CN108314333A - A kind of Electrostatic Absorption preparation method of Graphene glass - Google Patents
A kind of Electrostatic Absorption preparation method of Graphene glass Download PDFInfo
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- CN108314333A CN108314333A CN201810412012.3A CN201810412012A CN108314333A CN 108314333 A CN108314333 A CN 108314333A CN 201810412012 A CN201810412012 A CN 201810412012A CN 108314333 A CN108314333 A CN 108314333A
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- Prior art keywords
- graphene
- glass
- graphene oxide
- preparation
- oxygen
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
- C03C2218/324—De-oxidation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention provides a kind of Electrostatic Absorption preparation method of Graphene glass.Full carbon face oxidative modification directly is carried out to high-quality graphene with oxidants such as potassium permanganate, obtains the equally distributed graphene oxide composite material of oxygen-containing group;Sheet glass carries out silanization after the concentrated sulfuric acid/hydrogenperoxide steam generator processing with APTMS, and glass surface can be formed NH3+, graphene oxide composite material is coated in glass surface with bar coating method, graphene oxide is restored with hydroiodic acid, obtains Graphene glass.The method of the present invention prepares the equally distributed graphene oxide composite material of oxygen-containing group, overcome the inhomogeneities being distributed from the outer layer oxygen-containing group that internally gradually oxidized zone comes in conventional oxidation graphene preparation process, under electrostatic adsorption, the equally distributed graphene oxide of oxygen-containing group can be closely pasted onto on amidized glass, graphene film is not easy to be destroyed in reduction process and requirement to equipment is relatively low, is suitable for industrial production.
Description
Technical field
The present invention relates to Graphene glass preparation fields, with the equally distributed graphene oxide composite material of oxygen-containing group and use
The amidized glass of APTES is evenly distributed under electrostatic adsorption and pastes close Graphene glass.
Background technology
Glass is a kind of amorphous silicic acid salt material, since its good translucency and cheap cost become daily life
In one of essential traditional building material.The two-dimensional layer material that graphene is made of carbon atom, the machine with superelevation
Tool intensity, electric conductivity, thermal conductivity and the transparency.Graphene and glass are combined together, on the basis of keeping the transparency, together
When assign simple glass electric conductivity, thermal conductivity and surface hydrophobic, can be applicable to thermochromism window, antifog form and light and urge
Change etc..Since the resistance of graphene itself is moderate, the heat that when energization generates is enough to make the color of able thermochromic to send out
It is raw to change, therefore can be as a kind of suitable window material.The heat that graphene generates when energization can also be used to remove material
Expect surface water mist, in the case of cold, using graphene itself hydrophobic property can also spontaneous inhibition water mist formed, stone
The black antifog form of alkene glass has been provided simultaneously with the ability of actively and passively anti-/ demisting.In the graphene that glass surface is directly grown
It has good uniformity, it can be as a kind of light-catalysed ideal substrate of recycling.By chemical method by photocatalyst
To Graphene glass surface, catalytic efficiency can be effectively promoted.Graphene glass has very important practical significance and reason
Value can expand the application space of glass, cause glass industries and added from the low value-added economizing type height that is applied to of high-volume
It is worth the revolutionary change of application.
Directly Graphene glass can be prepared in glass surface growth graphene.Liu Zhongfan etc. utilizes chemical vapor deposition
Method glass surface catalytic pyrolysis is overcome by the accuracy controlling to reacting gas concentration, growth temperature and growth time
Forerunner's ability of immigrants is low, and carbon fragment is in the problems such as substrate surface transfer ability is weak, and success is real on pyroceram and simple glass
The controllable growth for having showed high-quality graphene film grows size and all well-proportioned graphene disk of distribution.This growth
The Graphene glass that method obtains, the excellent specific properties such as the interfacial contact with glass and graphene is good, interface is pollution-free, still
Complex process, equipment requirement is high, expends big, unsuitable practical application.Liquid phase film or transfer also can be used in Graphene glass
Method obtains, i.e., coats grapheme material or be transferred on glass.For example, Li et al. people utilizes LB membrane technologies in gas
Liquid interface is prepared for graphene film, is from the bottom up picked up graphene film with glass to obtain Graphene glass.Such method
The hydrophobicity of glass surface, graphene can not be overcome to paste the problems such as not close with glass surface, the graphene film of acquisition is not
There are problems that surface and interface pollution avoidablely, to seriously affect the performance of Graphene glass.Therefore, develop a kind of operation letter
New method single, at low cost, yield is high is that one in presently relevant application study is crucial.
Invention content
The present invention provides a kind of Electrostatic Absorption preparation method of Graphene glass, with the equally distributed oxidation of oxygen-containing group
Grapheme material and with 3- aminopropyl triethoxysilanes (APTES) amidized glass, obtains under electrostatic adsorption
It is even to be distributed and paste close Graphene glass.
The present invention adopts the following technical scheme that:
A kind of Electrostatic Absorption preparation method of Graphene glass, includes the following steps:
(1) it uses the oxidants such as potassium permanganate directly to carry out full carbon face oxidative modification to high-quality graphene, obtains oxygen-containing
The equally distributed graphene oxide composite material of group;
(2) sheet glass carries out silanization after the concentrated sulfuric acid/hydrogenperoxide steam generator processing with APTMS, and glass surface can be by shape
At NH3 +, graphene oxide composite material is coated in glass surface with bar coating method, graphene oxide is restored with hydroiodic acid, is obtained
Graphene glass.
Oxidant includes permanganate, chlorate, ferrite, chromate, persulfate etc. in step (1).
The source of high-quality graphene includes that various methods from top to bottom obtain high-quality graphene from graphite in step (1)
Method, such as mechanical stripping method, turbulene method, supercritical methanol technology.
Oxygen-containing group includes carboxyl, hydroxyl, carbonyl and epoxy group in step (1).
Oxidizer is the 25-400% of high-quality graphene quality, oxidization time 0.5-6h in step (1).
It is dry toluene to carry out solvent in silanization process to glass with APTMS in step (2), and temperature is 110 DEG C, reflux
12-24h, ATPES are excessive.
Hydroiodic acid mass fraction is preferably 30% in step (2), and the recovery time is preferably 5min.
The present invention has following advantage:
(1) present invention can prepare the equally distributed graphene oxide composite material of oxygen-containing group, overcome conventional oxidation graphene
The inhomogeneities being distributed from the outer layer oxygen-containing group that internally gradually oxidized zone comes in preparation process, under electrostatic adsorption,
The equally distributed graphene oxide of oxygen-containing group can be closely pasted onto on amidized glass, the graphene film in reduction process
It is not easy to be destroyed.
(2) the equally distributed graphene oxide composite material of oxygen-containing group can be in lower point obtained of oxygen content
Property is dissipated, reduces oxidization time, reduces destruction of the reducing agent to film in oxidation process.
(3) it is hydrophobic to overcome glass surface, graphene pastes untight disadvantage with glass surface, and to the requirement of equipment
It is relatively low, it is suitable for industrial production.
Description of the drawings
Fig. 1 is that the method for the present invention prepares grapheme material SEM figures.
Fig. 2 is Graphene glass optical picture.
Specific implementation mode
Of the invention for ease of understanding, 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 helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) 60g Iodide Bromide is uniformly mixed with 100mg expanded graphites, is packed into protection gas Ar gas, is enclosed within 100mL glass
In glass bottle, vial is placed in 100 DEG C of oil bath environment, is heated 48h, is prepared graphite intercalation compound.
(2) graphite intercalation compound is taken out and is filtered from vial rapidly, be put into the water heating kettle that volume is 50mL,
10mL aqueous solutions are added into water heating kettle, fix water heating kettle equipment rapidly.
(3) water heating kettle is heated to 180 DEG C, 1h, reaction is kept to finish, take out sample, cleaning sample obtains high quality stone
Black alkene powder aggregates.
(4) 50mg graphenes are put into the concentrated sulfuric acid that volume is 20mL, 100mg sodium chlorate are added, in ice-water bath
4h is reacted, graphene oxide is obtained after cleaning.
(5) 50mg graphite oxides are substantially soluble in 20mL deionized waters and obtain graphite oxide solution.
(6) glass is placed in the concentrated sulfuric acid/hydrogenperoxide steam generator, the concentrated sulfuric acid (mass fraction 98%) and hydrogen peroxide (matter
It is that 30%) volume ratio is 7: 3 to measure score, handles 1h at room temperature, obtains hydroxylating glass.
(7) excess APTMS is added in 100mL dry toluenes, hydroxylating glass is put into, temperature maintains 110 DEG C, returns
Flow 12-24h.
(8) glass is taken out and is cleaned with ethyl alcohol, graphene oxide composite material is coated in glass surface with bar coating method.
(9) hydroiodic acid for being 30% with mass fraction restores graphene oxide, and time 5min obtains graphene glass
Glass.
Embodiment 2
(1) by the anhydrous FeCl of 0.3g3It being mixed with 0.05g expanded graphites, vacuum tightness, 1h is warming up to 380 DEG C, maintains 12h,
Prepare graphite intercalation compound.Graphite intercalation compound is dissolved in dilute hydrochloric acid solution, filters drying, for use.
(2) graphite intercalation compound is put into rapidly to the supercritical CO that volume is 50mL2In device, to supercritical CO2Device
The middle hydrogen peroxide solution that 5mL mass fractions are added and are 30%, fixes rapidly equipment.
(3) by high supercritical CO2Device is heated to 38 DEG C, and boost in pressure to 75atm keeps 1h, reaction to finish, and takes out sample
Product, cleaning sample obtain graphene powder aggregation.
(4) 50mg graphenes are put into the concentrated sulfuric acid that volume is 20mL, 100mg sodium chlorate are added, in ice-water bath
4h is reacted, graphene oxide is obtained after cleaning.
(5) 50mg graphite oxides are substantially soluble in 20mL deionized waters and obtain graphite oxide solution.
(6) glass is placed in the concentrated sulfuric acid/hydrogenperoxide steam generator, the concentrated sulfuric acid (mass fraction 98%) and hydrogen peroxide (matter
It is that 30%) volume ratio is 7: 3 to measure score, handles 1h at room temperature, obtains hydroxylating glass.
(7) excess APTMS is added in 100mL dry toluenes, hydroxylating glass is put into, temperature maintains 110 DEG C, returns
Flow 12h.
(8) glass is taken out and is cleaned with ethyl alcohol, graphene oxide composite material is coated in glass surface with bar coating method.
(9) hydroiodic acid for being 30% with mass fraction restores graphene oxide, and time 5min obtains graphene glass
Glass.
Fig. 1 is that the present embodiment prepares grapheme material SEM figures.
Fig. 2 is that the present embodiment prepares Graphene glass optical picture.
Embodiment 3
(1) by the anhydrous FeCl of 0.3g3It being mixed with 0.05g expanded graphites, vacuum tightness, 1h is warming up to 380 DEG C, maintains 12h,
Prepare graphite intercalation compound.Graphite intercalation compound is dissolved in dilute hydrochloric acid solution, filters drying, for use.
(2) graphite intercalation compound is put into rapidly to the supercritical CO that volume is 50mL2In device, to supercritical CO2Device
The middle hydrogen peroxide solution that 5mL mass fractions are added and are 30%, fixes rapidly equipment.
(3) by high supercritical CO2Device is heated to 38 DEG C, and boost in pressure to 75atm keeps 1h, reaction to finish, and takes out sample
Product, cleaning sample obtain graphene powder aggregation.
(4) 50mg graphenes are put into the concentrated sulfuric acid that volume is 20mL, 100mg sodium chlorate are added, in ice-water bath
4h is reacted, graphene oxide is obtained after cleaning.
(5) 50mg graphite oxides are substantially soluble in 20mL deionized waters and obtain graphite oxide solution.
(6) glass is placed in the concentrated sulfuric acid/hydrogenperoxide steam generator, the concentrated sulfuric acid (mass fraction 98%) and hydrogen peroxide (matter
It is that 30%) volume ratio is 7: 3 to measure score, handles 1h at room temperature, obtains hydroxylating glass.
(7) excess APTMS is added in 100mL dry toluenes, hydroxylating glass is put into, temperature maintains 110 DEG C, returns
Stream is for 24 hours.
(8) glass is taken out and is cleaned with ethyl alcohol, graphene oxide composite material is coated in glass surface with bar coating method.
(9) hydroiodic acid for being 30% with mass fraction restores graphene oxide, and time 5min obtains graphene glass
Glass.
Embodiment 4
(1) by the anhydrous FeCl of 0.3g3It being mixed with 0.05g expanded graphites, vacuum tightness, 1h is warming up to 380 DEG C, maintains 12h,
Prepare graphite intercalation compound.Graphite intercalation compound is dissolved in dilute hydrochloric acid solution, filters drying, for use.
(2) graphite intercalation compound is put into rapidly to the supercritical CO that volume is 50mL2In device, to supercritical CO2Device
The middle hydrogen peroxide solution that 5mL mass fractions are added and are 30%, fixes rapidly equipment.
(3) by high supercritical CO2Device is heated to 38 DEG C, and boost in pressure to 75atm keeps 1h, reaction to finish, and takes out sample
Product, cleaning sample obtain graphene powder aggregation.
(4) 50mg graphenes are put into the concentrated sulfuric acid that volume is 20mL, 200mg sodium chlorate are added, in ice-water bath
2h is reacted, graphene oxide is obtained after cleaning.
(5) 50mg graphite oxides are substantially soluble in 20mL deionized waters and obtain graphite oxide solution.
(6) glass is placed in the concentrated sulfuric acid/hydrogenperoxide steam generator, the concentrated sulfuric acid (mass fraction 98%) and hydrogen peroxide (matter
It is that 30%) volume ratio is 7: 3 to measure score, handles 1h at room temperature, obtains hydroxylating glass.
(7) excess APTMS is added in 100mL dry toluenes, hydroxylating glass is put into, temperature maintains 110 DEG C, returns
Flow 12h.
(8) glass is taken out and is cleaned with ethyl alcohol, graphene oxide composite material is coated in glass surface with bar coating method.
(9) hydroiodic acid for being 30% with mass fraction restores graphene oxide, and time 5min obtains graphene glass
Glass.
Applicant states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological processes, 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, the selection etc. of concrete mode all fall within the present invention's
Within protection domain and the open scope.
Claims (7)
1. a kind of Electrostatic Absorption preparation method of Graphene glass, includes the following steps:
(1) it uses the oxidants such as potassium permanganate directly to carry out full carbon face oxidative modification to high-quality graphene, obtains oxygen-containing group
Equally distributed graphene oxide composite material;
(2) sheet glass carries out silanization after the concentrated sulfuric acid/hydrogenperoxide steam generator processing with APTMS, and glass surface can be formed NH3 +, graphene oxide composite material is coated in glass surface with bar coating method, graphene oxide is restored with hydroiodic acid, obtains graphite
Alkene glass.
2. preparation method according to claim 1, which is characterized in that oxidant described in step (1) include permanganate,
Chlorate, ferrite, chromate, persulfate etc..
3. preparation method according to claim 1, which is characterized in that the source of high-quality graphene described in step (1)
Including the method that various methods from top to bottom obtain high-quality graphene from graphite, such as mechanical stripping method, turbulene method, supercritical methanol technology
Deng.
4. preparation method according to claim 1, which is characterized in that oxygen-containing group described in step (1) includes carboxyl, hydroxyl
Base, carbonyl and epoxy group.
5. preparation method according to claim 1, which is characterized in that oxidizer is high quality described in step (1)
The 25-400% of graphene quality, oxidization time 0.5-6h.
6. preparation method according to claim 1, which is characterized in that carry out silicon to glass with APTMS described in step (2)
Solvent is dry toluene in alkanisation, and temperature is 110 DEG C, and flow back 12-24h, and ATPES is excessive.
7. preparation method according to claim 1, which is characterized in that hydroiodic acid mass fraction is preferred described in step (2)
It is 30%, the recovery time is preferably 5min.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110027292A (en) * | 2019-04-23 | 2019-07-19 | 盐城师范学院 | A kind of preparation method of the antifog Graphene glass of waterproof |
CN110357449A (en) * | 2019-07-16 | 2019-10-22 | 嘉兴学院 | A kind of graphene oxide electro-conductive glass and preparation method thereof |
CN113311160A (en) * | 2021-06-17 | 2021-08-27 | 山东科讯生物芯片技术有限公司 | Micro-fluidic biochip for rapidly detecting SARS-CoV-2 antigen and IgG/IgM antibody |
CN115818974A (en) * | 2022-12-26 | 2023-03-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for generating graphene coating on glass surface |
CN115818974B (en) * | 2022-12-26 | 2024-04-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for generating graphene coating on glass surface |
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Cited By (6)
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CN110027292A (en) * | 2019-04-23 | 2019-07-19 | 盐城师范学院 | A kind of preparation method of the antifog Graphene glass of waterproof |
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CN115818974A (en) * | 2022-12-26 | 2023-03-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for generating graphene coating on glass surface |
CN115818974B (en) * | 2022-12-26 | 2024-04-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for generating graphene coating on glass surface |
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Application publication date: 20180724 |