CN110240156B - Graphene concentrated polycondensation adhesive and preparation method and application thereof - Google Patents
Graphene concentrated polycondensation adhesive and preparation method and application thereof Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/182—Graphene
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
Abstract
The invention discloses a graphene concentrated polycondensation adhesive which comprises a graphene nanosheet core, a double-soluble surface active coating, a non-ionic surface active colloid and the like. The volume of the graphene nanosheet core is 10-30%, the volume of the double-soluble surface active coating film is 20-50%, and the volume of the non-ionic surface active colloid is 20-70%. The graphene concentrated poly-gel has the unique properties of high dispersion, high activity, high wetting, high conduction, high permeability, high adsorption, high foam, high specific surface, high corrosion resistance, high wear resistance and the like, and is safe and environment-friendly. Can be diluted by oil, water, gas, acid liquor, alkali liquor, emulsion, paint, cement paste, resin and the like, and is widely applied to the fields of oil and gas exploitation, geothermal development and conduction, energy conservation, permeation, corrosion prevention and the like.
Description
Technical Field
The invention relates to graphene, in particular to graphene condensed glue, a preparation method of the graphene condensed glue and application of the graphene condensed glue.
Background
The graphene is a novel nano-sheet material with super large specific surface area, super strong electric and heat conducting performance, compression resistance, wear resistance and corrosion resistance.
How to innovate and develop the unique performance of the graphene nano material, the graphene nano material is efficiently applied to the fields of oil and gas production increase, geothermal development and conduction, energy conservation, corrosion prevention and the like, and is a hot spot and difficult point problem of global attention and research.
Graphene dispersion liquid prepared by the existing patents and technologies, such as electrophoresis, ultrasound, modification and the like, is not seen or is not prepared into graphene concentrated polycondensation glue, and then the graphene concentrated polycondensation glue is diluted and applied at will according to different requirements. The surface modified graphene is difficult to maintain or completely recover the unique properties of graphene nano-sheets, such as surface adsorption, wear resistance, wettability, conductivity and the like. The graphene dispersion liquid at present has the advantages of low graphene content, high dispersant content, poor general compatibility and safety and environmental protection, high preparation and use costs, no contribution to full play of unique performance of graphene, and more contribution to safe, environment-friendly, efficient transportation, storage and large-scale application.
Disclosure of Invention
One of the purposes of the invention is to provide a graphene concentrated poly-condensation adhesive which has unique performances of high dispersion, high activity, high wetting, high conduction, high permeation, high adsorption, high foam, high specific surface, high corrosion resistance, high wear resistance and the like, can be diluted by oil, water, gas, acid liquor, alkali liquor, emulsion, paint, cement paste, resin and the like at high power, and is widely applied to the fields of oil and gas exploitation, geothermal development and conduction, energy conservation, permeation, corrosion resistance and the like.
The technical scheme is as follows: a graphene concentrated polymerization adhesive is composed of a graphene nanosheet core, a double-soluble surface active coating, a non-ionic surface active colloid and the like. The volume of the graphene nanosheet core is 10-30%, the volume of the double-soluble surface active coating film is 20-50%, and the volume of the nonionic surface active colloid is 20-70%.
Preferably, the double-soluble surface active coating is a double-soluble surfactant which is soluble in both a water solvent and an organic solvent and has a boiling point higher than 150 ℃.
Preferably, the double soluble surfactant is polyethylene glycol, polyglycerol, sucrose ester, alkylolamide, sorbitan ester or a mixture thereof.
Preferably, the nonionic surfactant colloid is a nonionic surfactant having a boiling point higher than 100 ℃.
Preferably, the nonionic surfactant is fluorocarbon, high-carbon fatty alcohol polyoxyethylene ether, high-carbon fatty acid polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyoxyethylene octadecanamine, fatty acid polyoxyethylene ester or a mixture thereof.
The second purpose of the invention is to provide a preparation method of the graphene condensed glue.
The technical scheme is as follows: a preparation method of graphene concentrated polycondensation adhesive comprises the following steps:
weighing graphene, a double-soluble surfactant and a nonionic surfactant according to a volume ratio, adding volatile environment-friendly dispersing agents such as ethanol, propanol and the like with the volume more than 1 time and the boiling point lower than 100 ℃, and uniformly stirring and mixing to prepare a graphene dispersion liquid;
and secondly, putting the graphene dispersion liquid formed in the step one into a pressure-resistant temperature-resistant nonmetal closed container, and heating by using microwaves. And (3) keeping the temperature at 90-100 ℃ until the volatile dispersing agent is completely evaporated and gasified, and forming high-dispersion graphene coating foam with other surfactants around the graphene concentrated coating. The graphene nanosheets are high in electric conduction, heat conduction and microwave adsorption capacity, and are preferentially and rapidly heated and magnetized, the volatile dispersing agents with low boiling points on the surfaces and the periphery of the graphene nanosheets are gasified to form bubbles, and the double-soluble surfactant with high boiling point forms a coating film on the surface of each graphene nanosheet.
Thirdly, stirring or ultrasonically vibrating the high-dispersion graphene coating foam formed in the pressure-resistant and temperature-resistant container to release gas to normal pressure, cooling to normal temperature, and condensing to obtain the graphene concentrated polymer gel.
The third purpose of the invention is to provide the application of the graphene condensed glue. The graphene concentrated poly-gel can be diluted by adding oil, gas, water, acid liquor, alkali liquor, emulsion, paint, cement slurry, resin and the like according to the actual application and use conditions of oil gas exploitation, geothermal development and conduction, energy conservation, energy storage, adsorption, corrosion prevention and the like.
The technical scheme is as follows: graphene poly-gel nano-foam/graphene poly-gel hot water or steam/graphene poly-gel nano-emulsion/graphene poly-gel nano-acid solution/graphene poly-gel nano-alkali solution/graphene poly-gel nano-paint/graphene poly-gel nano-pore cement stone/graphene poly-gel nano-resin. The graphene poly-gel nano foam is prepared by diluting the graphene concentrated poly-gel with water and injecting the diluted graphene concentrated poly-gel and inert gas into a foam generator; the hot water or steam for graphene glue polymerization is prepared by diluting the concentrated graphene glue polymerization with water and then heating; the graphene poly-gel nano emulsion is prepared by diluting the graphene concentrated poly-gel with emulsion; the graphene poly-gel nano acid solution is prepared by diluting the graphene concentrated poly-gel with an organic acid solution or an inorganic acid solution; the graphene poly-gel nano alkali liquor is prepared by diluting the graphene concentrated poly-gel alkali liquor; the graphene poly-gel nano paint is prepared by diluting the graphene concentrated poly-gel with paint; the graphene poly-glue nanopore set cement is prepared by diluting the graphene concentrated poly-glue with cement slurry; the graphene poly-gel nano resin is prepared by diluting the graphene concentrated poly-gel with resin.
The invention principle is as follows:
in the invention, the volatile diluent mainly plays a role in temporary dispersion during dispersion, all the diluent is gasified into bubbles to form high-dispersion graphene nanosheet foam during microwave heating and concentration, and finally all the high-dispersion graphene nanosheet foam is evaporated and volatilized to be released; when the double-soluble surfactant is heated and concentrated by microwaves, the graphene nanosheets are quickly heated and magnetized and dispersed and arranged due to high conductivity of the graphene nanosheets and high adsorbability of the double-soluble surfactant to the microwaves, a double-soluble surface active concentrated molecular film is formed on the surface of the graphene nanosheets to wrap the surface of the graphene nanosheets so as to modify the surface of the graphene nanosheets, the graphene nanosheets are prevented from aggregating, the modified concentrated molecular film can be dissolved in a water solvent or an organic solvent to play a role of the surfactant when diluted and applied, and the graphene nanosheets which lose a coated film can restore unique performances such as surface activity, adsorbability, conductivity, wear resistance and corrosion resistance; the nonionic surfactant becomes a continuous phase dispersant of the graphene coating film during microwave heating concentration, and is soluble in both water solvents and organic solvents during dilution application, so that the nonionic surfactant plays a role of the nonionic surfactant.
Compared with the prior art, the invention has the following beneficial effects:
1. the performance is unique: the graphene concentrated poly-gel prepared by the invention has the unique performances of high dispersion, high activity, high wetting, high conduction, high permeation, high adsorption, high foam, high specific surface, high corrosion resistance, high wear resistance and the like.
2. The use is convenient: the graphene concentrated poly-gel provided by the invention is highly concentrated, good in compatibility and convenient to transport and use. At normal temperature, oil, gas, water, acid liquor, alkali liquor, paint, cement paste, resin and the like can be added easily in any proportion for mixing and dilution, and the dispersing agent has the advantages of good dispersibility, strong stability, simple operation and convenient use.
3. The application is wide: the graphene concentrated poly-gel can be mixed with oil, gas, water, acid liquor, alkali liquor, emulsion, paint, cement slurry, drilling fluid, fracturing fluid, resin and the like, can be diluted efficiently at any proportion in a high-power way, and can be widely applied to the fields of oil and gas exploitation, geothermal development, energy conservation, conduction, permeation, corrosion prevention and the like.
4. Safety and environmental protection: the graphene concentrated poly-gel prepared by the invention has the advantages of no acid, no alkali, no dust, no water, no toxicity, no harm, neutrality, stability, corrosion resistance, temperature resistance, safety in production, transportation, storage and use, and environmental protection. Description of the terms
The invention discloses graphene concentrated poly-condensation glue, which is high-dispersity graphene coated jelly formed by firstly dispersing and then concentrating graphene.
Drawings
Fig. 1 is a microscopic morphology of the graphene condensed hydrogel in example 1 of the present invention.
Detailed Description
The invention will be further explained with reference to the drawings.
A preparation method of graphene concentrated polycondensation adhesive comprises the following steps:
weighing graphene, a double-soluble surfactant and a nonionic surfactant according to a volume ratio, sequentially adding a volatile environment-friendly dispersing agent such as ethanol, propanol and the like with the total volume more than 1 time and the boiling point lower than 100 ℃ into a closed container, and uniformly stirring and mixing to prepare a graphene dispersion liquid;
and secondly, putting the graphene dispersion liquid formed in the step one into a pressure-resistant temperature-resistant closed nonmetal container, and heating by using microwaves. Due to the fact that the graphene nanosheets are high in electric conduction, heat conduction and microwave adsorption capacity, rapid heating and magnetization are performed preferentially, the volatile dispersing agents with low boiling points on the surfaces and the periphery of the graphene nanosheets are gasified to form bubbles, and the double-soluble surfactant with high boiling points forms a coating film on the surface of each graphene nanosheet. And (3) keeping the temperature at 90-100 ℃ until the volatile dispersing agent is completely evaporated and gasified, and forming high-dispersion graphene coating foam with other surfactants around the graphene concentrated coating.
Thirdly, stirring or ultrasonically vibrating the high-dispersion graphene coating foam formed in the pressure-resistant and temperature-resistant container to release gas to normal pressure, cooling to normal temperature, and condensing to obtain the graphene concentrated polymer gel.
Example 1 preparation of graphene condensation Polymer
200 ml of graphene, 300 ml of polyethylene glycol double-soluble surfactant, 500 ml of fluorocarbon nonionic surfactant and 1000 ml of absolute ethyl alcohol volatile dispersant are measured respectively. Adding absolute ethyl alcohol, graphene, fluorocarbon and polyethylene glycol into a closed container in sequence, and uniformly stirring to form a neutral graphene dispersion liquid;
and secondly, adding the neutral graphene dispersion liquid formed in the step one into a temperature-resistant and pressure-resistant nonmetal closed container, heating by using microwaves and keeping the temperature at 90-100 ℃ until the volatile diluent is completely evaporated and gasified to form the high-dispersion graphene nano foamed adhesive. In the step, the surface of the graphene is heated, the volatile diluent on the surface of the graphene is gradually evaporated and gasified, the double-soluble dispersing agent and the nonionic surfactant on the surface of the graphene are gradually concentrated to form a film, and the graphene is wrapped, so that the surface of the graphene is modified and is not easy to aggregate.
And thirdly, naturally cooling the formed graphene high-dispersion nano foamed glue to normal temperature under normal pressure, and finally condensing the graphene high-dispersion nano foamed glue into 900 ml of graphene concentrated condensation glue with unique performances of high dispersion, high activity, high wetting, high conduction, high permeation, high adsorption, high foaming, high specific surface, high corrosion resistance, high wear resistance and the like. In the graphene concentrated poly-colloid, the core of a graphene nanosheet accounts for 22.2% of the total volume, the double-soluble surface active coating accounts for 33.3% of the total volume, and the non-ionic surface active colloid accounts for 44.5% of the total volume.
The graphene gel concentrate prepared in this example is shown in fig. 1.
Example 2 graphene poly-gel nanofoam
The graphene concentrated gel prepared by the method in example 1 is diluted by adding 1000-10000 times (volume multiple) of water, and then the diluted solution and inert gases such as nitrogen, carbon dioxide and the like are respectively injected into a foam generator to be mixed to form the nano graphene gel foam with high dispersion, high activity, high wetting, high conductivity and high stability. The nano graphene poly-gel foam is used for foam drilling, foam cementing, foam acidification, foam acid fracturing, foam flooding, foam gas production, foam drainage, foam cleaning, foam fire extinguishing and the like of oil and gas fields.
Example 3 graphene gel-forming hot water or steam
The graphene concentrated poly gel prepared by the method in the embodiment 1 is diluted by 1000-5000 times (volume multiple) of water and then heated to form graphene poly gel hot water or steam with characteristics of high dispersion, high activity, high wetting, high heat conductivity and the like, and then the graphene poly gel hot water or steam is injected into a thick oil or oil sand layer for huff and puff or displacement, so that the thick oil and the oil sand are efficiently exploited, and the thermal efficiency, the yield and the recovery rate are improved.
Example 4 graphene poly-gel nanoemulsion
The concentrated graphene gel prepared by the method in example 1 is diluted by oil-water emulsion with 1000-.
Example 5 graphene poly-colloid nano acid solution
The graphene concentrated poly-gel prepared by the method in the embodiment 1 is diluted by adding 1000-10000 times (volume multiple) of organic acid solution or inorganic acid solution to prepare the graphene poly-gel nano acid solution with the characteristics of high dispersion, high activity, high wetting, high specific surface, high corrosion resistance and the like, and the graphene poly-gel nano acid solution is used for the operations of acid cleaning, acidification, acid fracturing and the like of oil-gas-water wells.
Example 6 graphene poly-gel nano-alkali solution
The graphene concentrated poly gel prepared by the method in example 1 is diluted by adding 1000-10000 times (volume times) of alkali liquor to prepare the graphene poly gel nano alkali liquor with the characteristics of high dispersion, high activity, high adsorption, high corrosion resistance and the like, and the graphene poly gel nano alkali liquor is used for oil displacement, carbon absorption, sulfur removal, corrosion resistance and the like.
Example 7 graphene poly gel nano-paint
The graphene concentrated poly gel prepared by the method in the embodiment 1 is diluted by adding 100-1000 times (volume times) of paint to prepare the graphene poly gel nano paint with the characteristics of high conductivity, high wear resistance, high corrosion resistance and the like, and the graphene poly gel nano paint can be used for ultrathin and efficient heat conduction, electric conduction, temperature resistance, wear resistance, corrosion resistance coatings and the like.
Example 8 graphene poly-cement nanopore cement
The graphene concentrated poly-gel prepared by the method in the embodiment 1 is diluted by adding 100-1000 times (volume multiple) of cement slurry to prepare the graphene poly-gel nanopore cement with the characteristics of high permeability, high conductivity, high wear resistance, high corrosion resistance and the like. The graphene glue-gathering nanopore cement is used for sponge city construction of permeable set cement fracturing, water control and sand control in oil and gas and geothermal exploitation, and permeable pavement, floor heating floor, breathable wall and the like.
Example 9 graphene poly-gel nanophase
The graphene concentrated poly-gel prepared by the method in the embodiment 1 is diluted by adding 100-1000 times (volume times) of resin to prepare the graphene poly-gel nano resin with the characteristics of high electric conductivity, high heat transfer, high wear resistance, high corrosion resistance and the like, and the graphene poly-gel nano resin is used for lightning arresters, antistatic devices, corrosion-resistant radiators, wear-resistant and corrosion-resistant coatings and the like in flammable and explosive places in the oil and gas field.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A graphene concentrated poly-gel comprises a graphene nano-sheet core, a double-soluble surface active coating and a non-ionic surface active colloid.
2. The graphene concentrated poly-gel as claimed in claim 1, wherein: the volume of the graphene nano-sheet core accounts for 10-30%, the volume of the double-soluble surface active coating accounts for 20-50%, and the volume of the double-soluble surface active colloid accounts for 20-70%.
3. The graphene concentrated poly-mer according to any one of claims 1 or 2, characterized in that: the double-soluble surface active coating is a double-soluble surfactant which is soluble in a water solvent and an organic solvent and has a boiling point higher than 150 ℃.
4. The graphene concentrated poly gel of claim 3, wherein: the double-soluble surfactant is polyethylene glycol, polyglycerol, alkylolamide or a mixture thereof.
5. The graphene concentrated poly-mer according to any one of claims 1 or 2, characterized in that: the nonionic surfactant colloid is a nonionic surfactant with a boiling point higher than 100 ℃.
6. The graphene concentrated poly-mer according to claim 5, characterized in that: the nonionic surfactant is fluorocarbon, high-carbon fatty alcohol polyoxyethylene ether, high-carbon fatty acid polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether, octadecylamine polyoxyethylene ether, fatty acid polyoxyethylene ester or a mixture thereof.
7. A method for preparing the graphene concentrated polycondensation adhesive as claimed in any one of claims 1 to 6, comprising the following steps:
weighing graphene, a double-soluble surfactant and a nonionic surfactant according to a volume ratio, sequentially adding ethanol or propanol volatile environment-friendly dispersing agent with the volume more than 1 time and the boiling point lower than 100 ℃, and uniformly stirring and mixing to prepare graphene dispersion liquid;
secondly, putting the graphene dispersion liquid formed in the step one into a pressure-resistant temperature-resistant nonmetal closed container, and heating by using microwaves; keeping the temperature at 90-100 ℃ until the volatile dispersant is completely evaporated and gasified, and concentrating graphene to coat other surfactants around the film to form high-dispersion graphene coating foam;
thirdly, stirring or ultrasonically vibrating the high dispersion graphene coating foam formed in the pressure-resistant and temperature-resistant nonmetal container to release gas to normal pressure, cooling to normal temperature, and finally condensing into the graphene condensed glue.
8. A graphene poly glue nanometer foam/graphene poly glue hot water or steam/graphene poly glue nanometer emulsion/graphene poly glue nanometer acid liquid/graphene poly glue nanometer alkali liquid/graphene poly glue nanometer paint/graphene poly glue nanometer cement slurry/graphene poly glue nanometer resin slurry is characterized in that: the graphene poly-gel nano-foam is prepared by diluting the graphene concentrated poly-gel of any one of claims 1 to 6 with water and introducing inert gas; the graphene poly-glue hot water or steam is prepared by diluting the graphene concentrated poly-glue according to any one of claims 1 to 6 with water and then heating; the graphene poly-gel nano-emulsion is prepared by diluting the graphene concentrated poly-gel of any one of claims 1-6 with an emulsion; the graphene poly-gel nano acid solution is prepared by diluting the graphene concentrated poly-gel of any one of claims 1 to 6 with an organic acid solution or an inorganic acid solution; the graphene polygel nano alkali liquor is prepared by diluting the graphene concentrated polygel alkali liquor of any one of claims 1 to 6; the graphene poly gel nano paint is prepared by diluting the graphene concentrated poly gel of any one of claims 1 to 6 with paint; the graphene poly-gel nanopore cement slurry is prepared by diluting the graphene concentrated poly-gel in any one of claims 1 to 6 with cement slurry; the graphene poly-gel nano-resin is prepared by diluting the graphene concentrated poly-gel of any one of claims 1 to 6 with resin.
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