CN105731440B - A kind of utilization phase change materials peel off the method for preparing graphene microchip - Google Patents
A kind of utilization phase change materials peel off the method for preparing graphene microchip Download PDFInfo
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Abstract
The present invention proposes that a kind of utilization phase change materials peel off the method for preparing graphene microchip.This method is using graphite as raw material, graphite powder is modified by using boric acid, phase change materials are made to insert graphite layers in the blown state, solid phase is changed into by liquid phase using phase change materials and occurs the microdefect that volume contraction is formed, pull open graphite layers, further, mechanical shearing is peeled off under freezing conditions, crystal grain embrittlement peels off graphite linings moment to phase change materials under freezing conditions, so as to obtain graphene microchip, the cost of graphene microchip is greatly reduced, make graphene microchip in rubber, plastics, coating, lubricating oil, the composites such as sewage disposal can largely be added and used.Preparation method of the present invention is easily controllable, and scale steady production can be achieved, and the auxiliary material that production process is used easily is cleaned and crystallized and reused after precipitation, is realized pollution-free preparation graphene microchip, is conducive to promoting the large-scale application of graphene.
Description
Technical field
The present invention relates to grapheme material field, and in particular to the preparation method of graphene microchip, more particularly to a kind of
The method for preparing graphene microchip is peeled off using phase change materials.
Background technology
Graphene is the flaky substance for referring exclusively to be made up of single carbon atom theoretically.At present, simplest method is logical
Mechanical phonograph recorder separation is crossed, directly cuts down graphene platelet from larger graphite crystal.It can also be made by expanded, friction
The surface of graphite produces flocculus, the graphene containing individual layer in the crystal of these flocculus shapes.But have the disadvantage that the above method is obtained
Thin slice filter out the graphene platelet of individual layer, its size is difficult to control, it is impossible to reliably manufacture stable graphene film.
Advanced graphene preparation method mainly takes vapour deposition process, in base after being decomposed at high temperature using gaseous carbon source
Catalytic growth on body surface face prepares graphene, and this method is to prepare high-quality and large area single-layer graphene important side
Method.But its working condition is more harsh, power consumption is big, and cost is high.Moreover, directly largely being added using gaseous carbon sources
The danger of production.
The country mainly uses graphite oxide reducing process to prepare the main method of graphene at present, and this method is to enter graphite
The processing of row Strong oxdiative, obtains after graphite oxide, then carries out stripping to it preparing graphene oxide, eventually pass reduction treatment and obtain
Graphene.Graphite oxide is warming up to 150 by Chinese invention patent 200810151807.X with certain heating rate under a high vacuum
~600 DEG C, 0.5~20H of constant temperature is maintained, graphene oxide sheet is obtained.Due to the meeting heavy damage graphene during Strong oxdiative
The structure of lamella, although pass through reduction treatment, the electron conjugated structure of graphene sheet layer obtains part recovery, gained graphene material
Still there is larger gap with high-quality graphene in the property indices of material.In addition, the oxidizing process of graphite is usually required
High-temperature process in need or make during substantial amounts of highly acid the oxidant such as concentrated sulfuric acid, concentrated nitric acid, potassium permanganate etc., and reduction
With the poisonous chemical substance such as hydrazine hydrate, sodium borohydride, not only energy consumption is big, and efficiency is low, and cost is high and pollutes environment.
Mechanical stripping method is a kind of to prepare the method simple and easy to apply of high-quality graphene with low cost.In order that stone
Peeling-off between layer of ink, the conventional stripping means of mechanical-physical stripping method have conventional ball mill, stirring ball-milling, grinding etc..But borrow
Grinding aid ball is ground to graphite composite powder, and this method is big due to the local pressure that applies, and powerful impulsive force can make graphene produce knot
Structure defect.Chinese invention patent application number 201280019582.7 discloses a kind of method for preparing graphene, passes through grinding, ball
Mill, airflow milling etc. grind 4 hours acquisition graphenes by ionic liquid.The stripping of graphite is promoted by ionic liquid, but is adopted
The graphene crystalline size obtained with prolonged grinding is small, and by ionic liquid graphene layer lattice can be made to be affected.
In fact, the preparation of single-layer graphene is also rested in a small amount of preparation in grams at present, large-scale industry
Also no one else can do for metaplasia production.But meanwhile, the excellent performance of graphene is badly in need of in composite, lubriation material, coating, sewage
The fields such as processing are widely applied, and prior art is difficult to meet this large-scale demand.Therefore using graphene as the stone of unit
Black alkene microplate turns into the optimal selection that graphene enters from research to application.Graphene microchip, as multi-layer graphene structure, but
The characteristic of graphene, such as conduction, heat conduction, printing opacity, flexibility etc. are kept very well, can be wide as a kind of industrial raw materials
It is added to generally in existing various basic materials, the performance to current material is improved.In order to obtain graphene microchip, in
State's invention number of patent application 201310579504.9 discloses the controllable graphene microchip preparation side of a kind of high-specific surface area, size
Method, this method prepares highly expanded multiplying power expanded graphite using big particle diameter expansible graphite as raw material under high temperature；Using organic matter as intercalation
In thing, blending insertion expanded graphite lamella, the high-temp combustion under certain atmosphere, the graphene that acquisition certain size is peeled off in expansion is micro-
Piece.However, it is necessary to higher subnormal ambient realizes the successful expansion of graphite oxide in the thermal expansion process of graphite oxide,
Its condition is harsher, and the requirement to equipment is high, it is impossible to continuous production, it is difficult to amplify, and restricts the development of graphene microchip.
The good characteristic that graphene microchip is possessed due to it, its application field is boundless, for example improves the heat conduction of plastic cement
And heat dispersion, plastic cement is conductive and antistatic modified, strengthens the intensity of plastic cement, and improves the wear-resisting of plastic cement, greasy property and resistance to
Corrosivity etc..Due to nano thickness, being easily uniformly combined with other materials such as polymeric material, and form good be combined
Interface, graphene microchip can take the high intensity of graphene, lubrication, high temperature resistant and conductive characteristic among composite to,
So as to design, prepare high-performance composite materials.Such as graphite alkene plastics, graphene rubber, Graphene conductive ink, graphene
It is all good application that coating, graphene, which inhale ripple hidden function plate, graphene radiating element, graphene functional coating etc.,.We
Expect to realize under conditions of graphene layer crystal structure is not damaged and efficiently peel off graphite to prepare graphene microchip, so as to be big
Scale application graphene provides technical support.
The content of the invention
In view of the above-mentioned problems, the present invention proposes that a kind of utilization phase change materials peel off the method for preparing graphene microchip.Should
Method is changed into solid phase by liquid phase using phase-change material and occurs the microdefect that volume contraction is formed, mechanical under freezing conditions
Shearing peel off obtain graphene microchip, the cost of graphene microchip is greatly reduced, make graphene microchip rubber, plastics, coating,
The composites such as lubricating oil, sewage disposal can largely be added and used.
To solve the above problems, the present invention uses following technical scheme：
A kind of utilization phase change materials peel off the method for preparing graphene microchip, it is characterised in that：Using phase change materials as
Intercalator, graphite powder interlayer is placed in by intercalator, and being changed into solid phase by liquid phase using phase change materials occurs volume contraction
The microdefect of formation, is peeled off by mechanical shearing and obtains graphene microchip, and specific method is as follows：
（1）Graphite powder and absolute methanol or absolute ethyl alcohol are pressed into quality 1:10-30, stirs 30-45min at ambient temperature
Well mixed, addition boric acid, which is stirred to boric acid, to be completely dissolved, and more than 24h is placed in closing, isolates absolute methanol or absolute ethyl alcohol,
Dry, obtain pretreating graphite powder, the addition of its mesoboric acid is the 3-5% of graphite powder quality；
（2）Phase change materials are heated under the conditions of 40-60 DEG C to be completely melt, by step（1）Obtained pretreatment stone
Ink powder is added in the phase change materials being completely melt, is disperseed 1-2h with 200-800r/min rotating speed high-speed stirred, is made phase in version
Material inserts the interlayer of graphite, naturally cools to room temperature, the wherein mass ratio of pretreating graphite powder and phase change materials is 1:
0.1-0.5；Be when phase change materials are room temperature be liquid phase under the conditions of crystalloid solid phase, 40-60 DEG C phase-change material；
(3）By step（2）Obtained intercalated graphite is added in mechanical shearing stripping off device, is maintained at by liquid nitrogen input
Under cryogenic conditions less than -15 DEG C, peel off to sheet thickness and be less than in the range of 50 nm, then discharge；
（4）By step（3）Obtained material is cleaned in cleaning machine with deionized water, ethanol, except maize without germ, phase turn
Become material, dry, obtain graphene microchip.
Described phase-change material is one kind in crystalloid, preferably positive certain herbaceous plants with big flowers acid, laurate, myristic acid in solid phase.
Described phase-change material is hydrated salt.
Described hydrated salt is in Sodium acetate trihydrate, five water sodium thiosulfate, disodium hydrogen phosphate, sal glauberi
One kind, be in molten condition at 40-60 DEG C, easily combined with the layer part of graphite, and in room temperature, hydrated salt is due to phase in version
To crystalline transformation, occurs volume contraction, so that microdefect is produced in graphite layers, further as hydrated salt crystal in low temperature
Easily occur embrittlement, thus under the cryogenic conditions less than -15 DEG C, can peel off graphite by mechanical shearing stripping off device turns into
Graphene microchip.
Described mechanical shearing stripping off device is conventional medium grinder such as agitating ball mill, planetary ball mill, shaken
Dynamic ball mill, rotary-tube type ball mill, sand mill, or airslide disintegrating mill such as flat air flow crusher, circulating tube type air-flow
It is pulverizer, rotary ejection type airslide disintegrating mill, injecting type airslide disintegrating mill, target formula airslide disintegrating mill, fluidized bed airflow pulverizer, right
Push-style airslide disintegrating mill, or high pressure grinding rolls.
The Van der Waals force of graphite powder interlayer causes graphite layers to be difficult to smoothly peel off, by can be effective in interlayer intercalation
Van der Waals force is reduced, but this intercalation is still to be difficult to separate graphite linings.Although having organic or inorganic intercalator at present,
But effect is unsatisfactory, particularly it is difficult to volume production and prepares graphene microchip.The characteristics of present invention is prominent is to propose that one kind utilizes phase
Transition material peels off the method for preparing graphene microchip, and this method is modified using graphite as raw material by using boric acid to graphite powder,
Phase-change material is set to insert graphite layers in the blown state, being changed into solid phase by liquid phase using phase-change material occurs volume receipts
Contract the microdefect formed, pulls open graphite layers, further, is peeled off under freezing conditions using mechanical shearing, and phase-change material is
Crystalloid, enbrittles, and crystal grain embrittlement under freezing conditions peels off graphite linings moment, so as to obtain graphene microchip.Enter one
Step, the present invention, as auxiliary agent is prepared, is easily cleaned using boric acid, phase-change material and crystallizes recycling after precipitation, realize nothing
Pollution prepares graphene microchip.
A kind of utilization phase change materials of the present invention peel off the method for preparing graphene microchip, realize large-scale production graphite
Alkene microplate, is greatly reduced the cost of graphene microchip, and graphene microchip has nano thickness, easily with other materials such as polymer
Material is uniformly combined, and forms good compound interface；With the characteristic such as excellent conduction, lubrication, corrosion-resistant, high temperature resistant.Can
A large amount of additions are used in the composites such as rubber, plastics, coating, lubricating oil, sewage disposal.
Tested by the graphene microchip obtained to preparation method of the present invention, its thickness is in the range of 15-50 nm, in stone
Black alkene stratiform accumulation body.By operating specification of the graphene microchip according to Nano filling, ABS is scattered in 3% mass fraction filling
In resin, the electrical conductivity of its composite reaches 2.6 × 10-4 S/cm。
A kind of utilization phase of the present invention turns material and becomes the method peeled off and prepare graphene microchip, compared with prior art, and it is dashed forward
The characteristics of going out and excellent effect are：
1st, graphite powder is modified using boric acid, phase-change material is inserted graphite layers in the blown state, utilize phase in version
Material is changed into solid phase by liquid phase and occurs the microdefect that volume contraction is formed, and pulls open graphite layers, becomes graphite and serve as reasons
The graphene microchip of graphene unit accumulation.
2nd, mechanical shearing is peeled off under freezing conditions, and crystal grain embrittlement makes graphite linings moment to phase change materials under freezing conditions
Peel off, so as to obtain graphene microchip.
3rd, preparation method of the present invention is easily controllable, and scale steady production, the auxiliary material that production process is used can be achieved
Easily clean and crystallize and reused after precipitation, realize pollution-free preparation graphene microchip, Productive statistics are small, cost is low, tool
There is significant market application value.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill
Various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A kind of utilization phase change materials peel off the method for preparing graphene microchip, and specific method is as follows：
（1）Graphite powder and absolute ethyl alcohol are pressed into quality 1:30,45min is stirred at ambient temperature and is well mixed, and adds boron
Acid stirring to boric acid is completely dissolved, and more than 24h is placed in closing, isolates absolute ethyl alcohol, is dried, is obtained pretreating graphite powder, its
The addition of mesoboric acid is the 4% of graphite powder quality；
（2）Sodium acetate trihydrate is heated under the conditions of 40 DEG C to be completely melt, by step（1）Obtained pretreating graphite powder
The Sodium acetate trihydrate being completely melt is added, 2h is disperseed with 500r/min rotating speed high-speed stirred, Sodium acetate trihydrate is inserted graphite
Interlayer, naturally cool to room temperature, wherein the mass ratio of pretreating graphite powder and Sodium acetate trihydrate is 1:0.4；
(3）By step（2）Obtained intercalated graphite is added in agitating ball mill stripping off device, is inputted and kept by liquid nitrogen
Under the cryogenic conditions less than -15 DEG C, peel off to sheet thickness and be less than in the range of 50nm, then discharge；
（4）By step（3）Obtained material is cleaned in cleaning machine with deionized water, except maize without germ, acetate trihydrate
Sodium, dries, obtains graphene microchip.
Embodiment 2
A kind of utilization phase change materials peel off the method for preparing graphene microchip, and specific method is as follows：
（1）Graphite powder and absolute methanol are pressed into quality 1:10,30min is stirred at ambient temperature and is well mixed, and adds boron
Acid stirring to boric acid is completely dissolved, and more than 24h is placed in closing, isolates absolute methanol, is dried, is obtained pretreating graphite powder, its
The addition of mesoboric acid is the 5% of graphite powder quality；
（2）Sal glauberi is heated under the conditions of 60 DEG C to be completely melt, by step（1）Obtained pretreating graphite powder
The sal glauberi being completely melt is added, 2h is disperseed with 200r/min rotating speed high-speed stirred, sal glauberi is inserted graphite
Interlayer, naturally cool to room temperature, wherein the mass ratio of pretreating graphite powder and sal glauberi is 1:0.5；
(3）By step（2）Obtained intercalated graphite is added in circulation pipe air flow crasher shearing stripping off device, is passed through
Liquid nitrogen input is maintained under the cryogenic conditions less than -15 DEG C, is peeled off to sheet thickness and is less than 50nm scopes, then discharges；
（4）By step（3）Obtained material is cleaned in cleaning machine with deionized water, except maize without germ, ten water sulfuric acid
Sodium, dries, obtains graphene microchip.
Embodiment 3
A kind of utilization phase change materials peel off the method for preparing graphene microchip, and specific method is as follows：
（1）Graphite powder and absolute ethyl alcohol are pressed into quality 1:15,45min is stirred at ambient temperature and is well mixed, and adds boron
Acid stirring to boric acid is completely dissolved, and more than 24h is placed in closing, isolates absolute ethyl alcohol, is dried, is obtained pretreating graphite powder, its
The addition of mesoboric acid is the 3% of graphite powder quality；
（2）Five water sodium thiosulfate are heated to being completely melt under the conditions of 50 DEG C, by step（1）Obtained pretreatment stone
Ink powder is added in five water sodium thiosulfate being completely melt, is disperseed 1h with 800r/min rotating speed high-speed stirred, is made five water thio
Sodium sulphate inserts the interlayer of graphite, naturally cools to the mass ratio of room temperature, wherein pretreating graphite powder and five water sodium thiosulfate
For 1:0.3；
(3）By step（2）Obtained intercalated graphite is added in target formula airslide disintegrating mill mechanical shearing stripping off device, is passed through
Liquid nitrogen input is maintained under the cryogenic conditions less than -15 DEG C, is peeled off to sheet thickness and is less than in the range of 50nm, then discharges；
（4）By step（3）Obtained material is cleaned in cleaning machine with deionized water, except maize without germ, five water are thio
Sodium sulphate, dries, obtains graphene microchip.
Embodiment 4
A kind of utilization phase change materials peel off the method for preparing graphene microchip, and specific method is as follows：
（1）Graphite powder and absolute methanol are pressed into quality 1:30,30min is stirred at ambient temperature and is well mixed, and adds boron
Acid stirring to boric acid is completely dissolved, and more than 24h is placed in closing, isolates absolute methanol, is dried, is obtained pretreating graphite powder, its
The addition of mesoboric acid is the 3% of graphite powder quality；
（2）Disodium hydrogen phosphate is heated under the conditions of 60 DEG C to be completely melt, by step（1）Obtained pretreatment
Graphite powder is added in the disodium hydrogen phosphate being completely melt, is disperseed 1.5h with 400r/min rotating speed high-speed stirred, is made ten
Phosphate dihydrate disodium hydrogen inserts the interlayer of graphite, naturally cools to room temperature, wherein pretreating graphite powder and ten hydrogen phosphate dihydrates two
The mass ratio of sodium is 1:0.1；
(3）By step（2）Obtained intercalated graphite is added in high pressure grinding rolls mechanical shearing stripping off device, defeated by liquid nitrogen
Enter and be maintained under the cryogenic conditions less than -15 DEG C, peel off to sheet thickness and be less than in the range of 50 nm, then discharge；
（4）By step（3）Obtained material is cleaned in cleaning machine with deionized water, except maize without germ, 12 water phosphorus
Sour disodium hydrogen, dries, obtains graphene microchip.
Embodiment 5
A kind of utilization phase change materials peel off the method for preparing graphene microchip, and specific method is as follows：
（1）Graphite powder and absolute methanol are pressed into quality 1:30,30min is stirred at ambient temperature and is well mixed, and adds boron
Acid stirring to boric acid is completely dissolved, and more than 24h is placed in closing, isolates absolute methanol, is dried, is obtained pretreating graphite powder, its
The addition of mesoboric acid is the 3% of graphite powder quality；
（2）Myristic acid is heated under the conditions of 60 DEG C to be completely melt, by step（1）Obtained pretreating graphite powder adds
Enter in the myristic acid being completely melt, 1.5h is disperseed with 400r/min rotating speed high-speed stirred, myristic acid is inserted graphite
Interlayer, naturally cools to room temperature, the wherein mass ratio of pretreating graphite powder and myristic acid is 1:0.1；
(3）By step（2）Obtained intercalated graphite is added in rotary ejection type airslide disintegrating mill mechanical shearing stripping off device, is led to
Cross liquid nitrogen input to be maintained under the cryogenic conditions less than -15 DEG C, peel off to sheet thickness and be less than in the range of 50 nm, then discharge；
（4）By step（3）Obtained material is cleaned in cleaning machine with deionized water, ethanol, except maize without germ, Pork and beans
Cool acid, dries, obtains graphene microchip.
Embodiment 6
A kind of utilization phase change materials peel off the method for preparing graphene microchip, and specific method is as follows：
（1）Graphite powder and absolute methanol are pressed into quality 1:10,30min is stirred at ambient temperature and is well mixed, and adds boron
Acid stirring to boric acid is completely dissolved, and more than 24h is placed in closing, isolates absolute methanol, is dried, is obtained pretreating graphite powder, its
The addition of mesoboric acid is the 5% of graphite powder quality；
（2）Laurate is heated under the conditions of 60 DEG C to be completely melt, by step（1）Obtained pretreating graphite powder is added
The laurate being completely melt, disperses 2h with 200r/min rotating speed high-speed stirred, laurate is inserted the interlayer of graphite, naturally cold
But to room temperature, wherein pretreating graphite powder and lauric mass ratio are 1:0.5；
(3）By step（2）Obtained intercalated graphite is added in circulation pipe air flow crasher shearing stripping off device, is passed through
Liquid nitrogen input is maintained under the cryogenic conditions less than -15 DEG C, is peeled off to sheet thickness and is less than 50nm scopes, then discharges；
（4）By step（3）Obtained material is cleaned in cleaning machine with deionized water, ethanol, except maize without germ, bay
Acid, dries, obtains graphene microchip.
Claims (7)
1. a kind of utilization phase change materials peel off the method for preparing graphene microchip, it is characterised in that：It is slotting using phase change materials
Layer agent, graphite powder interlayer is placed in by intercalator, and being changed into solid phase by liquid phase using phase change materials occurs volume contraction shape
Into microdefect, peeled off by mechanical shearing and obtain graphene microchip, specific method is as follows：
（1）Graphite powder and absolute methanol or absolute ethyl alcohol are pressed into quality 1:10-30, stirs 30-45min mixing at ambient temperature
Uniformly, addition boric acid, which is stirred to boric acid, is completely dissolved, and more than 24h is placed in closing, isolates absolute methanol or absolute ethyl alcohol, is done
It is dry, pretreating graphite powder is obtained, the addition of its mesoboric acid is the 3-5% of graphite powder quality；
（2）Phase change materials are heated under the conditions of 40-60 DEG C to be completely melt, by step（1）Obtained pretreating graphite powder
Add in the phase change materials being completely melt, 1-2h is disperseed with 200-800r/min rotating speed high-speed stirred, makes phase change materials
The interlayer of graphite is inserted, room temperature is naturally cooled to, the wherein mass ratio of pretreating graphite powder and phase change materials is 1:0.1-
0.5；Be when phase change materials are room temperature be liquid phase under the conditions of crystalloid solid phase, 40-60 DEG C phase-change material；
(3）By step（2）Obtained intercalated graphite is added in mechanical shearing stripping off device, is maintained at low by liquid nitrogen input
In under -15 DEG C of cryogenic conditions, peel off to sheet thickness and be less than in the range of 50 nm, then discharge；
（4）By step（3）Obtained material is cleaned in cleaning machine with deionized water, ethanol, except maize without germ, phase in version material
Material, dries, obtains graphene microchip.
2. a kind of utilization phase change materials peel off the method for preparing graphene microchip according to claim 1, it is characterised in that：
Described phase-change material is one kind in positive certain herbaceous plants with big flowers acid, laurate, myristic acid.
3. a kind of utilization phase change materials peel off the method for preparing graphene microchip according to claim 1, it is characterised in that：
Described phase-change material is hydrated salt.
4. a kind of utilization phase change materials peel off the method for preparing graphene microchip according to claim 3, it is characterised in that：
Described hydrated salt is one kind in Sodium acetate trihydrate, five water sodium thiosulfate, disodium hydrogen phosphate, sal glauberi.
5. a kind of utilization phase change materials peel off the method for preparing graphene microchip according to claim 1, it is characterised in that：
Described mechanical shearing stripping off device be agitating ball mill, planetary ball mill, vibrator, rotary-tube type ball mill or
Sand mill.
6. a kind of utilization phase change materials peel off the method for preparing graphene microchip according to claim 1, it is characterised in that：
Described mechanical shearing stripping off device be flat air flow crusher, circulation pipe air flow crasher, rotary ejection type airslide disintegrating mill,
Injecting type airslide disintegrating mill, target formula airslide disintegrating mill, fluidized bed airflow pulverizer or Counter-impact flow pulverizer.
7. a kind of utilization phase change materials peel off the method for preparing graphene microchip according to claim 1, it is characterised in that：
Described mechanical shearing stripping off device is high pressure grinding rolls.
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