CN104843679B - The method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping - Google Patents
The method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping Download PDFInfo
- Publication number
- CN104843679B CN104843679B CN201510156136.6A CN201510156136A CN104843679B CN 104843679 B CN104843679 B CN 104843679B CN 201510156136 A CN201510156136 A CN 201510156136A CN 104843679 B CN104843679 B CN 104843679B
- Authority
- CN
- China
- Prior art keywords
- micro crystal
- crystal graphite
- suspension
- precipitation
- revs
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The present invention relates to a kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, belong to grapheme material preparing technical field.This method is：By micro crystal graphite powder and N methyl pyrrolidones, N, N dimethylformamides, N, more than one in N dimethyl acetamides and butyrolactone are well mixed with the mixed solution of o-dichlorohenzene, and micro crystal graphite concentration is 1~30mg mL‑1；Load closed container and be heated to 180~210 DEG C of stirring >=24h；With the lasting processing >=10min of 80~100W ultrasounds in 0~5 DEG C；Centrifuge and collect precipitation；It is distributed in methanol, ethanol, isopropanol or normal propyl alcohol, centrifuges and collect precipitation；It is distributed in water, centrifuges and collect precipitation；It is distributed in water, solid is frozen into≤10min, is dried in vacuo, obtains micro crystal graphite alkene.This method cost of raw material is low, and grade is high, and reserves are big, prepares simply, with low cost, can amplify production.
Description
Technical field
The present invention relates to a kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, belong to grapheme material
Preparing technical field.
Background technology
Graphene, is to be interconnected to hexagonal gridding between a kind of individual layer laminated structure being made up of carbon atom, carbon atom.
Graphene possesses theoretical value 2630m2g-1Bigger serface, 200000cm2V-1s-1High electron mobility, excellent printing opacity
Property and mechanical strength so that graphene in electronic device (such as：Field-effect transistor, transparency electrode, solar cell etc.), energy storage
Device is (such as：Ultracapacitor, lithium ion battery etc.), the neck such as energy conversion device (such as hydrogen storage, photoelectric conversion, fuel cell)
Domain is widely applied, and causes the extensive concern of global scientific research personnel.
Matter of utmost importance in the research and application of graphene is exactly the preparation of graphene.Originally, graphene is by machinery
Stripping method is obtained from highly oriented pyrolytic graphite, but the amount of graphene that methods described is obtained is considerably less, it is difficult to reach some sections
Grind and practical application purpose.At present, preparing the method for graphene mainly includes：Epitaxial growth method, electrochemical process, You Jihe
Cheng Fa, chemical vapour deposition technique and oxidation-reduction method etc..Wherein, oxidation-reduction method can realize prepared by batch, using the widest
It is general, but the defect obtained by oxidation-reduction method on graphene sheet layer is more, causes graphene partial properties to decline or lose, and system
Standby process complexity is cumbersome, and the cycle is long；Substantial amounts of strong acid and oxidant are needed to use during chemical oxidation and intercalation, pays higher
Cost, the nitrogen oxides produced in reacted acid pickle and course of reaction can cause environmental pollution.Except oxidation-reduction method
Outside, other prepare graphene method yield it is smaller, the basic research of small range is only applicable to, it is difficult to meet the need of actual production
Will.So far, also without that really can be adapted to the excellent process of industrialized production, this has become the application of limitation graphene,
The significant obstacle for hindering it to develop.
At present, the method for redox volume production graphene, using natural phaneritric crystalline flake graphite as raw material, in recent years I
State's high-quality crystalline flake graphite exhaustive exploitation.The grade of China's micro crystal graphite ore is high, reserves are big, but prepares stone by micro crystal graphite
The method of black alkene is rarely reported, and science research input is more short of.
The content of the invention
For defect present in prior art, peeled off it is an object of the invention to provide one kind by micro crystal graphite solvent heat
The method for preparing micro crystal graphite alkene, methods described preparation process is simple, with low cost, can amplify production.
The purpose of the present invention is realized by following technical scheme.
A kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step is as follows：
(1) micro crystal graphite powder is well mixed with solvent 1, obtains the suspension 1 of black, wherein, micro crystal graphite it is dense
Spend for 1mg mL-1~30mg mL-1；
Wherein, the solvent 1 is the mixed solution of organic reagent and o-dichlorohenzene, and the organic reagent is N- methylpyrroles
One or more of alkanone, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide and butyrolactone；It is preferred that organic reagent and neighbour two
The volume ratio of chlorobenzene is 4:1~1:3；The mixing is preferably first stirred, then ultrasonic disperse, the ultrasonic power be preferably 80W~
100W；
(2) suspension 1 for obtaining step (1) is fitted into closed container, is heated to 180 DEG C~210 DEG C and keeps described
Temperature, stirring reaction >=24h terminates, in the course of reaction, and the organic agent molecule in the solvent 1 carries out equal to graphite
Even intercalation, peel off, obtain the suspension 2 of black；
Wherein, the closed container should can prevent the corrosion of the suspension 1, can select polytetrafluoroethylene (PTFE) as interior
The reactor of lining；Stirring can be realized, preferably closed container bottom surface by adding magneton into the closed container with magnetic agitation
The diameter proportion of diameter and magneton is 2:1~5:1；Heating can be realized using baking oven；It is preferred that stirring reaction 24h~72h；
(3) suspension 2 for obtaining step (2) is cooled to after room temperature, and ultrasonically treated, ultrasonic work(is carried out in 0 DEG C~5 DEG C
Rate is 80W~100W, continues >=10min, obtains the suspension 3 of black；
Suspension 2 is cooled to after room temperature, can be carried out in ice-water bath ultrasonically treated；It is preferred that ultrasonically treated carried out several times,
Continue 10min~30min every time；
(4) suspension 3 for obtaining step (3) is centrifuged, and is collected lower sediment, is obtained precipitation 1；
It is preferred that the rotating speed of the centrifugation is 5000 revs/min~8000 revs/min, 10min~30min is centrifuged；
(5) precipitation 1 for obtaining step (4), which is distributed in solvent 2, forms homogeneous suspension 4, centrifuges, and collects lower floor
Precipitation, obtains precipitation 2；
The solvent 2 is methanol, ethanol, isopropanol or normal propyl alcohol；It is preferred that scattered with 100W~500W power ultrasonic
It is centrifuged after 30min~60min；It is preferred that the rotating speed of the centrifugation is 5000 revs/min~8000 revs/min,
Centrifuge 10min~30min；Preferred steps (5) are carried out >=2 times；
(6) precipitation 2 for obtaining step (5), which is distributed in water, forms homogeneous suspension 5, centrifuges, and collects lower floor and sinks
Form sediment, obtain precipitation 3；
It is preferred that the purity of water is water more than distilled water purity；It is preferred that disperseing 30min with 100W~500W power ultrasonic
It is centrifuged after~60min；It is preferred that the rotating speed of the centrifugation is 4000 revs/min~8000 revs/min, centrifugation
10min~30min；Preferred steps (6) are carried out >=2 times；
(7) precipitation 3 for obtaining step (6), which is distributed in water, forms homogeneous suspension 6, and suspension 6 is cold in≤10min
Solid is frozen into, then is dried in vacuo, micro crystal graphite alkene is obtained；
It is preferred that water is the water more than distilled water purity；It is preferred that ultrasonic disperse, ultrasonic power is 80W~100W, ultrasound
5min~10min；It is preferred to use liquid nitrogen to be freezed.
Beneficial effect
1. the invention provides a kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described letter
It is single, easy and reliable, meanwhile, green non-pollution, yield is high, and required equipment is simple, can mass produce；
2. the invention provides a kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described institute
Raw material micro crystal graphite cost is low, and grade is high, and China's storage level is enriched；During the chemical reagent that uses can reclaim profit
With, the supernatant liquor after being centrifuged in such as step (4) is recyclable, and the stripping as solvent 1 for next group micro crystal graphite is used,
Supernatant liquor after being centrifuged in step (5) is recyclable, is used as the solvent 2 in step (5)；
3. the invention provides a kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described is obtained
The number of plies of the micro crystal graphite alkene arrived is a small number of layer graphenes below 7 layers, is expected to be used as super light material, catalyst carrier, micro-nano
Electronic device, and energy storage and composite；
4. the invention provides a kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described makes
The chip of micro crystal graphite be less than crystalline flake graphite, with micro crystal graphite produce graphene not only by be greatly reduced graphene into
This, while will also make up market to small size, the demand of graphene with high specific surface；Solve graphene preparation side in the prior art
The method cycle is long, it is difficult to meet the shortcoming of industrialized production, while the advantage of the micro crystal graphite resource using China's abundant；
5. the invention provides a kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step
Suddenly temperature is 0 DEG C~5 DEG C in (3), can prevent temperature is too high micro crystal graphite alkene is reunited or is stacked again, step (5) purpose exists
In washing away the solvent 1 that is remained in suspension 4, step (6) purpose is to wash away the solvent 2 remained in suspension 5.
Brief description of the drawings
The photo for the black suspension 1 that Fig. 1 obtains for step (1) in embodiment 1.
Fig. 2 is the X-ray powder diffraction test result figure of the final product obtained in embodiment 1.
Fig. 3 is the scanning electron microscope diagram of the final product obtained in embodiment 1.
Fig. 4 is the transmission electron microscope figure of the final product obtained in embodiment 1.
Fig. 5 is that the resolution ratio of the final product obtained in embodiment 1 is 0.2nm transmission electron microscope figures.
Embodiment
The present invention, but not limited to this are described in detail with specific embodiment below in conjunction with the accompanying drawings.
In following examples, the baking oven is purchased from the BAO-50 type convection ovens for applying all triumphant experimental instruments and equipment limited.
Embodiment 1
A kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step is as follows：
(1) 35mg micro crystal graphite powder is weighed, is added in 35mL solvents 1, the solvent 1 is by 1-METHYLPYRROLIDONE and neighbour
Dichloro-benzenes is with volume ratio 1:1 mixes, and stirs 30min, then ultrasonically treated 30min, ultrasonic power is 80W, makes microlite
Ink is well mixed with solvent 1, obtains the suspension 1 of black, as shown in figure 1, wherein, the concentration of micro crystal graphite is 1mg mL-1；
(2) suspension 1 for obtaining step (1) is fitted into the reactor that 50mL basal diameters are 5cm, the reactor
Inner lining material is polytetrafluoroethylene (PTFE), and a diameter of 2.5cm magneton is put into reactor, and reactor is closed, is added in an oven
Heat is to 180 DEG C and keeps the temperature, and stirring reaction 24h obtains the suspension 2 of black；
(3) suspension 2 that step (2) is obtained in question response kettle is cooled to after room temperature, is transferred in beaker, in ice-water bath
Carry out ultrasonically treated 3 times, each ultrasonic power is 90W, continues 10min, obtains the suspension 3 of black；
(4) suspension 3 for obtaining step (3) is transferred in 15mL centrifuge tube, is carried out with 5000 revs/min of rotating speed
Centrifuge, centrifuge 10min, supernatant liquor is reclaimed, collect lower sediment, obtain precipitation 1；
(5) precipitation 1 for obtaining step (4) is distributed in 50mL absolute ethyl alcohol, is 100W ultrasounds point through ultrasonic power
Dissipate after 60min, be transferred in 50mL centrifuge tube, be centrifuged with 5000 revs/min of rotating speed, will after centrifugation 10min
Supernatant liquor is reclaimed, and collects lower sediment；Repeat it is described operation once, will this step collection lower sediment be distributed to 50mL
Absolute ethyl alcohol in, through ultrasonic power be 100W ultrasonic disperses 60min after, be transferred in 50mL centrifuge tube, with 5000 revs/min
The rotating speed of clock is centrifuged, and after centrifugation 10min, supernatant liquor is reclaimed, lower sediment is collected, obtains precipitation 2；
(6) precipitation 2 for obtaining step (5) is distributed in 50mL distilled water, is 100W ultrasonic disperses through ultrasonic power
After 60min, it is transferred in 15mL centrifuge tube, is centrifuged with 4000 revs/min of rotating speed, after centrifugation 10min, is outwelled
Supernatant liquor, collects lower sediment；Repeat the operation once, will the lower sediment of this step collection be distributed to 50mL steaming
In distilled water, after being 100W ultrasonic disperses 60min through ultrasonic power, it is transferred in 15mL centrifuge tube, with 4000 revs/min turn
Speed is centrifuged, and after centrifugation 10min, outwells supernatant liquor, collects lower sediment, obtain precipitation 3；
(7) precipitation 3 for obtaining step (6) is added in 5mL distilled water, and ultrasonic disperse 5min, ultrasonic power is 80W,
Obtain the aqueous solution of precipitation 3, the aqueous solution for precipitating 3 freeze in liquid nitrogen, then is dried in vacuo, vacuum for 8~
12MPa, obtains final product.
Final product is tested as follows：
(1) X-ray powder diffraction is tested：As a result it is as shown in Figure 2, it is seen that the spy that graphene sheet layer is stacked is occurred in that in Fig. 2
Levy diffraction maximum 25o, it is micro crystal graphite alkene to illustrate final product；
(2) Raman spectrum is tested：The ratio between the D peak intensities and G peak intensities of final product (I is understood from test resultD/IG)；D
Peak represents SP3The vibration absorption peak of the bonding model of hydridization carbon, such as：" C-C ", " C-O ", " C=O " etc., G peaks represent SP2Hydridization carbon
Bonding model vibration absorption peak, i.e.,：" C=C ", ID/IGValue for 0.11, G peak intensities it is larger, illustrate the knot of final product
Structure is not destroyed；Show that final product defect is less by Raman test result, quality is higher；
(3) Electron microscopy：SEM testing result is as shown in figure 3, transmission electron microscope is detected
As a result as shown in fig. 4, it can be seen that final product be tens nanometer to a few micrometers of lamellar structure；Randomly choose final product
On (a) point and (b) point carry out resolution ratio be 0.2nm transmission electron microscopes detect, as a result as shown in Figure 5, it is seen that finally produce
The lamella of thing (a) point is 7 layers, and the lamella of final product (b) point is 3 layers.
Embodiment 2
A kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step is as follows：
(1) weigh 9g micro crystal graphite powder, add in 1500mL solvents 1, the solvent 1 by DMF and
O-dichlorohenzene is with volume ratio 1:3 mix, and stir 30min, then ultrasonically treated 30min, ultrasonic power is 100W, makes crystallite
Graphite is well mixed with solvent 1, obtains the suspension 1 of black, wherein, the concentration of micro crystal graphite is 6mg mL-1；
(2) suspension 1 for obtaining step (1) is fitted into the reactor that 2000mL basal diameters are 15cm, the reaction
The inner lining material of kettle is polytetrafluoroethylene (PTFE), and a diameter of 3cm magneton is put into reactor, and reactor is closed, in an oven
It is heated to 210 DEG C and keeps the temperature, stirring reaction 72h obtains the suspension 2 of black；
(3) suspension 2 that step (2) is obtained in question response kettle is cooled to after room temperature, is transferred in beaker, in ice-water bath
Carry out ultrasonically treated 3 times, each ultrasonic power is 100W, continues 30min, obtains black suspension 3；
(4) suspension 3 for obtaining step (3) is transferred in 300mL centrifuge tube, and the rotating speed with 8000 revs/min enters
Row is centrifuged, and centrifuges 10min, supernatant liquor is reclaimed, and is collected lower sediment, is obtained precipitation 1；
(5) precipitation 1 for obtaining step (4) is distributed in 1000mL absolute methanol, is 500W ultrasounds through ultrasonic power
After scattered 30min, it is transferred in 300mL centrifuge tube, is centrifuged with 6000 revs/min of rotating speed, centrifuges 20min
Afterwards, supernatant liquor is reclaimed, collects lower sediment；Repeat the operation once, will the lower sediment collected of this step it is scattered
Into 1000mL absolute methanol, after being 500W ultrasonic disperses 30min through ultrasonic power, it is transferred in 300mL centrifuge tube, with
6000 revs/min of rotating speed is centrifuged, and after centrifugation 20min, supernatant liquor is reclaimed, lower sediment is collected, is sunk
Shallow lake 2；
(6) precipitation 2 for obtaining step (5) is distributed in 1000mL distilled water, is 500W ultrasounds point through ultrasonic power
Dissipate after 30min, be transferred in 300mL centrifuge tube, be centrifuged with 5000 revs/min of rotating speed, after centrifugation 20min,
Supernatant liquor is outwelled, lower sediment is collected；Repeat it is described operation once, will this step collection lower sediment be distributed to
In 1000mL distilled water, after being 500W ultrasonic disperses 30min through ultrasonic power, it is transferred in 300mL centrifuge tube, with 5000
Rev/min rotating speed be centrifuged, after centrifugation 20min, outwell supernatant liquor, collect lower sediment, obtain precipitation 3；
(7) precipitation 3 for obtaining step (6) is added in 20mL distilled water, ultrasonic disperse 10min, and ultrasonic power is
100W, obtains the aqueous solution of precipitation 3, and the aqueous solution for precipitating 3 freeze in liquid nitrogen, then is dried in vacuo, vacuum for 8~
12MPa, obtains final product.
Final product is tested as follows：
(1) X-ray powder diffraction is tested：As a result the characteristic diffraction peak 25 that graphene sheet layer is stacked is occurred in thato, illustrate final
Product is micro crystal graphite alkene；
(2) Raman spectrum is tested：The ratio between D peak intensities and G peak intensities of final product (I as can be known from the resultsD/IG)；D peaks generation
Table SP3The vibration absorption peak of the bonding model of hydridization carbon, such as：" C-C ", " C-O ", " C=O " etc., G peaks represent SP2Hydridization carbon into
The vibration absorption peak of key model, i.e.,：" C=C ", ID/IGValue for 0.13, G peak intensities it is larger, illustrate the structure of final product simultaneously
Do not destroy；Show that final product defect is less by Raman test result, quality is higher；
(3) Electron microscopy：, can from SEM testing result and transmission electron microscope testing result
It is tens nanometer to a few micrometers of lamellar structure with the final product seen；Randomly choose (a) point and (b) point on final product
Carry out resolution ratio to detect for 0.2nm transmission electron microscopes, as a result show the lamella of final product below 7 layers.
Embodiment 3
A kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step is as follows：
(1) 22.5g micro crystal graphite powder is weighed, is added in 750mL solvents 1, the solvent 1 is by DMA
With o-dichlorohenzene with volume ratio 1:2 mix, and stir 30min, then ultrasonically treated 30min, ultrasonic power is 100W, is made micro-
Spar ink is well mixed with solvent 1, obtains the suspension 1 of black, wherein, the concentration of micro crystal graphite is 30mg mL-1；
(2) suspension 1 for obtaining step (1) is fitted into the reactor that 1000mL basal diameters are 10cm, the reaction
The inner lining material of kettle is polytetrafluoroethylene (PTFE), and a diameter of 2.5cm magneton is put into reactor, and reactor is closed, in baking oven
In be heated to 210 DEG C and keep the temperature, stirring reaction 72h obtains the suspension 2 of black；
(3) suspension 2 that step (2) is obtained in question response kettle is cooled to after room temperature, is transferred in beaker, in ice-water bath
Carry out ultrasonically treated 3 times, each ultrasonic power is 100W, continues 20min, obtains the suspension 3 of black；
(4) suspension 3 for obtaining step (3) is transferred in 300mL centrifuge tube, and the rotating speed with 7000 revs/min enters
Row is centrifuged, and centrifuges 30min, supernatant liquor is reclaimed, and is collected lower sediment, is obtained precipitation 1；
(5) precipitation 1 for obtaining step (4) is distributed in 1000mL anhydrous normal propyl alcohol, super for 200W through ultrasonic power
Sound disperses after 50min, is transferred in 300mL centrifuge tube, is centrifuged with 6000 revs/min of rotating speed, centrifuges 30min
Afterwards, supernatant liquor is reclaimed, collects lower sediment；Repeat the operation once, will the lower sediment collected of this step it is scattered
To 1000mL without in normal propyl alcohol, after being 200W ultrasonic disperses 50min through ultrasonic power, it is transferred in 300mL centrifuge tube, with
6000 revs/min of rotating speed is centrifuged, and after centrifugation 30min, supernatant liquor is reclaimed, lower sediment is collected, is sunk
Shallow lake 2；
(6) precipitation 2 for obtaining step (5) is distributed in 1000mL distilled water, is 200W ultrasounds point through ultrasonic power
Dissipate after 50min, be transferred in 300mL centrifuge tube, be centrifuged with 5000 revs/min of rotating speed, after centrifugation 30min,
Supernatant liquor is outwelled, lower sediment is collected；Repeat it is described operation once, will this step collection lower sediment be distributed to
In 1000mL distilled water, after being 200W ultrasonic disperses 50min through ultrasonic power, it is transferred in 300mL centrifuge tube, with 5000
Rev/min rotating speed be centrifuged, after centrifugation 30min, outwell supernatant liquor, collect lower sediment, obtain precipitation 3；
(7) precipitation 3 for obtaining step (6) is added in 100mL distilled water, ultrasonic disperse 10min.Ultrasonic power is
100W, obtains the aqueous solution of precipitation 3, and the aqueous solution for precipitating 3 freeze in liquid nitrogen, then is dried in vacuo, vacuum for 8~
12MPa, obtains final product.
Final product is tested as follows：
(1) X-ray powder diffraction is tested：As a result the characteristic diffraction peak 25 that graphene sheet layer is stacked is occurred in thato, illustrate final
Product is micro crystal graphite alkene；
(2) Raman spectrum is tested：The ratio between D peak intensities and G peak intensities of final product (I as can be known from the resultsD/IG)；D peaks generation
Table SP3The vibration absorption peak of the bonding model of hydridization carbon, such as：" C-C ", " C-O ", " C=O " etc., G peaks represent SP2Hydridization carbon into
The vibration absorption peak of key model, i.e.,：" C=C ", ID/IGValue for 0.13, G peak intensities it is larger, illustrate the structure of final product simultaneously
Do not destroy；Show that final product defect is less by Raman test result, quality is higher；
(3) Electron microscopy：, can from SEM testing result and transmission electron microscope testing result
It is tens nanometer to a few micrometers of lamellar structure with the final product seen；Randomly choose (a) point and (b) point on final product
Carry out resolution ratio to detect for 0.2nm transmission electron microscope, as a result show the lamella of final product below 7 layers.
Embodiment 4
A kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step is as follows：
(1) weigh 11g micro crystal graphite powder, add in 750mL solvents 1, the solvent 1 by DMA,
1-METHYLPYRROLIDONE and o-dichlorohenzene are with volume ratio 1:1:1 mixes, and stirs 30min, then ultrasonically treated 30min, surpasses
Acoustical power is 100W, micro crystal graphite is well mixed with solvent 1, obtains the suspension 1 of black, wherein, the concentration of micro crystal graphite
For 15mg mL-1；
(2) suspension 1 for obtaining step (1) is fitted into the reactor that 1000mL basal diameters are 15cm, the reaction
The inner lining material of kettle is polytetrafluoroethylene (PTFE), and a diameter of 3cm magneton is put into reactor, and reactor is closed, in an oven
It is heated to 200 DEG C and keeps the temperature, stirring reaction 60h obtains the suspension 2 of black；
(3) suspension 2 that step (2) is obtained in question response kettle is cooled to after room temperature, is transferred in beaker, in ice-water bath
Carry out ultrasonically treated 3 times, each ultrasonic power is 90W, continues 15min, obtains the suspension 3 of black；
(4) suspension 3 for obtaining step (3) is transferred in 100mL centrifuge tube, and the rotating speed with 6000 revs/min enters
Row is centrifuged, and centrifuges 20min, supernatant liquor is reclaimed, and is collected lower sediment, is obtained precipitation 1；
(5) precipitation 1 for obtaining step (4) is distributed in 800mL anhydrous isopropyl alcohol, is 300W ultrasounds through ultrasonic power
After scattered 45min, it is transferred in 100mL centrifuge tube, is centrifuged with 5000 revs/min of rotating speed, centrifuges 30min
Afterwards, supernatant liquor is reclaimed, collects lower sediment；Repeat the operation once, will the lower sediment collected of this step it is scattered
Into 800mL anhydrous isopropyl alcohol, after being 300W ultrasonic disperses 45min through ultrasonic power, it is transferred in 100mL centrifuge tube,
It is centrifuged with 5000 revs/min of rotating speed, after centrifugation 30min, supernatant liquor is reclaimed, lower sediment is collected, obtains
Precipitation 2；
(6) precipitation 2 for obtaining step (5) is distributed in 1000mL distilled water, is 300W ultrasounds point through ultrasonic power
Dissipate after 45min, be transferred in 100mL centrifuge tube, be centrifuged with 5000 revs/min of rotating speed, after centrifugation 30min,
Supernatant liquor is outwelled, lower sediment is collected；Repeat it is described operation once, will this step collection lower sediment be distributed to
In 1000mL distilled water, after being 300W ultrasonic disperses 45min through ultrasonic power, it is transferred in 100mL centrifuge tube, with 5000
Rev/min rotating speed be centrifuged, after centrifugation 30min, outwell supernatant liquor, collect lower sediment, obtain precipitation 3；
(7) precipitation 3 for obtaining step (6) is added in 50mL distilled water, and ultrasonic disperse 8min, ultrasonic power is 90W,
Obtain the aqueous solution of precipitation 3, the aqueous solution for precipitating 3 freeze in liquid nitrogen, then is dried in vacuo, vacuum for 8~
12MPa, obtains final product.
Final product is tested as follows：
(1) X-ray powder diffraction is tested：As a result the characteristic diffraction peak 25 that graphene sheet layer is stacked is occurred in thato, illustrate final
Product is micro crystal graphite alkene；
(2) Raman spectrum is tested：The ratio between D peak intensities and G peak intensities of final product (I as can be known from the resultsD/IG)；D peaks generation
Table SP3The vibration absorption peak of the bonding model of hydridization carbon, such as：" C-C ", " C-O ", " C=O " etc., G peaks represent SP2Hydridization carbon into
The vibration absorption peak of key model, i.e.,：" C=C ", ID/IGValue for 0.12, G peak intensities it is larger, illustrate the structure of final product simultaneously
Do not destroy；Show that final product defect is less by Raman test result, quality is higher；
(3) Electron microscopy：, can from SEM testing result and transmission electron microscope testing result
It is tens nanometer to a few micrometers of lamellar structure with the final product seen；Randomly choose (a) point and (b) point on final product
Carry out resolution ratio to detect for 0.2nm transmission electron microscope, as a result show the lamella of final product below 7 layers.
Embodiment 5
A kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step is as follows：
(1) 4.5g micro crystal graphite powder is weighed, is added in 450mL solvents 1, the solvent 1 is by butyrolactone and o-dichlorohenzene
With volume ratio 3:1 mixes, and stirs 30min, then ultrasonically treated 30min, ultrasonic power is 90W, make micro crystal graphite with it is molten
Agent 1 is well mixed, and obtains the suspension 1 of black, wherein, the concentration of micro crystal graphite is 10mg mL-1；
(2) suspension 1 for obtaining step (1) is fitted into the reactor that 500mL basal diameters are 6cm, the reactor
Inner lining material be polytetrafluoroethylene (PTFE), be put into a diameter of 3cm magneton, reactor is closed, 200 DEG C are heated in an oven simultaneously
The temperature is kept, stirring reaction 36h obtains the suspension 2 of black；
(3) suspension 2 that step (2) is obtained in question response kettle is cooled to after room temperature, is transferred in beaker, in ice-water bath
Carry out ultrasonically treated 3 times, each ultrasonic power is 80W, continues 15min, obtains the suspension 3 of black；
(4) suspension 3 for obtaining step (3) is transferred in 100mL centrifuge tube, and the rotating speed with 7500 revs/min enters
Row is centrifuged, and centrifuges 15min, supernatant liquor is reclaimed, and is collected lower sediment, is obtained precipitation 1；
(5) precipitation 1 for obtaining step (4) is distributed in 500mL absolute ethyl alcohol, is 400W ultrasounds point through ultrasonic power
Dissipate after 40min, be transferred in 100mL centrifuge tube, be centrifuged with 7000 revs/min of rotating speed, after centrifugation 15min,
Supernatant liquor is reclaimed, lower sediment is collected；Repeat it is described operation once, will this step collection lower sediment be distributed to
In 500mL absolute ethyl alcohol, after being 400W ultrasonic disperses 40min through ultrasonic power, it is transferred in 100mL centrifuge tube, with
7000 revs/min of rotating speed is centrifuged, and after centrifugation 15min, supernatant liquor is reclaimed, lower sediment is collected, is sunk
Shallow lake 2；
(6) precipitation 2 for obtaining step (5) is distributed in 500mL distilled water, is 400W ultrasonic disperses through ultrasonic power
After 40min, it is transferred in 100mL centrifuge tube, is centrifuged with 6000 revs/min of rotating speed, after centrifugation 15min, is fallen
Fall supernatant liquor, collect lower sediment；Repeat it is described operation once, will this step collection lower sediment be distributed to 500mL
Distilled water in, through ultrasonic power be 400W ultrasonic disperses 40min after, be transferred in 100mL centrifuge tube, with 6000 revs/min
The rotating speed of clock is centrifuged, and after centrifugation 15min, outwells supernatant liquor, collects lower sediment, obtain precipitation 3；
(7) precipitation 3 for obtaining step (6) is added in 50mL distilled water, and ultrasonic disperse 7min, ultrasonic power is 90W,
Obtain the aqueous solution of precipitation 3, the aqueous solution for precipitating 3 freeze in liquid nitrogen, then is dried in vacuo, vacuum for 8~
12Mpa, obtains final product.
Final product is tested as follows：
(1) X-ray powder diffraction is tested：As a result the characteristic diffraction peak 25 that graphene sheet layer is stacked is occurred in thato, illustrate final
Product is micro crystal graphite alkene；
(2) Raman spectrum is tested：The ratio between D peak intensities and G peak intensities of final product (I as can be known from the resultsD/IG)；D peaks generation
Table SP3The vibration absorption peak of the bonding model of hydridization carbon, such as：" C-C ", " C-O ", " C=O " etc., G peaks represent SP2Hydridization carbon into
The vibration absorption peak of key model, i.e.,：" C=C ", ID/IGValue for 0.10, G peak intensities it is larger, illustrate the structure of final product simultaneously
Do not destroy；Raman test result shows that final product defect is less, and quality is higher；
(3) Electron microscopy：, can from SEM testing result and transmission electron microscope testing result
It is tens nanometer to a few micrometers of lamellar structure with the final product seen；Randomly choose (a) point and (b) point on final product
Carry out resolution ratio to detect for 0.2nm transmission electron microscope, as a result show the lamella of final product below 7 layers.
Embodiment 6
A kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step is as follows：
(1) 0.15g micro crystal graphite powder is weighed, is added in 75mL solvents 1, the solvent 1 is by 1-METHYLPYRROLIDONE, fourth
Lactone and o-dichlorohenzene are with volume ratio 0.5:0.5:1 mixes, and stirs 30min, then ultrasonically treated 30min, ultrasonic power
For 80W, micro crystal graphite is well mixed with solvent 1, obtain the suspension 1 of black, wherein, the concentration of micro crystal graphite is 2mg
mL-1；
(2) suspension 1 for obtaining step (1) is fitted into the reactor that 100mL basal diameters are 6cm, the reactor
Inner lining material be polytetrafluoroethylene (PTFE), a diameter of 2cm magneton is put into reactor, reactor is closed, in an oven plus
Heat is to 190 DEG C and keeps the temperature, and stirring reaction 24h obtains the suspension 2 of black；
(3) suspension 2 that step (2) is obtained in question response kettle is cooled to after room temperature, is transferred in beaker, in ice-water bath
Carry out ultrasonically treated 3 times, each ultrasonic power is 80W, continues 15min, obtains the suspension 3 of black；
(4) suspension 3 for obtaining step (3) is transferred in 20mL centrifuge tube, is carried out with 5000 revs/min of rotating speed
Centrifuge, centrifuge 15min, supernatant liquor is reclaimed, collect lower sediment, obtain precipitation 1；
(5) precipitation 1 for obtaining step (4) is distributed in 100mL anhydrous isopropyl alcohol, is 250W ultrasounds through ultrasonic power
After scattered 60min, it is transferred in 20mL centrifuge tube, is centrifuged with 6000 revs/min of rotating speed, after centrifugation 20min,
Supernatant liquor is reclaimed, lower sediment is collected；Repeat it is described operation once, will this step collection lower sediment be distributed to
In 100mL anhydrous isopropyl alcohol, after being 250W ultrasonic disperses 60min through ultrasonic power, it is transferred in 20mL centrifuge tube, with
6000 revs/min of rotating speed is centrifuged, and after centrifugation 20min, supernatant liquor is reclaimed, lower sediment is collected, is sunk
Shallow lake 2；
(6) precipitation 2 for obtaining step (5) is distributed in 100mL distilled water, is 250W ultrasonic disperses through ultrasonic power
After 60min, it is transferred in 20mL centrifuge tube, is centrifuged with 5000 revs/min of rotating speed, after centrifugation 20min, is outwelled
Supernatant liquor, collects lower sediment；Repeat it is described operation once, will this step collection lower sediment be distributed to 100mL's
In distilled water, after being 250W ultrasonic disperses 60min through ultrasonic power, it is transferred in 20mL centrifuge tube, with 5000 revs/min
Rotating speed is centrifuged, and after centrifugation 20min, outwells supernatant liquor, collects lower sediment, obtain precipitation 3；
(7) precipitation 3 for obtaining step (6) is added in 10mL distilled water, and ultrasonic disperse 9min, ultrasonic power is 80W,
Obtain the aqueous solution of precipitation 3, the aqueous solution for precipitating 3 freeze in liquid nitrogen, then is dried in vacuo, vacuum for 8~
12MPa, obtains final product.
Final product is tested as follows：
(1) X-ray powder diffraction is tested：As a result the characteristic diffraction peak 25 that graphene sheet layer is stacked is occurred in thato, illustrate final
Product is micro crystal graphite alkene；
(2) Raman spectrum is tested：The ratio between D peak intensities and G peak intensities of final product (I as can be known from the resultsD/IG)；D peaks generation
Table SP3The vibration absorption peak of the bonding model of hydridization carbon, such as：" C-C ", " C-O ", " C=O " etc., G peaks represent SP2Hydridization carbon into
The vibration absorption peak of key model, i.e.,：" C=C ", ID/IGValue for 0.09, G peak intensities it is larger, illustrate the structure of final product simultaneously
Do not destroy；Show that final product defect is less by Raman test result, quality is higher；
(3) Electron microscopy：, can from SEM testing result and transmission electron microscope testing result
It is tens nanometer to a few micrometers of lamellar structure with the final product seen；Randomly choose (a) point and (b) point on final product
Carry out resolution ratio to detect for 0.2nm transmission electron microscope, as a result show the lamella of final product below 7 layers.
Embodiment 7
A kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step is as follows：
(1) weigh 30g micro crystal graphite powder, add in 1500mL solvents 1, the solvent 1 by 1-METHYLPYRROLIDONE, N,
Dinethylformamide and o-dichlorohenzene are with volume ratio 1.5:1.5:1 mixes, and stirs 30min, then ultrasonically treated
30min, ultrasonic power is 100W, micro crystal graphite is well mixed with solvent 1, obtains the suspension 1 of black, wherein, microlite
The concentration of ink is 20mg mL-1；
(2) suspension 1 for obtaining step (1) is fitted into the reactor that 2000mL basal diameters are 15cm, the reaction
The inner lining material of kettle is polytetrafluoroethylene (PTFE), and a diameter of 6cm magneton is put into reactor, and reactor is closed, in an oven
It is heated to 200 DEG C and keeps the temperature, stirring reaction 24h obtains the suspension 2 of black；
(3) suspension 2 that step (2) is obtained in question response kettle is cooled to after room temperature, is transferred in beaker, in ice-water bath
Carry out ultrasonically treated 3 times, each ultrasonic power is 80W, continues 30min, obtains the suspension 3 of black；
(4) suspension 3 for obtaining step (3) is transferred in 200mL centrifuge tube, and the rotating speed with 5000 revs/min enters
Row is centrifuged, and centrifuges 10min, supernatant liquor is reclaimed, and is collected lower sediment, is obtained precipitation 1；
(5) precipitation 1 for obtaining step (4) is distributed in 800mL absolute ethyl alcohol, is 500W ultrasounds point through ultrasonic power
Dissipate after 50min, be transferred in 100mL centrifuge tube, be centrifuged with 8000 revs/min of rotating speed, after centrifugation 30min,
Supernatant liquor is reclaimed, lower sediment is collected；Repeat it is described operation once, will this step collection lower sediment be distributed to
In 800mL absolute ethyl alcohol, after being 500W ultrasonic disperses 50min through ultrasonic power, it is transferred in 100mL centrifuge tube, with
8000 revs/min of rotating speed is centrifuged, and after centrifugation 30min, supernatant liquor is reclaimed, lower sediment is collected, is sunk
Shallow lake 2；
(6) precipitation 2 for obtaining step (5) is distributed in 900mL distilled water, is 500W ultrasonic disperses through ultrasonic power
After 50min, it is transferred in 100mL centrifuge tube, is centrifuged with 4000 revs/min of rotating speed, after centrifugation 30min, is fallen
Fall supernatant liquor, collect lower sediment；Repeat it is described operation once, will this step collection lower sediment be distributed to 900mL
Distilled water in, through ultrasonic power be 500W ultrasonic disperses 50min after, be transferred in 100mL centrifuge tube, with 4000 revs/min
The rotating speed of clock is centrifuged, and after centrifugation 30min, outwells supernatant liquor, collects lower sediment, obtain precipitation 3；
(7) precipitation 3 for obtaining step (6) is added in 20mL distilled water, and ultrasonic disperse 5min, ultrasonic power is 80W,
Obtain the aqueous solution of precipitation 3, the aqueous solution for precipitating 3 freeze in liquid nitrogen, then is dried in vacuo, vacuum for 8~
12MPa, obtains final product.
Final product is tested as follows：
(1) X-ray powder diffraction is tested：As a result the characteristic diffraction peak 25 that graphene sheet layer is stacked is occurred in thato, illustrate final
Product is micro crystal graphite alkene；
(2) Raman spectrum is tested：The ratio between D peak intensities and G peak intensities of final product (I as can be known from the resultsD/IG)；D peaks generation
Table SP3The vibration absorption peak of the bonding model of hydridization carbon, such as：" C-C ", " C-O ", " C=O " etc., G peaks represent SP2Hydridization carbon into
The vibration absorption peak of key model, i.e.,：" C=C ", ID/IGValue for 0.12, G peak intensities it is larger, illustrate the structure of final product simultaneously
Do not destroy；Show that final product defect is less by Raman test result, quality is higher；
(3) Electron microscopy：, can from SEM testing result and transmission electron microscope testing result
It is tens nanometer to a few micrometers of lamellar structure with the final product seen；Randomly choose (a) point and (b) point on final product
Carry out resolution ratio to detect for 0.2nm transmission electron microscope, as a result show the lamella of final product below 7 layers.
Embodiment 8
A kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step is as follows：
(1) weigh 25g micro crystal graphite powder, add in 1500mL solvents 1, the solvent 1 by 1-METHYLPYRROLIDONE, N,
N- dimethyl acetamides, butyrolactone and o-dichlorohenzene are with volume ratio 1:1:1:1 mixes, and stirs 30min, then ultrasonically treated
30min, ultrasonic power is 100W, micro crystal graphite is well mixed with solvent 1, obtains the suspension 1 of black, wherein, microlite
The concentration of ink is 17mg mL-1；
(2) suspension 1 for obtaining step (1) is fitted into the reactor that 2000mL basal diameters are 15cm, the reaction
The inner lining material of kettle is polytetrafluoroethylene (PTFE), and a diameter of 4cm magneton is put into reactor, and reactor is closed, in an oven
It is heated to 180 DEG C and keeps the temperature, stirring reaction 70h obtains the suspension 2 of black；
(3) suspension 2 that step (2) is obtained in question response kettle is cooled to after room temperature, is transferred in beaker, in ice-water bath
Carry out ultrasonically treated 3 times, each ultrasonic power is 90W, continues 30min, obtains the suspension 3 of black；
(4) suspension 3 for obtaining step (3) is transferred in 100mL centrifuge tube, and the rotating speed with 6000 revs/min enters
Row is centrifuged, and centrifuges 30min, supernatant liquor is reclaimed, and is collected lower sediment, is obtained precipitation 1；
(5) precipitation 1 for obtaining step (4) is distributed in 900mL absolute ethyl alcohol, is 200W ultrasounds point through ultrasonic power
Dissipate after 50min, be transferred in 100mL centrifuge tube, be centrifuged with 6000 revs/min of rotating speed, after centrifugation 30min,
Supernatant liquor is reclaimed, lower sediment is collected；Repeat it is described operation once, will this step collection lower sediment be distributed to
In 900mL absolute ethyl alcohol, after being 200W ultrasonic disperses 50min through ultrasonic power, it is transferred in 100mL centrifuge tube, with
6000 revs/min of rotating speed is centrifuged, and after centrifugation 30min, supernatant liquor is reclaimed, lower sediment is collected, is sunk
Shallow lake 2；
(6) precipitation 2 for obtaining step (5) is distributed in 700mL distilled water, is 400W ultrasonic disperses through ultrasonic power
After 40min, it is transferred in 100mL centrifuge tube, is centrifuged with 5000 revs/min of rotating speed, after centrifugation 20min, is fallen
Fall supernatant liquor, collect lower sediment；Repeat it is described operation once, will this step collection lower sediment be distributed to 700mL
Distilled water in, through ultrasonic power be 400W ultrasonic disperses 40min after, be transferred in 100mL centrifuge tube, with 5000 revs/min
The rotating speed of clock is centrifuged, and after centrifugation 20min, outwells supernatant liquor, collects lower sediment, obtain precipitation 3；
(7) precipitation 3 for obtaining step (6) is added in 60mL distilled water, and ultrasonic disperse 8min, ultrasonic power is 90W,
Obtain the aqueous solution of precipitation 3, the aqueous solution for precipitating 3 freeze in liquid nitrogen, then is dried in vacuo, vacuum for 8~
12MPa, obtains final product.
Final product is tested as follows：
(1) X-ray powder diffraction is tested：As a result the characteristic diffraction peak 25 that graphene sheet layer is stacked is occurred in thato, illustrate final
Product is micro crystal graphite alkene；
(2) Raman spectrum is tested：The ratio between D peak intensities and G peak intensities of final product (I as can be known from the resultsD/IG)；D peaks generation
Table SP3The vibration absorption peak of the bonding model of hydridization carbon, such as：" C-C ", " C-O ", " C=O " etc., G peaks represent SP2Hydridization carbon into
The vibration absorption peak of key model, i.e.,：" C=C ", ID/IGValue for 0.14, G peak intensities it is larger, illustrate the structure of final product simultaneously
Do not destroy；Show that final product defect is less by Raman test result, quality is higher；
(3) Electron microscopy：, can from SEM testing result and transmission electron microscope testing result
It is tens nanometer to a few micrometers of lamellar structure with the final product seen；Randomly choose (a) point and (b) point on final product
Carry out resolution ratio to detect for 0.2nm transmission electron microscope, as a result show the lamella of final product below 7 layers.
Embodiment 9
A kind of method for preparing micro crystal graphite alkene by micro crystal graphite solvent heat stripping, methods described step is as follows：
(1) weigh 3.6g micro crystal graphite powder, add in 900mL solvents 1, the solvent 1 by 1-METHYLPYRROLIDONE, N,
N- dimethyl acetamides, N,N-dimethylformamide, butyrolactone and o-dichlorohenzene are with volume ratio 1:1:1:1:1 mixes, and stirs
30min is mixed, then ultrasonically treated 30min, ultrasonic power is 100W, micro crystal graphite is well mixed with solvent 1, obtains black
Suspension 1, wherein, the concentration of micro crystal graphite is 4mg mL-1；
(2) suspension 1 for obtaining step (1) is fitted into the reactor that 1200mL basal diameters are 12cm, the reaction
The inner lining material of kettle is polytetrafluoroethylene (PTFE), and a diameter of 4cm magneton is put into reactor, and reactor is closed, in an oven
It is heated to 200 DEG C and keeps the temperature, stirring reaction 65h obtains the suspension 2 of black；
(3) suspension 2 that step (2) is obtained in question response kettle is cooled to after room temperature, is transferred in beaker, in ice-water bath
Carry out ultrasonically treated 3 times, each ultrasonic power is 90W, continues 10min, obtains black suspension 3；
(4) suspension 3 for obtaining step (3) is transferred in 50mL centrifuge tube, is carried out with 8000 revs/min of rotating speed
Centrifuge, centrifuge 30min, supernatant liquor is reclaimed, collect lower sediment, obtain precipitation 1；
(5) precipitation 1 for obtaining step (4) is distributed in 500mL anhydrous isopropyl alcohol, is 500W ultrasounds through ultrasonic power
After scattered 30min, it is transferred in 100mL centrifuge tube, is centrifuged with 8000 revs/min of rotating speed, centrifuges 20min
Afterwards, supernatant liquor is reclaimed, collects lower sediment；Repeat the operation once, will the lower sediment collected of this step it is scattered
Into 500mL anhydrous isopropyl alcohol, after being 500W ultrasonic disperses 30min through ultrasonic power, it is transferred in 100mL centrifuge tube,
It is centrifuged with 8000 revs/min of rotating speed, after centrifugation 20min, supernatant liquor is reclaimed, lower sediment is collected, obtains
Precipitation 2；
(6) precipitation 2 for obtaining step (5) is distributed in 500mL distilled water, is 200W ultrasonic disperses through ultrasonic power
After 60min, it is transferred in 100mL centrifuge tube, is centrifuged with 7000 revs/min of rotating speed, after centrifugation 10min, outwells upper strata clear
Liquid, collects lower sediment；Repeat the operation once, will the lower sediment of this step collection be distributed to 500mL distilled water
In, after being 200W ultrasonic disperses 60min through ultrasonic power, it is transferred in 100mL centrifuge tube, with 7000 revs/min of rotating speed
It is centrifuged, after centrifugation 10min, outwells supernatant liquor, collect lower sediment, obtain precipitation 3；
(7) precipitation 3 for obtaining step (6) is added in 20mL distilled water, ultrasonic disperse 7min, and ultrasonic power is
100W, obtains the aqueous solution of precipitation 3, and the aqueous solution for precipitating 3 freeze in liquid nitrogen, then is dried in vacuo, vacuum for 8~
12MPa, obtains final product.
Final product is tested as follows：
(1) X-ray powder diffraction is tested：As a result the characteristic diffraction peak 25 that graphene sheet layer is stacked is occurred in thato, illustrate final
Product is micro crystal graphite alkene；
(2) Raman spectrum is tested：The ratio between D peak intensities and G peak intensities of final product (I as can be known from the resultsD/IG)；D peaks generation
Table SP3The vibration absorption peak of the bonding model of hydridization carbon, such as：" C-C ", " C-O ", " C=O " etc., G peaks represent SP2Hydridization carbon into
The vibration absorption peak of key model, i.e.,：" C=C ", ID/IGValue for 0.11, G peak intensities it is larger, illustrate the structure of final product simultaneously
Do not destroy；Show that final product defect is less by Raman test result, quality is higher；
(3) Electron microscopy：, can from SEM testing result and transmission electron microscope testing result
It is tens nanometer to a few micrometers of lamellar structure with the final product seen；Randomly choose (a) point and (b) point on final product
Carry out resolution ratio to detect for 0.2nm transmission electron microscope, as a result show the lamella of final product below 7 layers.
The present invention include but is not limited to above example, it is every carried out under the principle of spirit of the present invention it is any equivalent
Replace or local improvement, all will be regarded as within protection scope of the present invention.
Claims (8)
1. a kind of method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping, it is characterised in that：Step is as follows：
(1) micro crystal graphite powder is well mixed with solvent 1, obtains suspension 1, the concentration of micro crystal graphite is 1mg mL-1~
30mg mL-1；
Solvent 1 is the mixed solution of organic reagent and o-dichlorohenzene, and organic reagent is 1-METHYLPYRROLIDONE, N, N- dimethyl methyls
One or more of acid amides, DMAC N,N' dimethyl acetamide and butyrolactone；
(2) suspension 1 is fitted into closed container, is heated to 180 DEG C~210 DEG C and keeps the temperature, stirring reaction >=24h
Terminate, obtain suspension 2；
(3) suspension 2 is cooled to after room temperature, carried out in 0 DEG C~5 DEG C it is ultrasonically treated, ultrasonic power be 80W~100W, hold
Continuous >=10min, obtains suspension 3；
(4) suspension 3 is centrifuged, collects lower sediment, obtain precipitation 1；
(5) precipitation 1 is distributed in solvent 2 and forms homogeneous suspension 4, centrifuged, collected lower sediment, obtain precipitation 2；
The solvent 2 is methanol, ethanol, isopropanol or normal propyl alcohol；
(6) precipitation 2 is distributed in water and forms homogeneous suspension 5, centrifuged, collected lower sediment, obtain precipitation 3；
(7) precipitation 3 is distributed in water and forms homogeneous suspension 6, suspension 6 is frozen into solid, then carried out true in≤10min
Sky is dried, and obtains micro crystal graphite alkene.
2. a kind of method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping according to claim 1, its feature
It is：In step (1), the volume ratio of organic reagent and o-dichlorohenzene is 4:1~1:3；It is mixed into and first stirs, then ultrasonic disperse；
Ultrasonic power is 80W~100W.
3. a kind of method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping according to claim 1, its feature
It is：In step (2), closed container is with reactor of the polytetrafluoroethylene (PTFE) as liner；Magneton is added into closed container to enter
Row magnetic agitation；The diameter proportion of closed container basal diameter and magneton is 2:1~5:1；Stirring reaction 24h~72h.
4. a kind of method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping according to claim 1, its feature
It is：In step (3), suspension 2 is cooled to after room temperature, is carried out in ice-water bath ultrasonically treated；It is ultrasonically treated to carry out several times,
Continue 10min~30min every time.
5. a kind of method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping according to claim 1, its feature
It is：In step (4), the rotating speed of centrifugation is 5000 revs/min~8000 revs/min, centrifuges 10min~30min.
6. a kind of method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping according to claim 1, its feature
It is：In step (5), it is centrifuged after disperseing 30min~60min with 100W~500W power ultrasonic；Centrifuge
Rotating speed be 5000 revs/min~8000 revs/min, centrifuge 10min~30min；Step (5) is carried out >=2 times.
7. a kind of method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping according to claim 1, its feature
It is：In step (6), the purity of water is water more than distilled water purity；With 100W~500W power ultrasonic disperse 30min~
It is centrifuged after 60min；The rotating speed of the centrifugation is 4000 revs/min~8000 revs/min, centrifugation 10min~
30min；Step (6) is carried out >=2 times.
8. a kind of method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping according to claim 1, its feature
It is：In step (7), water is the water more than distilled water purity；Ultrasonic disperse, ultrasonic power is 80W~100W, ultrasonic 5min
~10min；Freezed using liquid nitrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510156136.6A CN104843679B (en) | 2015-04-03 | 2015-04-03 | The method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510156136.6A CN104843679B (en) | 2015-04-03 | 2015-04-03 | The method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104843679A CN104843679A (en) | 2015-08-19 |
| CN104843679B true CN104843679B (en) | 2017-09-26 |
Family
ID=53843730
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510156136.6A Active CN104843679B (en) | 2015-04-03 | 2015-04-03 | The method that micro crystal graphite alkene is prepared by micro crystal graphite solvent heat stripping |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104843679B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293482A (en) * | 2015-12-01 | 2016-02-03 | 张扬威 | Solvothermal stripping preparation method of graphene |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101882035B1 (en) * | 2010-06-25 | 2018-07-25 | 내셔널 유니버시티 오브 싱가포르 | Methods of forming graphene by graphite exfoliation |
| CN102431999B (en) * | 2011-09-22 | 2014-07-02 | 中国科学院金属研究所 | Method for preparing high-quality graphene |
| CN103213979A (en) * | 2013-05-10 | 2013-07-24 | 山西大同大学 | Method for preparing graphene by solvent-thermal process |
| CN103253659B (en) * | 2013-05-23 | 2015-09-23 | 渤海大学 | A kind of ultrasonic wave peels off the method for preparing graphite alkene |
| FR3009298B1 (en) * | 2013-07-31 | 2018-06-08 | Univ Bordeaux 1 | DIELS-ALDER REACTION-ASSISTED GRAPHITE EXFOLIATION METHOD |
| CN103626169A (en) * | 2013-11-06 | 2014-03-12 | 华东师范大学 | Preparation method of graphene quantum dot |
| CN103880002B (en) * | 2014-04-04 | 2015-12-16 | 厦门凯纳石墨烯技术股份有限公司 | A kind of continuous prodution graphene powder full scale plant and method thereof |
| CN103922323A (en) * | 2014-04-10 | 2014-07-16 | 华侨大学 | Method for preparing small-diameter graphene |
| CN104058396A (en) * | 2014-07-14 | 2014-09-24 | 复旦大学 | Method for preparing large-size high-quality graphene with controllable number of layers |
-
2015
- 2015-04-03 CN CN201510156136.6A patent/CN104843679B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104843679A (en) | 2015-08-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104724699B (en) | Method for preparing biomass graphene employing cellulose as raw material | |
| CN104843680B (en) | The method that graphene is prepared by micro crystal graphite batch | |
| CN102464313B (en) | Preparation method of graphene | |
| CN104475074B (en) | The preparation of boron doping hollow carbon balls and the application in cathode in direct methanol fuel cells | |
| CN105060289A (en) | Method for preparing fewer-layer graphene on basis of biomass waste | |
| CN102173414A (en) | Method for preparing graphene oxide by chemical peeling | |
| CN102583338B (en) | High-quality graphene powder and preparation method thereof | |
| CN104692363B (en) | Method for preparing graphene through hypergravity technology | |
| CN104692368B (en) | A kind of Graphene prepared as raw material with cellulose and preparation method thereof | |
| CN106024410B (en) | A kind of graphene-based electrode material for super capacitor of high power capacity and preparation method thereof | |
| CN105185599A (en) | Super-capacitor carbon composite material, preparation method therefor, and application of super-capacitor carbon composite material | |
| CN104211123A (en) | Preparation method for manganese oxide nano rods | |
| CN102275939A (en) | Preparation method of two-dimensional porous silica nanosheet | |
| CN103359709A (en) | Preparation method of nitrogen-doped graphene | |
| CN107845508A (en) | A kind of super capacitor material MoO2/ graphene/g C3N4Preparation method | |
| CN103922323A (en) | Method for preparing small-diameter graphene | |
| CN106206052B (en) | A kind of porous carbon composite electrode material of three-dimensional graphite alkenyl N doping and preparation method thereof | |
| CN104891479A (en) | Plant-based graphene and preparation method thereof | |
| CN107640761A (en) | The preparation method and stored energy application of graphene/carbon acid hydrogen nickel nanocube three-dimensional composite material | |
| CN107230784A (en) | A kind of spherical graphite alkene/mangano-manganic oxide composite and preparation method and application | |
| CN109592684B (en) | Petal spherical titanium carbide Ti3C2Mxene and preparation method and application thereof | |
| CN104511290B (en) | Preparation method of visible-light-driven photocatalyst nano spherical MoSe2 material | |
| CN108054020A (en) | A kind of preparation method and application of nitrogen-doped carbon particle/graphitized carbon nitrogen composite material | |
| CN105321726B (en) | High magnification active carbon/Activated Graphite alkene combination electrode material and preparation method thereof | |
| CN103078120B (en) | Ferrous silicate lithium ion battery cathode material with hierarchical structure and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |