CN108033442A - A kind of method that high speed peels off white graphite alkene - Google Patents
A kind of method that high speed peels off white graphite alkene Download PDFInfo
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- CN108033442A CN108033442A CN201711306580.7A CN201711306580A CN108033442A CN 108033442 A CN108033442 A CN 108033442A CN 201711306580 A CN201711306580 A CN 201711306580A CN 108033442 A CN108033442 A CN 108033442A
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- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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Abstract
The present invention relates to nano-graphene Material Field, specifically disclose a kind of method that high speed peels off white graphite alkene, after white graphite alkene (h BN) powder, surfactant, decentralized medium are mixed evenly the present invention according to a certain percentage, stir and peel off under high-speed condition, be specially：Low whipping speed is to be stirred stripping under the mixer of 5000 18000rpm, or injection stripping is carried out under the high pressure homogenizer of the pressure more than 50Mpa；After stripping, gained slurry is dried with ethanol wash, obtains white graphite alkene powder.This method can be effectively peeled off h BN particles, and the prepared white graphite alkene obtained has the characteristics that the number of plies is few, specific surface area is big, particle diameter is big, crystal structure is complete, and stripping means is simple, fast and effective, has significant market value.
Description
Technical field
The present invention relates to nano-graphene Material Field, and in particular to a kind of method that high speed peels off white graphite alkene.
Background technology
The discovery of graphene has triggered research boom of the scientific circles to two-dimensional material.The hexagonal boron nitride of individual layer or few layer
Also known as white graphite alkene (h-BN), is a kind of new two-dimensional material, is netted with the honeycomb that SP2 hydridization is formed by B/N atoms
Structure laminar crystalline material, because its structure is similar with graphene and referred to as white graphite alkene.White graphite alkene density is low, specific strength is high,
But white graphite alkene energy gap is up to 6.0ev, is a kind of excellent insulator.The thermal conductivity factor of white graphite alkene is high, has good
Thermal conductivity, can serve as composite material filler to improve its heat conductivility, be one of highest material of current thermal conductivity, very
Multi-field, such as photoelectron, magnetic energy, energy storage, catalysis field have broad application prospects；Have high temperature resistant, corrosion resistance, in sky
Still possess good chemical stability under more than 1000 DEG C and saline-alkali environment in gas atmosphere, can apply to anti-oxidant and corrosion-resistant painting
The fields such as layer；Friction coefficient is low, is industrially widely used frequently as a kind of lubricant of function admirable.
, at present still cannot be extensive although h-BN two-dimensional materials possess many excellent performances and are widely applied prospect
Preparation possesses structural integrity, h-BN two-dimensional materials of good performance.Traditional micromechanics is peeled off, and is to be peeled off h-BN using adhesive tape,
Although prepared h-BN structural integrities but yield is too low, it is not suitable for industrial mass production；Chemical liquid phase stripping etc. is commonly used
Poisonous and hazardous organic solvent, and oxidation and ion insertion etc. have its physical arrangement and electronic structure certain influence, it is prepared
The h-BN electric properties obtained are bad.Chemical vapour deposition technique can accurately control the h-BN numbers of plies, and prepared h-BN mass is good, but
Its is with high costs.As it can be seen that existing white graphite alkene preparation method, still lack the quality that can take into account graphene and industrialized production
It is required that this greatly limits its application.How economically the excellent white graphite alkene of production performance is also the emphasis studied at present
One of, further, since white graphite alkene possesses high Van der Waals force there are huge specific surface area, cause white graphite alkene piece easily to produce
Raw irreversible reunion, therefore improve its dispersiveness and be equally applied to that there is larger meaning.
The content of the invention
In view of this, it is necessary to for it is above-mentioned the problem of, there is provided a kind of method that high speed peels off white graphite alkene.This method energy
White graphite alkene particle is effectively peeled off at a high speed, and the prepared white graphite alkene obtained is with particle is uniform, the number of plies is few, specific surface area is big, pure
The characteristics of high is spent, can be dispersed in well in alcohol equal solvent, tens of days is preserved and does not produce reunion settlement action.And this method is grasped
It is simple to make process, cost is low, is suitably applied industrial production.
To achieve the above object, the present invention takes following technical solution：
The method that the high speed of the present invention peels off white graphite alkene, including：By white graphite alkene (h-BN) powder, surfactant,
After decentralized medium is mixed evenly, stirs and peel off under high-speed condition；
Stripping is stirred under the high-speed condition is specially：Low whipping speed is to be carried out under the mixer of 5000-18000rpm
Stirring is peeled off, and the mass ratio of white graphite alkene (h-BN) powder and surfactant is 1:50-10:1；The white graphite alkene
(h-BN) it is 1 mass ratio to be added with decentralized medium:100-1:2000；Whipping process reduces system temperature, total stirring using frozen water
Time is 10-240h；Or
Injection stripping is carried out under the high pressure homogenizer more than 50Mpa pressure；White graphite alkene (h-BN) powder and table
The mass ratio of face activating agent is 1:1-500:1；It is 1 that the white graphite alkene (h-BN) adds mass ratio with decentralized medium:3-1:
500；
After the completion of stripping, gained slurry uses ethanol wash, then dries, and obtains white graphite alkene powder.
The present invention in stripping process, the surface energy of decentralized medium close to white graphite alkene surface energy when (25-45mJ/
m2), stripping has highest efficiency and optimal effect, simultaneously as the change of h-BN stripping processes system viscosity is greatly, addition is suitable
The decentralized medium of amount can adjust the range of viscosities of system, keep solution good fluidity in peel-off device, not putty.B in h-BN,
N atoms are respectively with faint positive electricity, negative electricity, and h-BN there are pi bond, with electric charge or the long-chain Louis with pi bond of matching
Acid, the surfactant of long-chain lewis base, can fully adsorb to form steric hindrance and electric charge steric hindrance on h-BN, can promote
Grind, prevent separated h-BN nanometer sheets from reuniting.
Further, the decentralized medium is low-molecular-weight alcohol and/or the aqueous solution of ketone.
As preference, the surface tension of the decentralized medium is about 25-40mJ/m2。
As preference, the aqueous solution of the low-molecular-weight alcohol and/or ketone, low-molecular-weight alcohol and/or the quality of ketone and water
Than for 1:10-2:1, more preferably 1:5-2:1.
As preference, the low-molecular-weight alcohol is：In methanol, ethanol, isopropanol, the tert-butyl alcohol, ethylene glycol etc. at least
It is a kind of；The low-molecular-weight ketone is acetone.
Further, the surfactant is in the surfactant of tool long-chain lewis acid or long-chain lewis base
It is at least one.Wherein the C atomicities of surfactant are more than 12.
As preference, the long-chain lewis acid is：Higher fatty acids, aliphatic ketone, alicyclic ketone, fatty aldehyde etc., and its
At least one of corresponding derivative；The long-chain lewis base is：At least one of aromatic compound, amine, ether etc..
As it is furthermore preferred that the long-chain lewis acid surfactant is：Palmitic acid, palmitic acid, stearic acid, oleic acid,
Linoleic acid, palmitic acid, 18 ketone, 3- methyl cyclotridecanone, ring tetradecane ketone, 16 ketone of 3-, palmital, arbricolin or eicosane
At least one of aldehyde etc.；
The long-chain lewis base surfactant is：Palmitamide, heptadecyl-amine, octadecylamine, oleyl amine, Cholestyramine, end amine
Base polyethylene glycol, polyphenylacetylene, polythiophene, kayexalate, detergent alkylate, 4- dodecyl polyanilines, polyoxyethylene
Octane alkylphenol ether, glycidol 12-14 alkyl ethers, six polyethyleneglycol margarons, four ethene glycol lists, ten tetraether, six poly- second
At least one of ten tetraether of glycol list etc..Further, after injection is peeled off once, since slurry fluidity changes, continue to add
Bonus point dispersion media, the additive amount of the decentralized medium are 1/5-5 times of original solvents quality, and cyclic spray stripping is once or once
More than.
Further, when injection is peeled off, the mass ratio of white graphite alkene (h-BN) powder and surfactant is 10:1-
100:1；It is 1 that the white graphite alkene (h-BN) adds mass ratio with decentralized medium:10-1:100.More preferably described white graphite alkene
(h-BN) mass ratio of powder and surfactant is 10:1；The white graphite alkene (h-BN) adds mass ratio with decentralized medium
1:100.Injection is peeled off is hit using the stream material of high-pressure slurry high speed convection in the case where match nozzle, material and homogenizing valve, material and
The impact and shearing force that high speed convection produces between material, cavitation caused by pressure sharp fall when material flows into homogeneous chamber
Peel off white graphite alkene.
Mixer high speed dispersion peel off white graphite alkene can because shearing force is excessive and the white graphite alkene to being stripped causes one
The particle diameter for determining degree diminishes, crystal structure is destroyed.And during spraying stripping white graphite alkene, flowed at high speeds using material
When, cavitation caused by the shearing force that is produced between material and homogenizing valve, material and material, pressure sharp fall peels off white graphite
Alkene, peels off white graphite alkene with ball grinding stirring and compares, and it is mostly high speed between fluid mechanics and homogenizing valve, logistics and material that injection, which is peeled off,
Shearing force caused by friction, the destructive smaller of dialogue graphene, comparatively lamella bigger, crystal structure are more complete.
Beneficial effects of the present invention are：
White graphite alkene piece particle diameter that the present invention peels off is big, thickness is thin, specific surface area is big：The prepared white graphite alkene number of plies
For 1-20 layers or so, the thickness of thin slice as low as 1 nanometer, grain size can be distributed in hundreds of nanometers to a few micrometers, specific surface area
Up to 100-1500m2/g.The prepared white graphite alkene obtained can be dispersed in the solution such as alcohol, acetone, water for a long time, not produced
Raw phenomena such as settling of reuniting.
Environmentally protective without strong acid/base, toxic organic additive etc. in preparation process of the present invention, production efficiency is high, yield
Greatly, and equipment is simple, of low cost, has a good application prospect.
Brief description of the drawings
Fig. 1 is the SEM photograph of the prepared white graphite alkene dispersion obtained of embodiment 1；
Fig. 2 is the AFM photos of the prepared white graphite alkene dispersion obtained of embodiment 1；
Fig. 3 is the SEM photograph of the prepared white graphite alkene obtained of embodiment 9.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is made further clearly and completely to describe.It should be noted that described embodiment is only the present invention one
Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing
Go out all other embodiments obtained under the premise of creative work, belong to the scope of protection of the invention.
Embodiment 1
The specific step of preparation process of the present embodiment：0.2g white graphites alkene (h-BN) is weighed in beaker, addition 150g ethanol
With 150g deionized waters, 4g ring tetradecane ketone is measured, is added in beaker, stirring is allowed to be completely dissolved.
By above-mentioned matched somebody with somebody solution high speed dispersor with 10000rpm high-speed stirred 72h, and system temperature is reduced with frozen water,
To prevent high-speed stirred from causing temperature to raise, decentralized medium loss is too fast.
Stirring centrifuges white graphite alkene after peeling off after ethanol wash, 60 DEG C of drying and processings in Muffle furnace
Obtain white graphite alkene dispersion product.
Fig. 1 is the SEM photograph of product obtained by the present embodiment, it can be seen that peeled off by stirring, it is white after stripping
Graphene nanometer sheet particle diameter is more than 250nm, and nanometer sheet thickness is below 10nm；Fig. 2 detects photo for atomic force microscope, in figure
Most of sheet thickness is 2nm, and part h-BN thickness can as low as 1nm or so.It is 470m by detecting specific surface area2/g。
Embodiment 2
The specific step of preparation process of the present embodiment：Weigh 0.5g white graphites alkene (h-BN), 200g ethanol and 200g deionizations
Water is stirred evenly in beaker with glass bar.10g oleic acid is measured, is put into beaker, stirring is completely dissolved it.
By above-mentioned matched somebody with somebody solution high speed dispersor with 13000rpm high-speed stirred 48h, and system temperature is reduced with frozen water.
Stirring centrifuges white graphite alkene after peeling off after ethanol wash, 60 DEG C of drying and processings in Muffle furnace
Obtain white graphite alkene dispersion product.
White graphite alkene nanometer sheet particle diameter after stripping is more than 250nm, and nanometer sheet thickness is below 10nm；Most of thin slice is thick
Spending can as low as 1nm or so for 3nm, part h-BN thickness.It is 350m by detecting specific surface area2/g。
Embodiment 3
The specific step of preparation process of the present embodiment：Weigh 0.2g white graphites alkene (h-BN), 100g acetone and 100g deionizations
Water is stirred evenly in beaker with glass bar.2g octadecylamines are measured in beaker, same stirring is completely dissolved it.
By above-mentioned matched somebody with somebody solution high speed dispersor with 13000rpm high-speed stirred 24h, and system temperature is reduced with frozen water.
Stirring centrifuges white graphite alkene after peeling off after ethanol wash, 60 DEG C of drying and processings in Muffle furnace
Obtain white graphite alkene dispersion product.
White graphite alkene nanometer sheet particle diameter after stripping is more than 250nm, and nanometer sheet thickness is below 10nm；Most of thin slice is thick
Spending can as low as 1nm or so for 5nm, part h-BN thickness.It is 200m by detecting specific surface area2/g。
Embodiment 4
The specific step of preparation process of the present embodiment：Weigh 0.5g white graphites alkene (h-BN), 150g acetone and 150g deionizations
Water, measures 4g ring tetradecane ketone, adds in beaker, and stirring is completely dissolved it.
By above-mentioned matched somebody with somebody solution high speed dispersor with 15000rpm high-speed stirred 15h, and system temperature is reduced with frozen water.
Stirring centrifuges white graphite alkene after peeling off after ethanol wash, 60 DEG C of drying and processings in Muffle furnace
Obtain white graphite alkene dispersion product.
White graphite alkene nanometer sheet particle diameter after stripping is more than 250nm, and nanometer sheet thickness is below 10nm；Most of thin slice is thick
Spending can as low as 1nm or so for 4nm, part h-BN thickness.It is 230m by detecting specific surface area2/g。
Embodiment 5
The specific step of preparation process of the present embodiment：Weigh 0.2g white graphites alkene (h-BN), 100g acetone and 200g deionizations
Water, measures 4g4- dodecyl polyanilines, is put into beaker, and stirring is allowed to be completely dissolved.
By above-mentioned matched somebody with somebody solution high speed dispersor with 18000rpm high-speed stirred 12h, and system temperature is reduced with frozen water.
Stirring centrifuges white graphite alkene after peeling off after ethanol wash, 60 DEG C of drying and processings in Muffle furnace
Obtain white graphite alkene dispersion product.
White graphite alkene nanometer sheet particle diameter after stripping is more than 250nm, and nanometer sheet thickness is below 10nm；Most of thin slice is thick
Spending can as low as 1nm or so for 5nm, part h-BN thickness.It is 250m by detecting specific surface area2/g。
Embodiment 6
The specific step of preparation process of the present embodiment：Weigh 0.2g white graphites alkene (h-BN), 100g isopropanols and 50g deionizations
Water, measures 4g palmitic acid, 4g arbricolins, is put into beaker, and stirring is allowed to be completely dissolved.
By above-mentioned matched somebody with somebody solution high speed dispersor with 10000rpm high-speed stirred 60h, and system temperature is reduced with frozen water.
Stirring centrifuges white graphite alkene after peeling off after ethanol wash, 60 DEG C of drying and processings in Muffle furnace
Obtain white graphite alkene dispersion product.
White graphite alkene nanometer sheet particle diameter after stripping is more than 250nm, and nanometer sheet thickness is below 10nm；Most of thin slice is thick
Spending can as low as 1nm or so for 2nm, part h-BN thickness.It is 480m by detecting specific surface area2/g。
Embodiment 7
The specific step of preparation process of the present embodiment：Weigh 5g white graphites alkene (h-BN), 1000 methanol, 500g acetone and
1500g deionized waters, measure six polyethyleneglycol margarons of 1g, are put into beaker, and stirring is allowed to be completely dissolved.
By above-mentioned matched somebody with somebody solution high speed dispersor with 8000rpm high-speed stirred 160h, and system temperature is reduced with frozen water.
Stirring centrifuges white graphite alkene after peeling off after ethanol wash, 60 DEG C of drying and processings in Muffle furnace
Obtain white graphite alkene dispersion product.
White graphite alkene nanometer sheet particle diameter after stripping is more than 250nm, and nanometer sheet thickness is below 10nm；Most of thin slice is thick
Spending can as low as 1nm or so for 2nm, part h-BN thickness.It is 740m by detecting specific surface area2/g。
Embodiment 8
The specific step of preparation process of the present embodiment：Weigh 5g white graphites alkene (h-BN), 2000 ethanol, the 500g tert-butyl alcohols and
2000g deionized waters, measure 1g oleyl amines, 1g glycidol 12-14 alkyl ethers, are put into beaker, and stirring is allowed to be completely dissolved.
By above-mentioned matched somebody with somebody solution high speed dispersor with 6000rpm high-speed stirred 220h, and system temperature is reduced with frozen water.
Stirring centrifuges white graphite alkene after peeling off after ethanol wash, 60 DEG C of drying and processings in Muffle furnace
Obtain white graphite alkene dispersion product.
White graphite alkene nanometer sheet particle diameter after stripping is more than 250nm, and nanometer sheet thickness is below 10nm；Most of thin slice is thick
Spending can as low as 1nm or so for 2nm, part h-BN thickness.It is 600m by detecting specific surface area2/g。
Embodiment 9
The specific step of preparation process of the present embodiment：Weigh 100g h-BN, 500g ethanol and 500g deionized waters and beaker
In, 4g polythiophenes are added, stirring is allowed to be completely dissolved.
Slurry is transferred in high pressure homogenizer barrel, starts high pressure homogenizer, is peeled off with 100mpa start high-pressure injections.
Often injection is peeled off once supplements 200g ethanol water (ethanol afterwards：Water quality ratio is 1:1), then injection stripping is carried out once；Such as
This spray repeatedly stripping 10 times after, by white graphite alkene after ethanol wash, 60 DEG C of drying and processings obtain Bai Shi in Muffle furnace
Black alkene product.
Fig. 1 is the SEM photograph of the present embodiment products obtained therefrom, it can be seen that being peeled off by spraying, obtained white stone
Black alkene nanometer sheet particle diameter is more than 250nm, and nanometer sheet thickness is below 10nm, and part h-BN thickness can as low as 1nm or so.Pass through inspection
Survey specific surface area is 380m2/g。
Embodiment 10
The specific step of preparation process of the present embodiment：100g h-BN, 500g ethanol and 500g deionized waters are weighed in beaker
In, stirred evenly with glass bar, add 10g oleyl amines, stirring is completely dissolved it.
Above-mentioned slurry is transferred to, is peeled off 5 times with 300mpa injections.It is water-soluble that often injection stripping once supplements 200g ethanol afterwards
Liquid (ethanol：Water quality ratio is 1:1) after the completion of, injection is peeled off, by white graphite alkene after ethanol wash, 60 DEG C in Muffle furnace
Drying and processing obtains white graphite alkene product.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and nanometer sheet thickness is below 10nm；Big portion
The thickness for dividing h-BN pieces is 4nm, and part h-BN thickness can as low as 1nm or so.It is 620m by detecting specific surface area2/g。
Embodiment 11
The specific step of preparation process of the present embodiment：100g h-BN, 500g acetone and 500g deionized waters are weighed in beaker
In, stirred evenly with glass bar, measure 2g palmitic acid, during addition is above-mentioned, equally stir to dissolve.
Will be above-mentioned, injection is carried out with 380mpa and is peeled off 4 times.Often injection in stripping process is sprayed to peel off once on supplement 300g
State aqueous acetone solution.White graphite alkene is passed through into ethanol wash after the completion of injection stripping, 60 DEG C of drying and processings obtain in Muffle furnace
White graphite alkene product.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and nanometer sheet thickness is below 10nm；Big portion
The thickness for dividing h-BN pieces is 4nm, and part h-BN thickness can as low as 1nm or so.It is 880m by detecting specific surface area2/g。
Embodiment 12
The specific step of preparation process of the present embodiment：100g h-BN, 200g acetone and 400g deionized waters are weighed, measures 4g
Octadecylamine, is put into beaker, and stirring is completely dispersed it.
Above-mentioned slurry is transferred in high pressure homogenizer barrel, starts high pressure homogenizer, 3 are peeled off with 300mpa high-pressure injections
It is secondary.Spray often injection in stripping process and peel off the once addition above-mentioned aqueous acetone solutions of 200g, to ensure, system possesses suitable stream
Dynamic property.Injection stripping is finished by white graphite alkene solution after ethanol wash, and 60 DEG C of drying and processings obtain Bai Shi in Muffle furnace
Black alkene product.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and nanometer sheet thickness is below 10nm, big portion
The thickness for dividing h-BN pieces is 3nm, and part h-BN thickness can as low as 1nm or so.It is 380m by detecting specific surface area2/g。
Embodiment 13
The specific step of preparation process of the implementation case：100g h-BN, 500g acetone and 500g deionized waters are weighed, is measured
4g 3- methyl cyclotridecanones, are put into beaker, and stirring is allowed to be completely dissolved.
Above-mentioned slurry is transferred in high pressure homogenizer barrel, starts high pressure homogenizer, is sprayed 2 times with 500mpa.Injection
Often injection is peeled off in stripping process once adds the above-mentioned aqueous acetone solutions of 500g afterwards, possesses suitable mobility with guarantee system.
Injection stripping is finished by white graphite alkene after ethanol wash, and 60 DEG C of drying and processings obtain white graphite alkene product in Muffle furnace.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and nanometer sheet thickness is below 10nm；Big portion
The thickness for dividing h-BN pieces is 4nm, and part h-BN thickness can as low as 1nm or so.It is 650m by detecting specific surface area2/g。
Embodiment 14
The specific step of preparation process of the implementation case：100g h-BN, the 250g tert-butyl alcohols, 250g acetone and 500g is weighed to go
Ionized water, measures 3g 3- methyl cyclotridecanones, is put into beaker, and stirring makes to be dispersed into uniform sizing material.
Above-mentioned slurry is transferred in high pressure homogenizer barrel, starts high pressure homogenizer, is peeled off 2 times with 600mpa injections.
Spray in stripping process, injection for the first time adds the above-mentioned 500g tert-butyl alcohols/aqueous acetone solution after peeling off, and possesses with guarantee system suitable
The mobility of conjunction.Injection stripping is finished by white graphite alkene after ethanol wash, and 60 DEG C of drying and processings obtain white in Muffle furnace
Graphene product.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and nanometer sheet thickness is below 10nm；Big portion
The thickness for dividing h-BN pieces is 4nm, and part h-BN thickness can as low as 1nm or so.It is 680m by detecting specific surface area2/g。
Embodiment 15
The specific step of preparation process of the implementation case：Weigh 100g h-BN, 250g methanol, 250g acetone and 500g go from
Sub- water, measures 3g palmitals, is put into beaker, and stirring is allowed to be uniformly dispersed.
Above-mentioned slurry is transferred to high pressure homogenizer barrel, starts high pressure homogenizer, is peeled off 10 times with 100mpa injections.Spray
Penetrate in stripping process, often spray the once addition above-mentioned methanol/acetone aqueous solutions of 200g.Injection stripping, which finishes, passes through white graphite alkene
After ethanol wash, 60 DEG C of drying and processings obtain white graphite alkene product in Muffle furnace.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and nanometer sheet thickness is below 10nm；Big portion
The thickness for dividing h-BN pieces is 5nm, and part h-BN thickness can as low as 1nm or so.It is 350m by detecting specific surface area2/g。
Embodiment 16
The specific step of preparation process of the implementation case：Weigh 10g h-BN, 250g methanol, 250 isopropanols and 500g go from
Sub- water, measures 10g polyoxyethylene octane alkylphenol ethers, is put into beaker, and stirring is allowed to be uniformly dispersed.
Above-mentioned slurry is transferred to high pressure homogenizer barrel, starts high pressure homogenizer, 2 are peeled off with 500mpa high-pressure injections
It is secondary.Spray in stripping process, often injection, which is peeled off, once adds the above-mentioned methanol/isopropanol aqueous solutions of 500g, possesses with guarantee system
Suitable mobility.Injection, which is peeled off, finishes by white graphite alkene after ethanol wash, and 60 DEG C of drying and processings obtain white in Muffle furnace
Graphene product.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and nanometer sheet thickness is below 5nm；Big portion
The thickness for dividing h-BN pieces is 2nm, and part h-BN thickness can as low as 1nm or so.It is 800m by detecting specific surface area2/g。
Embodiment 17
The specific step of preparation process of the present embodiment：100g h-BN, 500g ethanol and 500g deionized waters are weighed in beaker
In, stirred evenly with glass bar, add 0.3g oleyl amines, stirring is completely dissolved it.
Above-mentioned slurry is transferred to, is peeled off 5 times with 300mpa injections.It is water-soluble that often injection stripping once supplements 200g ethanol afterwards
Liquid (ethanol：Water quality ratio is 1:1) after the completion of, injection is peeled off, by white graphite alkene after ethanol wash, 60 DEG C in Muffle furnace
Drying and processing obtains white graphite alkene product.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and nanometer sheet thickness is below 10nm；Big portion
The thickness for dividing h-BN pieces is 8nm, and part h-BN thickness can as low as 5nm or so.It is 220m by detecting specific surface area2/g。
Embodiment 18
The specific step of preparation process of the implementation case：Weigh 5g h-BN, the 500g tert-butyl alcohols, 500g acetone and 1000g go from
Sub- water, measures 3g 3- methyl cyclotridecanones, is put into beaker, and stirring makes to be dispersed into uniform sizing material.
Above-mentioned slurry is transferred in high pressure homogenizer barrel, starts high pressure homogenizer, is peeled off 2 times with 600mpa injections.
Injection stripping is finished by white graphite alkene after ethanol wash, and 60 DEG C of drying and processings obtain white graphite alkene product in Muffle furnace.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and nanometer sheet thickness is below 10nm；Big portion
The thickness for dividing h-BN pieces is 7nm, and part h-BN thickness can as low as 6nm or so.It is 280m by detecting specific surface area2/g。
Embodiment 19
The specific step of preparation process of this comparative example：100g h-BN, 500g acetone and 500g deionized waters are weighed, measures 4g
Octadecylamine, is put into beaker, and stirring is completely dispersed it.
Above-mentioned slurry is transferred in high pressure homogenizer barrel, starts high pressure homogenizer, is peeled off 10 times with 50mpa injections.
Once addition 100g aqueous acetone solutions are often sprayed in injection stripping process.Injection stripping is finished passes through alcohol by white graphite alkene solution
After washing, 60 DEG C of drying and processings obtain white graphite alkene product in Muffle furnace.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and nanometer sheet thickness is below 10nm；Pass through
Detection specific surface area is 105m2/g。
Comparative example 1
The specific step of preparation process of the present embodiment：0.2g white graphites alkene (h-BN) is weighed in beaker, addition 150g ethanol
With 150g deionized waters, 4g ring tetradecane ketone is measured, is added in beaker, stirring is allowed to be completely dissolved.
By above-mentioned matched somebody with somebody solution high speed dispersor with 10000rpm high-speed stirred 5h, and system temperature is reduced with frozen water.
Stirring centrifuges white graphite alkene after peeling off after ethanol wash, and 60 DEG C of drying and processings obtain Bai Shi in Muffle furnace
Black alkene dispersion product.
White graphite alkene nanometer sheet particle diameter after stripping is more than 250nm, and nanometer sheet thickness is largely more than 20nm；Partial sheet
Thickness is 50nm, and part h-BN thickness can as low as 5nm or so.It is 60m by detecting specific surface area2/g。
Comparative example 2
The specific step of preparation process of the present embodiment：0.2g white graphites alkene (h-BN) is weighed in beaker, addition 150g ethanol
With 150g deionized waters, surfactant is not added with.
By above-mentioned matched somebody with somebody solution high speed dispersor with 10000rpm high-speed stirred 80h, and system temperature is reduced with frozen water.
Stirring centrifuges white graphite alkene after peeling off after ethanol wash, and 60 DEG C of drying and processings obtain Bai Shi in Muffle furnace
Black alkene dispersion product.
White graphite alkene nanometer sheet particle diameter after stripping is more than 250nm, and nanometer sheet thickness is largely more than 20nm；Partial sheet
Thickness is 50nm, and part h-BN thickness can as low as 5nm or so.It is 30m by detecting specific surface area2/g。
Comparative example 3
The specific step of preparation process of this comparative example：100g h-BN, 500g acetone and 500g deionized waters are weighed, measures 4g
Octadecylamine, is put into beaker, and stirring is completely dispersed it.
Above-mentioned slurry is transferred in high pressure homogenizer barrel, starts high pressure homogenizer, is peeled off 10 times with 30mpa injections.
Once addition 100g aqueous acetone solutions are often sprayed in injection stripping process.Injection stripping is finished passes through alcohol by white graphite alkene solution
After washing, 60 DEG C of drying and processings obtain white graphite alkene product in Muffle furnace.
The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, and the thickness of most of h-BN pieces is 40nm,
It is 30m by detecting specific surface area2/g。
Comparative example 4
The specific step of preparation process of this comparative example：100g h-BN, 500g acetone and 500g deionized waters are weighed, is not added with table
Face activating agent.
Above-mentioned slurry is transferred in high pressure homogenizer barrel, starts high pressure homogenizer, is peeled off 4 times with 200mpa injections.
Spray often injection in stripping process and peel off once addition 100g aqueous acetone solutions, possess suitable mobility with guarantee system.
Injection stripping is finished by white graphite alkene after ethanol wash, and 60 DEG C of drying and processings obtain white graphite in Muffle furnace
Alkene product.The obtained white graphite alkene nanometer sheet particle diameter of the present embodiment is more than 250nm, nanometer sheet thickness 40nm or so.Pass through inspection
Survey specific surface area is 48m2/g。
Embodiment described above only expresses the several embodiments of the present invention, its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (9)
1. a kind of method that high speed peels off white graphite alkene, it is characterised in that including：White graphite alkene (h-BN) powder, surface are lived
Property agent, decentralized medium be mixed evenly after, stir and peel off under high-speed condition；
It is that stirring stripping is specially under high-speed condition that the high speed, which is peeled off,：Low whipping speed is the mixer of 5000-18000rpm
Under be stirred stripping, the mass ratio of white graphite alkene (h-BN) powder and surfactant is 1:50-10:1；The white stone
It is 1 that black alkene (h-BN) adds mass ratio with decentralized medium:100-1:2000；Whipping process reduces system temperature using frozen water, always
Mixing time is 10-240h；Or
Injection stripping is carried out under the high pressure homogenizer more than 50Mpa pressure；White graphite alkene (h-BN) powder is lived with surface
Property agent mass ratio be 1:1-500:1；It is 1 that the white graphite alkene (h-BN) adds mass ratio with decentralized medium:3-1:500；
After the completion of stripping, gained slurry uses ethanol wash, then dries, and obtains white graphite alkene powder.
2. the method that high speed according to claim 1 peels off white graphite alkene, it is characterised in that the decentralized medium is low point
The aqueous solution of son amount alcohol and/or ketone.
3. the method that high speed according to claim 2 peels off white graphite alkene, it is characterised in that the low-molecular-weight alcohol and/
Or the mass ratio of the aqueous solution of ketone, low-molecular-weight alcohol and/or ketone and water is 1:10-2:1.
4. the method that high speed according to claim 2 peels off white graphite alkene, it is characterised in that the low-molecular-weight alcohol is：
At least one of methanol, ethanol, isopropanol, the tert-butyl alcohol, ethylene glycol；The low-molecular-weight ketone is acetone.
5. the method that high speed according to claim 1 peels off white graphite alkene, it is characterised in that the surfactant is tool
At least one of surfactant of long-chain lewis acid or long-chain lewis base.
6. the method that high speed according to claim 5 peels off white graphite alkene, it is characterised in that the long-chain lewis acid
For：Higher fatty acids, aliphatic ketone, alicyclic ketone, fatty aldehyde, and its at least one of corresponding derivative；The long-chain Louis
Alkali is：At least one of aromatic compound, amine, ether.
7. the method that high speed according to claim 6 peels off white graphite alkene, it is characterised in that the long-chain lewis acid table
Face activating agent is：Palmitic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, palmitic acid, 18 ketone, 3- methyl cyclotridecanone, ring ten
At least one of four alkanones, 16 ketone of 3-, palmital, arbricolin or eicosane aldehyde；
The long-chain lewis base surfactant is：Palmitamide, heptadecyl-amine, octadecylamine, oleyl amine, Cholestyramine, end amido gather
Ethylene glycol, polyphenylacetylene, polythiophene, kayexalate, detergent alkylate, 4- dodecyl polyanilines, polyoxyethylene octane
Alkylphenol ether, glycidol 12-14 alkyl ethers, six polyethyleneglycol margarons, four ethene glycol lists, ten tetraether, six polyethylene glycol
At least one of single ten tetraethers.
8. the method that high speed according to claim 1 peels off white graphite alkene, it is characterised in that after injection is peeled off once, by
Change in slurry fluidity, continue to add decentralized medium, the additive amount of the decentralized medium is the 1/5-5 of original solvents quality
Times, cyclic spray peels off once or more.
9. the method that high speed according to claim 1 peels off white graphite alkene, it is characterised in that described white when injection is peeled off
The mass ratio of graphene (h-BN) powder and surfactant is 10:1-100:1；The white graphite alkene (h-BN) and decentralized medium
It is 1 to add mass ratio:10-1:100.
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| CN110255513A (en) * | 2019-06-19 | 2019-09-20 | 常州兴烯石墨烯科技有限公司 | A kind of hydrophilic modifying white graphite alkene and preparation method thereof |
| CN113264778A (en) * | 2021-05-17 | 2021-08-17 | 厦门理工学院 | Boron nitride composite ceramic and preparation method and application thereof |
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| CN106865508A (en) * | 2016-12-12 | 2017-06-20 | 广东纳路纳米科技有限公司 | A kind of method that white graphite alkene is peeled off in high speed dispersion |
| CN113025283B (en) * | 2019-12-25 | 2022-06-17 | 东莞新能德科技有限公司 | Phase change material, preparation method thereof and electronic component |
| CN113247868B (en) * | 2021-04-14 | 2022-11-11 | 佛山市晟鹏科技有限公司 | Two-dimensional material and preparation method and application thereof |
| KR102644774B1 (en) * | 2021-05-04 | 2024-03-08 | 티엠티피 랩스, 아이엔씨. | Apparatus and method for exfoliating graphite |
| CN115368758A (en) * | 2022-09-13 | 2022-11-22 | 安徽大学 | Non-ionic surfactant non-covalent modified boron nitride heat-conducting filler and heat-conducting composite material based on same |
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