CN114873586A - Preparation method of graphene material dispersion liquid - Google Patents
Preparation method of graphene material dispersion liquid Download PDFInfo
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- CN114873586A CN114873586A CN202210446493.6A CN202210446493A CN114873586A CN 114873586 A CN114873586 A CN 114873586A CN 202210446493 A CN202210446493 A CN 202210446493A CN 114873586 A CN114873586 A CN 114873586A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 231
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 212
- 239000000463 material Substances 0.000 title claims abstract description 164
- 239000006185 dispersion Substances 0.000 title claims abstract description 124
- 239000007788 liquid Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 58
- 239000002904 solvent Substances 0.000 claims abstract description 68
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 20
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
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- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
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- 238000002604 ultrasonography Methods 0.000 claims description 4
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- 238000004299 exfoliation Methods 0.000 claims description 2
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- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 2
- 239000008158 vegetable oil Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 description 20
- 239000010687 lubricating oil Substances 0.000 description 18
- 239000010689 synthetic lubricating oil Substances 0.000 description 18
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- 239000010439 graphite Substances 0.000 description 13
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 8
- 238000005265 energy consumption Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 4
- 239000005457 ice water Substances 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 239000007800 oxidant agent Substances 0.000 description 4
- 235000010333 potassium nitrate Nutrition 0.000 description 4
- 239000004323 potassium nitrate Substances 0.000 description 4
- 239000012286 potassium permanganate Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/135—Carbon
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- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a preparation method of a graphene material dispersion liquid. The preparation method comprises the following steps: (1) mixing a graphene material with a low-viscosity solvent to obtain a first dispersion liquid; (2) mixing the first dispersion liquid obtained in the step (1) with a high-viscosity solvent to obtain a second dispersion liquid; (3) removing the low-viscosity solvent from the second dispersion liquid obtained in the step (2) to obtain the graphene material dispersion liquid. The preparation method of the graphene material dispersion liquid provided by the invention can realize uniform dispersion of the graphene material in the high-viscosity solvent, greatly reduce the time required for dispersion of the graphene material in the high-viscosity solvent, improve the dispersion efficiency of the graphene material in the high-viscosity solvent, and has the advantages of simple process and low cost.
Description
Technical Field
The invention belongs to the technical field of graphene materials, and particularly relates to a preparation method of a graphene material dispersion liquid.
Background
The graphene is represented by sp 2 The two-dimensional nano material formed by the hybridization of carbon atoms in a hexagonal arrangement has high electrical conductivity, thermal conductivity and mechanical strength. Under the action of friction, graphiteThe lamina layer can rotate, and the friction force is converted into the rotating force. Furthermore, when multi-layer graphene in which single-layer graphene is stacked is rubbed, graphene sheets may slip with each other. Therefore, the graphene has excellent friction resistance and is an excellent lubricating oil additive. In addition, graphene can absorb infrared radiation and has good heat transfer efficiency. Therefore, the graphene can be used as an additive to improve the combustion efficiency of oil products.
At present, the graphene is mainly dispersed in oil products by an ultrasonic method or by adding a dispersing agent. Generally, a certain mass of graphene material is added into an oil product, and the graphene is dispersed in different oil products through ultrasound or the assistance of a dispersing agent. For example, CN107338086A discloses a lubricating oil additive of graphene doped composite dispersant and a preparation method thereof, wherein the preparation method comprises the following steps: the single-layer or multi-layer graphene and the specific composite dispersant are added into the lubricating oil by in-situ modification and ultrasonic dispersion methods, so that the sedimentation and agglomeration of the graphene are reduced, and the antifriction and antiwear performance of the graphene in the lubricating oil is exerted. However, the preparation method requires doping of a composite dispersant, and the content of dispersed graphene is small.
CN111621350A discloses a preparation method of graphene lubricating oil for vehicles, which comprises the following steps: mixing the modified graphene with nano lubricating oil, adding a dispersing agent, and carrying out ultrasonic treatment to obtain the graphene lubricating oil. The graphene improves the lubricating performance of the lubricating oil, but a dispersant needs to be added, the ultrasonic time is long, and the energy consumption is high.
CN106118826A discloses a modified graphene lubricating oil with high dispersibility and high affinity and a preparation method thereof, the preparation method comprises the following steps: (1) gradually adding the modified graphene, the dispersing agent, the affinity agent, the anti-foaming agent and the preservative into the base oil, and uniformly stirring; (2) and (2) stirring the mixture obtained in the step (1) while carrying out ultrasonic oscillation to obtain the modified graphene lubricating oil. The modified graphene in the lubricating oil is uniformly dispersed, so that excellent anti-wear and anti-friction effects can be realized, and the lubricating oil has good mechanical protection and excellent stability and oxidation resistance. However, the graphene lubricating oil is high in cost and energy consumption.
A common drawback in the prior art is that most oils have a higher viscosity, especially lubricating oils, and as the viscosity increases, their anti-friction properties increase. Due to the fact that strong pi-pi stacking interaction exists between graphene sheet layers, higher energy consumption is often needed for achieving the dispersion of aggregated graphene in a high-viscosity solvent. Moreover, the effect of direct ultrasonic dispersion is not good, and the dispersed graphene is easy to re-aggregate along with the time extension, so that the performance of the oil product is further reduced.
Therefore, developing a graphene material dispersion method with high dispersion efficiency, good stability, low energy consumption and low cost in high-viscosity oil products is an urgent problem to be solved in the field.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a graphene material dispersion liquid. The preparation method of the graphene material dispersion liquid enables the graphene material to be high in dispersion efficiency in a high-viscosity solution and good in stability, improves the friction reduction performance of the graphene material, and is simple in process and low in cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a preparation method of a graphene material dispersion, including the following steps:
(1) mixing a graphene material with a low-viscosity solvent to obtain a first dispersion liquid;
(2) mixing the first dispersion liquid obtained in the step (1) with a high-viscosity solvent to obtain a second dispersion liquid;
(3) removing the low-viscosity solvent from the second dispersion liquid obtained in the step (2) to obtain the graphene material dispersion liquid.
In the invention, the graphene material is uniformly dispersed in the low-viscosity solvent by uniformly dispersing the graphene material in the low-viscosity solvent, and then is mixed with the high-viscosity solvent. Because the diffusion speed of the low-viscosity solvent molecules in the high-viscosity solvent is far higher than that of the agglomerated graphene in the high-viscosity solvent, the low-viscosity solvent molecules can carry the dispersed graphene material to be uniformly mixed with the high-viscosity solvent molecules, so that the graphene material is further uniformly mixed with the high-viscosity solvent, and then the low-viscosity solvent molecules are removed, so that the graphene material is uniformly dispersed in the high-viscosity solvent, and the stability and the friction reduction performance of the graphene material are improved. Compared with other dispersing methods, the method does not need to modify the graphene material or introduce other additives such as a dispersing agent and the like to help dispersion, can avoid the introduction of impurities, reduces the cost, and improves the quality of high-viscosity solvents, especially oil products.
Preferably, the graphene material comprises a graphene material prepared by an electrochemical stripping method and/or a graphene material prepared by reducing graphene oxide.
In the invention, the specific steps of preparing the graphene material by adopting an electrochemical stripping method comprise:
and in the presence of electrolyte, taking the graphite foil as a working electrode and taking an inert metal or carbon electrode as a counter electrode, and electrolyzing to obtain the graphene material.
Preferably, the electrolyte comprises any one of ammonium sulfate, potassium sulfate, sodium sulfate, potassium chloride, sodium hydroxide, sulfuric acid, or tetrabutylammonium hydroxide, or a combination of at least two thereof.
Preferably, the concentration of the electrolyte is 0.05-2M, for example, 0.06M, 0.1M, 0.5M, 1M, 2M and the like.
Preferably, the inert metal electrode includes any one of a platinum electrode, a gold electrode, or a graphite electrode.
Preferably, the distance between the working electrode and the counter electrode is 1.5 to 10cm, and may be, for example, 1.5cm, 1.8cm, 2cm, 2.2cm, 2.4cm, 3cm, 4cm, 5cm, 6cm, 7cm, 8cm, 9cm, or the like.
Preferably, the voltage of the electrolysis is 5-15V, for example, 6V, 8V, 10V, 12V, 14V and the like.
Preferably, the electrolysis time is 5-15 min, for example, 6min, 8min, 10min, 12min, 14min and the like.
Preferably, the electrolysis further comprises the steps of suction filtration, washing and drying.
Preferably, the drying temperature is 40 to 80 ℃, for example, 50 ℃, 60 ℃, 70 ℃ and the like.
In the invention, the graphene material prepared by reducing graphene oxide is prepared by a hummers method, and the specific steps include:
taking graphite as a raw material, and stripping the graphite by using an oxidant to obtain graphene oxide; and reducing the graphene oxide to obtain the graphene material.
Preferably, the oxidant comprises a combination of concentrated sulphuric acid, potassium nitrate and potassium permanganate.
Preferably, the mass ratio of the concentrated sulfuric acid to the graphite is (20-200): 1, and may be, for example, 25:1, 30:1, 40:1, 50:1, 60:1, 80:1, 100:1, 120:1, 140:1, 160:1, 180:1, and the like.
Preferably, the mass ratio of the potassium permanganate to the graphite is (2-20): 1, and for example, the mass ratio can be 4:1, 6:1, 8:1, 10:1, 12:1, 14:1, 16:1, 18:1, and the like.
The mass ratio of potassium nitrate to graphite is preferably (0.2 to 5: 1), and may be, for example, 0.4:1, 0.8:1, 1:1, 1.5:1, 2:1, 2.5:1, 3:1, 3.5:1, 4:1, 4.5:1, or the like.
In the invention, the reaction condition for stripping the graphene by using the oxidant comprises the steps of reacting for 30min under the ice-water bath condition, heating to 35 ℃ for reacting for 6h, and continuing the ice-water bath reaction for 2h to obtain the graphene oxide.
Preferably, the reducing agent used for the reduction comprises hydrazine hydrate.
Preferably, the mass ratio of hydrazine hydrate to graphene oxide is (1-5): 1, and may be, for example, 1:1, 1.5:1, 2:1, 3:1, 4:1, or the like.
According to the invention, the graphene reduction and oxidation process comprises the steps of reacting for 1h at 95 ℃, and then washing and drying to obtain the graphene material.
According to the invention, the graphene material prepared by adopting an electrochemical stripping method or reducing graphene oxide can be used for obtaining the graphene material with low oxygen content, can be rapidly dispersed in a low-viscosity solvent, and further improves the dispersion of the graphene material in a high-viscosity solvent.
Preferably, the thickness of the graphene material is 1-3 nm, and for example, the thickness can be 1nm, 2nm, or 3 nm.
Preferably, the graphene material has a sheet size of 500nm to 2 μm, and may be, for example, 600nm, 800nm, 1 μm, 2 μm, or the like.
Preferably, the viscosity of the low-viscosity solvent in step (1) is not more than 3 mPas at 20 ℃, and may be, for example, 0.2 mPas, 0.4 mPas, 0.8 mPas, 1 mPas, 1.2 mPas, 1.4 mPas, 1.6 mPas, 1.8 mPas, 2 mPas, 2.2 mPas, 2.4 mPas, 2.6 mPas, 2.8 mPas, or the like.
Preferably, the low viscosity solvent comprises any one of ethanol, propanol, tetrahydrofuran, N-dimethylformamide, dimethylsulfoxide, or acetonitrile, or a combination of at least two thereof.
In the present invention, the graphene is easily dispersed into a low viscosity solvent.
Preferably, the volume of the low-viscosity solvent is 0.05 to 2mL, and may be, for example, 0.1mL, 0.2mL, 0.4mL, 0.6mL, 0.8mL, 1mL, 1.5mL, 1.8mL, or the like, based on 1mg of the mass of the graphene material.
Preferably, the mixing of step (1) comprises performing under ultrasonic conditions.
Preferably, the power of the ultrasound is 50-500W, such as 60W, 80W, 100W, 150W, 200W, 250W, 300W, 350W, 400W, 460W, 470W, 480W, 490W, 500W, 510W, 520W, 530W, 540W, etc.
Preferably, the time of the ultrasonic treatment is 5-30 min, for example, 6min, 8min, 10min, 12min, 15min, 18min, 20min, 22min, 24min, 26min, 28min and the like.
Preferably, the content of the graphene material in the first dispersion liquid in the step (1) is 0.02 to 5% by mass, and may be, for example, 0.04%, 0.06%, 0.08%, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 4.5%, or the like.
The viscosity of the high-viscosity solvent in the step (2) is preferably not less than 100 mPas, and may be, for example, 120 mPas, 140 mPas, 160 mPas, 180 mPas, 200 mPas, or the like at 20 ℃.
Preferably, the high viscosity solvent includes any one of or a combination of at least two of engine oil, vegetable oil, silicone oil, paraffin wax, or oleic acid.
In the present invention, the engine oil refers to lubricating oil.
Preferably, the mixing method of step (2) comprises physical shaking and/or stirring.
Preferably, the mixing time in step (2) is 1-5 min, for example, 1min, 2min, 3min, 4min, 5min, etc.
Preferably, the method for removing the low-viscosity solvent of step (3) comprises heating evaporation and/or direct suction.
In the present invention, the direct suction means that when the low-viscosity solvent and the high-viscosity solvent are separated from each other, the low-viscosity solvent is directly sucked away, thereby removing the low-viscosity solvent.
The volume ratio of the low-viscosity solvent to the high-viscosity solvent is preferably (0.05-10): 1, and may be, for example, 0.07:1, 0.1:1, 0.5:1, 1:1, 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, or the like.
Preferably, the graphene material in the graphene material dispersion liquid is 0.02 to 5% by mass, and may be, for example, 0.04%, 0.06%, 0.08%, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 4.5% by mass or the like.
In the invention, the graphene material is in a specific content range, so that the dispersion effect of the graphene material can be ensured, and the abrasion resistance of the graphene material can also be ensured; the content is too low to play a role in friction resistance, the content is too high, and the dispersion effect is poor.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) ultrasonically mixing a graphene material and a low-viscosity solvent for 5-30 min under the condition that the power is 50-500W to obtain a first dispersion liquid;
(2) mixing the first dispersion liquid obtained in the step (1) with a high-viscosity solvent for 1-5 min to obtain a second dispersion liquid;
(3) removing the low-viscosity solvent from the second dispersion liquid obtained in the step (2) by heating evaporation and/or direct suction to obtain the graphene material dispersion liquid; the mass percentage of graphene in the graphene material dispersion liquid is 0.02-5%.
According to the invention, the graphene material is prepared by an electrochemical stripping method or reduction of graphene oxide, and then the graphene material is dispersed in a high-viscosity solvent by means of a low-viscosity solvent, so that the graphene material has better dispersibility, stability and abrasion resistance in oil products.
The recitation of numerical ranges herein includes not only the above-recited values, but also any values between any of the above-recited numerical ranges not recited, and for brevity and clarity, is not intended to be exhaustive of the specific values encompassed within the range.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the graphene material dispersion liquid, the graphene material is dispersed in the low-viscosity solvent, then the graphene material is mixed with the high-viscosity solvent, and finally the low-viscosity solvent is removed, so that the graphene material is uniformly dispersed in the high-viscosity solvent, the dispersion efficiency is high, the graphene material is kept stand for 48 hours without sedimentation and agglomeration, the friction reduction performance of the graphene material is improved, the friction coefficient is less than or equal to 0.103, the friction force is less than or equal to 5.033kgf, and the diameter of a friction spot is less than or equal to 0.46 mm; and other auxiliary agents are not needed, so that the introduction of impurities is avoided, and the method is low in energy consumption, low in cost, simple in process and good in universality.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of a graphene material dispersion liquid provided in embodiment 1 of the present invention;
fig. 2 is a scanning electron microscope image of the graphene material provided in preparation example 1 of the present invention;
fig. 3 is a graph illustrating a dispersion effect of a graphene material in absolute ethanol in a preparation method of a graphene material dispersion solution provided in example 1;
fig. 4 is a graph showing the dispersion effect of the graphene material in the mixed solvent of absolute ethanol and synthetic lubricating oil in the preparation method of the graphene material dispersion provided in example 1;
fig. 5 is a diagram illustrating a dispersion effect of a graphene material in a synthetic lubricating oil in a preparation method of a graphene material dispersion solution provided in example 1;
FIG. 6 is a graph showing the dispersion effect of the graphene material dispersion liquid in example 1 after standing for 48 hours;
fig. 7 is a graph illustrating the effect of dispersing graphene materials in oleic acid in the preparation method of the graphene material dispersion provided in example 2;
fig. 8 is a graph illustrating a dispersion effect of a graphene material in N, N-dimethylformamide in a preparation method of a graphene material dispersion solution provided in example 3;
fig. 9 is a graph showing the effect of dispersing a graphene material in a mixed solvent of N, N-dimethylformamide and synthetic lubricating oil in the method for preparing a graphene material dispersion solution provided in example 3;
the lower layer is N, N-dimethylformamide, and the upper layer is synthetic lubricating oil dispersed with graphene materials;
fig. 10 is a graph showing the dispersion effect of the graphene material in the preparation method of the graphene material dispersion liquid provided in comparative example 1.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The materials used in the examples and comparative examples of the present invention are as follows:
synthesizing lubricating oil: daoqi, SP 0W-20 lubricating oil
Preparation example 1
The graphene material is prepared by adopting an electrochemical stripping method and comprises the following specific steps:
graphite foil as working electrode, platinum wire as counter electrode, and 0.1M (NH) 4 ) 2 SO 4 A strip of electrolyte with a distance of 2cm between the working electrode and the counter electrode and an electrolysis voltage of 10VElectrolyzing for 10min under the condition to obtain graphene dispersion liquid; and (3) carrying out suction filtration and washing on the graphene dispersion liquid, and drying in an oven at 60 ℃ overnight to obtain the electrochemically stripped graphene material (the thickness is 1 nm).
The structure of the graphene material provided in preparation example 1 was characterized by using a scanning electron microscope (SU 8220, hitachi corporation), and the result is shown in fig. 2, which shows that the sheet size of the graphene material is 500nm to 2 μm.
Preparation example 2
A graphene material, which is different from preparation example 1 only in that 1MH is used in the preparation method 2 SO 4 As an electrolyte, a graphene material with a thickness of 2nm was obtained, and other steps and parameters were the same as those of preparation example 1.
Preparation example 3
The graphene material is prepared by adopting a conventional method for reducing graphene oxide, and comprises the following specific steps:
taking graphite as a raw material, stripping the graphite by using concentrated sulfuric acid, potassium nitrate and potassium permanganate as oxidants, reacting for 30min under the condition of ice-water bath, heating to 35 ℃, reacting for 6h, and continuing the ice-water bath reaction for 2h to obtain graphene oxide; then, reducing the graphene oxide by using hydrazine hydrate as a reducing agent, reacting for 1h at the temperature of 95 ℃, washing and drying to obtain the graphene material; the mass ratio of the concentrated sulfuric acid to the graphite is 80:1, the mass ratio of the potassium nitrate to the graphite is 1.2:1, and the mass ratio of the potassium permanganate to the graphite is 6: 1; the mass ratio of the hydrazine hydrate to the graphene oxide is 3: 1.
Preparation example 4
The graphene material is different from the graphene material prepared in the preparation example 1 only in that the electrolyte is prepared by adopting KNO with the concentration of 1.5M 3 And (3) dissolving to obtain a graphene material with the thickness of 50nm, wherein other steps and parameters are the same as those of preparation example 1.
Preparation example 5
The graphene is only different from preparation example 1 in that the graphene is prepared by a ball milling method, and the method comprises the following specific steps: dispersing a graphite material into an aqueous solution containing sodium carboxymethylcellulose, grinding for 6 hours by using a ball mill, and stripping to obtain a graphene dispersion liquid; and carrying out suction filtration and washing on the graphene dispersion liquid, and drying in an oven at 60 ℃ overnight to obtain the mechanically-peeled graphene material.
Example 1
The embodiment provides a preparation method of a graphene material dispersion liquid, which comprises the following specific steps:
(1) weighing 5mg of the graphene material provided in preparation example 1 in 5mL of absolute ethyl alcohol, and performing ultrasonic treatment for 20min under the condition that the ultrasonic power is 500W to obtain a uniform first dispersion liquid;
(2) transferring the first dispersion liquid into 5mL of synthetic lubricating oil, and shaking and mixing for 20s to obtain a second dispersion liquid;
(3) and transferring the second dispersion liquid to an open culture dish, and heating the second dispersion liquid on a hot table at 80 ℃ for 30min to obtain the graphene material dispersion liquid.
In the present invention, a schematic flow chart of the preparation method of the graphene material dispersion liquid provided in example 1 is shown in fig. 1.
In the invention, the dispersion effect of the graphene material in absolute ethyl alcohol is shown in fig. 3; the dispersion effect in the mixed solvent of absolute ethyl alcohol and synthetic lubricating oil is shown in FIG. 4; the dispersion effect in synthetic lubricating oils is shown in FIG. 5.
The dispersion effect of the graphene material after allowing the graphene material dispersion liquid obtained in example 1 to stand for 48 hours is shown in fig. 6.
Example 2
The embodiment provides a preparation method of a graphene material dispersion liquid, which comprises the following specific steps:
(1) weighing 5mg of the graphene material provided in preparation example 2 in 2mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 20min under the condition that the ultrasonic power is 500W to obtain a uniform first dispersion liquid;
(2) transferring the first dispersion liquid into 5mL of oleic acid, and shaking and mixing for 20s to obtain a second dispersion liquid;
(3) and transferring the second dispersion liquid to an open culture dish, and heating the second dispersion liquid on a hot table at 80 ℃ for 30min to obtain the graphene material dispersion liquid.
In the present invention, the dispersion effect of the graphene material in oleic acid is shown in fig. 7.
Example 3
The embodiment provides a preparation method of a graphene material dispersion liquid, which comprises the following specific steps:
(1) weighing 5mg of the graphene material provided in preparation example 1 in 5mL of N, N-dimethylformamide, and performing ultrasonic treatment for 5min under the condition that the ultrasonic power is 500W to obtain a uniform first dispersion liquid;
(2) transferring the first dispersion liquid into 5mL of synthetic lubricating oil, shaking and mixing for 20s, and standing for 1min to obtain a layered second dispersion liquid;
(3) and directly sucking the lower layer of N, N-dimethylformamide in the layered second dispersion liquid by using a dropper to obtain the graphene material dispersion liquid.
In the invention, the dispersion effect of the graphene material in N, N-dimethylformamide is shown in fig. 8; the dispersing effect in the mixed solvent of N, N-dimethylformamide and synthetic lubricating oil is shown in fig. 9; wherein, the lower layer is N, N-dimethylformamide, and the upper layer is synthetic lubricating oil dispersed with graphene materials.
In the present invention, the first dispersion liquid is mixed with the synthetic lubricating oil, and after shaking, the graphene material may be transferred into the synthetic lubricating oil.
Example 4
The present embodiment provides a method for preparing a graphene material dispersion, which is different from that in embodiment 1 only in that the graphene material provided in preparation example 3 is selected as the graphene material in step (1), and other steps and parameters are the same as those in embodiment 1.
Example 5
The present embodiment provides a method for preparing a graphene material dispersion, which is different from that in embodiment 1 only in that the graphene material provided in preparation example 4 is selected as the graphene material in step (1), and other steps and parameters are the same as those in embodiment 1.
Example 6
This example provides a method for preparing a graphene material dispersion, which is different from example 1 only in that the graphene material in step (1) is the graphene material provided in preparation example 5, and other steps and parameters are the same as those in example 1.
Comparative example 1
The present comparative example provides a graphene material dispersion, which is different from example 1 only in that the graphene material is dispersed without using absolute ethanol, and the specific steps include:
weighing 5mg of the graphene material provided in preparation example 1 in 5mL of synthetic lubricating oil, and performing ultrasonic treatment for 20min under the condition that the ultrasonic power is 500W to obtain the graphene material dispersion liquid.
In the present invention, the dispersion effect of the graphene material in the preparation method of the graphene material dispersion liquid provided in comparative example 1 is shown in fig. 10.
Performance testing
(1) Dispersion efficiency: observing whether the solid graphene material exists in the graphene material dispersion liquid obtained in the embodiments 1-6 and the comparative example 1, if the solid graphene material does not exist, marking the solid graphene material as "excellent", and if the content of the solid graphene material is less than 20%, marking the solid graphene material as "better"; if the content of the solid graphene material is more than or equal to 20%, marking as 'poor';
(2) stability: standing the graphene material dispersion liquid provided in the examples 1-6 and the comparative example 1 for 48 hours, observing whether the graphene material dispersion liquid is settled and agglomerated, and dividing the graphene material dispersion liquid into 3 grades according to the observation result, wherein the grades are respectively 'no precipitation', 'partial precipitation' and 'full precipitation';
(3) friction reduction: the friction coefficient, friction force and friction spot diameter of the graphene material dispersion liquid provided in examples 1 to 6 and the synthetic lubricating oil of the undispersed graphene material provided in comparative example 1 were tested by using an MS-10A four-ball friction tester.
The specific test results are shown in table 1:
TABLE 1
Wherein "-" in Table 1 indicates that the test for abrasion resistance was not performed; only the dispersibility of the graphene material needs to be tested in the oleic acid; the "synthetic lubricating oil" in table 1 is labeled with "NA" because no graphene material is added and its dispersibility is not considered.
As can be seen from the above table, according to the preparation method of the graphene material dispersion liquid provided by the invention, the graphene material is dispersed in the low-viscosity solvent, then mixed with the high-viscosity solvent, and finally the low-viscosity solvent is removed, so that the graphene material is uniformly dispersed in the high-viscosity solvent, the dispersion efficiency is high, the graphene material does not settle or agglomerate after standing for 48 hours, the friction reduction performance of the graphene material is improved, other auxiliaries are not needed, the introduction of impurities is avoided, the energy consumption is low, the cost is low, and the process is simple. As can be seen from examples 1 and 3, the friction coefficient of the synthetic lubricating oil is 0.08 to 0.09 by adopting the specific dispersion method of the invention; the friction force is 4.62-4.82 kgf; the diameter of the friction spot is 0.41-0.46 mm, and the friction reducing performance is good.
From examples 1 to 4, it can be seen that the graphene material obtained by electrochemical exfoliation or reduction of graphene oxide has good dispersibility and stability in a high-viscosity solvent by the preparation method of the present invention, and the preparation method of the graphene dispersion liquid provided by the present invention has good universality, and is suitable for not only lubricating oil but also other high-viscosity solvents.
As can be seen from comparison between example 1 and example 5, when the thickness of the graphene material is too large, dispersibility is poor and abrasion resistance is poor; as can be seen from comparison between example 1 and example 6, the graphene material prepared by other methods has poor dispersibility and poor abrasion resistance; as can be seen from comparison between example 1 and comparative example 1, when the low-viscosity solvent is not used for assisting dispersion, the graphene is not dispersed in the high-viscosity solvent after long-time ultrasonic processing, and the wear resistance of the synthetic lubricating oil is poor; compared with synthetic lubricating oil without the graphene material, the wear resistance is greatly improved.
In conclusion, the preparation method of the graphene material dispersion liquid provided by the invention not only improves the dispersion efficiency and stability of the graphene material and improves the friction reduction performance of the graphene material, but also does not need to introduce other additives to help dispersion, does not need to help dispersion by long-time ultrasound, has low energy consumption, low cost and simple process, is a dispersion method of the graphene material which is easier to industrialize, has universality and provides a solution for quickly and simply preparing functional graphene oil.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of a graphene material dispersion liquid is characterized by comprising the following steps:
(1) mixing a graphene material with a low-viscosity solvent to obtain a first dispersion liquid;
(2) mixing the first dispersion liquid obtained in the step (1) with a high-viscosity solvent to obtain a second dispersion liquid;
(3) removing the low-viscosity solvent from the second dispersion liquid obtained in the step (2) to obtain the graphene material dispersion liquid.
2. The preparation method according to claim 1, wherein the graphene material in step (1) comprises a graphene material prepared by an electrochemical exfoliation method and/or a graphene material prepared by reducing graphene oxide;
preferably, the thickness of the graphene material is 1-3 nm.
3. The production method according to claim 1 or 2, characterized in that the low-viscosity solvent of step (1) has a viscosity of 3 mPas or less at 20 ℃;
preferably, the low viscosity solvent comprises any one or a combination of at least two of ethanol, propanol, tetrahydrofuran, N-dimethylformamide, dimethyl sulfoxide or acetonitrile;
preferably, the volume of the low-viscosity solvent is 0.05-2 mL calculated by the mass of the graphene material being 1 mg.
4. The method of any one of claims 1 to 3, wherein the mixing of step (1) comprises performing under ultrasonic conditions.
5. The preparation method according to claim 4, wherein the power of the ultrasound is 50-500W;
preferably, the time of the ultrasonic treatment is 5-30 min.
6. The preparation method according to any one of claims 1 to 5, wherein the graphene material is contained in the first dispersion liquid in the step (1) in an amount of 0.02 to 5% by mass.
7. The preparation method according to any one of claims 1 to 6, wherein the viscosity of the high-viscosity solvent in the step (2) is not less than 100mPa.s at 20 ℃;
preferably, the high viscosity solvent includes any one of or a combination of at least two of engine oil, vegetable oil, silicone oil, paraffin wax, or oleic acid.
8. The method according to any one of claims 1 to 7, wherein the mixing in step (2) comprises physical shaking and/or stirring;
preferably, the mixing time in the step (2) is 1-5 min.
9. The method according to any one of claims 1 to 8, wherein the removing of the low-viscosity solvent in step (3) comprises heating evaporation and/or direct suction;
preferably, the volume ratio of the low-viscosity solvent to the high-viscosity solvent is (0.05-10): 1;
preferably, the mass percentage of the graphene material in the graphene material dispersion liquid is 0.02-5%.
10. The method according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) ultrasonically mixing a graphene material and a low-viscosity solvent for 5-30 min under the condition that the power is 50-550W to obtain a first dispersion liquid;
(2) mixing the first dispersion liquid obtained in the step (1) with a high-viscosity solvent for 1-5 min to obtain a second dispersion liquid;
(3) removing the low-viscosity solvent from the second dispersion liquid obtained in the step (2) by heating and evaporation and/or direct suction to obtain the graphene material dispersion liquid; the mass percentage of the graphene material in the graphene material dispersion liquid is 0.02-5%.
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