CN110127671A - A kind of general preparative methods of redox graphene group compound film - Google Patents
A kind of general preparative methods of redox graphene group compound film Download PDFInfo
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08K3/02—Elements
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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
Abstract
A kind of general preparative methods of redox graphene group compound film, this method prepares graphite oxide alkenyl mixed liquor first, graphene oxide group compound film is prepared by modes such as vacuum filtration, spin coating, drop coating, blade coating, coatings, it puts it into reaction vessel and is sealed after liquid is added, redox graphene group compound film is prepared by hydro-thermal or solvothermal reaction at a certain temperature.Mixed liquor also may include polymer, organic nano material, inorganic nano material, metal nano material etc. in addition to comprising graphene oxide.Universality of the present invention is strong, and preparation process is simple and convenient；Redox graphene group compound film obtained can also further high temperature reduction, graphene reducing degree is higher, crystalline texture is more perfect redox graphene group compound film is made；Good using redox graphene group compound film stability made from this method, thickness, loose performance is adjustable, and the thermal conductivity, conductance, catalytic performance etc. of composite membrane are adjusted according to different composite.
Description
Technical field
The present invention relates to a kind of general preparative methods of redox graphene group compound film.
Background technique
Graphene-based composite material has a wide range of applications in fields such as the energy, environment, chemical industry.For example, graphene
Group compound film substance separation, catalysis, lithium ion battery, supercapacitor, in terms of all have important research value
And application value.However, the slightly solubility of graphene greatly limits the research and application of the composite material based on graphene.
Thus, the good graphene oxide of people elder generation synthesizing water-solubility carries out it with other materials compound to prepare graphite oxide alkenyl
Composite material, then graphene-structured, synthesizing graphite alkene based composites, such as airsetting are repaired by electronation or high temperature thermal reduction
Glue, fiber and film.However, the graphene-based composite membrane flexility or stabilization of directly electronation or high temperature thermal reduction synthesis
Property is poor, limits the potential application range of graphene-based composite membrane.
Summary of the invention
The purpose of the present invention is exactly directed to above-mentioned the problems of the prior art and to provide a kind of redox graphene base multiple
Close the general preparative methods of film.
In order to improve the flexibility and stability of graphene-based composite membrane, the present invention is using graphene oxide as raw material, by it
It carries out after uniformly mixing dispersion, is such as filtered by vacuum by certain way, spin coating, drop coating, blade coating, coating mode with other materials
Graphene oxide group compound film is prepared, then puts it into closed container and carries out hydro-thermal or solvothermal reaction preparation stability
Good redox graphene group compound film.According to needs are applied, the flexility of graphene-based composite membrane can also be dredged
Loose performance, electric property and thermal property are adjusted.Film obtained is with good stability；Film flexility depends on adding
Add that substance, whether there is or not the flexility of support substrate and support substrate itself.The technology of the present invention universality is strong, operation is convenient, green
Environmental protection.
The purpose of the present invention is achieved through the following technical solutions: a kind of redox graphene group compound film preparation
Method, comprising the following steps:
(1) graphite oxide alkenyl mixed liquor is prepared, mixed liquor also includes polymer, organic in addition to comprising graphene oxide
It nano material, inorganic nano material, metal nano material and is used to prepare in inorganic or metal nano material predecessor
It is one or more；
(2) graphite oxide alkenyl mixed liquor obtained in step (1) passed through into certain way such as vacuum filtration, spin coating, drop coating, scraped
The modes such as painting, coating are prepared into graphene oxide group compound film.
(3) graphene oxide group compound film obtained in step (2) is put into reaction vessel, is added in the reaction vessel
It is sealed after liquid, carries out hydro-thermal reaction or solvent thermal reaction for a period of time at a certain temperature, redox graphene is made
Group compound film.
In step (1), the graphite oxide alkenyl mixed liquor can be directly formulated, and multiple steps can also be divided to distinguish
After the solution or dispersion liquid of preparing or prepare different material, remix, used in solvent be that water and polarity are organic molten
One of agent is a variety of, and a certain amount of acidic or alkaline substances can also be added as needed.
In step (1), the concentration of graphene oxide is generally no greater than 30 mg/mL in the graphite oxide alkenyl mixed liquor,
But it is not limited to concentrations above.It is preferred that 5-20 mg/mL.
In step (1), in the graphite oxide alkenyl mixed liquor in addition to graphene oxide, the additive amount of other materials is general
Not higher than 2 times of added graphene oxide quality, but it is not limited to the above additive amount.
In step (1), the polymer is mainly water-soluble polymer and other polar solvent dissolubility polymer.
In step (1), the organic nano material mainly includes two-dimension polymer.
In step (1), the inorganic nano material include silicon, fullerene, active carbon, graphene, carbon nanotube, carbon black,
Black squama, graphite alkene, Mxene, titanium dioxide, silicon nitride, boron nitride, molybdenum disulfide, ferroso-ferric oxide, stannic oxide, titanium dioxide
The nanometers such as titanium, cobaltosic oxide, nickel hydroxide, mangano-manganic oxide, cadmium sulfide, zinc oxide, titanium dioxide rubidium, cadmium telluride, zinc sulphide
Material but it is not limited to the above substance.
In step (1), the metal nano material includes but is not limited to gold, silver, foil, lead, nickel, copper, germanium etc..
In step (1), the graphene oxide dispersion can be added reducing agent, reducing agent include but is not limited to hydrazine hydrate,
Sodium borohydride, glucose, ascorbic acid, sodium ascorbate, ethylene glycol, diethylene glycol, hydroquinone, hydrobromic acid, hydroiodic acid and
One of acetic acid is a variety of.
In step (1), crosslinking agent can be added in the graphene oxide dispersion, and such as diamines substance contains amino and mercapto
Substance, 1,4- butanediol diglycidyl ether, glyoxal, formaldehyde, glyoxalic acid, citric acid, fumaric acid of base etc..
In step (2), the graphene oxide group compound film of the preparation can also further progress crosslinking, prepare it is more stable
Graphene oxide group compound film.
In step (3), the reaction vessel including but not limited to by glass, metal, polyethylene, polypropylene, polyparaphenylene,
Polytetrafluoroethylene (PTFE) material is made into or equipped with by materials such as glass, metal, polyethylene, polypropylene, polyparaphenylene, polytetrafluoroethylene (PTFE)
It is made into the reaction vessel of liner.
In step (3), the liquid is one of water, polar organic solvent, liquid reducer, liquid cross-linker or more
Mixture is planted, acidic or alkaline substances can also be added in liquid as needed.
In step (3), the certain temperature is generally 100-300 DEG C；Described a period of time is generally 2 h -24 h, but not
It is limited to the above reaction time, preferably 5-10h.
Obtained redox graphene group compound film includes with support substrate or the oxygen reduction without support substrate
Fossil mertenyl composite membrane.
The present invention has the advantages that compared with prior art
1, the technology of the present invention prepares graphite oxide alkenyl mixed liquor in a liquid first, then be such as filtered by vacuum by certain way,
The modes such as spraying, spin coating, blade coating, coating prepare graphene oxide group compound film.At a certain temperature, by it in confined space
Hydrothermal reduction reaction or solvothermal reaction are carried out, redox graphene group compound film is prepared, is a kind of completely new system
The inventive technique of standby redox graphene group compound film；
2, universality of the present invention is strong, and preparation process is simple and convenient；
3, redox graphene group compound film obtained can also further high temperature reduction, be made graphene reducing degree more
Redox graphene group compound film high, crystalline texture is more perfect；
4, redox graphene group compound film stability obtained is good, and thickness, loose performance is adjustable, adjustable according to different composite
Save thermal conductivity, conductance, the catalytic performance etc. of composite membrane；
5, the flexibility of redox graphene group compound film obtained depend on composition and component content, whether there is or not support substrates
And the flexility of support substrate.
Detailed description of the invention
Fig. 1 is composite membrane appearance schematic diagram prepared by the present invention, and wherein A is the reduction-oxidation graphite prepared in embodiment 1
Alkene/composite membrane of polyvinyl alcohol, B illustrate that redox graphene/composite membrane of polyvinyl alcohol flexibility is fine.
Specific embodiment
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
It is bright, it should not be understood as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment, all belong to the scope of protection of the present invention.
Embodiment 1:
Step (1): dispersing the graphene oxide of 0.5 g in the water of 100 mL, stirs 8 h, and 20 min of ultrasound obtain 5
The graphene oxide dispersion of mg/mL；
Step (2): 1 g polyvinyl alcohol is dissolved in the poly-vinyl alcohol solution that 10 mg/mL are configured in 100 mL water；
Step (3): preparation in the graphene oxide dispersion and 1 mL step (2) prepared in 0.5 mL step (1) is taken respectively
Poly-vinyl alcohol solution is scattered in again in 200 mL water, prepares graphene oxide/polyvinyl alcohol mixed liquor；
Step (4): the graphene oxide/polyvinyl alcohol mixed liquor that step (3) are prepared is taken out on the organic film that diameter is about 4cm
Filter into graphene oxide/polyvinyl alcohol mixed liquor composite membrane.
Step (5): the graphene oxide/polyvinyl alcohol composite membrane prepared in step (4) is put into polytetrafluoroethyllining lining
Afterwards, 1 mL water is added, reaction kettle is put it into after sealing, then carry out it is closed after reaction kettle is put into 120o10 are carried out in C baking oven
The reaction of h hydrothermal reduction, obtains redox graphene/composite membrane of polyvinyl alcohol.
The composite membrane mechanical strength that this method obtains is higher, and flexibility is good.
Embodiment 2:
Step (1): dispersing 1 g graphene oxide in the water of 200 mL, stirs 10 h, 5 min of ultrasound, obtains oxidation stone
Black alkene dispersion liquid；
Step (2): the carbon nanotube and 10 mL second two of 0.01 g are added in the graphene oxide dispersion obtained by step (1)
Amine and 5 g sodium ascorbates after stirring 1 h, 10 min of ultrasound, take out 0.2 mL and are diluted in 100 mL water, after 5 min of ultrasound
Film forming is filtered on the organic film that diameter is about 4 mm, and graphene oxide/carbon nano-tube compound film is made.
Step (3): graphene oxide/carbon nano-tube compound film obtained in step (2) is put into 150 mL polytetrafluoroethyl-nes
In alkene liner, is sealed after the mixed liquor of 1 mL water, 1 mL ethyl alcohol and 0.1 mL ethylene glycol is added, inner liner of reaction kettle is put into reaction
In kettle, 130 are put into after closedoThe reaction of 10 h solvothermals is carried out in C baking oven, obtains redox graphene/carbon nanometer
Pipe composite membrane.
Redox graphene/carbon nano-tube compound film that this method obtains all has well in water and organic solvent
Stability, and flexibility is also preferable.
Embodiment 3:
Step (1): dispersing 1 g graphene oxide in the water of 200 mL, stirs 10 h, 10 min of ultrasound, obtains oxidation stone
Black alkene dispersion liquid；
Step (2): taking the middle gained graphene oxide dispersion of 5 mL steps (1) and 2 mL ethyl alcohol in 10 mL vials respectively,
It after stirring 10 min, is added 0.5 mL butyl titanate (precursor for belonging to above-mentioned inorganic nano material), stirring 30
Ultrasound 2min again after min, is filtered into graphene oxide group compound film.
Step (3): the graphene oxide group compound film in step (2) is put into polytetrafluoroethyllining lining, and 1 mL is added
It is sealed after water, then puts it into after reaction kettle and carry out closed, reaction kettle is put into 150oHydro-thermal reaction is carried out in C vacuum drying oven
12 h obtain redox graphene/titanium dioxide composite film.
Redox graphene/titanium dioxide composite film that this method obtains has photocatalysis performance, under illumination condition
Can degradating organic dye, such as methyl blue.
Embodiment 4:
Step (1): dispersing 1 g graphene oxide in the water of 200 mL, stirs 10 h, 2 min of ultrasound, obtains oxidation stone
Black alkene dispersion liquid；
Step (2): the graphene oxide dispersion obtained by the step (1) be added 0.05 g carbon nanotube and 10 mL ethylenediamines and
10 mL ethylene glycol are configured to graphene oxide/carbon nanotube mixed liquor after stirring 1 h, 2 min of ultrasound.
Step (3): 1 g polyvinyl alcohol is added in the water of 100 mL, 70oPoly- second is configured to after being dissolved under C
Enolate solution.
Step (4): the graphene oxide/carbon nanotube mixed liquor prepared in 0.2 mL step (2) is taken to be added to 100 mL
In water, after adding the polyvinyl alcohol water solution prepared in 0.1 mL step (3), 10 min of ultrasound, be configured to graphene oxide/
Carbon nanotube/polyvinyl alcohol mixed liquor.
Step (5): mixed liquor in step (4) is filtered into the graphene oxide/carbon nano-tube/poly second for being about 4 cm at diameter
Enol composite membrane.
Step (6): the graphene oxide/carbon nanotube/polyvinyl alcohol composite membrane prepared in step (5) is put into 100 mL
In polytetrafluoroethyllining lining, then the mixed liquor of the hydrazine hydrate of 2 mL ethyl alcohol, 0.5 mL ethylene glycol and 0.1 mL is added thereto, it is close
It is honored as a queen and is put into 100 mL reaction kettles, be put into 120 after reaction kettle is sealedoSolvothermal is carried out in C baking oven reacts 15 h, system
Obtain graphene oxide/carbon nanotube/polyvinyl alcohol composite membrane.
The graphene oxide that this method obtains/carbon nanotube/polyvinyl alcohol composite membrane stability is good, and flexibility is good, can
With curling.
Embodiment 5:
Step (1): dispersing 2 g graphene oxides in the water of 200 mL, stirs 10 h, 2 min of ultrasound, obtains oxidation stone
Black alkene dispersion liquid；
Step (2): the graphene oxide dispersion for taking 5 mL steps (1) to prepare is separately added into thereto in 10 mL vials
Gold nano grain solution, 0.1mL ethylenediamine and the 0.01 mL hydrazine hydrate of the 0.1mg/mL of 0.2mL after 10 min of ultrasound, passes through
Rubbing method prepares graphene oxide/gold composite membrane on the hydrophily organic film that diameter is about 2.5cm after drying at room temperature.
Step (3): graphene oxide/gold composite membrane obtained in step (2) is put into 50 mL polytetrafluoroethyllining linings
In, it is sealed after the mixed liquor of 1 mL water and 0.01mL hydrazine hydrate is added, inner liner of reaction kettle is put into reaction kettle, is put into after closed
150 o8 h of C baking oven hydrothermal reduction, obtains redox graphene/gold composite membrane.
In this preparation method the addition of gold nano grain and the addition of reducing agent be able to improve film electric conductivity and
The reducing degree of graphene oxide.
Embodiment 6:
Step (1): dispersing 1 g graphene oxide in the DMF of 100 mL, stirs 10 h, 2 min of ultrasound, obtains oxidation stone
Black alkene dispersion liquid；
Step (2): 1 g polyacrylonitrile is dissolved in 100 mLDMF at 80 DEG C, prepares 10 mg/mL polyacrylonitrile solutions；
Step (3): it takes prepared in graphene oxide dispersion and 0.02 step (3) obtained in 0.05 mL step (1) respectively
Polyacrylonitrile solution is added in 50 mL DMF, and it is mixed to be configured to graphene oxide/polyacrylonitrile after 1 h of stirring, 10 min of ultrasound
Close liquid；
Step (4): graphene oxide/polyacrylonitrile mixed liquor that step (3) are prepared is on the organic film that diameter is about 4 cm
Filter into graphene oxide/polyacrylonitrile compound film；
Step (5): the graphene oxide/polyacrylonitrile compound film prepared in step (4) is put into 150 mL polytetrafluoroethylene (PTFE)
In lining, seals, inner liner of reaction kettle is put into reaction kettle, then put it into 160 after 2 mL DMF are addedoIt is carried out in C baking oven molten
Agent heat-treats 4 h, obtains redox graphene/polyacrylonitrile compound film.
Oxidation graphene oxide/the polyacrylonitrile compound film prepared in this preparation method has good flexibility and stabilization
Property.
Above-described embodiment is used to explain the present invention, rather than limits the invention, in spirit and right of the invention
It is required that protection scope in, to any modifications or changes for making of the present invention, fall within protection scope of the present invention.
Claims (11)
1. a kind of general preparative methods of redox graphene group compound film, it is characterised in that: be by being filtered by vacuum, revolving
Painting, drop coating, blade coating or coating method prepare graphene oxide group compound film, then put it into closed container carry out hydro-thermal or
Solvothermal reaction prepares redox graphene group compound film, specifically includes the following steps:
(1) prepare graphite oxide alkenyl mixed liquor, in mixed liquor in addition to comprising graphene oxide, while also comprising polymer, have
It machine nano material, inorganic nano material, metal nano material and is used to prepare in inorganic or metal nano material predecessor
It is one or more；
(2) graphite oxide alkenyl mixed liquor obtained in step (1) is passed through into vacuum filtration, spin coating, drop coating, blade coating or coating side
Formula is prepared into graphene oxide group compound film；
(3) graphene oxide group compound film obtained in step (2) is put into reaction vessel, liquid is added in the reaction vessel
After seal, carry out hydro-thermal reaction or solvent thermal reaction for a period of time at a certain temperature, it is multiple that redox graphene base be made
Close film.
2. the general preparative methods of redox graphene group compound film according to claim 1, it is characterised in that: step
(1) in, the graphite oxide alkenyl mixed liquor can be directly formulated in a liquid, and multiple steps can also be divided to prepare respectively
Or after preparing the solution or dispersion liquid of different material, remix, used in liquid be in water and polar organic solvent
It is one or more, a certain amount of acidic or alkaline substances can also be added as needed.
3. the general preparative methods of redox graphene group compound film according to claim 1, it is characterised in that: step
(1) in, the concentration of graphene oxide is not more than 30 mg/mL, preferably 5-20 mg/mL in the graphite oxide alkenyl mixed liquor.
4. the general preparative methods of redox graphene group compound film according to claim 1, it is characterised in that: step
(1) in, in the graphite oxide alkenyl mixed liquor in addition to graphene oxide, the additive amount of other materials is not higher than added oxygen
2 times of graphite alkene quality.
5. the general preparative methods of redox graphene group compound film according to claim 1, it is characterised in that: step
(1) in, the polymer is water-soluble polymer or other polar solvent dissolubility polymer.
6. the general preparative methods of redox graphene group compound film according to claim 1, it is characterised in that: step
(1) in, the organic nano material mainly includes two-dimension polymer；The inorganic nano material includes silicon, fullerene, activity
Charcoal, graphene, carbon nanotube, carbon black, black squama, graphite alkene, Mxene, titanium dioxide, silicon nitride, boron nitride, molybdenum disulfide, four
Fe 3 O, stannic oxide, titanium dioxide, cobaltosic oxide, nickel hydroxide, mangano-manganic oxide, cadmium sulfide, zinc oxide, dioxy
Change rubidium, cadmium telluride, zinc sulfide nano-material；The metal nano material is gold, silver, foil, lead, nickel, copper, germanium.
7. the general preparative methods of redox graphene group compound film according to claim 1, it is characterised in that: step
(1) in, reducing agent can be added in the graphene oxide dispersion, reducing agent includes hydrazine hydrate, sodium borohydride, glucose, resists
One of bad hematic acid, sodium ascorbate, ethylene glycol, diethylene glycol, hydroquinone, hydrobromic acid, hydroiodic acid and acetic acid are a variety of.
8. the general preparative methods of redox graphene group compound film according to claim 1, it is characterised in that: step
(1) in, crosslinking agent can be added in the graphene oxide dispersion, such as diamines substance, the substance containing amino and sulfydryl, Isosorbide-5-Nitrae-
Butanediol diglycidyl ether, glyoxal, formaldehyde, glyoxalic acid, citric acid, fumaric acid etc..
9. the general preparative methods of redox graphene group compound film according to claim 1, it is characterised in that: step
Suddenly in (3), the liquid be one of water, polar organic solvent, liquid reducer, liquid cross-linker or a variety of mixtures,
Acidic or alkaline substances can also be added in liquid as needed.
10. the general preparative methods of redox graphene group compound film according to claim 1, it is characterised in that: step
Suddenly in (3), the certain temperature is generally 100-300 DEG C；Described a period of time is 2 h -24 h, preferably 5-10h.
11. the general preparative methods of redox graphene group compound film according to claim 1, it is characterised in that: step
Suddenly in (3), in step (3), the redox graphene group compound film includes with support substrate or without support substrate
Redox graphene group compound film.
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| CN113353924A (en) * | 2021-07-29 | 2021-09-07 | 西南科技大学 | Preparation method and application of fluorinated graphene photo-thermal conversion film for laser ignition |
| CN114348997A (en) * | 2021-12-29 | 2022-04-15 | 杭州嘉悦智能设备有限公司 | Nitrogen-doped graphene-metal nanoparticle film and preparation method thereof |
| CN114538422A (en) * | 2022-01-21 | 2022-05-27 | 西南交通大学 | Graphene alternating film with porous-micro air bag structure, preparation method and application |
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