will be taken out simultaneously inside and outside crucible 6 with mechanical pump, reaches 4Pa hereinafter, being then turned on to resistance unit vacuum meter registration
Molecular pump reaches 8 × 10 to pumping high vacuum inside and outside crucible 6, to ionization module vacuum meter registration-3Pa is vacuumized hereinafter, can close
Unit；Snorkel 13 (the first snorkel) and lower snorkel 19 (the second snorkel) in opening, at the same it is logical to crucible 6 and cavity 18
Enter high purity inert gas Ar；The pressure difference between crucible 6 and cavity 18 is set to reach 50Kpa by differential pressure sensor；Then ring is opened
Shape heater 8 heats the raw material in crucible 6, keeps the temperature 15min after reaching predetermined temperature；Later on agitating unit, leaf
Piece 7 rotates horizontally, and work 20min is sufficiently mixed melt 17 uniformly；Then the pulse of trapezoidal wave is inputted to Piexoelectric actuator 1
Signal, Piexoelectric actuator 1 drive drive rod 5 to pump, melt 17 are typed it out from micropore, form drop
20；It is constantly added in crucible 6 after melting sources to be added from feed inlet 3, guarantees that the amount of melt in crucible is constant；Drop 20 is dropping
It falls in pipe 21 and solidifies to form microballoon without container, fall in collecting chamber 12；After due-in collection, stop ring heater 8 and blade
7, feed inlet 3 is closed, drive rod 5 is risen, secondly closes upper snorkel 13, lower snorkel 19；After waiting 30min, close cold
But collecting chamber 12 is opened in water 15, takes out monodisperse carbosphere.
Embodiment 2
The mono-dispersion microballoon of charcoal is prepared, charcoal raw material is fitted into crucible 6 of the customization with centre bore first, charge weight is big
About the 3/4 of 6 capacity of crucible；Then nanopore device 10 is fixed on to the underface of crucible 6, guarantee the centre bore of crucible 6 with it is micro-
Hole is in same vertical line；Drive rod 5 is fixed on right above 6 centre bore of crucible, thermocouple temperature measuring apparatus is loaded onto, closes fire door
9；First low vacuum will be taken out simultaneously inside and outside crucible 6 with mechanical pump, reaches 4Pa hereinafter, being then turned on to resistance unit vacuum meter registration
Molecular pump reaches 8 × 10 to pumping high vacuum inside and outside crucible 6, to ionization module vacuum meter registration-3Pa is vacuumized hereinafter, can close
Unit；Snorkel 13 and lower snorkel 19 in opening, while high purity inert gas Ar is passed through to crucible 6 and cavity 18；Pass through pressure
Poor inductor makes the pressure difference between crucible 6 and cavity 18 reach 45Kpa；Then ring heater 8 is opened to the raw material in crucible 6
It is heated, keeps the temperature 15min after reaching predetermined temperature；Later on agitating unit, blade 7 rotate horizontally, and work 20min makes to melt
Body 17 is sufficiently mixed uniformly；Then the pulse signal of trapezoidal wave is inputted to Piexoelectric actuator 1, Piexoelectric actuator 1, which drives, to be passed
Lever 5 pumps, and melt 17 is typed it out from micropore, forms drop 20；From charging after melting sources to be added
It is constantly added in crucible 6 in mouth 3, guarantees that the amount of melt in crucible is constant；Drop 20 solidifies to be formed without container in landing pipe 21
Microballoon is fallen in collecting chamber 12；After due-in collection, stop ring heater 8 and blade 7, feed inlet 3 is closed, by drive rod 5
It rises, secondly closes upper snorkel 13, lower snorkel 19；After waiting 30min, cooling water 15 is closed, opens collecting chamber 12, is taken out
Monodisperse carbosphere.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
Describe in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in protection of the invention
Within the scope of.
Claims (10)
1. a kind of device for preparing monodisperse carbosphere characterized by comprising
Reaction chamber, top are equipped with feed inlet；
Reactor, is arranged inside reaction chamber and its bottom is equipped with centre bore, and reactor is used for fused materials；
Piezoelectricity gear unit, is arranged in inside reactor and one end can squeeze out the material in reactor out of centre bore；
Micropore unit, centrally disposed hole bottom, for controlling the size for forming particle；
Heating unit is used for heating response device；And
Vacuum unit, to provide pressure difference inside and outside reactor.
2. the device according to claim 1 for preparing monodisperse carbosphere, which is characterized in that
The inside reactor is equipped with the agitating unit for stirring material；
Preferably, the agitating unit includes blade；The blade rotates horizontally；The axle center of the blade and the piezoelectricity pass
The axle center of moving cell is on a vertical line；
Preferably, the reaction chamber side wall is equipped with gas vent；It is equipped in gas vent in the connection reaction chamber to shield
The vent valve in portion and outside atmosphere.
3. the device according to claim 1 for preparing monodisperse carbosphere, which is characterized in that
Contact angle between the reactor and micropore unit and melt is all larger than 90 degree, and the two does not react；
Preferably, the reactor includes crucible；
Preferably, the reaction chamber is equipped with the watch window for real-time observing response device.
4. the device according to claim 1 for preparing monodisperse carbosphere, which is characterized in that
The piezoelectricity gear unit includes piezoelectric ceramics, thermal insulation board and drive rod, and the thermal insulation board is arranged above drive rod, institute
Stating drive rod bottom end can protrude into the centre bore in reactor；
Preferably, the aperture of the micropore unit is 0.05-0.8mm；
Preferably, the heating unit includes heater；
As further preferred, the heater is annular；
As further preferred, the heater is resistance heater；
Preferably, the vacuum unit includes:
First snorkel is arranged in reactor head, for adjusting the pressure of inside reactor；
Second snorkel is arranged on reaction chamber side wall, for adjusting the pressure inside reaction chamber；And
Third snorkel is connected to the first snorkel and the second snorkel, and third snorkel is equipped with for adjusting reactor
The third breather pipe valve of pressure difference between reaction chamber.
5. the device according to claim 1 for preparing monodisperse carbosphere, which is characterized in that
The device for preparing monodisperse carbosphere further includes the collector unit for collecting product, and collector unit setting is being reacted
Below room；
Preferably, the collector unit includes landing pipe and collecting chamber, landing pipe is arranged between reaction chamber and collecting chamber, system
The monodisperse carbosphere got ready enters the collecting chamber from landing pipe；
Preferably, the device for preparing monodisperse carbosphere further includes the water cooling unit for cooling down reaction chamber, the water
Cold unit includes cooling water intake and cooling water outlet；
Preferably, the device for preparing monodisperse carbosphere further includes the branch that reaction chamber bottom is arranged in and plays a supportive role
Frame.
6. a kind of obtain the preparation method of micron size carbosphere using any one of such as claim 1-5 described device,
It is characterized by comprising the following steps:
(1) the molten condition carbon material in reactor is mixed with solvent, obtains carbon material one after cooling；
(2) it is sprayed from micropore unit under the action of piezoelectricity gear unit after melting carbon material one and forms drop, drop is cold
But microballoon is formed afterwards to get the micron size carbosphere is arrived.
7. preparation method according to claim 6, which is characterized in that
The internal and external pressure difference of reactor described in step (1) is 1-10Kpa；
Preferably, forming the process of drop described in step (2) specifically: preset pulse letter is arranged after melting carbon material
Number, by pumping for the state modulator drive rod of pulse waveform regulated, carbon material is made to spray shape from nanopore device
At drop；
As further preferred, pulse signal described in step (2) is trapezoidal wave, and the rising time of the trapezoidal wave is
50-1000 μ s keeps being 500-5000 μ s along the time, and the failing edge time is 500-5000 μ s；
Preferably, the method for the cooling of drop described in step (2) includes natural cooling in landing pipe；
Preferably, the sphericity for the micron size carbosphere being prepared in step (2) is distributed S50≥0.94。
8. preparation method according to claim 6, which is characterized in that
Incubation step is carried out after the fusing step of carbon material one described in step (2)；
Preferably, being stirred step again after one incubation step of carbon material in step (2)；
As further preferred, the whipping step specifically: the piezoelectricity gear unit is before unlatching, the leaf of agitating unit
Piece first works 10-30min, keeps melt dispersion uniform；
Preferably, the process of the preparation method has continuity, the continuity is to make to react by continuous adding raw materials
The amount of indoor melt remains unchanged realization.
9. a kind of be prepared or using such as any one of claim 6-8 using device as described in any one in claim 1-5
The monodisperse carbosphere that the preparation method obtains.
10. electrode material, isotropic carbon/stone of the monodisperse carbosphere as claimed in claim 9 in lithium ion secondary battery
Application in the packing material field of ink material and performance liquid chromatographic column.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116272645A (en) * | 2023-05-11 | 2023-06-23 | 中建环能科技股份有限公司 | Sewage denitrification carrier preparation system and preparation method |
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| JP2011084429A (en) * | 2009-10-15 | 2011-04-28 | Osaka Gas Co Ltd | Carbon material, and method for producing carbon material and graphite material |
| CN102363524A (en) * | 2011-06-30 | 2012-02-29 | 江苏国正新材料科技有限公司 | Preparation method of high-efficiency carbon material hollow spheres |
| CN106488819A (en) * | 2014-06-20 | 2017-03-08 | 维洛3D公司 | Equipment, system and method for 3 D-printing |
| CN104550988A (en) * | 2015-01-28 | 2015-04-29 | 大连理工大学 | Method and device for preparation of superfine spherical metal powder on basis of uniform droplet spray method |
| CN107824793A (en) * | 2017-10-31 | 2018-03-23 | 中国科学院过程工程研究所 | A kind of device and method for preparing ultra-fine single dispersion metal microballoon |
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| CN116272645A (en) * | 2023-05-11 | 2023-06-23 | 中建环能科技股份有限公司 | Sewage denitrification carrier preparation system and preparation method |
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