CN107857258A - A kind of method of full carbon face oxidation adjusting function graphite alkene functional group species - Google Patents
A kind of method of full carbon face oxidation adjusting function graphite alkene functional group species Download PDFInfo
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Abstract
The present invention provides a kind of method of full carbon face oxidation adjusting function graphite alkene functional group species.First, high-quality graphene raw material is prepared using turbulene method or Asia/supercritical process.Further full carbon face is carried out using specific oxidant, concentrated acid system and additive to high-quality graphene to aoxidize, obtained the regulatable functionalization graphene material of functional group species.The inventive method reaction time is short, control the species of graphene oxy radical, laminated structure destruction to graphene is small, overcome the problem of graphene is difficult to handle and easily accumulated, so as to impart the further processing characteristics of graphene and handlability, the holding of the better performances of graphene is realized, and then is applied in fields such as desalinization, anticorrosion with coat, photoelectric device and energy storages.
Description
Technical field
The present invention relates to functionalization graphene preparation field, especially with specific oxidant, concentrated acid and additive to height
Quality graphene carries out full carbon face oxidation and prepares the method for adjusting the regulatable functionalization graphene of functional group's species.
Background technology
Graphene is one kind completely by sp2The thickness that the carbon atom of hydridization is formed is only monoatomic layer or several monoatomic layers
Quasi- two dimensional crystal material, transparent, thermal conductivity factor is high, and its electron mobility is high under normal temperature, at the same be also most thin in the world but also most
Hard nano material.Grapheme material can high-performance optical electrical part, gas sensor, composite, field emmision material and
The fields such as energy stores obtain extensive use.The graphene of structural integrity is combined by the carbon hexatomic ring without any labile bond
The two dimensional crystal formed, the inert state in its surface, chemical stability is high, weaker with the interaction of solvent, between piece and piece
There is stronger Van der Waals force, easily produce aggregation, it is insoluble in water and conventional organic solvent, this is further to graphene
Research and application cause great difficulty.In order to give full play to its advantageous property, and improve its molding processibility, such as improve
Dissolubility and dispersiveness in the base, it is necessary to which effective functionalization is carried out to graphene.Meanwhile functional group determines compound
Property, the compound containing certain functional group possess the chemical property of this functional group., can be with by introducing specific functional group
Assign graphene new property, further expand its application field.Control to graphene oxide functional group, help to formulate phase
The reduction strategy answered, improve the electric conductivity of redox graphene；In addition, the surface chemistry of graphene oxide is formed to material
Mechanical property and biology performance have a significant impact.Such as Dai etc. has synthesized a kind of carboxy-modified oxidation using chloroactic acid method
Graphene, and graphene oxide Pegylation is formed into NGO and is used for pharmaceutical carrier and cell imaging etc. with PEG compounds
Research.Yang et al. utilizes a kind of solion containing Amino End Group under the conditions of existing for no any surfactant,
Covalent bond functionalization is carried out to graphene oxide, can be in water, DMF (DMF) and dimethyl sulfoxide (DMSO)
(DMSO) disperse in equal solvent；Wang et al. carries out covalent bond functionalization, warp to graphene oxide with SSS (PSS)
After crossing the reduction of hydrazine hydrate steam, water miscible GNs-PSS can obtain；By octadecylamine (ODA) and the covalent bond of graphene oxide
Reaction, and to obtain the GNs-ODA of organophilic solvent after hydroquinones backflow reduction.
Graphene oxide is most typical functionalization graphene, the officials such as carboxyl, epoxy radicals, hydroxyl, carbonyl on lamella be present
It can roll into a ball, these groups can introduce specific functional group, realize different functions as the avtive spot of reaction kinetic.Control
The surface functional group species of graphene oxide, it is possible to the performance of controlled material, such as the control to graphene oxide functional group
For system for improving reduction efficiency, improving the electric conductivity of redox graphene has important facilitation；But due to covalent bond
After various groups are introduced during functionalization, original conjugated structure is destroyed, is existed very in terms of electric conductivity with graphene
Big difference；In addition, the oxidizing process of graphite usually require a large amount of highly acid oxidants for example the concentrated sulfuric acid, concentrated nitric acid, dichromic acid and
Potassium permanganate, sodium nitrate etc.；And high-temperature process is needed in mesh reduction process or uses the toxic chemicals such as hydrazine, dimethylhydrazine
Matter, not only energy consumption is big, efficiency is low, cost is high but also pollution environment.
By summarizing above, the species of graphene oxide oxy radical is controlled, further to prepare different types of function
Graphite alkene is provided convenience, and the electric conductivity to improve redox graphene has important facilitation.In function graphite
A kind of controllable functionalization graphene functional group species, oxygen content be low, dispersible, structure is broken there is an urgent need to develop for alkene preparation field
The new method of bad small functionalization graphene, and then apply and led in desalinization, anticorrosion with coat, photoelectric device and energy storage etc.
Domain.
The content of the invention
The defects of to overcome prior art, solution functional group species can not regulate and control, oxygen content is high, structure destroys big ask
Topic, propose a kind of method of full carbon face oxidation adjusting function graphite alkene functional group species.The functionalization graphene side of the present invention
Method can accomplish that functional group's species is controllable, and the laminated structure destruction of graphene is small, what graphene was difficult to handle and easily accumulated
Problem is effectively alleviated, and graphene obtains further processing characteristics and handlability.
The present invention adopts the following technical scheme that：
A kind of method of full carbon face oxidation adjusting function graphite alkene functional group species, comprises the following steps：
(1) send out reactant in the intercalator and solution of graphite intercalation compound as raw material with graphite intercalation compound
Raw redox reaction, high-quality graphene is efficiently prepared using turbulene method or Asia/supercritical process；
(2) carry out full carbon face to high-quality graphene using specific oxidant, concentrated acid and additive to aoxidize, obtained
The main hydroxylating graphene comprising hydroxyl and epoxy radicals mainly wraps carboxylic carboxylated grapheme material.
The intercalator of graphite intercalation compound is metal or metal halide, specially potassium, sodium, lithium, potassium sodium in step (1)
Alloy, lodine chloride, aluminium chloride, nickel chloride, antimony chloride, iron chloride or antimony fluoride.
Into solution, addition can include ethanol, sodium borohydride by the material of intercalator reaction between graphite flake layer in step (1)
Solution, hydrazine hydrate solution, hydrogenperoxide steam generator etc. and all substances that gas is produced in intercalator course of reaction, hydrogen peroxide matter
It is 30% to measure solubility, and hydrazine hydrate mass ratio is 30%, and sodium borohydride solution need to be configured as the alkaline solution that PH is 13.
Turbulene method is to rotate to produce shearing force using liquid at high speed in step (1), and graphite flake layer is effectively peeled off
A kind of method.
Step (1) Central Asia/supercritical process is to utilize the water of subcritical state or supercritical carbon dioxide etc. pair
A kind of method that graphite flake layer is effectively peeled off.
Oxidant, concentrated acid in step (2), including chlorate, potassium permanganate, bichromate etc., concentrated acid include the concentrated sulfuric acid, dense
Nitric acid and perchloric acid etc..
Additive is hydrogen peroxide, deionized water etc. in step (2).
Full carbon face oxidation uses the mass ratio of oxidant and graphene as 0.5~6 in step (2), and preferably 3.
Full carbon face oxidation uses the time as 0.5h-8h in step (2), preferably 3h.
Full carbon face oxidation uses temperature as 0 DEG C -20 DEG C in step (2), preferably 0 DEG C.
Low oxygen content, which refers to oxygen content in functionalization graphene material and accounts for the ratio of carbon oxygen element gross mass, in step (2) is less than
30%, preferably 10%-20%.
The present invention has following advantage：
(1) requirement of the present invention to equipment is relatively low, and the used time is short, and oxidizer is few, suitable for industry or laboratory operation.
(2) the full carbon face oxidation proposed in the present invention is different from from edge to inside progressively entering in conventional graphite oxidizing process
Row carbon face aoxidizes, and can control the species of graphene oxide oxy radical, prepares hypoxic graphene oxide, overcome graphite
The problem of alkene is difficult to handle and easily accumulated, so as to impart the further processing characteristics of graphene and handlability, realize
The holdings of the better performances of graphene.
Brief description of the drawings
Fig. 1 is the XPS figures that the inventive method prepares hydroxylating graphene.
Fig. 2 is the XPS figures that the inventive method prepares carboxylated graphene.
Fig. 3 is the infrared absorption spectra that the inventive method prepares hydroxylating graphene.
Fig. 4 is the infrared absorption spectra that the inventive method prepares carboxylated graphene.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for help and understands the present invention, is not construed as the concrete restriction to the present invention.
Embodiment 1
(1) by the anhydrous FeCl of 0.3g3It is well mixed with 0.05g expanded graphites, vacuum tightness is in 20mL specification vacuum ampullas
In, 1h is warming up to 380 DEG C, maintains 12h.Black product is dissolved in dilute hydrochloric acid solution, filters drying, it is stand-by.
(2) intercalation compound is taken out, be distributed in 50mL organic solvent 1-METHYLPYRROLIDONEs, prepare the outstanding of 5mg/mL
Supernatant liquid.
(3) 10mL suspension is taken to be put into the container for the turbulent flow generator that volume is 2L.
(4) 10mL sodium borohydride alkaline aqueous solution is added into container.
(5) turbulent flow generator is maintained to 10000r/m rotating speed, keeps 1h, reaction finishes, and takes out sample, and cleaning sample obtains
To graphene powder aggregation.
(6) by 20mL H2SO4(0 DEG C) maintains 0.5 hour in frozen water.
(7) original grapheme material 30mg is added in the concentrated sulfuric acid, is stirred 10 minutes.
(8) 120mg sodium chlorate is put into the solution of the concentrated sulfuric acid and graphene, stirred 4 hours at room temperature.
(9) product repeated centrifugation is washed, ultrasound obtains the hydroxylating graphene solution disperseed in water.
Fig. 1 is the XPS figures that the inventive method prepares hydroxylating graphene.
Fig. 3 is the infrared absorption spectra that the inventive method prepares hydroxylating graphene.
Embodiment 2
(1) by the anhydrous FeCl of 0.3g3It is well mixed with 0.05g expanded graphites, vacuum tightness is in 20mL specification vacuum ampullas
In, 1h is warming up to 380 DEG C, maintains 12h.Black product is dissolved in dilute hydrochloric acid solution, filters drying, it is stand-by.
(2) intercalation compound is taken out, be distributed in 50mL organic solvent 1-METHYLPYRROLIDONEs, prepare the outstanding of 5mg/mL
Supernatant liquid.
(3) 10mL suspension is taken to be put into the container for the turbulent flow generator that volume is 2L.
(4) 10mL sodium borohydride alkaline aqueous solution is added into container.
(5) turbulent flow generator is maintained to 10000r/m rotating speed, keeps 1h, reaction finishes, and takes out sample, and cleaning sample obtains
To graphene powder aggregation.
(6) by 20mL H2SO4(0 DEG C) maintains 0.5 hour in frozen water.
(7) original grapheme material 30mg is added in the concentrated sulfuric acid, is stirred 10 minutes.
(8) by H that 120mg sodium chlorate and 0.1mL mass fractions are 30%2O2It is put into the solution of the concentrated sulfuric acid and graphene
In, stir 4 hours at room temperature.
(9) product repeated centrifugation is washed, ultrasound obtains the carboxylated graphene solution disperseed in water.
Fig. 2 is the XPS figures that the inventive method prepares carboxylated graphene.
Fig. 4 is the infrared absorption spectra that the inventive method prepares carboxylated graphene.
Embodiment 3
(1) by the anhydrous FeCl of 0.3g3It is well mixed with 0.05g expanded graphites, vacuum tightness is in 20mL specification vacuum ampullas
In, 1h is warming up to 380 DEG C, maintains 12h.Product is dissolved in dilute hydrochloric acid solution, filters drying, it is stand-by.
(2) intercalation compound is taken out, be distributed in 50mL organic solvent 1-METHYLPYRROLIDONEs, prepare the outstanding of 5mg/mL
Supernatant liquid.
(3) 2mL suspension is taken to be put into volume as in 50mL water heating kettles.
(4) mass fraction that 4mL is added into water heating kettle is 30% hydrogen peroxide solution, fixes water heating kettle rapidly and sets
It is standby.
(5) water heating kettle is heated to 160 DEG C, keeps 1h, reaction finishes, and takes out sample, and cleaning sample obtains Graphene powder
Last aggregation.
(6) by 20mL H2SO4(0 DEG C) maintains 0.5 hour in frozen water.
(7) original grapheme material 30mg is added in the concentrated sulfuric acid, is stirred 10 minutes.
(8) 120mg sodium chlorate is put into the solution of the concentrated sulfuric acid and graphene, stirred 4 hours at room temperature.
(9) product repeated centrifugation is washed, ultrasound obtains the hydroxylating graphene solution disperseed in water.
Embodiment 4
(1) by the anhydrous FeCl of 0.3g3It is well mixed with 0.05g expanded graphites, vacuum tightness is in 20mL specification vacuum ampullas
In, 1h is warming up to 380 DEG C, maintains 12h.Product is dissolved in dilute hydrochloric acid solution, filters drying, it is stand-by.
(2) intercalation compound is taken out, be distributed in 50mL organic solvent 1-METHYLPYRROLIDONEs, prepare the outstanding of 5mg/mL
Supernatant liquid.
(3) 2mL suspension is taken to be put into volume as in 50mL water heating kettles.
(4) mass fraction that 4mL is added into water heating kettle is 30% hydrogen peroxide solution, fixes water heating kettle rapidly and sets
It is standby.
(5) water heating kettle is heated to 160 DEG C, keeps 1h, reaction finishes, and takes out sample, and cleaning sample obtains Graphene powder
Last aggregation.
(6) by 20mL H2SO4(0 DEG C) maintains 0.5 hour in frozen water.
(7) original grapheme material 30mg is added in the concentrated sulfuric acid, is stirred 10 minutes.
(8) by H that 120mg sodium chlorate and 0.1mL mass fractions are 30%2O2It is put into the solution of the concentrated sulfuric acid and graphene
In, stir 4 hours at room temperature.
(9) product repeated centrifugation is washed, ultrasound obtains the carboxylated graphene solution disperseed in water.
Embodiment 5
(1) by the anhydrous FeCl of 0.3g3It is well mixed with 0.05g expanded graphites, vacuum tightness is in 20mL specification vacuum ampullas
In, 1h is warming up to 380 DEG C, maintains 12h.Product is dissolved in dilute hydrochloric acid solution, filters drying, it is stand-by.
(2) intercalation compound is taken out, be distributed in 50mL organic solvent 1-METHYLPYRROLIDONEs, prepare the outstanding of 5mg/mL
Supernatant liquid.
(3) it is 50mL supercritical COs to take 2mL suspension to be put into volume2In kettle.
(4) to supercritical CO2The mass fraction that 4mL is added in kettle is 30% hydrogen peroxide solution, fixes super face rapidly
Boundary CO2Kettle.
(5) by supercritical CO2Kettle is heated to 35 DEG C, keeps 1h, and reaction finishes, and takes out sample, and cleaning sample obtains graphite
Alkene powder aggregates.
(6) by 20mL H2SO4(0 DEG C) maintains 0.5 hour in frozen water.
(7) original grapheme material 30mg is added in the concentrated sulfuric acid, is stirred 10 minutes.
(8) 120mg sodium chlorate is put into the solution of the concentrated sulfuric acid and graphene, stirred 4 hours at room temperature.
(9) product repeated centrifugation is washed, ultrasound obtains the hydroxylating graphene solution disperseed in water.
Embodiment 6
(1) by the anhydrous FeCl of 0.3g3It is well mixed with 0.05g expanded graphites, vacuum tightness is in 20mL specification vacuum ampullas
In, 1h is warming up to 380 DEG C, maintains 12h.Product is dissolved in dilute hydrochloric acid solution, filters drying, it is stand-by.
(2) intercalation compound is taken out, be distributed in 50mL organic solvent 1-METHYLPYRROLIDONEs, prepare the outstanding of 5mg/mL
Supernatant liquid.
(3) it is 50mL supercritical COs to take 2mL suspension to be put into volume2In kettle.
(4) to supercritical CO2The mass fraction that 4mL is added in kettle is 30% hydrogen peroxide solution, fixes super face rapidly
Boundary CO2Kettle.
(5) by supercritical CO2Kettle is heated to 35 DEG C, keeps 1h, and reaction finishes, and takes out sample, and cleaning sample obtains graphite
Alkene powder aggregates.
(6) by 20mL H2SO4(0 DEG C) maintains 0.5 hour in frozen water.
(7) original grapheme material 30mg is added in the concentrated sulfuric acid, is stirred 10 minutes.
(8) by H that 120mg sodium chlorate and 0.1mL mass fractions are 30%2O2It is put into the solution of the concentrated sulfuric acid and graphene
In, stir 4 hours at room temperature.
(9) product repeated centrifugation is washed, ultrasound obtains the carboxylated graphene solution disperseed in water.
Applicant states that the present invention illustrates the detailed process equipment of the present invention and technological process by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, selection of concrete mode etc., all fall within the present invention's
Within the scope of protection domain and disclosure.
Claims (11)
1. a kind of method of full carbon face oxidation adjusting function graphite alkene functional group species, comprises the following steps：
(1) make reactant in the intercalator and solution of graphite intercalation compound that oxygen occur as raw material with graphite intercalation compound
Change reduction reaction, high-quality graphene is efficiently prepared using turbulene method or Asia/supercritical process；
(2) carry out full carbon face to high-quality graphene using specific oxidant, concentrated acid and additive to aoxidize, obtain main
Hydroxylating graphene comprising hydroxyl and epoxy radicals mainly wraps carboxylic carboxylated grapheme material.
2. preparation method according to claim 1, it is characterised in that graphite intercalation compound described in step (1) is inserted
Layer agent is metal or metal halide, specially potassium, sodium, lithium, sodium-potassium eutectic, lodine chloride, aluminium chloride, nickel chloride, antimony chloride, chlorine
Change iron or antimony fluoride.
3. preparation method according to claim 1, it is characterised in that addition can be with stone into solution described in step (1)
The material of ink sheet interlayer intercalator reaction includes ethanol, sodium borohydride solution, hydrazine hydrate solution, hydrogenperoxide steam generator etc. and intercalation
The all substances of gas are produced in agent course of reaction, hydrogen peroxide quality solubility is 30%, and hydrazine hydrate mass ratio is 30%, boron hydrogen
The alkaline solution that PH is 13 need to be configured as by changing sodium solution.
4. preparation method according to claim 1, it is characterised in that turbulene method described in step (1) is to utilize liquid height
Speed rotation produces shearing force, a kind of method being effectively peeled off to graphite flake layer.
5. preparation method according to claim 1, it is characterised in that Asia/supercritical process described in step (1) is utilization
A kind of method that water or supercritical carbon dioxide of subcritical state etc. are effectively peeled off to graphite flake layer.
6. preparation method according to claim 1, it is characterised in that oxidant, concentrated acid described in step (2), including chlorine
Hydrochlorate, potassium permanganate, bichromate etc., concentrated acid include the concentrated sulfuric acid, concentrated nitric acid and perchloric acid etc..
7. preparation method according to claim 1, it is characterised in that additive described in step (2) be hydrogen peroxide, go from
Sub- water etc..
8. preparation method according to claim 1, it is characterised in that full carbon face oxidation is using oxidation described in step (2)
The mass ratio of agent and graphene is 0.5~6, preferably 3.
9. preparation method according to claim 1, it is characterised in that full carbon face oxidation uses the time described in step (2)
For 0.5h-8h, preferably 3h.
10. preparation method according to claim 1, it is characterised in that full carbon face oxidation uses temperature described in step (2)
For 0 DEG C -20 DEG C, preferably 0 DEG C.
11. preparation method according to claim 1, it is characterised in that low oxygen content refers to function fossil described in step (2)
In black alkene material oxygen content account for carbon oxygen element gross mass ratio be less than 30%, preferably 10%-20%.
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| CN108314024A (en) * | 2018-04-24 | 2018-07-24 | 盐城师范学院 | A kind of plasma preparation method of transparent graphene conductive film |
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