CN113214884B - Preparation method of super-regular graphene-based lubricating grease - Google Patents
Preparation method of super-regular graphene-based lubricating grease Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/02—Carbon; Graphite
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
Abstract
The invention belongs to the technical field of materials, and relates to a preparation method of super-regular graphene-based lubricating grease. The invention takes concentrated sulfuric acid and potassium permanganate as oxidants to be mixed with graphite powder; dropping hydrogen peroxide water solution; adding a high-concentration strong alkali solution after stirring; carrying out suction filtration and washing treatment on the obtained suspension, and then reducing at high temperature to obtain surface super-regular graphene lamellar powder; carrying out ball milling treatment on graphene powder; respectively dissolving the obtained graphene powder and the basic lubricating grease by using an organic solvent, mixing the graphene powder and the basic lubricating grease to obtain an emulsion, and homogenizing the emulsion; heating in water bath to evaporate all the organic solvent and restore the semi-solid state of the lubricating grease; and cooling and repeatedly grinding to obtain the super-regular graphene-based lubricating grease. The method adopts the modes of dissolution-evaporation-macroscopic dispersion-microscopic homogenization to disperse the ultra-regular graphene sheets into the base lubricating grease, has excellent lubricating effect, and can be widely applied to the fields of engineering machinery, aerospace, passenger vehicles, military equipment and the like.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of super-regular graphene-based lubricating grease.
Background
The development of modern mechanical equipment puts forward more and more rigorous requirements on the performances of prolonging the service life of the equipment, reducing power consumption, realizing green sustainable development and the like. The method for improving the lubricating performance of the equipment is the simplest and most effective method for reducing energy consumption and prolonging the service life of the equipment. Because the lubricating grease has good high-temperature stability and excellent bearing capacity, the lubricating grease becomes one of the most widely used lubricating media at present, and is more generally used under severe working conditions such as heavy load, high speed, high temperature, dustiness and the like. Zinc dialkyldithiophosphates (ZDDPs) are the most commonly used antiwear and antioxidant additives in conventional lubricants. However, global sustainable development concepts impose severe restrictions on the use of ZDDPs containing harmful elements such as sulfur and phosphorus. Therefore, in order to meet the lubricating requirements of mechanical equipment, improve the wear-resistant and friction-reducing performance and reduce the emission of toxic and harmful elements, scientific field and industrial research gradually focus on exploring the feasibility of taking graphene as a lubricating medium additive so as to replace the traditional wear-resistant and antioxidant additive containing harmful elements such as phosphorus, sulfur and the like represented by ZDDPs.
The laminated structure and the surface regularity of the graphene have obvious influence on the lubricating performance, the smoother the surface is, the fewer defects such as atoms and folds are, and the more obvious the wear-resistant and friction-reducing performance is. The existing methods for preparing graphene mainly comprise a mechanical stripping method, a vapor deposition method and a chemical stripping method. The high-quality graphene sheets with regular surface atom arrangement and regular sheet morphology can be prepared by both a mechanical stripping method and a gas-phase deposition method, but the graphene sheets have the disadvantages of high process cost, low production efficiency, complex process and the like, and are difficult to be applied to large-scale industrial preparation of additives. The chemical stripping method has the advantages of high production efficiency, simple process and low preparation cost, and is the most reliable preparation method of graphene as an industrial lubricating additive. But the problems of uneven sheet quality, more surface defects and the like exist, and the improvement of the wear-resistant and friction-reducing performance of the graphene is not facilitated. Therefore, the development of graphene which can be prepared efficiently and cheaply and has a super-regular lamellar structure is an urgent problem to be solved by researchers in the lubrication field.
Disclosure of Invention
The invention aims to provide a preparation method of super-regular graphene-based lubricating grease, which is simple in preparation process and low in cost and is expected to realize large-scale industrial production.
The invention provides a preparation method of super-regular graphene-based lubricating grease, which comprises the following steps:
(1) in a low-temperature water bath at 35 ℃, taking graphite powder as a preparation raw material, and carrying out oxidation treatment on the graphite powder by using concentrated sulfuric acid and potassium permanganate, wherein the particle size of the graphite powder is 1000-1800 meshes; during oxidation treatment, the mass ratio of the graphite powder to the concentrated sulfuric acid to the potassium permanganate is as follows: graphite powder, namely concentrated sulfuric acid and potassium permanganate, wherein the potassium permanganate is 1, (30-50) and (3-5), and the heat preservation time is 20-30 minutes to obtain a mixed solution containing graphite oxide; placing the mixed solution in a constant-temperature water bath for heat preservation treatment, and performing electromagnetic stirring;
(2) adding deionized water into the mixed liquid obtained in the step (1), wherein the mass ratio of the added deionized water to the graphite powder is (120-150): 1, until no bubbles are generated and the mixed liquid becomes dark purple, then carrying out heat preservation treatment on the mixed liquid, carrying out electromagnetic stirring at the temperature of 40-60 ℃ in a constant-temperature water bath for 60-80 minutes, and then dropwise adding aqueous hydrogen peroxide with the weight concentration of 3040 wt% at the dropwise adding speed of 0.50.8 ml/s until the mixed liquid becomes golden yellow completely; then keeping the temperature for 1020 minutes;
(3) after heat preservation treatment is carried out on the golden yellow mixed liquid in the step (2), strong alkali aqueous solution is dropwise added until the mixed liquid is alkaline;
(4) carrying out suction filtration treatment on the mixed liquid obtained in the step (3), and carrying out high-temperature thermal reduction treatment on the obtained filter cake, wherein the temperature of the high-temperature thermal reduction is 150-200 ℃, and the time of the high-temperature reduction is 4-7 hours;
(5) and (3) carrying out acid washing, water washing and drying treatment on the product obtained in the step (4) for multiple times, wherein the acid washing solvent is a dilute hydrochloric acid aqueous solution with the weight percentage concentration of 5-10 wt%, the water washing solvent is high-purity water, the drying treatment temperature is 50-60 ℃, and the drying time is 3-4 hours. Performing ball milling treatment on the super-regular graphene powder, wherein the rotating speed of the ball milling treatment is 400-600 r/min, and the ball milling time is 2-3 hours;
(6) dissolving the graphene powder prepared in the step (5) by using an organic solvent to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is (8-10): 1; simultaneously dissolving the basic lubricating grease by using an organic solvent to obtain a second mixture, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1 (1.3-1.6); mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base lubricating grease is 0.05-1 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no massive lubricating grease exists, so as to obtain an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 400-600W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 35-45 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers a semi-solid state;
(8) and (4) cooling the product obtained in the step (7) to room temperature, and then grinding for multiple times to obtain the uniformly mixed super-regular graphene-based lubricating grease.
The preparation method of the super-regular graphene-based lubricating grease provided by the invention has the following advantages:
(1) according to the preparation method of the super-regular graphene-based lubricating grease, the graphene sheet layer with the super-regular surface morphology is prepared by adopting a chemical stripping process, so that the defects of low production efficiency, complex process flow, high preparation cost and the like of graphene prepared by a mechanical stripping method and a vapor deposition method in the prior art are overcome; meanwhile, the damage influence of the redox reaction in the existing method on the graphene sheet layer is controlled to be extremely low, so that the method has great industrial application value.
(2) The preparation method adopts the modes of dissolution-evaporation-macroscopic dispersion-microscopic homogenization to disperse the ultra-regular graphene lamella into the base grease, the dispersion effect is uniform, and the chemical components in the base grease are stable.
(3) The super-regular graphene-based lubricating grease prepared by the method has excellent anti-wear and anti-friction effects, can effectively improve the surface wear condition of a friction pair, meets the application requirements under extreme working conditions such as heavy load and high temperature, and has wide application prospects in the fields of engineering machinery, aerospace, passenger vehicles, military equipment and the like.
Drawings
Fig. 1 is a scanning electron microscope image of a super-regular graphene sheet layer in example 1 of the present invention. The graph a is an image of a plurality of super-regular graphene sheets, and the graph b is an image of a single super-regular graphene sheet.
Fig. 2 is a high-resolution transmission electron microscope image of the super-regular graphene sheet layer of embodiment 1 of the present invention.
Fig. 3 is a raman spectrum of the super-regular graphene in example 1 of the present invention.
Fig. 4 is a graph comparing the friction coefficients of the super-regular graphene and the commercial graphene of example 1 of the present invention as a grease lubricant additive.
Detailed Description
The preparation method of the super-regular graphene-based lubricating grease provided by the invention comprises the following steps:
(1) in a low-temperature water bath at 35 ℃, taking graphite powder as a preparation raw material, and carrying out oxidation treatment on the graphite powder by using concentrated sulfuric acid and potassium permanganate, wherein the particle size of the graphite powder is 1000-1800 meshes; during oxidation treatment, the mass ratio of the graphite powder to the concentrated sulfuric acid to the potassium permanganate is as follows: graphite powder, namely concentrated sulfuric acid and potassium permanganate, wherein the potassium permanganate is 1, (30-50) and (3-5), and the heat preservation time is 20-30 minutes to obtain a mixed solution containing graphite oxide; placing the mixed solution in a constant-temperature water bath for heat preservation treatment, and performing electromagnetic stirring;
(2) adding deionized water into the mixed liquid obtained in the step (1), wherein the mass ratio of the added deionized water to the graphite powder is (120-150): 1, until no bubbles are generated and the mixed liquid becomes dark purple, then carrying out heat preservation treatment on the mixed liquid, carrying out electromagnetic stirring at the temperature of 40-60 ℃ in a constant-temperature water bath for 60-80 minutes, and then dropwise adding aqueous hydrogen peroxide with the weight concentration of 3040 wt% at the dropwise adding speed of 0.50.8 ml/s until the mixed liquid becomes golden yellow completely; followed by incubation for 1020 minutes.
(3) After heat preservation treatment is carried out on the golden yellow mixed liquid in the step (2), strong alkali aqueous solution is dropwise added until the mixed liquid is alkaline;
(4) carrying out suction filtration treatment on the mixed liquid obtained in the step (3), and carrying out high-temperature thermal reduction treatment on the obtained filter cake, wherein the temperature of the high-temperature thermal reduction is 150-200 ℃, and the time of the high-temperature reduction is 4-7 hours;
(5) and (3) carrying out acid washing, water washing and drying treatment on the product obtained in the step (4) for multiple times, wherein the acid washing solvent is a dilute hydrochloric acid aqueous solution with the weight percentage concentration of 5-10 wt%, the water washing solvent is high-purity water, the drying treatment temperature is 50-60 ℃, and the drying time is 3-4 hours. Performing ball milling treatment on the super-regular graphene powder, wherein the rotating speed of the ball milling treatment is 400-600 r/min, and the ball milling time is 2-3 hours;
(6) dissolving the graphene powder prepared in the step (5) by using an organic solvent to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is (8-10): 1; simultaneously dissolving the basic lubricating grease by using an organic solvent to obtain a second mixture, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1 (1.3-1.6); mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base lubricating grease is 0.05-1 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no massive lubricating grease exists, so as to obtain an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 400-600W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 35-45 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers a semi-solid state;
(8) and (4) cooling the product obtained in the step (7) to room temperature, and then grinding for multiple times to obtain the uniformly mixed super-regular graphene-based lubricating grease.
In the step (2) of the preparation method, deionized water is added at a speed of 400-500 mL/min; the temperature of the heat preservation treatment is 40-60 ℃, and preferably 45-50 ℃.
In the step (3) of the preparation method, the solute of the strong alkali aqueous solution is one of potassium hydroxide, sodium hydroxide and lithium hydroxide solid, the weight percentage concentration of the strong alkali aqueous solution is 3040 wt%, and the speed of adding the strong alkali aqueous solution is 0.2-0.3 ml/s; the pH value of the mixed solution is 9-11.
In the step (6) of the preparation method, the organic solvent is one or a mixture of more of petroleum ether, absolute ethyl alcohol, acetone, ethyl acetate and methanol.
In the step (8) of the preparation method, the grinding treatment comprises grinding treatment of a ball mill and a three-roll grinder, and the rotating speed of the ball mill is 300 revolutions per minute; the rotating speed of a fast roller of the three-roller grinder is 200-250 r/min, and the grinding fineness is 5-12 microns.
The following describes in detail specific embodiments of the present invention. All embodiments are exemplary and intended to be illustrative of the invention, and should not be construed as limiting the invention.
Example 1
(1) Weighing 5.0g of 1200-mesh commercial graphite powder, adding the graphite powder into 225.0g of concentrated sulfuric acid liquid batch by batch very slowly in a water bath environment at 4 ℃, after the two are fully and uniformly mixed, uniformly and stably adding 20.0g of potassium permanganate solid particles into the mixed liquid, preserving heat for 30 minutes under the condition of constant-temperature water bath, and carrying out electromagnetic stirring treatment.
(2) 600.0g of deionized water was added to the mixed solution, and the mixture was kept at 50 ℃ for 60 minutes while being subjected to electromagnetic stirring treatment. After the heat preservation is finished, the hydrogen peroxide aqueous solution with the weight percentage concentration of 30 wt% is slowly dripped until the solution is completely golden yellow, and then the heat preservation is carried out for 15 minutes.
(3) Slowly dropwise adding a 30 wt% potassium hydroxide aqueous solution to the mixed liquid under electromagnetic stirring until the pH of the mixed liquid becomes 10, followed by electromagnetic stirring for 40 minutes.
(4) And carrying out suction filtration on the mixed liquid, and placing the suction filtration product in a vacuum drying oven at 180 ℃ for high-temperature reduction for 5 hours.
(5) And repeatedly cleaning the dried product by using 8 wt% of dilute hydrochloric acid solution and high-purity aqueous solution, performing suction filtration again, and then placing the product in a vacuum drying oven at 60 ℃ for heat preservation for 3 hours. And performing ball milling treatment on the dried product, wherein the ball milling rotation speed is 500 r/min, and the ball milling time is 2 hours, so as to finally obtain the super-regular graphene sheet layer.
(6) Dissolving the graphene powder prepared in the step (5) by using a petroleum ether solution to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is 8: 1; simultaneously dissolving the basic lubricating grease by using an organic solvent, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1:1.5, so as to obtain a second mixture; mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base grease is 0.5 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no blocky lubricating grease exists, obtaining an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 600W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 40 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers to a semi-solid state;
(8) after the lubricating grease is cooled to room temperature, carrying out ball milling treatment for 1 hour, wherein the ball milling rotation speed is 300 revolutions per minute, and repeating for 3 times; and (5) grinding the ball-milled lubricating grease by using a three-roll grinder, and repeating for 3 times. Finally obtaining the super-regular graphene lubricating grease with the mass concentration of 0.5 wt%.
The morphology and the crystallization state of the prepared super-regular graphene sheet layer are analyzed by using a JMS-IT field emission scanning electron microscope, a JEM-2010 high-resolution transmission electron microscope and an HR800l Raman spectrometer, and the detection results are respectively shown in FIG. 1, FIG. 2 and FIG. 3. Fig. 1 is an SEM image of a super-regular graphene sheet layer and an EDS energy spectrum of a carbon element, fig. 2 is an HRTEM image of a super-regular graphene sheet layer, and fig. 3 is a Raman spectrum of a super-regular graphene sheet layer. As can be seen from fig. 1 and 2, the graphene sheet layer prepared by the method has extremely flat surface appearance and extremely regular edge structure. As can be seen from FIG. 3, the intensity ratio I of the D peak to the G peak of the grapheneD/IGThe value is only 0.15, which shows that the internal crystal structure is complete and the defects are few.
The prepared super-regular graphene lubricating grease and related comparative materials were subjected to tribology performance tests, and the test results are shown in fig. 4 and table 1. Compared with commercial graphene and commercial graphite, the super-regular graphene prepared by the method has better lubricating property.
TABLE 1 comparison of lubricating properties of super-regular graphene grease and other comparative materials
Example 2
(1) Weighing 5.0g of 1500-mesh commercial graphite powder, adding the graphite powder into 250.0g of concentrated sulfuric acid liquid batch by batch very slowly in a water bath environment at 4 ℃, uniformly mixing the graphite powder and the concentrated sulfuric acid liquid, uniformly and stably adding 15.0g of potassium permanganate solid particles into the mixed liquid, preserving heat for 30 minutes under the condition of constant-temperature water bath, and carrying out electromagnetic stirring treatment.
(2) 600.0g of deionized water was added to the mixed solution, and the mixture was kept at 50 ℃ for 60 minutes while being subjected to electromagnetic stirring treatment. After the heat preservation is finished, the hydrogen peroxide aqueous solution with the weight percentage concentration of 30 wt% is slowly dripped until the solution is completely golden yellow, and then the heat preservation is carried out for 15 minutes.
(3) To the mixed liquid was slowly added dropwise an aqueous solution of 35 wt% sodium hydroxide under electromagnetic stirring until the pH of the mixed liquid was 9, followed by electromagnetic stirring for 40 minutes.
(4) And carrying out suction filtration on the mixed liquid, and placing the suction filtration product in a vacuum drying oven at 200 ℃ for high-temperature reduction for 7 hours.
(5) And repeatedly cleaning the dried product by using 8 wt% of dilute hydrochloric acid solution and high-purity aqueous solution, performing suction filtration again, and then placing the product in a vacuum drying oven at 50 ℃ for heat preservation for 4 hours. And performing ball milling treatment on the dried product, wherein the ball milling rotation speed is 500 r/min, and the ball milling time is 2 hours, so as to finally obtain the super-regular graphene sheet layer.
(6) Dissolving the graphene powder prepared in the step (5) with an absolute ethyl alcohol solution to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is 10: 1; simultaneously dissolving the basic lubricating grease by using an organic solvent, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1:1.6, so as to obtain a second mixture; mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base grease is 0.5 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no massive lubricating grease exists, obtaining an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 400W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 40 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers to a semi-solid state;
(8) after the lubricating grease is cooled to room temperature, carrying out ball milling treatment for 1 hour, wherein the ball milling rotation speed is 300 revolutions per minute, and repeating for 3 times; and (5) grinding the ball-milled lubricating grease by using a three-roll grinder, and repeating for 3 times. Finally obtaining the super-regular graphene lubricating grease with the mass concentration of 0.5 wt%.
Example 3
(1) Weighing 1800-mesh commercial graphite powder 5.0g, adding the graphite powder into concentrated sulfuric acid liquid 175.0g batch by batch very slowly in a water bath environment at 4 ℃, after the two are fully and uniformly mixed, uniformly and stably adding potassium permanganate solid particles 25.0g into the mixed liquid, preserving the heat for 30 minutes under the condition of constant-temperature water bath, and carrying out electromagnetic stirring treatment.
(2) 600.0g of deionized water was added to the mixed solution, and the mixture was kept at 50 ℃ for 60 minutes while being subjected to electromagnetic stirring treatment. After the heat preservation is finished, the hydrogen peroxide aqueous solution with the weight percentage concentration of 30 wt% is slowly dripped until the solution is completely golden yellow, and then the heat preservation is carried out for 15 minutes.
(3) Slowly dropwise adding a 40 wt% lithium hydroxide aqueous solution to the mixed liquid under electromagnetic stirring until the pH of the mixed liquid is 11, followed by electromagnetic stirring for 40 minutes.
(4) And carrying out suction filtration on the mixed liquid, and placing the suction filtration product in a vacuum drying oven at 160 ℃ for high-temperature reduction for 4 hours.
(5) And repeatedly cleaning the dried product by using 8 wt% of dilute hydrochloric acid solution and high-purity aqueous solution, performing suction filtration again, and then placing the product in a vacuum drying oven at 50 ℃ for heat preservation for 4 hours. And performing ball milling treatment on the dried product, wherein the ball milling rotation speed is 500 r/min, and the ball milling time is 2 hours, so as to finally obtain the super-regular graphene sheet layer.
(6) Dissolving the graphene powder prepared in the step (5) with an acetone solution to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is 10: 1; simultaneously dissolving the basic lubricating grease by using an organic solvent, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1:1.3, so as to obtain a second mixture; mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base grease is 0.5 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no blocky lubricating grease exists, obtaining an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 500W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 45 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers to a semi-solid state;
(8) after the lubricating grease is cooled to room temperature, carrying out ball milling treatment for 1 hour, wherein the ball milling rotation speed is 300 revolutions per minute, and repeating for 3 times; and (5) grinding the ball-milled lubricating grease by using a three-roll grinder, and repeating for 3 times. Finally obtaining the super-regular graphene lubricating grease with the mass concentration of 0.5 wt%.
Example 4
(1) Weighing 5.0g of 1000-mesh commercial graphite powder, adding the graphite powder into 150.0g of concentrated sulfuric acid liquid batch by batch very slowly in a water bath environment at 4 ℃, uniformly mixing the graphite powder and the concentrated sulfuric acid liquid, uniformly and stably adding 15.0g of potassium permanganate solid particles into the mixed liquid, preserving heat for 30 minutes under the condition of constant-temperature water bath, and carrying out electromagnetic stirring treatment.
(2) 700.0g of deionized water was added to the mixed solution, and the mixture was kept at 50 ℃ for 60 minutes while being subjected to electromagnetic stirring treatment. After the heat preservation is finished, the hydrogen peroxide aqueous solution with the weight percentage concentration of 30 wt% is slowly dripped until the solution is completely golden yellow, and then the heat preservation is carried out for 15 minutes.
(3) Slowly dropwise adding a 30 wt% potassium hydroxide aqueous solution to the mixed liquid under electromagnetic stirring until the pH of the mixed liquid becomes 10, followed by electromagnetic stirring for 40 minutes.
(4) And carrying out suction filtration on the mixed liquid, and placing the suction filtration product in a vacuum drying oven at 180 ℃ for high-temperature reduction for 4 hours.
(5) And repeatedly cleaning the dried product by using 8 wt% of dilute hydrochloric acid solution and high-purity aqueous solution, performing suction filtration again, and then placing the product in a vacuum drying oven at 60 ℃ for heat preservation for 4 hours. And performing ball milling treatment on the dried product, wherein the ball milling rotation speed is 500 r/min, and the ball milling time is 2 hours, so as to finally obtain the super-regular graphene sheet layer.
(6) Dissolving the graphene powder prepared in the step (5) with an ethyl acetate solution to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is 10: 1; simultaneously dissolving the basic lubricating grease by using an organic solvent, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1:1.5, so as to obtain a second mixture; mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base grease is 0.5 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no blocky lubricating grease exists, obtaining an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 500W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 45 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers to a semi-solid state;
(8) after the lubricating grease is cooled to room temperature, carrying out ball milling treatment for 1 hour, wherein the ball milling rotation speed is 300 revolutions per minute, and repeating for 3 times; and (5) grinding the ball-milled lubricating grease by using a three-roll grinder, and repeating for 3 times. Finally obtaining the super-regular graphene lubricating grease with the mass concentration of 0.5 wt%.
Example 5
(1) Weighing 5.0g of 1200-mesh commercial graphite powder, adding the graphite powder into 225.0g of concentrated sulfuric acid liquid batch by batch very slowly in a water bath environment at 4 ℃, after the two are fully and uniformly mixed, uniformly and stably adding 25.0g of potassium permanganate solid particles into the mixed liquid, preserving heat for 30 minutes under the condition of constant-temperature water bath, and carrying out electromagnetic stirring treatment.
(2) 700.0g of deionized water was added to the mixed solution, and the mixture was kept at 50 ℃ for 60 minutes while being subjected to electromagnetic stirring treatment. After the heat preservation is finished, the hydrogen peroxide aqueous solution with the weight percentage concentration of 30 wt% is slowly dripped until the solution is completely golden yellow, and then the heat preservation is carried out for 15 minutes.
(3) Slowly dropwise adding a 30 wt% potassium hydroxide aqueous solution to the mixed liquid under electromagnetic stirring until the pH of the mixed liquid becomes 9, followed by electromagnetic stirring for 40 minutes.
(4) And carrying out suction filtration on the mixed liquid, and placing the suction filtration product in a vacuum drying oven at 200 ℃ for high-temperature reduction for 7 hours.
(5) And repeatedly cleaning the dried product by using 8 wt% of dilute hydrochloric acid solution and high-purity aqueous solution, performing suction filtration again, and then placing the product in a vacuum drying oven at 55 ℃ for heat preservation for 3 hours. And performing ball milling treatment on the dried product, wherein the ball milling rotation speed is 500 r/min, and the ball milling time is 2 hours, so as to finally obtain the super-regular graphene sheet layer.
(6) Dissolving the graphene powder prepared in the step (5) by using a methanol solution to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is 10: 1; simultaneously dissolving the basic lubricating grease by using an organic solvent, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1:1.5, so as to obtain a second mixture; mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base grease is 0.5 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no blocky lubricating grease exists, obtaining an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 500W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 45 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers to a semi-solid state;
(8) after the lubricating grease is cooled to room temperature, carrying out ball milling treatment for 1 hour, wherein the ball milling rotation speed is 300 revolutions per minute, and repeating for 3 times; and (5) grinding the ball-milled lubricating grease by using a three-roll grinder, and repeating for 3 times. Finally obtaining the super-regular graphene lubricating grease with the mass concentration of 0.5 wt%.
Example 6
(1) Weighing 5.0g of 1200-mesh commercial graphite powder, adding the graphite powder into 225.0g of concentrated sulfuric acid liquid batch by batch very slowly in a water bath environment at 4 ℃, after the two are fully and uniformly mixed, uniformly and stably adding 25.0g of potassium permanganate solid particles into the mixed liquid, preserving heat for 30 minutes under the condition of constant-temperature water bath, and carrying out electromagnetic stirring treatment.
(2) 600.0g of deionized water was added to the mixed solution, and the mixture was kept at 50 ℃ for 60 minutes while being subjected to electromagnetic stirring treatment. After the heat preservation is finished, the hydrogen peroxide aqueous solution with the weight percentage concentration of 30 wt% is slowly dripped until the solution is completely golden yellow, and then the heat preservation is carried out for 20 minutes.
(3) Slowly dropwise adding a 30 wt% potassium hydroxide aqueous solution to the mixed liquid under electromagnetic stirring until the pH of the mixed liquid becomes 11, followed by electromagnetic stirring for 40 minutes.
(4) And carrying out suction filtration on the mixed liquid, and placing the suction filtration product in a vacuum drying oven at 150 ℃ for high-temperature reduction for 7 hours.
(5) And repeatedly cleaning the dried product by using 8 wt% of dilute hydrochloric acid solution and high-purity aqueous solution, performing suction filtration again, and then placing the product in a vacuum drying oven at 55 ℃ for heat preservation for 3 hours. And performing ball milling treatment on the dried product, wherein the ball milling rotation speed is 500 r/min, and the ball milling time is 2 hours, so as to finally obtain the super-regular graphene sheet layer.
(6) Dissolving the graphene powder prepared in the step (5) by using a petroleum ether and absolute ethyl alcohol solution in a mass ratio of 10:1 to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is 10: 1; simultaneously dissolving the basic lubricating grease by using an organic solvent, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1:1.5, so as to obtain a second mixture; mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base grease is 0.5 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no blocky lubricating grease exists, obtaining an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 500W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 45 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers to a semi-solid state;
(8) after the lubricating grease is cooled to room temperature, carrying out ball milling treatment for 1 hour, wherein the ball milling rotation speed is 300 revolutions per minute, and repeating for 3 times; and (5) grinding the ball-milled lubricating grease by using a three-roll grinder, and repeating for 3 times. Finally obtaining the super-regular graphene lubricating grease with the mass concentration of 0.5 wt%.
Example 7
(1) Weighing 5.0g of 1200-mesh commercial graphite powder, adding the graphite powder into 225.0g of concentrated sulfuric acid liquid batch by batch very slowly in a water bath environment at 4 ℃, after the two are fully and uniformly mixed, uniformly and stably adding 25.0g of potassium permanganate solid particles into the mixed liquid, preserving heat for 30 minutes under the condition of constant-temperature water bath, and carrying out electromagnetic stirring treatment.
(2) 600.0g of deionized water was added to the mixed solution, and the mixture was kept at 50 ℃ for 60 minutes while being subjected to electromagnetic stirring treatment. After the heat preservation is finished, the hydrogen peroxide aqueous solution with the weight percentage concentration of 30 wt% is slowly dripped until the solution is completely golden yellow, and then the heat preservation is carried out for 20 minutes.
(3) Slowly dropwise adding a 30 wt% potassium hydroxide aqueous solution to the mixed liquid under electromagnetic stirring until the pH of the mixed liquid becomes 11, followed by electromagnetic stirring for 40 minutes.
(4) And carrying out suction filtration on the mixed liquid, and placing the suction filtration product in a vacuum drying oven at 150 ℃ for high-temperature reduction for 4 hours.
(5) And repeatedly cleaning the dried product by using 8 wt% of dilute hydrochloric acid solution and high-purity aqueous solution, performing suction filtration again, and then placing the product in a vacuum drying oven at 55 ℃ for heat preservation for 3 hours. And performing ball milling treatment on the dried product, wherein the ball milling rotation speed is 500 r/min, and the ball milling time is 2 hours, so as to finally obtain the super-regular graphene sheet layer.
(6) Dissolving the graphene powder prepared in the step (5) by using a petroleum ether and acetone solution in a mass ratio of 10:1 to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is 9: 1; simultaneously dissolving the basic lubricating grease by using an organic solvent, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1:1.5, so as to obtain a second mixture; mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base grease is 0.5 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no blocky lubricating grease exists, obtaining an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 500W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 45 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers to a semi-solid state;
(8) after the lubricating grease is cooled to room temperature, carrying out ball milling treatment for 1 hour, wherein the ball milling rotation speed is 300 revolutions per minute, and repeating for 3 times; and (5) grinding the ball-milled lubricating grease by using a three-roll grinder, and repeating for 3 times. Finally obtaining the super-regular graphene lubricating grease with the mass concentration of 0.5 wt%.
Example 8
(1) Weighing 5.0g of 1200-mesh commercial graphite powder, adding the graphite powder into 225.0g of concentrated sulfuric acid liquid batch by batch very slowly in a water bath environment at 4 ℃, after the two are fully and uniformly mixed, uniformly and stably adding 25.0g of potassium permanganate solid particles into the mixed liquid, preserving heat for 30 minutes under the condition of constant-temperature water bath, and carrying out electromagnetic stirring treatment.
(2) 600.0g of deionized water was added to the mixed solution, and the mixture was kept at 50 ℃ for 60 minutes while being subjected to electromagnetic stirring treatment. After the heat preservation is finished, the hydrogen peroxide aqueous solution with the weight percentage concentration of 30 wt% is slowly dripped until the solution is completely golden yellow, and then the heat preservation is carried out for 20 minutes.
(3) Slowly dropwise adding a 30 wt% potassium hydroxide aqueous solution to the mixed liquid under electromagnetic stirring until the pH of the mixed liquid becomes 11, followed by electromagnetic stirring for 40 minutes.
(4) And carrying out suction filtration on the mixed liquid, and placing the suction filtration product in a vacuum drying oven at 180 ℃ for high-temperature reduction for 5 hours.
(5) And repeatedly cleaning the dried product by using 8 wt% of dilute hydrochloric acid solution and high-purity aqueous solution, performing suction filtration again, and then placing the product in a vacuum drying oven at 55 ℃ for heat preservation for 3 hours. And performing ball milling treatment on the dried product, wherein the ball milling rotation speed is 500 r/min, and the ball milling time is 2 hours, so as to finally obtain the super-regular graphene sheet layer.
(6) Dissolving the graphene powder prepared in the step (5) by using an acetone and absolute ethyl alcohol solution in a mass ratio of 10:1 to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is 9: 1; simultaneously dissolving the basic lubricating grease by using an organic solvent, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1:1.5, so as to obtain a second mixture; mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base grease is 0.5 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no blocky lubricating grease exists, obtaining an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 500W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 45 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers to a semi-solid state;
(8) after the lubricating grease is cooled to room temperature, carrying out ball milling treatment for 1 hour, wherein the ball milling rotation speed is 300 revolutions per minute, and repeating for 3 times; and (5) grinding the ball-milled lubricating grease by using a three-roll grinder, and repeating for 3 times. Finally obtaining the super-regular graphene lubricating grease with the mass concentration of 0.5 wt%.
Example 9
(1) Weighing 5.0g of 1200-mesh commercial graphite powder, adding the graphite powder into 250.0g of concentrated sulfuric acid liquid batch by batch very slowly in a water bath environment at 4 ℃, uniformly mixing the graphite powder and the concentrated sulfuric acid liquid, uniformly and stably adding 25.0g of potassium permanganate solid particles into the mixed liquid, preserving heat for 30 minutes under the condition of constant-temperature water bath, and carrying out electromagnetic stirring treatment.
(2) 600.0g of deionized water was added to the mixed solution, and the mixture was kept at 50 ℃ for 60 minutes while being subjected to electromagnetic stirring treatment. After the heat preservation is finished, the hydrogen peroxide aqueous solution with the weight percentage concentration of 30 wt% is slowly dripped until the solution is completely golden yellow, and then the heat preservation is carried out for 20 minutes.
(3) Slowly dropwise adding a 30 wt% potassium hydroxide aqueous solution to the mixed liquid under electromagnetic stirring until the pH of the mixed liquid becomes 10, followed by electromagnetic stirring for 40 minutes.
(4) And carrying out suction filtration on the mixed liquid, and placing the suction filtration product in a vacuum drying oven at 180 ℃ for high-temperature reduction for 6 hours.
(5) And repeatedly cleaning the dried product by using 8 wt% of dilute hydrochloric acid solution and high-purity aqueous solution, performing suction filtration again, and then placing the product in a vacuum drying oven at 55 ℃ for heat preservation for 3 hours. And performing ball milling treatment on the dried product, wherein the ball milling rotation speed is 500 r/min, and the ball milling time is 2 hours, so as to finally obtain the super-regular graphene sheet layer.
(6) Dissolving the graphene powder prepared in the step (5) by using a petroleum ether and methanol solution in a mass ratio of 10:1 to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is 9: 1; simultaneously dissolving the basic lubricating grease by using an organic solvent, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1:1.5, so as to obtain a second mixture; mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the base grease is 0.5 wt%;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no blocky lubricating grease exists, obtaining an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 500W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 45 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers to a semi-solid state;
(8) after the lubricating grease is cooled to room temperature, carrying out ball milling treatment for 1 hour, wherein the ball milling rotation speed is 300 revolutions per minute, and repeating for 3 times; and (5) grinding the ball-milled lubricating grease by using a three-roll grinder, and repeating for 3 times. Finally obtaining the super-regular graphene lubricating grease with the mass concentration of 0.5 wt%.
Claims (1)
1. A preparation method of super-regular graphene-based lubricating grease is characterized by comprising the following steps:
(1) in a low-temperature water bath at 3-5 ℃, taking graphite powder as a preparation raw material, and carrying out oxidation treatment on the graphite powder by using concentrated sulfuric acid and potassium permanganate, wherein the particle size of the graphite powder is 1000-1800 meshes; during oxidation treatment, the mass ratio of the graphite powder to the concentrated sulfuric acid to the potassium permanganate is as follows: graphite powder, namely concentrated sulfuric acid and potassium permanganate, wherein the potassium permanganate is 1, (30-50) and (3-5), and the heat preservation time is 20-30 minutes to obtain a mixed solution containing graphite oxide; placing the mixed solution in a constant-temperature water bath for heat preservation treatment, and performing electromagnetic stirring;
(2) adding deionized water into the mixed liquid obtained in the step (1) at a speed of 400-500 mL/min, wherein the mass ratio of the added deionized water to the graphite powder is (120-150): 1, until no bubbles are generated and the mixed liquid becomes dark purple, then carrying out heat preservation treatment on the mixed liquid, carrying out electromagnetic stirring at the temperature of 45-50 ℃ in a thermostatic water bath for 60-80 minutes, then dropwise adding a hydrogen peroxide aqueous solution with the weight concentration of 30-40 wt% at a speed of 0.5-0.8 mL/s until the mixed liquid becomes golden yellow completely; then preserving the heat for 10-20 minutes;
(3) after heat preservation treatment is carried out on the golden yellow mixed solution in the step (2), dropwise adding a strong alkali aqueous solution until the mixed solution is alkaline, wherein the solute of the strong alkali aqueous solution is one of potassium hydroxide, sodium hydroxide and lithium hydroxide solids, the weight percentage concentration of the strong alkali aqueous solution is 30-40 wt%, and the adding speed of the strong alkali aqueous solution is 0.2-0.3 ml/s; the pH value of the mixed solution is 9-11;
(4) carrying out suction filtration treatment on the mixed liquid obtained in the step (3), and carrying out high-temperature thermal reduction treatment on the obtained filter cake, wherein the temperature of the high-temperature thermal reduction is 150-200 ℃, and the time of the high-temperature reduction is 4-7 hours;
(5) carrying out acid washing, water washing and drying treatment on the product obtained in the step (4) for multiple times, wherein the acid washing solvent is a dilute hydrochloric acid aqueous solution with the weight percentage concentration of 5-10 wt%, the water washing solvent is high-purity water, the drying treatment temperature is 50-60 ℃, and the drying time is 3-4 hours; performing ball milling treatment on the super-regular graphene powder, wherein the rotating speed of the ball milling treatment is 400-600 r/min, and the ball milling time is 2-3 hours;
(6) dissolving the graphene powder prepared in the step (5) by using an organic solvent to obtain a first mixture, wherein the mass ratio of the organic solvent to the graphene powder is (8-10): 1; simultaneously dissolving the basic lubricating grease by using an organic solvent to obtain a second mixture, wherein the mass ratio of the organic solvent to the basic lubricating grease is 1 (1.3-1.6); mixing the first mixture and the second mixture with each other to obtain a third mixture; in the third mixture, the mass concentration of the graphene powder in the basic lubricating grease is 0.05-1 wt%, and the organic solvent is one or more of petroleum ether, absolute ethyl alcohol, acetone, ethyl acetate and methanol;
(7) mechanically stirring the third mixed solution obtained in the step (6) until no massive lubricating grease exists, so as to obtain an emulsion containing the super-regular graphene, and then carrying out ultrasonic homogenization treatment on the emulsion, wherein the power of the ultrasonic homogenization treatment is 400-600W, and the treatment time is 2 hours; placing the emulsion in a constant-temperature water bath for electromagnetic stirring, wherein the temperature of the constant-temperature water bath is 35-45 ℃, and the electromagnetic stirring time is 4 hours until the lubricating grease recovers a semi-solid state;
(8) cooling the product obtained in the step (7) to room temperature, and then grinding for multiple times to obtain the uniformly mixed super-regular graphene-based lubricating grease, wherein the grinding comprises grinding by a ball mill and a three-roll grinder, and the rotating speed of the ball mill is 300 revolutions per minute; the rotating speed of a fast roller of the three-roller grinder is 200-250 r/min, and the grinding fineness is 5-12 microns.
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