CN114480001B - Molybdenum disulfide nano lubricating oil capable of stably existing and preparation method thereof - Google Patents
Molybdenum disulfide nano lubricating oil capable of stably existing and preparation method thereof Download PDFInfo
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 136
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 126
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002199 base oil Substances 0.000 claims abstract description 108
- 239000002270 dispersing agent Substances 0.000 claims abstract description 47
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 31
- 239000011259 mixed solution Substances 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 19
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 18
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 18
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 18
- 239000005642 Oleic acid Substances 0.000 claims description 18
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 18
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 18
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 18
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 17
- 238000003760 magnetic stirring Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 12
- 239000003921 oil Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 6
- 230000001050 lubricating effect Effects 0.000 abstract description 11
- 231100000241 scar Toxicity 0.000 abstract description 7
- 239000000725 suspension Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 9
- 238000012986 modification Methods 0.000 description 8
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- 238000010586 diagram Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004939 coking Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
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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
-
- 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
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
- C10M2201/066—Molybdenum sulfide
-
- 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
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
-
- 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
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
-
- 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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- 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
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/08—Thiols; Sulfides; Polysulfides; Mercaptals
- C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/04—Detergent property or dispersant property
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- Chemical & Material Sciences (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention discloses a kind of energy stabilizingThe molybdenum disulfide nanometer lubricating oil and the preparation method thereof exist, wherein, the molybdenum disulfide nanometer lubricating oil is composed of molybdenum disulfide powder, dispersant mixed liquid and base oil; in the molybdenum disulfide nanometer lubricating oil, the mass fraction of the dispersant mixed liquid is 8-15 wt%, and the mass fraction of the molybdenum disulfide powder is 0.1-1.0 wt%; the preparation method comprises the following steps: adding molybdenum disulfide powder into the dispersant mixed solution to obtain a mixed reaction system; heating the mixed reaction system, magnetically stirring, and naturally cooling after the reaction is finished to obtain a dispersant modified molybdenum disulfide mixed solution; and mixing the dispersant modified molybdenum disulfide mixed solution with the base oil, and performing ultrasonic dispersion treatment to obtain the molybdenum disulfide nano lubricating oil. MoS of the invention 2 The nanometer lubricating oil can exist stably, the diameter of the wear scar under the extreme pressure condition can be reduced remarkably, and the lubricating property of the base oil is improved remarkably.
Description
Technical Field
The invention relates to the technical field of nano lubricating oil. In particular to molybdenum disulfide nanometer lubricating oil capable of stably existing and a preparation method thereof.
Background
The existing research shows that the nano lubricating oil has excellent extreme pressure performance, wear resistance and antifriction performance compared with base oil, has higher bearing capacity and lubricating performance under the conditions of high temperature, heavy load and the like, and the nano particles can repair furrows generated by local peak contact, thereby improving the surface flatness. Molybdenum disulfide (MoS) 2 ) Similar to graphene, the molybdenum disulfide has an obvious layered structure, the lubricating property of the molybdenum disulfide depends on the specific crystal structure of the molybdenum disulfide, and the molybdenum disulfide is connected between layers only by weak van der Waals force, so that the molybdenum disulfide has the characteristic of easy shearing. The molybdenum disulfide layer is of an S-Mo-S sandwich structure, and the excellent bearing capacity is reflected by strong in-plane rigidity along the thickness direction. Thus, MoS 2 The lubricating oil composition can be used as a lubricating oil nano additive or a solid lubricating material and has excellent friction performance.
MoS 2 The nano material has excellent friction performance but MoS 2 The high specific surface energy and high surface atomic activity of the nano-particles enable MoS 2 The nano particles are easy to mutually adsorb in the lubricating oil to generate aggregation to influence the quality of the lubricating oil, thereby directly influencing MoS 2 The nanometer lubricating oil is applied to actual working conditions. Therefore, a MoS capable of stably existing was developed 2 The nano lubricating oil has great significance for improving the lubrication and heat transfer of contact parts.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide the molybdenum disulfide nano lubricating oil capable of stably existing and the preparation method thereof, so as to solve the existing MoS 2 Molybdenum disulfide in the nanometer lubricating oil is easy to adsorb each other to generate aggregation, the suspension stability is poor, the preparation process is complex and the like.
In order to solve the technical problems, the invention provides the following technical scheme:
a molybdenum disulfide nanometer lubricating oil capable of stably existing is composed of molybdenum disulfide powder, dispersant mixed liquor and base oil; in the molybdenum disulfide nanometer lubricating oil, the mass fraction of the dispersant mixed liquid is 8-15 wt%, and the mass fraction of molybdenum disulfide powder is 0.1-1.0 wt%;
the dispersant mixed solution consists of oleic acid, oleylamine and n-dodecyl mercaptan, and the mass ratio of the oleic acid to the oleylamine to the n-dodecyl mercaptan is (0.8-1.2): (1.8-2.2): (0.8-1.2); the oleic acid, the oleylamine and the n-dodecyl mercaptan can be used as a single dispersant to increase the suspension stability of the molybdenum disulfide nano lubricating oil, but researches show that the oleic acid, the oleylamine and the n-dodecyl mercaptan are not ideal in stabilizing effect when used singly, and the mixed dispersant obtained by mixing the oleic acid, the oleylamine and the n-dodecyl mercaptan according to the proportion has the best dispersing performance on molybdenum disulfide particles and is beneficial to improving the lubricating property of the molybdenum disulfide nano lubricating oil.
According to the molybdenum disulfide nanometer lubricating oil capable of stably existing, the mass fraction of the dispersant mixed solution is 12wt%, and the mass ratio of oleic acid, oleylamine and n-dodecyl mercaptan in the dispersant mixed solution is 1:2: 1. in the test, the mass fraction of the dispersant mixed solution is too large or too small, which is not beneficial to the dispersion of the molybdenum disulfide particles, and when the mass fraction of the dispersant mixed solution is 12wt%, the mass ratio of the oleic acid to the oleylamine to the n-dodecyl mercaptan is 1:2:1, the suspension stability and the lubricating property of the molybdenum disulfide nano lubricating oil are better than those of molybdenum disulfide lubricating oil with a single dispersant or a mixture of any two dispersants.
According to the molybdenum disulfide nanometer lubricating oil capable of stably existing, the particle size of molybdenum disulfide powder is 50-200 nm, and the mass fraction of the molybdenum disulfide powder is 0.3-0.5 wt%. Too small a particle size of the molybdenum disulfide powder increases the cost of the lubricating oil, while too large a particle size tends to decrease its suspension stability. If the added amount of molybdenum disulfide is too small, it is difficult to provide a sufficient lubricating effect, and if it is too large, it is liable to settle due to aggregation of particles.
The molybdenum disulfide nanometer lubricating oil capable of stably existing is characterized in that the base oil is industrial white oil, and the base oil is one or a combination of two or more of 32# base oil, 46# base oil, 68# base oil, 100# base oil, 150# base oil, 250# base oil, 300# base oil or 400# base oil.
The molybdenum disulfide nanometer lubricating oil capable of stably existing is prepared by the following steps: the kinematic viscosity of the 32# base oil is 28-35 mm 2 The kinematic viscosity of the 46# base oil is 42-50 mm 2 The kinematic viscosity of the 68# base oil is 65-71 mm 2 The kinematic viscosity of the 100# base oil is 95-105 mm 2 The kinematic viscosity of the 150# base oil is 145-155 mm 2 The kinematic viscosity of the No. 250 base oil is 240-260 mm 2 The kinematic viscosity of 300# base oil is 290-310 mm 2 The kinematic viscosity of the 400# base oil is 380-420 mm 2 /s。
A preparation method of molybdenum disulfide nano lubricating oil capable of stably existing comprises the following steps:
step A: oleic acid, oleylamine and n-dodecyl mercaptan are mixed according to the mass ratio of (0.8-1.2): (1.8-2.2): (0.8-1.2) to obtain a dispersant mixed solution;
and B: adding molybdenum disulfide powder into the dispersant mixed solution to obtain a mixed reaction system; heating the mixed reaction system, magnetically stirring, and naturally cooling after the reaction is finished to obtain a dispersant modified molybdenum disulfide mixed solution;
and C: mixing the dispersant modified molybdenum disulfide mixed solution with the base oil, performing ultrasonic dispersion treatment, and obtaining molybdenum disulfide nano lubricating oil after the ultrasonic dispersion treatment is finished;
in the molybdenum disulfide nanometer lubricating oil, the mass fraction of the dispersant mixed liquid is 8-15 wt%, and the mass fraction of the molybdenum disulfide powder is 0.1-1.0 wt%.
According to the preparation method of the molybdenum disulfide nano lubricating oil capable of stably existing, in the molybdenum disulfide nano lubricating oil, the mass fraction of the dispersant mixed liquid is 12wt%, and the mass fraction of the molybdenum disulfide powder is 0.3-0.5 wt%; the mass ratio of oleic acid, oleylamine and n-dodecyl mercaptan in the dispersant mixed solution is 1:2: 1; the particle size of the molybdenum disulfide powder is 50-200 nm;
the base oil is industrial white oil, and the base oil is one or a combination of two or more of 32# base oil, 46# base oil, 68# base oil, 100# base oil, 150# base oil, 250# base oil, 300# base oil or 400# base oil;
at 40 ℃ conditions: the kinematic viscosity of the 32# base oil is 28-35 mm 2 The kinematic viscosity of the 46# base oil is 42-50 mm 2 The kinematic viscosity of the 68# base oil is 65-71 mm 2 The kinematic viscosity of the 100# base oil is 95-105 mm 2 The kinematic viscosity of the 150# base oil is 145-155 mm 2 The kinematic viscosity of the No. 250 base oil is 240-260 mm 2 The kinematic viscosity of 300# base oil is 290-310 mm 2 The kinematic viscosity of the 400# base oil is 380-420 mm 2 /s。
The preparation method of the molybdenum disulfide nanometer lubricating oil capable of stably existing comprises the following steps: controlling the temperature of the mixed reaction system to be 170-190 ℃, and carrying out magnetic stirring for 1.5-2.5 h, wherein the rotating speed of the magnetic stirring is 500-800 r/min. If the reaction temperature of the mixed reaction system is too low, the modification effect is poor, and even difficult to realize, and if the reaction temperature is too high, coking failure of the mixed reaction system is easily caused. In addition, the magnetic stirring time and the magnetic stirring rotating speed can also influence the modification effect of the molybdenum disulfide, if the magnetic stirring time is too short, the modification process of the molybdenum disulfide cannot be completely modified, and if the stirring time is too long, the operation time is increased, and the preparation efficiency is reduced; if the rotation speed of the magnetic stirring is too low, the modification reaction is not facilitated, but if the rotation speed of the magnetic stirring is too high, the droplets splash, and the operation safety is affected.
The preparation method of the molybdenum disulfide nanometer lubricating oil capable of stably existing comprises the following steps: controlling the temperature of the mixed reaction system to be 180 ℃, and carrying out magnetic stirring for 2h, wherein the rotating speed of the magnetic stirring is 600 r/min. Under the reaction condition, the molybdenum disulfide particles are easier to disperse after surface modification, and the prepared molybdenum disulfide lubricating oil has good suspension stability and better lubricating property.
The preparation method of the molybdenum disulfide nanometer lubricating oil capable of stably existing comprises the following steps: the power of ultrasonic dispersion is 1080W, the temperature of ultrasonic dispersion is 110 ℃, the coking and failure of lubricating oil can be easily caused by overhigh temperature, and the ultrasonic dispersion is not facilitated by overlow temperature; the working mode of ultrasonic dispersion is as follows: after ultrasonic dispersion for 1 second, pausing for 1 second, then continuing ultrasonic dispersion for 1 second, pausing for 1 second; this ultrasonic dispersion mode of operation was cycled for 90 min. The ultrasonic mode has high dispersion efficiency, if the ultrasonic working time is too long, the temperature of the lubricating oil is easily too high, and the temperature control is not facilitated, and if the ultrasonic working time is too short, the ultrasonic efficiency is reduced, and the dispersion effect is not good.
The technical scheme of the invention achieves the following beneficial technical effects:
the invention realizes the MoS by selecting a specific dispersant and controlling the proportion of each component in the dispersant and the addition amount of the dispersant 2 And (3) surface modification of the nanoparticles. One step earlier on MoS than adding dispersant directly to base oil 2 The surface modification of the nanoparticles can increase MoS 2 Repulsive force between nano particlesEffectively prevents agglomeration and enhances MoS 2 The dispersion stability of the nanoparticles in the lubricating oil is improved, and the excellent lubricating property of the nano lubricating oil is exerted. MoS prepared by the invention 2 The nano lubricating oil can stably exist, and no obvious aggregation and sedimentation phenomenon exists after 20 days; and the MoS prepared by the invention is relative to the base oil 2 The nanometer lubricating oil can obviously reduce the wear scar diameter under the extreme pressure condition, can improve the limit load, the limit temperature and the limit speed of an oil film under the long-grinding condition (the limit load, the limit temperature and the limit speed represent the maximum running load, the maximum running temperature and the maximum running speed before the oil film between friction pairs breaks), and obviously improves the lubricating property of the base oil.
The dispersing agent used in the invention is oleic acid, oleylamine and n-dodecyl mercaptan with the mass ratio of 1:2:1, the formula is simple, the cost is lower, the environment is friendly, the preparation process is simple, and the time consumption of the preparation process is shorter. MoS configured by adopting method of the invention 2 The nano lubricating oil can stably exist, and the suspension stability of the nano lubricating oil can be continuously maintained only by simple mechanical shaking after the nano lubricating oil is placed for a long time (more than one month).
Drawings
FIG. 1 is a simplified experimental operation of step B in example 1 of the present invention;
FIG. 2 is a simplified experimental operation of step C in example 1 of the present invention;
FIG. 3 is a real beat diagram of the molybdenum disulfide nanometer lubricating oil prepared in example 1 of the present invention;
FIG. 4 is a real image of the molybdenum disulfide nanometer lubricant oil prepared in example 1 of the present invention after being left for 20 days;
FIG. 5 is a real beat diagram of the molybdenum disulfide nanometer lubricating oil prepared by the comparative example 1 of the present invention;
FIG. 6 is a real image of the molybdenum disulfide nanometer lubricant prepared in comparative example 1 of the present invention after being left for 3 days;
FIG. 7 is a graph of the load and friction coefficient of the molybdenum disulfide nanometer lubricating oil and 32# base oil prepared in example 1 of the present invention as a function of time;
FIG. 8 is a graph showing the results of a limit load test of the molybdenum disulfide nano lubricating oil prepared in example 1 of the present invention;
FIG. 932 # base oil ultimate load test results plot;
FIG. 10 is a comparison of the wear scar diameters of the molybdenum disulfide nanometer lubricating oil prepared in example 1 of the present invention and the 32# base oil.
FIG. 11 different base oils and their corresponding mass fraction of 0.5wt% MoS 2 And (5) comparing the wear scar diameters of the nano lubricating oil.
Detailed Description
Example 1
In the embodiment, the molybdenum disulfide nano lubricating oil capable of stably existing consists of molybdenum disulfide powder, dispersant mixed liquor and base oil; in the molybdenum disulfide nanometer lubricating oil, the mass fraction of the dispersant mixed liquid is 12wt%, and the mass fraction of the molybdenum disulfide powder is 0.5 wt%; the dispersant mixed liquid is composed of Oleic acid (chemical formula C) 18 H 34 O 2 ) Oleylamine (formula C) 18 H 37 N) and N-dodecyl mercaptan (1-Dodecanethiol, formula C) 12 H 26 S), the mass ratio of oleic acid, oleylamine and n-dodecyl mercaptan is 1:2: 1; the particle size of the molybdenum disulfide powder is 50-200 nm; the base oil is 32# base oil and is industrial-grade white oil.
The preparation method of the molybdenum disulfide nanometer lubricating oil capable of stably existing comprises the following steps:
step A: adding 9g of oleic acid, 18g of oleylamine and 9g of n-dodecyl mercaptan into a beaker together for mixing to obtain a dispersant mixed solution;
and B: adding 1.5g of molybdenum disulfide powder into the dispersant mixed solution to obtain a mixed reaction system; after stirring sufficiently with a glass rod, the beaker was placed on the surface of a heating table, and the temperature of the heating table was set to 180 ℃. Meanwhile, dispersing by using magnetic stirring, setting the rotating speed to be 600r/min, keeping the temperature of the mixed reaction system at 180 ℃, finishing the reaction after 2 hours of magnetic stirring, and naturally cooling to room temperature to obtain a dispersing agent modified molybdenum disulfide mixed solution; FIG. 1 is the present step for MoS 2 The experimental operation diagram of modifying the powder is shown;
and C: modifying the dispersantThe mixed solution of molybdenum disulfide and 262.5g of base oil (the base oil used in the present embodiment is No. 32 base oil, and the kinematic viscosity of the base oil at 40 ℃ is 28-35 mm 2 Mixing, fully stirring by using a glass rod, and then performing ultrasonic dispersion treatment by using an ultrasonic processor, wherein the specific setting parameter of the ultrasonic dispersion is 90% of the rated power of 1200W, and the working mode is as follows: the ultrasonic dispersion and the interval time are both 1 second (namely after 1 second of ultrasonic dispersion, pausing for 1 second, continuing to perform ultrasonic dispersion for 1 second, pausing for 1 second, and circulating in the same way), the temperature is controlled to be 110 ℃ during ultrasonic dispersion, and the molybdenum disulfide nano lubricating oil is naturally cooled to the room temperature after continuously dispersing for 90 minutes to obtain the molybdenum disulfide nano lubricating oil; FIG. 2 is a simplified diagram of the experimental operation in this step.
FIGS. 7 to 9 show No. 32 base oils and MoS in example 1 2 And comparing the limit load of the nano lubricating oil. Where the abscissa in fig. 7 represents the duration of the experiment and the ordinate represents the friction coefficient and the load, respectively. The load increased with the increase of the experimental time, the critical load of the base oil No. 32 was 50N, at which the oil film breaking friction coefficient suddenly increased, and severe gluing wear occurred on the friction surface, as shown in FIG. 8. MoS 2 The limit load of the nano lubricating oil was 520N, and the frictional surface was only slightly abraded at a load of 500N, as shown in fig. 9. Shows MoS 2 The nanometer lubricating oil can obviously improve the critical load of an oil film (increased from 50N to 500N) and reduce the abrasion of a friction surface compared with base oil.
FIG. 10 shows base oil # 32 and MoS in example 1 2 And (5) comparing the wear scar diameters of the nano lubricating oil. In the extreme pressure characteristic experiment, the set parameters are 650N of load and 1500r/min of rotating speed. The MoS can be known from the figure 2 The diameter of the wear-scar of the nano lubricating oil is 0.74mm, and the diameter of the wear-scar is reduced by about 43 percent compared with that of the base oil of 1.31mm, which shows that the introduction of the molybdenum disulfide can obviously reduce the diameter of the wear-scar under the extreme pressure characteristic.
Comparative example 1
The preparation method of the molybdenum disulfide nano lubricating oil in the comparative example comprises the following steps: adding 1.5g of molybdenum disulfide powder into 36g of base oil, and heating and stirring by the same method as in the step B of the embodiment 1 to obtain a molybdenum disulfide dispersion liquid; and then, mixing the molybdenum disulfide dispersion liquid with 262.5g of base oil by the same method as in the step C of the embodiment 1, and carrying out ultrasonic dispersion treatment, so as to obtain the molybdenum disulfide nano lubricating oil after the treatment is finished. The base oil used in this comparative example was the same as in example 1, and the molybdenum disulfide powder used was the same as in example 1.
Fig. 3 to 6 are stability test results of the lubricating oils prepared in example 1 and comparative example 1. Fig. 3 and 4 are real-time photographs of the nano-lubricating oil prepared in example 1 and the nano-lubricating oil after being left for 20 days, respectively, and it can be seen from the photographs that the molybdenum disulfide nano-lubricating oil prepared in example 1 has no obvious aggregation and sedimentation phenomenon after being left for 20 days, which indicates that the nano-lubricating oil has excellent suspension stability. In contrast, fig. 5 and 6 are real-time images of the nano-lubricating oil prepared in comparative example 1 and the nano-lubricating oil after standing for 3 days, and it can be seen from the images that after standing for 3 days, the molybdenum disulfide particles in the nano-lubricating oil in comparative example 1 almost completely settled, and the upper layer was transparent base oil, which indicates that the suspension stability was poor. In addition, the molybdenum disulfide nano lubricating oil in example 1 can keep the suspension stability after being placed for a long time (more than one month) only by simple mechanical shaking, while the lubricating oil prepared in comparative example 1 can not keep the suspension stability after being placed for 3 days by simple mechanical shaking.
Example 2
In the embodiment, the molybdenum disulfide nano lubricating oil capable of stably existing consists of molybdenum disulfide powder, dispersant mixed liquor and base oil; in the molybdenum disulfide nanometer lubricating oil, the mass fraction of the dispersant mixed liquid is 12wt%, and the mass fraction of the molybdenum disulfide powder is 0.3 wt%; the dispersant mixed solution is prepared from Oleic acid, (Oleic acid, chemical formula C 18 H 34 O 2 ) Oleylamine (formula C) 18 H 37 N) and N-dodecyl mercaptan (1-Dodecanethiol, formula C) 12 H 26 S), the mass ratio of oleic acid, oleylamine and n-dodecyl mercaptan is 1:2: 1; the particle size of the molybdenum disulfide powder is 50-200 nm; the base oil is 150# base oil and is also industrial grade white oil.
The preparation method of the molybdenum disulfide nanometer lubricating oil capable of stably existing comprises the following steps:
step A: adding 9g of oleic acid, 18g of oleylamine and 9g of n-dodecyl mercaptan into a beaker together for mixing to obtain a dispersant mixed solution;
and B: adding 0.9g of molybdenum disulfide powder into the dispersant mixed solution to obtain a mixed reaction system; after stirring sufficiently with a glass rod, the beaker was placed on the surface of a heating table, and the temperature of the heating table was set to 180 ℃. Meanwhile, dispersing by using magnetic stirring, setting the rotating speed to be 600r/min, keeping the temperature of the mixed reaction system at 180 ℃, finishing the reaction after 2 hours of magnetic stirring, and naturally cooling to room temperature to obtain a dispersing agent modified molybdenum disulfide mixed solution;
and C: the dispersant modified molybdenum disulfide mixed solution and 263.1g of base oil (the base oil used in the embodiment is 150# base oil, and the kinematic viscosity of the base oil at 40 ℃ is 145-155 mm 2 Mixing, fully stirring by using a glass rod, and then performing ultrasonic dispersion treatment by using an ultrasonic processor, wherein the specific setting parameter of the ultrasonic dispersion is 90% of the rated power of 1200W, and the working mode is as follows: the ultrasonic dispersion and the interval time are both 1 second (namely after 1 second of ultrasonic dispersion, pausing for 1 second, continuing to perform ultrasonic dispersion for 1 second, pausing for 1 second, and circulating in the same way), the temperature is controlled to be 110 ℃ during ultrasonic dispersion, the continuous dispersion is performed for 90min, and then the molybdenum disulfide nano lubricating oil is naturally cooled to the room temperature, so that the molybdenum disulfide nano lubricating oil is obtained.
In other embodiments, 46# base oil, 68# base oil, 100# base oil, 250# base oil, 300# base oil, or 400# base oil may be used (XX # base oil means that the kinematic viscosity is about XXmm at 40 ℃. (XX # base oil means that the kinematic viscosity is about XXmm) 2 Mixing any one of the molybdenum disulfide and the dispersant modified molybdenum disulfide mixed solution to prepare molybdenum disulfide nanometer lubricating oil; the molybdenum disulfide nanometer lubricating oil which is not easy to aggregate and settle and has good suspension stability can be realized, and the suspension stability can be continuously maintained only by simple mechanical shaking after the molybdenum disulfide nanometer lubricating oil is placed for a long time (more than one month).
FIG. 11 shows different base oils and 0.5wt% MoS prepared using different base oils 2 Comparison of wear scar diameters for Nano-Lubricants. In an extreme pressure characteristic experiment, the set parameters are 650N load, 1500r/min rotating speed and 28-35 mm kinematic viscosity at 40 ℃ from low-viscosity base oil (32# base oil) 2 (s) to high viscosity base oil (400# base oil, kinematic viscosity at 40 ℃ 380-420 mm) 2 S) MoS prepared by the same method as in example 1 2 The nano lubricating oil can obviously reduce the average wear scar diameter of the steel ball, which shows that the lubricating property of the base oil with different viscosities can be effectively improved by adopting the preparation method of the invention. In addition, the higher the viscosity of the base oil is, the better the suspension stability of the prepared molybdenum disulfide nano lubricating oil is, and by adopting the preparation method provided by the invention, even if the 32# base oil with the minimum viscosity is adopted, the prepared molybdenum disulfide nano lubricating oil can also keep the suspension stability for more than 20 days.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are possible which remain within the scope of the appended claims.
Claims (2)
1. A preparation method of molybdenum disulfide nano lubricating oil capable of stably existing is characterized by comprising the following steps:
step A: mixing oleic acid, oleylamine and n-dodecyl mercaptan according to a mass ratio of 1:2:1 to obtain a dispersant mixed solution;
and B: adding molybdenum disulfide powder into the dispersant mixed solution to obtain a mixed reaction system; heating the mixed reaction system, magnetically stirring, and naturally cooling after the reaction is finished to obtain a dispersant modified molybdenum disulfide mixed solution;
and C: mixing the dispersant modified molybdenum disulfide mixed solution with base oil, performing ultrasonic dispersion treatment, and obtaining molybdenum disulfide nano lubricating oil after the ultrasonic dispersion treatment is finished;
in the molybdenum disulfide nanometer lubricating oil, the mass fraction of the dispersant mixed liquid is 12wt%, and the mass fraction of molybdenum disulfide powder is 0.3-0.5 wt%; the particle size of the molybdenum disulfide powder is 50-200 nm;
in the step B: controlling the temperature of the mixed reaction system to be 180 ℃, and carrying out magnetic stirring for 2 hours at the rotating speed of 600 r/min;
in the step C: the power of ultrasonic dispersion is 1080W, and the temperature of ultrasonic dispersion is 110 ℃; the working mode of ultrasonic dispersion is as follows: after ultrasonic dispersion for 1 second, pausing for 1 second, then continuing ultrasonic dispersion for 1 second, pausing for 1 second; this ultrasonic dispersion mode of operation was cycled for 90 min.
2. The method for preparing the molybdenum disulfide nanometer lubricating oil capable of being stably existed according to claim 1, wherein the base oil is industrial-grade white oil, and the base oil is one or a combination of two or more of 32# base oil, 46# base oil, 68# base oil, 100# base oil, 150# base oil, 250# base oil, 300# base oil or 400# base oil;
at 40 ℃ conditions: the kinematic viscosity of the 32# base oil is 28-35 mm 2 The kinematic viscosity of the 46# base oil is 42-50 mm 2 The kinematic viscosity of the 68# base oil is 65-71 mm 2 The kinematic viscosity of the 100# base oil is 95-105 mm 2 The kinematic viscosity of the 150# base oil is 145-155 mm 2 The kinematic viscosity of the No. 250 base oil is 240-260 mm 2 The kinematic viscosity of 300# base oil is 290-310 mm 2 The kinematic viscosity of the 400# base oil is 380-420 mm 2 /s。
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