CN111363609A - Modified graphene lubricating oil and preparation method thereof - Google Patents
Modified graphene lubricating oil and preparation method thereof 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular compounds
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- 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
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- 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
- C10M2201/05—Metals; Alloys
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- 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
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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- 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
- C10M2201/087—Boron oxides, acids or salts
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- 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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/022—Ethene
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/08—Aldehydes; Ketones
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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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
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- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/287—Partial esters
- C10M2207/289—Partial esters containing free hydroxy groups
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- 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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/08—Amides
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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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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- 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
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/049—Phosphite
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Abstract
The invention belongs to the field of lubricating oil, and particularly relates to modified graphene lubricating oil and a preparation method thereof. The graphene lubricating oil additive is prepared from 10-20 parts of stearic acid, 10-15 parts of oleic acid, 50-70 parts of acetone, 10-30 parts of graphene powder, 5-8 parts of concentrated sulfuric acid, 5-9 parts of molybdenum powder microspheres, 4-8 parts of chromium powder microspheres, 5-10 parts of iron oxide microspheres, 10-15 parts of phentriazumizole, 9-18 parts of di-N-butyl phosphite, 8-16 parts of lithium fluoroborate, 10-30 parts of basic white oil, 4-8 parts of montmorillonite, 5-10 parts of N, N-dimethylformamide, 2-5 parts of lanolin magnesium soap, 5-8 parts of glyceryl monostearate, 8-12 parts of sodium polyethylene and 10-20 parts of a silane coupling agent in parts by mass; and then adding the graphene lubricating oil additive into 100-120 parts of base oil, and dispersing for 1h to obtain the lubricating oil modified graphene lubricating oil. The modified graphene lubricating oil produced by the invention can be well dispersed in commercial lubricating oil, the extreme pressure lubricating property of the modified graphene lubricating oil can be obviously improved, and the modified graphene lubricating oil has the characteristics of temperature reduction, drying and shock absorption.
Description
Technical Field
The invention belongs to the field of lubricating oil, and particularly relates to modified graphene lubricating oil and a preparation method thereof.
Background
Graphene is a two-dimensional carbon atom crystal with a special structure and a single atom thickness, so that the novel material with excellent self-lubricating, mechanical and thermal properties has a good application prospect in the field of lubricating oil, but the use of the novel material is limited due to poor dispersibility and easy agglomeration in the lubricating oil.
In order to improve the dispersion stability of graphene in lubricating oil and the extreme pressure lubrication performance of the lubricating oil, the dispersion stability of the graphene is synergistically improved by improving the formula of the lubricating oil and modifying the graphene.
Disclosure of Invention
One object of the present invention is to provide a modified graphene lubricating oil.
The modified graphene lubricating oil comprises the following raw materials in parts by weight: 10-20 parts of stearic acid, 10-15 parts of oleic acid, 50-70 parts of acetone, 10-30 parts of graphene powder, 5-8 parts of concentrated sulfuric acid, 5-9 parts of molybdenum powder microspheres, 4-8 parts of chromium powder microspheres, 5-10 parts of iron oxide microspheres, 10-15 parts of benzotriazole, 9-18 parts of di-N-butyl phosphite, 8-16 parts of lithium fluoroborate, 10-30 parts of basic white oil, 4-8 parts of montmorillonite, 5-10 parts of N, N-dimethylformamide, 2-5 parts of lanolin magnesium soap, 5-8 parts of glyceryl monostearate, 8-12 parts of sodium polyethylene, 10-20 parts of a silane coupling agent and 100-120 parts of base oil.
Another objective of the present invention is to provide a preparation method of the modified graphene lubricating oil.
The preparation method of the modified graphene lubricating oil comprises the following steps:
step one, adding stearic acid and oleic acid into acetone, magnetically stirring for 30min, adding graphene powder, continuously stirring for 1h, and then dropwise adding concentrated sulfuric acid to obtain black slurry; putting the black slurry into a round-bottom flask, connecting with a condensation reflux device, keeping the temperature of the round-bottom flask constant in a constant-temperature water bath at 50 ℃ for 3 hours to obtain slurry and a filter cake, then carrying out suction filtration on the slurry, washing the slurry for 3 times by using absolute ethyl alcohol, and putting the filter cake into a vacuum oven to be dried for 8 hours at 80 ℃; finally, crushing the dried filter cake for 30s to obtain modified graphene powder;
adding the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the glyceryl monostearate and the sodium polyethylene into the mixed solution, uniformly mixing, performing closed-end frosting for 48 hours, standing for 48 hours to obtain an additive without graphene powder, adding a silane coupling agent and the modified graphene powder into the additive without the graphene powder, and stirring for 3 hours to obtain the graphene lubricating oil additive;
and step three, adding the graphene lubricating oil additive into the base oil, dispersing for 1h to obtain lubricating oil modified graphene lubricating oil, then placing the prepared sample in a place which is at normal temperature and is away from light, and standing for 90 d to obtain the modified graphene lubricating oil.
Wherein the crushing speed of the filter cake in the first step is 35000 r/min.
And adding the molybdenum powder microspheres, the chromium powder microspheres, the iron oxide microspheres, the benzotriazole, the di-n-butyl phosphite and the lithium fluoborate into the base white oil in the second step, wherein the dispersion speed is 4000r/min at room temperature, the closed grinding speed is 3000r/min, and the reaction temperature is 100 ℃.
And step two, uniformly mixing the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the stearic acid monoglyceride and the sodium polyethylene, then carrying out closed-cell sanding at the speed of 3000r/min and the reaction temperature of 140 ℃, and standing for 48 hours at the temperature of 140 ℃.
Wherein the speed of dispersing the graphene lubricating oil additive in the lubricating oil for 1h in the third step is 3500 r/min.
Compared with the prior art, the modified graphene lubricating oil produced by the invention can be well dispersed in commercial lubricating oil and the extreme pressure lubricating property of the lubricating oil is obviously improved, and the modified graphene lubricating oil has the characteristics of cooling, drying and damping, can improve the running condition of equipment and plays a role in protecting and repairing a friction surface; the modified graphene lubricating oil improves the dispersibility of graphene and the lubricating property of base oil, the dispersibility of graphene in the lubricating oil is enhanced by the synergistic effect, and the formed stable graphene film-oil film double-lubricating-layer structure can obviously improve the lubricating condition of equipment.
Detailed Description
The following detailed description of embodiments of the invention is intended to be illustrative, and not to be construed as limiting the invention.
Example 1
Embodiment 1 provides a modified graphene lubricating oil, which comprises the following raw materials in parts by weight: 20 parts of stearic acid, 15 parts of oleic acid, 55 parts of acetone, 20 parts of graphene powder, 8 parts of concentrated sulfuric acid, 9 parts of molybdenum powder microspheres, 7 parts of chromium powder microspheres, 5 parts of iron oxide microspheres, 10 parts of benzotriazole, 18 parts of di-N-butyl phosphite, 16 parts of lithium fluoroborate, 15 parts of basic white oil, 5 parts of montmorillonite, 8 parts of N, N-dimethylformamide, 3 parts of lanolin magnesium soap, 8 parts of glycerol monostearate, 12 parts of sodium polyethylene, 12 parts of a silane coupling agent and 120 parts of basic oil.
The preparation method of the modified graphene lubricating oil provided in embodiment 1 includes the following steps: step one, adding stearic acid and oleic acid into acetone, magnetically stirring for 30min, adding graphene powder, continuously stirring for 1h, and then dropwise adding concentrated sulfuric acid to obtain black slurry; putting the black slurry into a round-bottom flask, connecting with a condensation reflux device, keeping the temperature of the round-bottom flask constant in a constant-temperature water bath at 50 ℃ for 3 hours to obtain slurry and a filter cake, then carrying out suction filtration on the slurry, washing the slurry for 3 times by using absolute ethyl alcohol, and putting the filter cake into a vacuum oven to be dried for 8 hours at 80 ℃; finally, crushing the dried filter cake for 30s to obtain modified graphene powder;
adding the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the glyceryl monostearate and the sodium polyethylene into the mixed solution, uniformly mixing, performing closed-end frosting for 48 hours, standing for 48 hours to obtain an additive without graphene powder, adding a silane coupling agent and the modified graphene powder into the additive without the graphene powder, and stirring for 3 hours to obtain the graphene lubricating oil additive;
and step three, adding the graphene lubricating oil additive into the lubricating oil, dispersing for 1h to obtain the lubricating oil modified graphene lubricating oil, then placing the prepared sample in a place which is at normal temperature and away from light, and standing for 90 d to obtain the modified graphene lubricating oil.
Wherein the crushing speed of the filter cake in the first step is 35000 r/min.
And adding the molybdenum powder microspheres, the chromium powder microspheres, the iron oxide microspheres, the benzotriazole, the di-n-butyl phosphite and the lithium fluoborate into the base white oil in the second step, wherein the dispersion speed is 4000r/min at room temperature, the closed grinding speed is 3000r/min, and the reaction temperature is 100 ℃.
And step two, uniformly mixing the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the stearic acid monoglyceride and the sodium polyethylene, then carrying out closed-cell sanding at the speed of 3000r/min and the reaction temperature of 140 ℃, and standing for 48 hours at the temperature of 140 ℃.
Wherein the speed of adding the graphene lubricating oil additive into the base oil for dispersing for 1h in the third step is 3500 r/min.
Example 2
Embodiment 2 provides a modified graphene lubricating oil, which comprises the following raw materials in parts by weight: 18 parts of stearic acid, 15 parts of oleic acid, 65 parts of acetone, 15 parts of graphene powder, 8 parts of concentrated sulfuric acid, 9 parts of molybdenum powder microspheres, 4 parts of chromium powder microspheres, 6 parts of iron oxide microspheres, 14 parts of benzotriazole, 10 parts of di-N-butyl phosphite, 10 parts of lithium fluoroborate, 25 parts of basic white oil, 5 parts of montmorillonite, 9 parts of N, N-dimethylformamide, 4 parts of lanolin magnesium soap, 6 parts of glycerol monostearate, 10 parts of sodium polyethylene, 18 parts of a silane coupling agent and 120 parts of basic oil.
The preparation method of the modified graphene lubricating oil provided in embodiment 2 includes the following steps: step one, adding stearic acid and oleic acid into acetone, magnetically stirring for 30min, adding graphene powder, continuously stirring for 1h, and then dropwise adding concentrated sulfuric acid to obtain black slurry; putting the black slurry into a round-bottom flask, connecting with a condensation reflux device, keeping the temperature of the round-bottom flask constant in a constant-temperature water bath at 50 ℃ for 3 hours to obtain slurry and a filter cake, then carrying out suction filtration on the slurry, washing the slurry for 3 times by using absolute ethyl alcohol, and putting the filter cake into a vacuum oven to be dried for 8 hours at 80 ℃; finally, crushing the dried filter cake for 30s to obtain modified graphene powder;
adding the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the glyceryl monostearate and the sodium polyethylene into the mixed solution, uniformly mixing, performing closed-end frosting for 48 hours, standing for 48 hours to obtain an additive without graphene powder, adding a silane coupling agent and the modified graphene powder into the additive without the graphene powder, and stirring for 3 hours to obtain the graphene lubricating oil additive;
and step three, adding the graphene lubricating oil additive into the lubricating oil, dispersing for 1h to obtain the lubricating oil modified graphene lubricating oil, then placing the prepared sample in a place which is at normal temperature and away from light, and standing for 90 d to obtain the modified graphene lubricating oil.
Wherein the crushing speed of the filter cake in the first step is 35000 r/min.
And adding the molybdenum powder microspheres, the chromium powder microspheres, the iron oxide microspheres, the benzotriazole, the di-n-butyl phosphite and the lithium fluoborate into the base white oil in the second step, wherein the dispersion speed is 4000r/min at room temperature, the closed grinding speed is 3000r/min, and the reaction temperature is 100 ℃.
And step two, uniformly mixing the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the stearic acid monoglyceride and the sodium polyethylene, then carrying out closed-cell sanding at the speed of 3000r/min and the reaction temperature of 140 ℃, and standing for 48 hours at the temperature of 140 ℃.
Wherein the speed of adding the graphene lubricating oil additive into the base oil for dispersing for 1h in the third step is 3500 r/min.
Example 3
Embodiment 3 provides a modified graphene lubricating oil, which comprises the following raw materials in parts by weight: 20 parts of stearic acid, 13 parts of oleic acid, 65 parts of acetone, 30 parts of graphene powder, 5 parts of concentrated sulfuric acid, 9 parts of molybdenum powder microspheres, 8 parts of chromium powder microspheres, 10 parts of iron oxide microspheres, 15 parts of benzotriazole, 18 parts of di-N-butyl phosphite, 16 parts of lithium fluoroborate, 30 parts of basic white oil, 4 parts of montmorillonite, 10 parts of N, N-dimethylformamide, 5 parts of lanolin magnesium soap, 8 parts of glyceryl monostearate, 12 parts of sodium polyethylene, 20 parts of a silane coupling agent and 120 parts of basic oil.
The preparation method of the modified graphene lubricating oil provided in example 3 includes the following steps: step one, adding stearic acid and oleic acid into acetone, magnetically stirring for 30min, adding graphene powder, continuously stirring for 1h, and then dropwise adding concentrated sulfuric acid to obtain black slurry; putting the black slurry into a round-bottom flask, connecting with a condensation reflux device, keeping the temperature of the round-bottom flask constant in a constant-temperature water bath at 50 ℃ for 3 hours to obtain slurry and a filter cake, then carrying out suction filtration on the slurry, washing the slurry for 3 times by using absolute ethyl alcohol, and putting the filter cake into a vacuum oven to be dried for 8 hours at 80 ℃; finally, crushing the dried filter cake for 30s to obtain modified graphene powder;
adding the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the glyceryl monostearate and the sodium polyethylene into the mixed solution, uniformly mixing, performing closed-end frosting for 48 hours, standing for 48 hours to obtain an additive without graphene powder, adding a silane coupling agent and the modified graphene powder into the additive without the graphene powder, and stirring for 3 hours to obtain the graphene lubricating oil additive;
and step three, adding the graphene lubricating oil additive into the base oil, dispersing for 1h to obtain lubricating oil modified graphene lubricating oil, then placing the prepared sample in a place which is at normal temperature and is away from light, and standing for 90 d to obtain the modified graphene lubricating oil.
Wherein the crushing speed of the filter cake in the first step is 35000 r/min.
And adding the molybdenum powder microspheres, the chromium powder microspheres, the iron oxide microspheres, the benzotriazole, the di-n-butyl phosphite and the lithium fluoborate into the base white oil in the second step, wherein the dispersion speed is 4000r/min at room temperature, the closed grinding speed is 3000r/min, and the reaction temperature is 100 ℃.
And step two, uniformly mixing the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the stearic acid monoglyceride and the sodium polyethylene, then carrying out closed-cell sanding at the speed of 3000r/min and the reaction temperature of 140 ℃, and standing for 48 hours at the temperature of 140 ℃.
Wherein the speed of dispersing the graphene lubricating oil additive in the lubricating oil for 1h in the third step is 3500 r/min.
Example 4
Embodiment 4 provides a modified graphene lubricating oil, which comprises the following raw materials in parts by weight: 12 parts of stearic acid, 12 parts of oleic acid, 54 parts of acetone, 15 parts of graphene powder, 7 parts of concentrated sulfuric acid, 8 parts of molybdenum powder microspheres, 5 parts of chromium powder microspheres, 8 parts of iron oxide microspheres, 12 parts of benzotriazole, 16 parts of di-N-butyl phosphite, 10 parts of lithium fluoroborate, 15 parts of basic white oil, 7 parts of montmorillonite, 8 parts of N, N-dimethylformamide, 5 parts of lanolin magnesium soap, 8 parts of stearic acid monoglyceride, 12 parts of sodium polyethylene, 20 parts of a silane coupling agent, and 100 parts of basic oil.
The preparation method of the modified graphene lubricating oil provided in example 4 includes the following steps: step one, adding stearic acid and oleic acid into acetone, magnetically stirring for 30min, adding graphene powder, continuously stirring for 1h, and then dropwise adding concentrated sulfuric acid to obtain black slurry; putting the black slurry into a round-bottom flask, connecting with a condensation reflux device, keeping the temperature of the round-bottom flask constant in a constant-temperature water bath at 50 ℃ for 3 hours to obtain slurry and a filter cake, then carrying out suction filtration on the slurry, washing the slurry for 3 times by using absolute ethyl alcohol, and putting the filter cake into a vacuum oven to be dried for 8 hours at 80 ℃; finally, crushing the dried filter cake for 30s to obtain modified graphene powder;
adding the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the glyceryl monostearate and the sodium polyethylene into the mixed solution, uniformly mixing, performing closed-end frosting for 48 hours, standing for 48 hours to obtain an additive without graphene powder, adding a silane coupling agent and the modified graphene powder into the additive without the graphene powder, and stirring for 3 hours to obtain the graphene lubricating oil additive;
and step three, adding the graphene lubricating oil additive into the base oil, dispersing for 1h to obtain lubricating oil modified graphene lubricating oil, then placing the prepared sample in a place which is at normal temperature and is away from light, and standing for 90 d to obtain the modified graphene lubricating oil.
Wherein the crushing speed of the filter cake in the first step is 35000 r/min.
And adding the molybdenum powder microspheres, the chromium powder microspheres, the iron oxide microspheres, the benzotriazole, the di-n-butyl phosphite and the lithium fluoborate into the base white oil in the second step, wherein the dispersion speed is 4000r/min at room temperature, the closed grinding speed is 3000r/min, and the reaction temperature is 100 ℃.
And step two, uniformly mixing the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the stearic acid monoglyceride and the sodium polyethylene, then carrying out closed-cell sanding at the speed of 3000r/min and the reaction temperature of 140 ℃, and standing for 48 hours at the temperature of 140 ℃.
Wherein the speed of adding the graphene lubricating oil additive into the base oil for dispersing for 1h in the third step is 3500 r/min.
Example 5
Embodiment 5 provides a modified graphene lubricating oil, which comprises the following raw materials in parts by weight: 14 parts of stearic acid, 10 parts of oleic acid, 50 parts of acetone, 10 parts of graphene powder, 6 parts of concentrated sulfuric acid, 8 parts of molybdenum powder microspheres, 7 parts of chromium powder microspheres, 6 parts of iron oxide microspheres, 10 parts of benzotriazole, 18 parts of di-N-butyl phosphite, 8 parts of lithium fluoroborate, 20 parts of basic white oil, 8 parts of montmorillonite, 5 parts of N, N-dimethylformamide, 2 parts of lanolin magnesium soap, 5 parts of glycerol monostearate, 8 parts of sodium polyethylene, 10 parts of a silane coupling agent and 100 parts of basic oil.
The preparation method of the modified graphene lubricating oil provided in example 5 includes the following steps: step one, adding stearic acid and oleic acid into acetone, magnetically stirring for 30min, adding graphene powder, continuously stirring for 1h, and then dropwise adding concentrated sulfuric acid to obtain black slurry; putting the black slurry into a round-bottom flask, connecting with a condensation reflux device, keeping the temperature of the round-bottom flask constant in a constant-temperature water bath at 50 ℃ for 3 hours to obtain slurry and a filter cake, then carrying out suction filtration on the slurry, washing the slurry for 3 times by using absolute ethyl alcohol, and putting the filter cake into a vacuum oven to be dried for 8 hours at 80 ℃; finally, crushing the dried filter cake for 30s to obtain modified graphene powder;
adding the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the glyceryl monostearate and the sodium polyethylene into the mixed solution, uniformly mixing, performing closed-end frosting for 48 hours, standing for 48 hours to obtain an additive without graphene powder, adding a silane coupling agent and the modified graphene powder into the additive without the graphene powder, and stirring for 3 hours to obtain the graphene lubricating oil additive;
and step three, adding the graphene lubricating oil additive into the base oil, dispersing for 1h to obtain lubricating oil modified graphene lubricating oil, then placing the prepared sample in a place which is at normal temperature and is away from light, and standing for 90 d to obtain the modified graphene lubricating oil.
Wherein the crushing speed of the filter cake in the first step is 35000 r/min.
And adding the molybdenum powder microspheres, the chromium powder microspheres, the iron oxide microspheres, the benzotriazole, the di-n-butyl phosphite and the lithium fluoborate into the base white oil in the second step, wherein the dispersion speed is 4000r/min at room temperature, the closed grinding speed is 3000r/min, and the reaction temperature is 100 ℃.
And step two, uniformly mixing the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the stearic acid monoglyceride and the sodium polyethylene, then carrying out closed-cell sanding at the speed of 3000r/min and the reaction temperature of 140 ℃, and standing for 48 hours at the temperature of 140 ℃.
Wherein the speed of dispersing the graphene lubricating oil additive in the lubricating oil for 1h in the third step is 3500 r/min.
In order to verify the reliability of the modified graphene lubricating oil, a load test and a wear test were performed.
Test 1
Load test, room temperature, 1500r/min,60 s.
Test 2
Abrasion test at 50 deg.C, load at 15kg, 500 r/min.
The blank is 100% base oil.
As can be seen from the table above, the addition of the graphene lubricating oil additive to the base oil reduces the diameter of the wear-scar, greatly increases the load of the four-ball machine load test, and improves the wear resistance.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. The modified graphene lubricating oil is characterized by comprising the following raw materials in parts by mass: 10-20 parts of stearic acid, 10-15 parts of oleic acid, 50-70 parts of acetone, 10-30 parts of graphene powder, 5-8 parts of concentrated sulfuric acid, 5-9 parts of molybdenum powder microspheres, 4-8 parts of chromium powder microspheres, 5-10 parts of iron oxide microspheres, 10-15 parts of benzotriazole, 9-18 parts of di-N-butyl phosphite, 8-16 parts of lithium fluoroborate, 10-30 parts of basic white oil, 4-8 parts of montmorillonite, 5-10 parts of N, N-dimethylformamide, 2-5 parts of lanolin magnesium soap, 5-8 parts of glyceryl monostearate, 8-12 parts of sodium polyethylene, 10-20 parts of a silane coupling agent and 100-120 parts of base oil.
2. A preparation method of modified graphene lubricating oil is characterized by comprising the following steps:
step one, adding stearic acid and oleic acid into acetone, magnetically stirring for 30min, adding graphene powder, continuously stirring for 1h, and then dropwise adding concentrated sulfuric acid to obtain black slurry; putting the black slurry into a round-bottom flask, connecting with a condensation reflux device, keeping the temperature of the round-bottom flask constant in a constant-temperature water bath at 50 ℃ for 3 hours to obtain slurry and a filter cake, then carrying out suction filtration on the slurry, washing the slurry for 3 times by using absolute ethyl alcohol, and putting the filter cake into a vacuum oven to be dried for 8 hours at 80 ℃; finally, crushing the dried filter cake for 30s to obtain modified graphene powder;
adding the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the glyceryl monostearate and the sodium polyethylene into the mixed solution, uniformly mixing, performing closed-end frosting for 48 hours, standing for 48 hours to obtain an additive without graphene powder, adding a silane coupling agent and the modified graphene powder into the additive without the graphene powder, and stirring for 3 hours to obtain the graphene lubricating oil additive;
and step three, adding the graphene lubricating oil additive into the base oil, dispersing for 1h to obtain lubricating oil modified graphene lubricating oil, then placing the prepared sample in a place which is at normal temperature and is away from light, and standing for 90 d to obtain the modified graphene lubricating oil.
3. The preparation method of the modified graphene lubricating oil according to claim 2, wherein the speed of crushing the filter cake in the first step is 35000 r/min.
4. The method of claim 2, wherein in the second step, the molybdenum powder microspheres, the chromium powder microspheres, the iron oxide microspheres, the benzotriazole, the di-n-butyl phosphite, and the lithium fluoborate are added to the base white oil, and the mixture is dispersed at the room temperature of 4000r/min, the closed-abrasive speed of 3000r/min, and the reaction temperature of 100 ℃.
5. The method for preparing the modified graphene lubricating oil according to claim 2, wherein the montmorillonite, the N, N-dimethylformamide, the lanolin magnesium soap, the stearic acid monoglyceride and the sodium polyethylene are uniformly mixed, then the speed of the closed-end sanding is 3000r/min, the reaction temperature is 140 ℃, and the temperature is kept for 48 hours at rest and is 140 ℃.
6. The preparation method of the modified graphene lubricating oil according to claim 2, wherein the speed of dispersing the graphene lubricating oil additive in the lubricating oil for 1h in the third step is 3500 r/min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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