CN105800545B - A method of removing preparation two-dimensional material - Google Patents
A method of removing preparation two-dimensional material Download PDFInfo
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- CN105800545B CN105800545B CN201610154564.XA CN201610154564A CN105800545B CN 105800545 B CN105800545 B CN 105800545B CN 201610154564 A CN201610154564 A CN 201610154564A CN 105800545 B CN105800545 B CN 105800545B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
- B81C1/0038—Processes for creating layers of materials not provided for in groups B81C1/00357 - B81C1/00373
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
A method of removing preparation two-dimensional material belongs to two-dimensional material technical field.The dispersion liquid of stratified material is passed through supergravity reactor, under the conditions of hypergravity, the removing certain time of stratified material " from top to bottom " is obtained into the two-dimension nano materials of single-layer or multi-layer in certain temperature and certain liquid phase environment.The present invention is had many advantages, such as simple process, is widely used, be easy to scale amplification using high-gravity technology liquid phase removing preparation two-dimensional material.
Description
Technical field:
The present invention relates to a kind of preparation methods of two-dimension nano materials, particularly prepare two wieners using liquid phase stripping method
Rice material, also belongs to the application that high-gravity technology prepares two-dimension nano materials field in removing, belongs to two-dimensional material technical field.
Background technique:
Two-dimension nano materials be space only have it is one-dimensional in the another bidimensional of nanoscale be not nanoscale substance, by
In the quantum size effect of nanometer phase, small-size effect, skin effect, macro quanta tunnel effect etc., have them
Different from original property, it is with a wide range of applications in numerous areas.
There are many method for preparing two-dimension nano materials, can be summarized as physical method, chemical method and physical-chemical process.Chemical method master
It to be chemical synthesis, at high cost, properties of product are uncontrollable.Physical-chemical process is mainly intercalation stripping method and electrochemical stripping
Method, ion insertion method are the highest method of current charge stripping efficiency, wide adaptation range.Its shortcomings that is that time-consuming, preparation condition is stringent
And remove the aggregation that intercalator easily leads to two-dimensional material.Electrochemical stripping method easily causes the variation of material composition, extensive to make
It is standby also more difficult.Physical method mainly includes solid phase stripping method and liquid phase stripping method.Solid phase stripping method is mainly mechanical stripping method, machine
Tool stripping method is the weak Van der Waals force that molecule interlayer is overcome by the viscous adhesion of adhesive tape, to achieve the purpose that removing.
This method is time saving, laborsaving, simple, quick, and not only charge stripping efficiency is high, and the two dimension that mechanical stripping method is prepared by this method
Material has original crystal structure.However the shortcomings that this method is that yield is extremely low, it is difficult to large scale preparation and poor repeatability.
Liquid phase stripping method mainly has organic solvent stripping method, ionic liquid stripping method, surfactant auxiliary water phase stripping method (such as liquid phase
Ultrasonic method) and mixed solvent stripping method.Liquid phase ultrasonic method is that stratified material powder is distributed in dispersing agent, is aided with ultrasonic hand
Section removes body phase powder at two-dimensional material, although this method extent of exfoliation and charge stripping efficiency are slightly below first two method, it
The characteristics of easy to operate, convenient and suitable high-volume, large-scale production is all the key that attract people.Especially recently in relation to water
The successful document report of removing preparation two-dimensional material under the conditions of phase, before the industrial applications for more having shown this preparation method
Scape.This method using organic solvent, the aqueous solution of surfactant, aqueous solutions of polymers and ionic liquid etc. as dispersion liquid,
Under the conditions of hypergravity, by stratified material remove at two-dimensional material, and can be uniform and stable be present in dispersion liquid.This method without
Need to pre-process directly liquid phase to remove, and have loose preparation condition, easy to operate, wide adaptation range and suitable large-scale production
The features such as.
Cross_flow rotating packed bed is a kind of technology of novel strengthening transfer process, is generated by high-speed rotating bed body
Powerful centrifugal force field simulates Elevated Gravity, more empty media under Elevated Gravity of solution-air, liquid-liquid and liquid-solid 2 phase or
In duct flow contact, generate huge shearing force can by liquid tear at micron to nano grade liquid film, brin and drop,
Microcosmic mixing and mass transport process are greatly strengthened.There is equipment size substantially to reduce with quality for it;Molecular mixing and transmitting
Process is highly enriched;Residence time of the material in equipment is extremely short (0.1~1.0s);It is easily operated, driving and parking, maintenance and repair
The advantages that facilitating.Hypergravity process intensification technology has been widely used in the multiphase mistake for needing to be strengthened to alternate transmittance process
Journey and need in phase or it is quasi- it is homogeneous in microcosmic mixed intensified mixing and reaction process, have been achieved with industrialization.Currently, by overweight
The rotary packed bed patent for being applied to removing preparation nano material of power, patent " a kind of gravity Method only delivered with laboratory
(application number: 201310645908.3), this method is made by carrying out pretreating graphite to graphite to the method for preparing graphene "
The interlamellar spacing of graphite increases, and later in high-gravity rotating bed middle removing pretreating graphite, obtains graphene.And by high-gravity technology
For being prepared in two-dimension nano materials by raw material directly removing of unpretreated stratified material, have not been reported.
Summary of the invention
The present invention provides a kind of method of novel removing preparation two-dimensional material, being capable of stripped laminar simple substance, transition metal
The stratified materials such as sulfide, transition metal oxide, obtain two-dimension nano materials.
The invention discloses a kind of methods of removing preparation two-dimensional material, which is characterized in that including process below and step
It is rapid:
Stratified material powder is weighed, is distributed in dispersion liquid, at a certain temperature, is passed through rotating packed bed reactor
In, it removes 0.5~10 hour, by changing the conditions such as hypergravity level and splitting time to change removing journey in stripping process
Degree, then by centrifuge separation, supernatant is the stable dispersions containing two-dimensional material.Dispersion liquid is filtered by miillpore filter
Two-dimensional material powder body material is obtained with freeze-drying.
The concentration of dispersion liquid is preferably standard with the dispersion performance to stratified material.
The dispersion liquid of stratified material of the present invention is according to common configuration method.Dispersion liquid has been configured first, then
It weighs stratified material powder to pour into configured dispersion liquid, stir evenly.Wherein:
Dispersion liquid can be liquid mixture or single liquid.
When dispersion liquid is mixture, dispersing agent therein are as follows: organic solvent such as NMP, isopropanol etc., surfactant such as gallbladder
Sour sodium, Qula logical, neopelex, lauryl sodium sulfate etc., polymer such as polyvinyl alcohol, polyethylene glycol, dispersion
Medium is water.
It can be water, organic solvent or ionic liquid such as 1- butyl -3- methylimidazole six when dispersion liquid is single liquid
Fluorophosphate, 1- butyl -3- methyl imidazolium tetrafluoroborate.Because different stratified materials surface nature and crystal structure not
Together, used dispersant is different, and concentration is also different, can be selected as needed.
The stratified material includes: graphite, molybdenum disulfide, boron nitride, kaolin, sericite, montmorillonite.
Rotating packed bed reactor of the present invention is the hypergravity swinging bed device having disclosed, including filler
The forms such as bed, deflector type helical duct rotating packed bed reactor (application reference number 91109255.2,91111028.3,
01268009.5,200520100685.3,02114174.6,200510032296.6), preferred cross_flow rotating packed bed.
Hypergravity level of the present invention refers to the centrifugal acceleration that rotor rotation generates in hypergravity swinging bed device
Size, usually indicated with the multiple of gravity acceleration g, it is main related with the revolving speed of rotor and the internal-and external diameter of rotor.Hypergravity
Horizontal grIt can be indicated with following formula:
In formula: n is rotor revolving speed per minute.
r1、r2The respectively inside and outside diameter of rotor.
Hypergravity level and splitting time of the invention is according to the size and concentration control of required two-dimensional material nanoscale twins
System is in certain range, and to guarantee to obtain, lamella is uniform, satisfactory two-dimensional material.Experimental result of the invention is, one
Determine in range, hypergravity level is higher, splitting time is longer, and the size of obtained two-dimensional material is smaller, and concentration is higher.
Temperature of the present invention is between 1-100 degrees Celsius.Splitting time is between 0.5-10 hours.Hypergravity is horizontal
For 100-2000g.
Traditional vacuum separation, miillpore filter suction filtration and freeze-drying of the present invention use conventional method.
Two-dimensional material prepared by the present invention is the nanometer sheet of single layer, two layers or few layer.
Of the invention is mainly characterized by: the dispersion liquid of stratified material is passed through supergravity reactor, under the conditions of hypergravity,
The removing certain time of stratified material " from top to bottom " is obtained into the two of single-layer or multi-layer in certain temperature and certain liquid phase environment
Dimension nano material.It is available not destroy that crystal structure, concentration is higher and the two-dimensional material of dispersion stable after the completion of removing,
Be conducive to practical application.The present invention can prepare most of two-dimensional material, such as graphene, two-dimentional molybdenum disulfide, nanometer kaolinite
Soil, nm-class boron nitride etc., and simple process, it is at low cost convenient for operation.The present invention is using the removing preparation of high-gravity technology liquid phase
Two-dimensional material has many advantages, such as simple process, is widely used, and is easy to scale amplification.
Detailed description of the invention
Fig. 1 outer circulation cross_flow rotating packed bed schematic diagram;
The names of the parts are as follows: 1. pedestals;2. motor;3. liquid outlet;4. bolt;5. cavity;6. gas access;7. spiral shell
Bolt;8. cavity gland;9. sealing;10. StoreFront formula liquid distribution trough;11. honeycomb duct type liquid distribution trough;12. gas vent;
13. bolt;14. reservoir;Filler core cylinder;16. gland;17. split drum type brake liquid re-distributor;18. filler;19.
Triangular pyramidal ring;20. turntable;21. bolt;22. sealing;23. key;24. bolt.
The rotary packed bed schematic diagram of recycle super-gravity in Fig. 2;
All parts title are as follows: 1. feed inlets;2. packing layer;3. cavity;4. discharge port;5. rotor;6. washing mouth;7. row
Port;8. temperature control collet;9. air inlet;10. liquid lifting unit;11. discharge port switchs.
1 UV, visible light spectrophotometric analysis figure of Fig. 3 embodiment;
1 scanning electron microscope of Fig. 4 embodiment.
The scanning electron microscope of Fig. 5 embodiment 8.
The scanning electron microscope of Fig. 6 embodiment 11.
The scanning electron microscope of Fig. 7 embodiment 12.
Specific embodiment
Invention is further explained with reference to the accompanying drawing, but the present invention is not limited to following embodiments.
The present invention can use outer circulation mode of operation, it may be assumed that the suspension of material to be stripped is placed in reservoir, by compacted
Dynamic pump is transported in hypergravity rotation packed column reactor, then is flowed back into storage tank by discharge port, recycles repeatedly, suspension warp
Later treatment process obtains the supernatant of two-dimensional material.The present invention can also within circulate operation mode, the i.e. suspension of release liner
Liquid is placed directly in hypergravity rotation packed column reactor, suspension continuous recirculation gas stripper wherein, then work after post treatment
Skill obtains the supernatant of two-dimensional material.
Embodiments of the present invention are further illustrated by implementing process as shown in Figure 1, 2:
As shown in Figure 1, the suspension of the bulk stratified material configured as needed is added in reservoir 14, reaction process
In, suspension agitated device premix stirs evenly, suspension is transported to honeycomb duct type liquid distribution trough 11 by peristaltic pump, and by
Its inner edge for being uniformly sprayed onto packing layer is flowed from inner edge to outer rim under the influence of centrifugal force, in packing layer 18, stratiform
Material granule is mainly by shearing force by the removing of " from top to bottom ".The work of two-dimensional nano piece under being stripped in dispersing agent
It is uniformly distributed in solution with lower.Two-dimensional material can be obtained in technique after post treatment.According to the dense of required two-dimensional material
The size of degree and lamella, setting recirculation gas stripper time, hypergravity are horizontal.
As shown in Fig. 2, the suspension of the stratified material configured as needed is added to hypergravity rotation filler by feed inlet 1
In bed reactor, start rotary drill reactor, suspension is drawn into packing layer 2, stratified material particle master by liquid lifting unit 10
It will be by shearing force by the removing of " from top to bottom ".Two-dimensional material can be obtained in technique after post treatment.According to required two
The concentration of material and the size of lamella are tieed up, setting recirculation gas stripper time, hypergravity are horizontal.
The packing layer of cross_flow rotating packed bed of the present invention includes, but are not limited to: the silk of metal material and nonmetallic materials
Net, porous plate, corrugated plating, foamed material or structured packing, the silk screen of preferred metal materials.
Embodiment
It is the non-limiting example of present invention preparation two-dimensional material below.The present invention should also include, without departing substantially from the present invention
The various changes that those of ordinary skill in the art are able to carry out under conditions of range.
Embodiment 1
The molybdenum disulfide powder 14g that average particle size is 1.5 μm is weighed as shown in Figure 1: to be distributed in the dispersion liquid of 350ml,
Dispersion liquid is the Qula water flowing solution of 13mg/mL.The dispersion liquid of molybdenum disulfide powder is added in reservoir 14, premix is uniform
Afterwards, start peristaltic pump and cross_flow rotating packed bed, raw material are sprayed onto packing layer 18 through honeycomb duct type liquid distribution trough 11
Edge, adjusting reactor hypergravity level be 1386g, exfoliation temperature be room temperature (25 DEG C), after continuously removing 10h, by from
The isolated supernatant containing two-dimentional molybdenum disulfide of the heart.By ultraviolet-uisible spectrophotometer and scanning electron microscope analysis, such as scheme
3, it is sheet and uniform in size, concentration is being 0.40mg/mL, and length is 260 rans, and the average number of plies is 5 layers.
Embodiment 2: in addition to following variations, remaining process is the same as embodiment 1.Splitting time is 5h, gained two dimension molybdenum disulfide
Concentration are as follows: 0.16mg/mL, length are 314 rans, and the average number of plies is 6 layers.
Embodiment 3: in addition to following variations, remaining process is the same as embodiment 1.Bulk stratified material is selected as boron nitride, dispersion liquid
For ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate, gained two dimension boron nitride concentration are as follows: 0.30mg/mL, length are
290 rans, the average number of plies are 5 layers.
Embodiment 4: in addition to following variations, remaining process is the same as embodiment 1.Dispersion liquid is the water-soluble of polymer polyethylene glycol
Liquid, concentration 10mg/mL, gained two dimension molybdenum disulfide concentration are as follows: 0.17mg/mL, length are 300 rans, the average number of plies 4
Layer.
Embodiment 5: in addition to following variations, remaining process is the same as embodiment 1.Cross_flow rotating packed bed is selected as interior circulation (such as
Fig. 2), hypergravity level is 347g.Gained two dimension curing molybdenum sheet concentration is 0.24mg/mL.
Embodiment 6: in addition to following variations, remaining process is the same as embodiment 1.Exfoliation temperature is 50 DEG C.Gained two dimension curing
Molybdenum concentration are as follows: 0.53mg/mL, length are 230 rans, and the average number of plies is 4 layers.
Embodiment 7: in addition to following variations, remaining process is the same as embodiment 1.Dispersion liquid is water-soluble using the sodium taurocholate of 5mg/mL
Liquid.Gained two dimension molybdenum disulfide concentration are as follows: 0.53mg/mL, length are as follows: 255nm or so, the average number of plies are 4 layers.
Embodiment 8
As shown in Figure 1: by metering, the suspension for the mica that configuration 400mL mass fraction is 5%, dispersing agent is deionization
Water.Suspension obtained is poured into reservoir.Wherein adjusting reactor hypergravity level is 347g, and exfoliation temperature is room temperature 25
DEG C, splitting time 10h.Obtain 0.80 μm of length or so of mica sheet, such as Fig. 4.
Embodiment 9: in addition to following variations, remaining process is the same as embodiment 8.Splitting time 5h, obtained product is through scanning electricity
The sericite piece that mirror analysis is 1.04 μm of average length.
Embodiment 10: in addition to following variations, remaining process is the same as embodiment 8.Hypergravity level is selected as 1386g.Obtained production
The sericite piece that product are 0.51 μm of average length through scanning electron microscope analysis.
Embodiment 11: by metering, the kaolinic suspension that configuration 400mL mass fraction is 5%, dispersing agent is deionization
Water.Suspension obtained is poured into reservoir.Wherein adjusting reactor hypergravity level is 347g, and exfoliation temperature is room temperature 25
DEG C, splitting time 10h.Obtained product is through scanning electron microscope analysis are as follows: the kaolin piece of 147.34nm, such as Fig. 5.
Embodiment 12:
It is as shown in Figure 2: by metering, to take 20g graphite powder, be scattered in the N-Methyl pyrrolidone (NMP) of 400mL, stir
12h is mixed, the NMP suspension of graphite is made.Suspension obtained is added to the chamber of cross_flow rotating packed bed by feed inlet 1
In body.Wherein adjusting reactor hypergravity level is 368g, and exfoliation temperature is room temperature (25 DEG C), splitting time 8h.Gained stone
Black alkene concentration is the supernatant of 0.17mg/mL, average 5 layers of the number of plies, such as Fig. 6.
Embodiment 13: in addition to following variations, remaining process is the same as embodiment 12.Exfoliation temperature is adjusted to 50 DEG C.Gained graphite
Alkene concentration is 0.20mg/mL, and length is 220 rans.
Embodiment 14: in addition to following variations, remaining process is the same as embodiment 12.Exfoliation temperature is adjusted to 90 DEG C.Gained graphite
Alkene concentration is 0.25mg/mL, and length is 220 rans.
Embodiment 15: in addition to following variations, remaining process is the same as embodiment 12.Dispersion liquid is changed to the sodium taurocholate of 0.5mg/mL
Aqueous solution.The concentration of gained graphene is 0.30mg/mL, and length is 200 rans.
Embodiment 16: in addition to following variations, remaining process is the same as embodiment 15.The 1- of 0.08mg/mL is added in dispersion liquid
Butyl -3- methylimidazole hexafluorophosphate, gained graphene concentration are 0.4mg/mL, and length is 180 rans.
Claims (6)
1. a kind of method of removing preparation two-dimensional material, which is characterized in that including process below and step:
Stratified material powder is weighed, is distributed in dispersion liquid, between 1-100 degrees Celsius, is passed through rotating packed bed reactor
In, it removes 0.5~10 hour, by change hypergravity level and splitting time condition to change extent of exfoliation in stripping process,
Then by centrifuge separation, supernatant is the stable dispersions containing two-dimensional material;Hypergravity level is 100-2000g.
2. a kind of method of removing preparation two-dimensional material described in accordance with the claim 1, which is characterized in that dispersion liquid passes through micropore
Filter membrane filters and freeze-drying obtains two-dimensional material powder body material.
3. a kind of method of removing preparation two-dimensional material described in accordance with the claim 1, which is characterized in that dispersion liquid is mixed for liquid
Close object or single liquid;When dispersion liquid is mixture, dispersing agent therein is selected from: organic solvent, surfactant, and dispersion is situated between
Matter is water;
It is water, organic solvent or ionic liquid when dispersion liquid is single liquid.
4. a kind of method of removing preparation two-dimensional material described in accordance with the claim 3, which is characterized in that organic solvent is selected from
NMP or isopropanol, surfactant are sodium taurocholate, Qula logical, neopelex or lauryl sodium sulfate, polyethylene
Alcohol, polyethylene glycol;
Ionic liquid is 1- butyl -3- methylimidazole hexafluorophosphate or 1- butyl -3- methyl imidazolium tetrafluoroborate.
5. a kind of method of removing preparation two-dimensional material described in accordance with the claim 1, which is characterized in that stratified material is stone
Ink, molybdenum disulfide, boron nitride, kaolin, sericite or montmorillonite.
6. a kind of method of removing preparation two-dimensional material described in accordance with the claim 1, which is characterized in that high-gravity rotating bed anti-
Answering device is the rotating packed bed reactor of packed bed or deflector type helical duct form.
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