CN106044920B - A kind of graphene microchip and preparation method thereof with network structure - Google Patents
A kind of graphene microchip and preparation method thereof with network structure Download PDFInfo
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- CN106044920B CN106044920B CN201610372745.XA CN201610372745A CN106044920B CN 106044920 B CN106044920 B CN 106044920B CN 201610372745 A CN201610372745 A CN 201610372745A CN 106044920 B CN106044920 B CN 106044920B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
Abstract
The graphene microchip and preparation method thereof with network structure that the invention discloses a kind of.The present invention in graphene microchip by being added grafted functional group, and during grafting in graphene microchip generate micropore method obtained it is a kind of with regular three-dimensional net structure, the graphene microchip that stability is good, adsorption rate is high, composite performance is excellent, the network structure graphene microchip adsorptivity with super strength, suitable for heavy metal adsorption, sewage treatment, greasy dirt collection, sea water desalination, drink water purifying, and can be carried out under wider temperature range, wider pH value range, wide ion component using.
Description
Technical field
The present invention relates to the technical fields of graphene, the in particular to technical field of Graphene derivative.
Background technique
Graphene is that a kind of carbon atom is closely arranged by regular hexagon as cellular plane atomic crystal structure, graphene
Distinctive planar structure makes it have the characteristic that many three-dimensional crystals do not have, if specific surface area is up to 2.6 × 103m2/g,
Thermal coefficient is up to 3 × 103W/(m.K), mechanical property is 1.06 × 103Gpa, Young's modulus 1.0TPa, mechanical strength
Up to 130Gpa is more than 100 times of steel.There is graphene stable regular hexagon lattice structure to make it have excellent conduction
Property, electron mobility is up to 1.5 × 104cm2/ (V.s), it is 2 times higher than the maximum mobility of semiconductor indium antimonide, than commercial silicon wafer
Maximum mobility it is 10 times high, furthermore graphene also has very high light transmission, room-temperature quantum tunnel-effect, unusual quantum suddenly
Your effect etc..
Come from structure, the super macromolecular substances that graphene is made of together countless phenyl ring polymerizations, thus
Graphene also has the response characteristic of poly-ring aromatic compounds to a certain extent, can be hydrogenated, be fluorinated, with it is other organic
Object polymerization etc..
Under normal conditions, C-C bond is very stable in graphene, inside be difficult to Lock-in missing carbon atom,
Therefore chemical property is sufficiently stable, but its edge has reactivity rich in dangling bond, scarce key or oxygen-containing functional group, can be with it
Its organic molecule is polymerize.And because preparing for graphene oxide is relatively easy, therefore using graphene oxide before
It is one of the most common means realizing graphene and polymerizeing with organic molecule that body, which is driven, with reacting for small organic molecule.
Shortage of water resources is one of the ultimate challenge that faces always of the whole world, account for 70% or more area of the earth be can not be direct
The seawater of reference has in still remaining freshwater resources and largely there is pollution, therefore sea water desalination and sewage treatment are to solve water
The big technical problem of the two of shortage of resources.During solving both of these problems, researcher has found that nano material is capable of providing
Subnano-class channel provides the transmission channel of high speed for hydrone, and prevents passing through for macromolecular simultaneously, so as to realize sea
The fast purification of the quick desalination and sewage of water.
Graphene is due to its sp2Honeycomb crystal structure that the close arrangement of hydbridized carbon atoms is formed and show special
Mass-transfer performance can introduce nano-pore or the packed structures of engineer on graphene film body, form the choosing of high-permeability
Selecting property permeable membrane, while the porous structure of graphene and its composite material makes it have the higher rate of adsorption, and high ratio table
Area makes it have bigger effective adsorption area, these characteristics integrate make graphene have fast and efficiently absorption with
Detergent power.
A kind of sewage treatment graphene macroform material is disclosed in Chinese patent application CN105126764A, is passed through
(1) it is ultrasonically treated graphene oxide water solution；(2) graphene oxide solution and graphene fiber film are added in reaction kettle, adds
Natural cooling after heat to constant temperature, freeze-drying have obtained a kind of gap structure prosperity, large specific surface area, the stone for sewage treatment
Black alkene material, preparation method of the present invention is simple, but the application performance of material is still not excellent enough, and speculates product according to preparation method
Yield may be lower.
One kind is disclosed in Chinese patent application CN102992305 can be used as lithium ion battery positive and negative electrode material, super electricity
Container electrode material, catalysis material and absorption, material for water treatment grapheme material, it is by using ultrasound that graphite oxide is equal
It is even to be dispersed in water, short chain alcohol is added thereafter and carries out the obtained porous graphene water of hydro-thermal reaction at 80 ~ 280 DEG C as reducing agent
Colloidal sol, then the porous graphene hydrosol is obtained into porous solid graphene through vacuum freeze drying.
Summary of the invention
It is an object of the invention to propose it is a kind of with regular three-dimensional net structure, stability is good, adsorption rate is high, compound
The graphene microchip haveing excellent performance, which is different from the grapheme material in above-mentioned published patent application, by graphite
Alkenyl body and other organic molecules are combined, and are non-fully made of graphite alkenes material, therefore have superior compound
Performance.
The present invention proposes the preparation method of the graphene microchip simultaneously.
Technical scheme is as follows:
A kind of graphene microchip with network structure, the graphene microchip of the network structure include graphene sheet layer structure
And the reticular structure of connection graphene film interlayer, the graphene sheet layer structure include at least two layers of graphene, the netted knot
Structure by mono- graphene sheet layer structure of an end Jie, it is another terminate in another adjacent graphene sheet layer structure, molecule
Organic molecule material composition interconnected between chain main body.
Preferably, the preparation method of the graphene microchip of network structure, it is characterised in that: the following steps are included:
(1) graphite is removed as graphene microchip；
(2) graphene microchip is prepared as by graphene oxide microplate by Hummers method or amendment Hummers；
(3) graphene oxide microplate is dispersed in water, sequentially add thereto ethylenediamine, o-phenylenediamine, p-phenylenediamine,
The bentonite that acrylamide, vinyl alcohol, acrylic acid coat reacts 6 ~ 12h at 80 ~ 110 DEG C, keeps magnetic agitation in reaction；
(4) it is centrifugated after the mixing liquid for completing step (3) being carried out strong stirring, light fraction is filtered again,
Obtained solid is presoma；
(5) presoma is carried out to reduction reaction with hydrogen under inert gas protection to get to network structure
Graphene microchip.
In above-mentioned steps, removing described in step (1) refers mainly to mechanical stripping, because of the invention mainly micro- using graphene
Piece, does not need the graphene of single layer especially, thus the removing be not necessarily it is high-precision, stringent, graphite is removed as single layer
Process.
The present invention has selected first to aoxidize graphene microchip, and its object is to improve graphene microchip and other functions
Group grafting ability, it is to be understood that if directly apply graphene, the present invention in small organic molecule can also with its into
Row functionalization, but the extent of reaction may be smaller, needs additional activator or only generates in graphene microchip edge.
Hummers method main process described in step (2) is that dense sulphur is added in graphene microchip and sodium nitrate under ice bath
In acid, then potassium permanganate is added by several times, control reaction temperature is no more than 20 DEG C, carries out reaction a period of time, heats up thereafter, is added
Deionized water adds appropriate hydrogen peroxide, thereafter heat filtering, is finally washed and is dried using dilute hydrochloric acid and deionized water, obtained
Graphene oxide microplate.The process of the amendment Hummers method is main are as follows: under ice bath, by graphene microchip and sodium nitrate
It is added in the concentrated sulfuric acid, is slow added into potassium permanganate, control reaction temperature is no more than 10 DEG C, takes after stirring 2h under condition of ice bath
Out, reaction 5d is stirred at room temperature thereafter, mixing liquid is diluted using dilute sulfuric acid thereafter, adds appropriate hydrogen peroxide,
It is centrifuged after being stirred to react 2h, is finally washed repeatedly using dilute sulfuric acid, hydrogen peroxide mixed solution and dilute hydrochloric acid and further uses distillation
Water washing, it is dry, obtain graphene oxide microplate.
It is that can increase graphene oxide microplate because ethylenediamine has activation effect that ethylenediamine is firstly added in step (3)
Grafting rate, while bentonite its purpose that acrylic acid cladding is added in step (3) be on the one hand to make acrylic acid also assist in into
In grafting, on the other hand with the consumption of acrylic acid, the bentonite of cladding is exposed in mixing liquid, swelling after contacting with water
The soil body accumulates rapid expanding, generates obvious impact to graphene oxide microplate, therefore generate graphene oxide microplate by bentonite
The micropore of occupy-place.
The stronger stirring of dispersion effect that strong stirring in step (4) refers to can be the big mechanical stirring of revolving speed,
It can be ultrasonic vibration, its object is to separate bentonite with the graphene oxide microplate of network structure.
The purpose of step (5) is graphene oxide microplate being reduced to graphene microchip, therefore improves its chemical stabilization
Property.
A kind of preferred embodiment of above-mentioned preparation method are as follows: the quality of the graphene oxide microplate and the ethylenediamine
For 6 ~ 10:1 ~ 3.
Another preferred embodiment of the preparation method are as follows: the matter of the graphene oxide microplate and the o-phenylenediamine
Amount is 6 ~ 10:1 ~ 3, and the mass ratio with the p-phenylenediamine is 6 ~ 10:2 ~ 5.
Another preferred embodiment of the preparation method are as follows: the matter of the graphene oxide microplate and the acrylamide
Amount is 6 ~ 10:2 ~ 5.
Another preferred embodiment of the preparation method are as follows:: the matter of the graphene oxide microplate and the vinyl alcohol
Amount is 6 ~ 10:1 ~ 3.
Another preferred embodiment of the preparation method are as follows: the graphene oxide microplate and acrylic acid cladding
Bentonitic quality is 6 ~ 10:1 ~ 3.
Another preferred embodiment of the preparation method are as follows: the temperature of reduction reaction described in the step (5) is 300
~ 500 DEG C, the time is 1 ~ 2h.
Another preferred embodiment of the preparation method are as follows: the preparation method for bentonite of the acrylic acid cladding are as follows:
Bentonite, isopropanol, acrylic acid and ammonium persulfate are added in flask, under stiring, 1 is heated at reflux in 80 ~ 90 DEG C of constant temperature ~
2h, maintains thereafter stirring, and 10 ~ 30min of natural cooling filters to get the bentonite coated to the acrylic acid.
The preparation method for bentonite of above-mentioned acrylic acid cladding it is further preferred are as follows: the acrylic acid and bentonitic matter
Amount is than being 1 ~ 3:2 ~ 10.
Using network structure of the invention graphene microchip when, water to be processed can be passed through thereon, hydrone from
Pass through in the micropore of graphene microchip, heavy metal ion or salt ion are blocked on outside graphene microchip, and are connected with graphene
Reticular structure organic molecule material have stronger water absorption function, micropore of the hydrone from graphene microchip can be accelerated
In the rate that passes through, while also there is microcellular structure inside the organic molecule of these reticular structures, can be filtered and inhale simultaneously
It is attached, enhance water purification ability, in addition, the organic molecule of these reticular structures is distributed between multiple graphene sheet layer structures, it is to be processed
It when water passes through wherein, is equivalent to and has carried out multiple filtering and absorption, the very high fresh water of cleanliness can be obtained.
The present invention in graphene microchip by being added grafted functional group, and during grafting in graphene microchip
Generate micropore method obtained it is a kind of with regular three-dimensional net structure, stability is good, adsorption rate is high, composite performance is excellent
Graphene microchip, the network structure graphene microchip adsorptivity with super strength, suitable for heavy metal adsorption, at sewage
Reason, greasy dirt collection, sea water desalination, drink water purifying, and can be in wider temperature range, wider pH value range, wide
Ion component under carry out using.
Specific embodiment
Embodiment 1:
(1) 10g graphite is removed using miniature extruder as graphene microchip；Test discovery graphene microchip is essentially 5
Layer or more graphene constitute；
(2) graphene microchip is prepared as by graphene oxide microplate by Hummers method, obtains graphene oxide microplate
16g；
(3) 2g bentonite, 10g isopropanol, 1g acrylic acid and 0.1g ammonium persulfate are added in flask, under stiring, in
80 DEG C of constant temperature are heated at reflux 2h, maintain stirring thereafter, and natural cooling 10min filters to get the bentonite coated to acrylic acid；
(4) it disperses graphene oxide microplate in 50g water, sequentially adds 1g ethylenediamine, 1g o-phenylenediamine, 5g thereto
The bentonite that p-phenylenediamine, 5g acrylamide, 1g vinyl alcohol, 1g acrylic acid coat, 12h is reacted at 80 DEG C, is kept in reaction
Magnetic agitation；
(5) by the mixing liquid frequency of use for completing step (3) to be centrifugated after the ultrasonic vibration 30min of 20kHz, weight
Matter part is bentonite, and light fraction is the mixing liquid of the graphene oxide microplate containing network structure, again by light fraction
Secondary filtering, obtained solid are presoma；
(6) presoma is reacted to 2h with hydrogen at 300 DEG C under inert gas protection to get to network knot
The graphene microchip of structure.
Embodiment 2
(1) 10g graphite is removed using miniature extruder as graphene microchip；Test discovery graphene microchip is essentially 5
Layer or more graphene constitute；
(2) graphene microchip is prepared as by graphene oxide microplate by Hummers method, obtains graphene oxide microplate
15g；
(3) 2.5g bentonite, 10g isopropanol, 1g acrylic acid and 0.1g ammonium persulfate are added in flask, under stiring,
It is heated at reflux 1h in 90 DEG C of constant temperature, maintains stirring thereafter, natural cooling 30min filters to get the swelling coated to acrylic acid
Soil；
(4) it disperses graphene oxide microplate in 70g water, sequentially adds 2g ethylenediamine, 2g o-phenylenediamine, 3g thereto
The bentonite that p-phenylenediamine, 3g acrylamide, 2g vinyl alcohol, 2g acrylic acid coat, 6h is reacted at 110 DEG C, is kept in reaction
Magnetic agitation；
(5) by the mixing liquid frequency of use for completing step (3) to be centrifugated after the ultrasonic vibration 20min of 30kHz, weight
Matter part is bentonite, and light fraction is the mixing liquid of the graphene oxide microplate containing network structure, again by light fraction
Secondary filtering, obtained solid are presoma；
(6) presoma is reacted to 1h with hydrogen at 500 DEG C under inert gas protection to get to network knot
The graphene microchip of structure.
Embodiment 3
(1) 10g graphite is removed using miniature extruder as graphene microchip；Test discovery graphene microchip is essentially 5
Layer or more graphene constitute；
(2) graphene microchip is prepared as by graphene oxide microplate by Hummers method, obtains graphene oxide microplate
15g；
(3) 3g bentonite, 15g isopropanol, 1g acrylic acid and 0.15g ammonium persulfate are added in flask, under stiring, in
80 DEG C of constant temperature are heated at reflux 1.5h, maintain stirring thereafter, and natural cooling 20min filters to get the swelling coated to acrylic acid
Soil；
(4) disperse graphene oxide microplate in 100g water, sequentially add thereto 3g ethylenediamine, 3g o-phenylenediamine,
The bentonite that 5g p-phenylenediamine, 5g acrylamide, 3g vinyl alcohol, 3g acrylic acid coat, 8h is reacted at 100 DEG C, is protected in reaction
Hold magnetic agitation；
(5) by the mixing liquid frequency of use for completing step (3) to be centrifugated after the ultrasonic vibration 30min of 40kHz, weight
Matter part is bentonite, and light fraction is the mixing liquid of the graphene oxide microplate containing network structure, again by light fraction
Secondary filtering, obtained solid are presoma；
(6) presoma is reacted to 2h with hydrogen at 400 DEG C under inert gas protection to get to network knot
The graphene microchip of structure.
Embodiment 4
(1) 10g graphite is removed using miniature extruder as graphene microchip；Test discovery graphene microchip is essentially 5
Layer or more graphene constitute；
(2) graphene microchip is prepared as by graphene oxide microplate by amendment Hummers method, it is micro- obtains graphene oxide
Piece 17g；
(3) 1g bentonite, 15g isopropanol, 1.5g acrylic acid and 0.1g ammonium persulfate are added in flask, under stiring,
It is heated at reflux 1.5h in 85 DEG C of constant temperature, maintains stirring thereafter, natural cooling 20min filters to get the swelling coated to acrylic acid
Soil；
(4) it disperses graphene oxide microplate in 70g water, sequentially adds 1.7g ethylenediamine, 1.7g neighbour's benzene two thereto
The bentonite that amine, 3g p-phenylenediamine, 3g acrylamide, 1.7g vinyl alcohol, 1.7g acrylic acid coat, reacts 10h at 100 DEG C,
Magnetic agitation is kept in reaction；
(5) by the mixing liquid frequency of use for completing step (3) to be centrifugated after the ultrasonic vibration 20min of 20kHz, weight
Matter part is bentonite, and light fraction is the mixing liquid of the graphene oxide microplate containing network structure, again by light fraction
Secondary filtering, obtained solid are presoma；
(6) presoma is reacted to 1.5h with hydrogen at 400 DEG C under inert gas protection to get to network
The graphene microchip of structure.
Embodiment 5
(1) 10g graphite is removed using miniature extruder as graphene microchip；Test discovery graphene microchip is essentially 5
Layer or more graphene constitute；
(2) graphene microchip is prepared as by graphene oxide microplate by amendment Hummers method, it is micro- obtains graphene oxide
Piece 18g；
(3) 3g bentonite, 15g isopropanol, 2g acrylic acid and 0.2g ammonium persulfate are added in flask, under stiring, in
90 DEG C of constant temperature are heated at reflux 1.5h, maintain stirring thereafter, and natural cooling 30min filters to get the swelling coated to acrylic acid
Soil；
(4) it disperses graphene oxide microplate in 80g water, sequentially adds 3g ethylenediamine, 2g o-phenylenediamine, 2g thereto
The bentonite that p-phenylenediamine, 3g acrylamide, 2g vinyl alcohol, 2g acrylic acid coat, 12h is reacted at 80 DEG C, is kept in reaction
Magnetic agitation；
(5) by the mixing liquid frequency of use for completing step (3) to be centrifugated after the ultrasonic vibration 10min of 30kHz, weight
Matter part is bentonite, and light fraction is the mixing liquid of the graphene oxide microplate containing network structure, again by light fraction
Secondary filtering, obtained solid are presoma；
(6) presoma is reacted to 1.5h with hydrogen at 500 DEG C under inert gas protection to get to network
The graphene microchip of structure.
Embodiment 6
(1) 10g graphite is removed using miniature extruder as graphene microchip；Test discovery graphene microchip is essentially 5
Layer or more graphene constitute；
(2) graphene microchip is prepared as by graphene oxide microplate by amendment Hummers method, it is micro- obtains graphene oxide
Piece 16g；
(3) 3g bentonite, 15g isopropanol, 2g acrylic acid and 0.15g ammonium persulfate are added in flask, under stiring, in
80 DEG C of constant temperature are heated at reflux 1h, maintain stirring thereafter, and natural cooling 10min filters to get the bentonite coated to acrylic acid；
(4) it disperses graphene oxide microplate in 100g water, sequentially adds 2g ethylenediamine, 1.7g neighbour's benzene two thereto
The bentonite that amine, 3g p-phenylenediamine, 2g acrylamide, 1.7g vinyl alcohol, 2g acrylic acid coat, reacts 10h, instead at 110 DEG C
Answer middle holding magnetic agitation；
(5) by the mixing liquid frequency of use for completing step (3) to be centrifugated after the ultrasonic vibration 15min of 40kHz, weight
Matter part is bentonite, and light fraction is the mixing liquid of the graphene oxide microplate containing network structure, again by light fraction
Secondary filtering, obtained solid are presoma；
(6) presoma is reacted to 2h with hydrogen at 500 DEG C under inert gas protection to get to network knot
The graphene microchip of structure.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application
Within scope and spirit.
Claims (8)
1. a kind of graphene microchip with network structure, it is characterised in that: the graphene microchip includes graphene sheet layer knot
Structure and the reticular structure for connecting graphene film interlayer, the graphene sheet layer structure includes at least two layers of graphene, described netted
Structure by mono- graphene sheet layer structure of an end Jie, it is another terminate in another adjacent graphene sheet layer structure, point
Organic molecule material composition interconnected between subchain main body；
The graphene microchip of the network structure by being prepared following preparation method:
(1) graphite is removed as graphene microchip；
(2) graphene microchip is prepared as by graphene oxide microplate by Hummers method or amendment Hummers；
(3) graphene oxide microplate is dispersed in water, sequentially adds ethylenediamine, o-phenylenediamine, p-phenylenediamine, propylene thereto
The bentonite that amide, vinyl alcohol, acrylic acid coat reacts 6 ~ 12h at 80 ~ 110 DEG C, keeps magnetic agitation in reaction；It is described
The preparation method for bentonite of acrylic acid cladding are as follows: bentonite, isopropanol, acrylic acid and ammonium persulfate are added in flask,
Under stirring, it is heated at reflux 1 ~ 2h in 80 ~ 90 DEG C of constant temperature, maintains stirring thereafter, 10 ~ 30min of natural cooling filters to get institute is arrived
State the bentonite of acrylic acid cladding；
(4) it is centrifugated, light fraction is filtered again, gained after the mixing liquid for completing step (3) being carried out strong stirring
Solid is presoma；
(5) presoma is carried out to reduction reaction with hydrogen under inert gas protection to get the stone with network structure is arrived
Black alkene microplate.
2. the graphene microchip according to claim 1 with network structure, it is characterised in that: the graphene oxide is micro-
The mass ratio of piece and the ethylenediamine is 6 ~ 10:1 ~ 3.
3. the graphene microchip according to claim 1 with network structure, it is characterised in that: the graphene oxide is micro-
The mass ratio of piece and the o-phenylenediamine is 6 ~ 10:1 ~ 3, and the mass ratio with the p-phenylenediamine is 6 ~ 10:2 ~ 5.
4. the graphene microchip according to claim 1 with network structure, it is characterised in that: the graphene oxide is micro-
The mass ratio of piece and the acrylamide is 6 ~ 10:2 ~ 5.
5. the graphene microchip according to claim 1 with network structure, it is characterised in that: the graphene oxide is micro-
The mass ratio of piece and the vinyl alcohol is 6 ~ 10:1 ~ 3.
6. the graphene microchip according to claim 1 with network structure, it is characterised in that: the graphene oxide is micro-
Piece and the bentonitic mass ratio of acrylic acid cladding are 6 ~ 10:1 ~ 3.
7. the graphene microchip according to claim 1 with network structure, it is characterised in that: the acrylic acid and swelling
The mass ratio of soil is 1 ~ 3:2 ~ 10.
8. the graphene microchip according to claim 1 with network structure, it is characterised in that: described in step (5) also
The temperature of original reaction is 300 ~ 500 DEG C, and the time is 1 ~ 2h.
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| CN106542598B (en) * | 2017-01-23 | 2024-02-09 | 北京大学 | Solar sea water desalting device |
| CN107416801B (en) * | 2017-09-08 | 2020-03-24 | 安徽玄同工业设计有限公司 | Preparation method of three-dimensional porous graphene |
| CN111320355A (en) * | 2019-11-21 | 2020-06-23 | 佛山科学技术学院 | Preparation method of efficient flocculant for sludge dewatering |
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|---|---|
| CN106044920A (en) | 2016-10-26 |
| WO2017206579A1 (en) | 2017-12-07 |
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