CN108929742B - Nano molybdenum disulfide lubricating oil and preparation method thereof - Google Patents
Nano molybdenum disulfide lubricating oil and preparation method thereof Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 133
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 150000001875 compounds Chemical class 0.000 claims abstract description 24
- 239000002199 base oil Substances 0.000 claims abstract description 20
- 150000001412 amines Chemical class 0.000 claims abstract description 19
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011733 molybdenum Substances 0.000 claims abstract description 15
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 15
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 12
- 239000011593 sulfur Substances 0.000 claims abstract description 12
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 235000016768 molybdenum Nutrition 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 7
- 239000003921 oil Substances 0.000 claims description 7
- 235000019198 oils Nutrition 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 5
- 239000011609 ammonium molybdate Substances 0.000 claims description 5
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 5
- 229940010552 ammonium molybdate Drugs 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- PWKSKIMOESPYIA-UHFFFAOYSA-N 2-acetamido-3-sulfanylpropanoic acid Chemical compound CC(=O)NC(CS)C(O)=O PWKSKIMOESPYIA-UHFFFAOYSA-N 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 4
- 239000008158 vegetable oil Substances 0.000 claims description 4
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- OKGXJRGLYVRVNE-UHFFFAOYSA-N diaminomethylidenethiourea Chemical compound NC(N)=NC(N)=S OKGXJRGLYVRVNE-UHFFFAOYSA-N 0.000 claims description 3
- BRWIZMBXBAOCCF-UHFFFAOYSA-N hydrazinecarbothioamide Chemical compound NNC(N)=S BRWIZMBXBAOCCF-UHFFFAOYSA-N 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 2
- 230000009467 reduction Effects 0.000 abstract description 10
- 239000006185 dispersion Substances 0.000 abstract description 6
- 239000007810 chemical reaction solvent Substances 0.000 abstract description 4
- 229910052961 molybdenite Inorganic materials 0.000 description 21
- 239000000243 solution Substances 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000010410 layer Substances 0.000 description 8
- 239000000314 lubricant Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 239000002135 nanosheet Substances 0.000 description 6
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 238000005461 lubrication Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000010705 motor oil Substances 0.000 description 5
- 239000002060 nanoflake Substances 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000002356 single layer Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000010696 ester oil Substances 0.000 description 3
- 229940057995 liquid paraffin Drugs 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 239000002480 mineral oil Substances 0.000 description 3
- 235000010446 mineral oil Nutrition 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000005078 molybdenum compound Substances 0.000 description 3
- 150000002752 molybdenum compounds Chemical class 0.000 description 3
- 230000008439 repair process Effects 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 125000004434 sulfur atom Chemical group 0.000 description 3
- 150000003464 sulfur compounds Chemical class 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 239000010693 vegetable lubricating oil Substances 0.000 description 3
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical group CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 2
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- KAJZYANLDWUIES-UHFFFAOYSA-N heptadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCCN KAJZYANLDWUIES-UHFFFAOYSA-N 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000003879 lubricant additive Substances 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 231100000241 scar Toxicity 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004201 L-cysteine Substances 0.000 description 1
- 235000013878 L-cysteine Nutrition 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
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- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
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Images
Classifications
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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
- C10M125/22—Compounds containing sulfur, selenium or tellurium
-
- 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
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
- C10N2020/01—Physico-chemical properties
- C10N2020/055—Particles related characteristics
- C10N2020/06—Particles of special shape or size
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention provides nano molybdenum disulfide lubricating oil and a preparation method thereof. The method for preparing the nano molybdenum disulfide lubricating oil comprises the following steps: (1) preparing reaction liquid, wherein the reaction liquid comprises a molybdenum-containing compound, a sulfur-containing compound and organic amine; (2) heating the reaction solution for reaction to obtain two-dimensional nano flaky molybdenum disulfide; (3) and dispersing the two-dimensional nano flaky molybdenum disulfide in base oil through ultrasonic dispersion to obtain the nano molybdenum disulfide lubricating oil. According to the preparation method provided by the invention, organic amine is used as a reaction solvent when the two-dimensional nano flaky molybdenum disulfide is prepared, so that not only can ultrathin two-dimensional nano flaky molybdenum disulfide be prepared, but also oleylamine molecules can be modified on the surface of the two-dimensional nano flaky molybdenum disulfide, the dispersion stability of the two-dimensional nano flaky molybdenum disulfide in lubricating oil is increased, and the friction reduction and wear resistance of the nano molybdenum disulfide lubricating oil are improved.
Description
Technical Field
The invention relates to the technical field of lubricating oil additive materials, in particular to nano molybdenum disulfide lubricating oil and a preparation method thereof.
Background
Currently, molybdenum disulfide (MoS)2) Is a kind of layered material with special structure, which is divided into single-layer MoS2And multilayer MoS2. Wherein the MoS is a single layer2Is a sandwich structure consisting of an upper layer of S atoms, a lower layer of S atoms and a middle layer of Mo atoms, and the Mo atoms and the S atoms are combined by covalent bonds. And multi-layer MoS2Then several single-layer MoS2Relying on the weaker van der waals force composition between the layers. Two-dimensional nano-sheet MoS due to ultra-thin layered structure2Shows a plurality of remarkable physical and chemical properties, and shows important application prospects in the fields of lubrication, catalysis, lithium ion batteries, supercapacitors, optoelectronic devices thereof and the like.
Over the past decades, MoS of various forms2Nanoparticles, e.g. nanoflowers, nanospheres, nanosheet structures and nano-fullerene-like MoS2Are used as lubricant additives. ResearcherGeneral MoS2The antifriction and antiwear mechanism of the particles used as the lubricating additive is ascribed to the three aspects of the ball effect, the interlayer slippage and the peeling transfer, and meanwhile, MoS is researched by a plurality of researchers2The friction-reducing and wear-resisting mechanism of the particles is mainly attributed to a transfer stripping mechanism. In addition, Chen et al report ultra-thin nano-platelet-shaped MoS2Can be transferred to a friction contact area easily and shows excellent extreme pressure performance. Thus, it can be seen that the two-dimensional nano-flake MoS using the ultra-thin structure2As a lubricant additive, excellent tribological properties can be obtained.
However, two-dimensional nano-platelet-shaped MoS2The preparation of (A) has always troubled researchers. Currently, two-dimensional nano-sheet MoS has been developed2The synthesis method mainly comprises a stripping method, a chemical vapor deposition method and a water/solvent thermal method. However, problems of yield, structure, morphology, cost and stability still limit two-dimensional nano-sheet MoS2Development and application of (1) exploring and preparing high-quality two-dimensional nano flaky MoS2The method of (2) is still a major problem in the related art. In addition, MoS is required2The particles are practically applied to lubricating oil, and the problem of dispersion stability of the particles in the lubricating oil needs to be solved. However, MoS2The particles have a high surface energy and a high tendency to spontaneously form agglomerates in the lubricating oil, which eventually precipitate in the lubricating oil. Thus, it can be seen that MoS is being produced2After granulation, it has been a technical problem to disperse the particles stably in the lubricating oil.
Disclosure of Invention
The present invention has been completed based on the following findings of the inventors:
the inventor finds that organic amine is used as a reaction solvent in the process of preparing the two-dimensional nano flaky molybdenum disulfide, so that the two-dimensional nano flaky molybdenum disulfide with an ultrathin layered structure can be quickly and efficiently prepared, and oleylamine molecules can be modified on the surface of the two-dimensional nano flaky molybdenum disulfide, so that the dispersion stability of the two-dimensional nano flaky molybdenum disulfide in lubricating oil is improved, and the friction reduction and wear resistance of the nano molybdenum disulfide lubricating oil are improved.
In view of the above, an object of the present invention is to provide a method for preparing a nano molybdenum disulfide lubricating oil with good dispersion stability of additives and higher friction reduction and wear resistance.
In a first aspect of the invention, a method for preparing nano molybdenum disulfide lubricating oil is provided.
According to an embodiment of the invention, the method comprises: (1) preparing reaction liquid, wherein the reaction liquid comprises a molybdenum-containing compound, a sulfur-containing compound and organic amine; (2) heating the reaction solution for reaction to obtain two-dimensional nano flaky molybdenum disulfide; (3) and dispersing the two-dimensional nano flaky molybdenum disulfide in base oil through ultrasonic dispersion to obtain the nano molybdenum disulfide lubricating oil.
The inventor finds that by adopting the preparation method of the embodiment of the invention and adopting organic amine as a reaction solvent during the preparation of the two-dimensional nano flaky molybdenum disulfide, not only can the ultrathin two-dimensional nano flaky molybdenum disulfide be prepared, but also the surface of the two-dimensional nano flaky molybdenum disulfide can be modified with oleylamine molecules, so that the dispersion stability of the two-dimensional nano flaky molybdenum disulfide in lubricating oil is improved, and the friction reduction and wear resistance of the nano molybdenum disulfide lubricating oil are further improved.
In addition, the preparation method according to the above embodiment of the present invention may further have the following additional technical features:
according to the embodiment of the invention, the chain length of the carbon chain of the organic amine is C16-C22.
According to an embodiment of the present invention, the molybdenum-containing compound is selected from at least one of sodium molybdate, ammonium molybdate and molybdenum acetylacetonate, and the sulfur-containing compound is selected from at least one of thioacetamide, L-cysteine, thiourea, guanylthiourea and thiosemicarbazide.
According to an embodiment of the invention, the molar ratio of the molybdenum compound to the sulfur compound is 1: (5-60), and based on the volume of the organic amine, the total mass concentration of the molybdenum-containing compound and the sulfur-containing compound is 0.01-1.5 g/mL.
According to an embodiment of the present invention, the step (2) further comprises: (2-1) stirring the reaction liquid under the protection of inert gas, heating to 100-130 ℃, preserving heat for 15-60 minutes, continuously heating to 150-200 ℃, preserving heat for 30-180 minutes, and cooling; (2-2) carrying out centrifugal separation on the cooled reaction liquid, washing the centrifugally separated precipitate and drying to obtain the two-dimensional nano flaky molybdenum disulfide.
According to an embodiment of the invention, the purity of the inert gas is greater than 99.9% and the washed organic solvent is selected from cyclohexane or ethanol.
In a second aspect of the present invention, a nano molybdenum disulfide lubricating oil is provided.
According to an embodiment of the invention, the nano molybdenum disulfide lubricating oil comprises two-dimensional nano flaky molybdenum disulfide and base oil.
The inventor finds that the two-dimensional nano flaky molybdenum disulfide of the nano molybdenum disulfide lubricating oil disclosed by the embodiment of the invention can be stably dispersed in the base oil, and the two-dimensional nano flaky molybdenum disulfide with an ultrathin layer-shaped structure can timely enter a friction contact area in a friction process to perform a friction chemical reaction with a friction surface to form a friction chemical reaction film, so that the direct contact of rough peaks is effectively avoided, and the reaction film can also fill and repair the wear surface, thereby greatly improving the friction reduction and wear resistance of the lubricating oil.
In addition, the nano molybdenum disulfide lubricating oil according to the above embodiment of the present invention may also have the following additional technical features:
according to the embodiment of the invention, oleylamine molecules are modified on the surface of the two-dimensional nano flaky molybdenum disulfide, and the chain length of carbon chains of the oleylamine molecules is C16-C22.
According to an embodiment of the present invention, the base oil includes at least one selected from the group consisting of liquid paraffin, synthetic oil, mineral oil, ester oil, vegetable oil, and lubricating oil.
According to the embodiment of the invention, the mass content of the two-dimensional nano flaky molybdenum disulfide is 1-4%.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing aspects of the invention are explained in the description of the embodiments with reference to the following drawings, in which:
FIG. 1 is a schematic flow chart of a method for preparing nano molybdenum disulfide lubricating oil according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of a method for preparing nano molybdenum disulfide lubricating oil according to another embodiment of the invention;
FIG. 3 is a scanning electron micrograph of two-dimensional nanosheet-shaped molybdenum disulfide according to one embodiment of the present invention;
FIG. 4 is an infrared spectrum of a two-dimensional nanosheet of molybdenum disulfide in accordance with one embodiment of the present invention;
FIG. 5 is a thermogravimetric plot of two-dimensional nanosheet-like molybdenum disulfide in accordance with one embodiment of the present invention;
FIG. 6 shows tribological performance test results of nano-sized molybdenum disulfide lubricant and pure engine oil in accordance with one embodiment of the present invention.
Detailed Description
The following examples of the present invention are described in detail, and it will be understood by those skilled in the art that the following examples are intended to illustrate the present invention, but should not be construed as limiting the present invention. Unless otherwise indicated, specific techniques or conditions are not explicitly described in the following examples, and those skilled in the art may follow techniques or conditions commonly employed in the art or in accordance with the product specifications.
In one aspect of the invention, the invention provides a method for preparing nano molybdenum disulfide lubricating oil. According to an embodiment of the present invention, referring to fig. 1, the preparation method includes:
s100: and preparing a reaction solution.
In the step, a reaction solution comprising a molybdenum-containing compound, a sulfur-containing compound and organic amine is prepared, and thus, the two-dimensional nano flaky molybdenum disulfide can be synthesized through subsequent heating reaction.
According to the embodiment of the invention, the chain length of the carbon chain of the organic amine in the reaction liquid can be C16-C22, so that the temperature resistance of the nano molybdenum disulfide lubricating oil added with the two-dimensional nano flaky molybdenum disulfide is better by adopting the long-chain organic amine, and the service performance of the prepared lubricating oil is improved. In some embodiments of the present invention, the organic amine is hexadecylamine, heptadecylamine or octadecylamine, and thus, the organic amine of the above kind is used as a solvent to synthesize the two-dimensional nano flaky molybdenum disulfide with high yield, and the long-chain organic amine can also modify the surface of the two-dimensional nano flaky molybdenum disulfide, so as to further improve the temperature resistance of the nano molybdenum disulfide lubricating oil.
According to an embodiment of the present invention, the molybdenum-containing compound may be selected from at least one of sodium molybdate, ammonium molybdate and molybdenum acetylacetonate, and the sulfur-containing compound may be selected from at least one of thioacetamide, L-cysteine, thiourea, guanylthiourea and thiosemicarbazide. Thus, molybdenum disulfide can be thermally synthesized in high yield by using the molybdenum-containing compound and the sulfur-containing compound of the above-mentioned kinds. In some embodiments of the present invention, the molybdenum compound may be sodium molybdate, and the sulfur compound may be thioacetamide or L-cysteine, so that the molybdenum disulfide can be thermally synthesized with high yield and the two-dimensional nano-flaky molybdenum disulfide has uniform morphology and particle size.
According to an embodiment of the invention, the molar ratio of molybdenum compound to said sulfur compound is 1: (5-60), and based on the volume of the organic amine, the total mass concentration of the molybdenum-containing compound and the sulfur-containing compound is 0.01-1.5 g/mL, so that the reaction solution composed of the raw materials in the above proportion can effectively regulate and control the morphology of the molybdenum disulfide particles into a two-dimensional nano sheet with an ultrathin layered structure.
S200: and heating the reaction solution for reaction to obtain the two-dimensional nano flaky molybdenum disulfide.
In the step, the reaction solution is heated to react, so as to obtain the two-dimensional nano flaky molybdenum disulfide. According to an embodiment of the present invention, referring to fig. 2, step S200 may further include:
s210: stirring the reaction solution under the protection of inert gas, heating the reaction solution in sections, reacting and cooling the reaction solution.
In the step, the reaction solution obtained in the step S100 is stirred under the protection of inert gas, heated to 100-130 ℃, kept warm for 15-60 minutes, continuously heated to 150-200 ℃, kept warm for 30-180 minutes, and then cooled. Therefore, side reactions are less under the protection of nitrogen, the yield is further improved, and the two-dimensional nano flaky molybdenum disulfide can fully have an ultrathin lamellar structure through sectional heating. According to the embodiment of the present invention, the purity of the inert gas is greater than 99.9%, so that the side reaction such as oxidation is prevented to reduce the synthesis yield of the molybdenum disulfide.
S220: and carrying out centrifugal separation on the cooled reaction liquid, washing the precipitate after the centrifugal separation, and drying to obtain the two-dimensional nano flaky molybdenum disulfide.
In this step, the reaction solution cooled in step S210 is centrifuged, and the centrifuged precipitate is washed and dried to obtain two-dimensional nano flaky molybdenum disulfide. According to the embodiment of the invention, the washed organic solvent can be selected from cyclohexane or ethanol, so that the centrifuged precipitate is washed 4 times by cyclohexane or ethanol, and high-purity two-dimensional nanosheet-shaped molybdenum disulfide can be obtained.
S300: and dispersing the two-dimensional nano flaky molybdenum disulfide in base oil through ultrasonic dispersion to obtain the nano molybdenum disulfide lubricating oil.
In the step, the two-dimensional nano flaky molybdenum disulfide prepared in the step S200 is dispersed in the base oil through ultrasonic dispersion to obtain the nano molybdenum disulfide lubricating oil, so that the two-dimensional nano flaky molybdenum disulfide with the surface modified with oleylamine molecules has oil solubility, and is easily and stably dispersed in the base oil, and the friction reduction and wear resistance of the nano molybdenum disulfide lubricating oil are effectively improved.
According to an embodiment of the present invention, the base oil includes at least one selected from the group consisting of liquid paraffin, synthetic oil, mineral oil, ester oil, vegetable oil and lubricating oil, so that the two-dimensional nano-flaky molybdenum disulfide having the oleylamine molecule modified on the surface thereof can be dispersed in the base oil of the above kind, thereby solving the problem of easy agglomeration of the lubricant.
In summary, according to the embodiments of the present invention, the present invention provides a preparation method, in which organic amine is used as a reaction solvent when two-dimensional nano-flake molybdenum disulfide is prepared, so that not only can ultrathin-layered two-dimensional nano-flake molybdenum disulfide be prepared, but also oleylamine molecules can be modified on the surface of the two-dimensional nano-flake molybdenum disulfide, thereby increasing the dispersion stability of the two-dimensional nano-flake molybdenum disulfide in lubricating oil, and further improving the friction reduction and wear resistance of the nano-molybdenum disulfide lubricating oil.
In another aspect of the invention, the invention provides nano molybdenum disulfide lubricating oil.
According to an embodiment of the invention, the nano molybdenum disulfide lubricating oil comprises two-dimensional nano flaky molybdenum disulfide and base oil. It should be noted that the "two-dimensional nanosheet-shaped molybdenum disulfide" herein specifically refers to an ultra-thin layer-shaped MoS having a lateral dimension of 20 to 30nm and consisting of only one or several atomic layers2. Thus, the two-dimensional nano flaky molybdenum disulfide can be stably dispersed in the base oil and has MoS with an ultrathin lamellar structure2The lubricating oil can easily enter a friction contact area in the friction process, and a friction chemical reaction film is formed by the friction chemical reaction between the lubricating oil and the friction surface, so that the direct contact of rough peaks is effectively avoided, and the reaction film can also fill and repair the worn surface, thereby greatly improving the friction reduction and wear resistance of the lubricating oil.
According to the embodiment of the invention, the surface of the two-dimensional nano flaky molybdenum disulfide is modified with oleylamine molecules, and the chain length of the carbon chain of the oleylamine molecules is C16-C22, so that the two-dimensional nano flaky MoS modified with oleylamine molecules on the surface2Can be directly dispersed in base oil, and is suitable for being directly used as a lubricating oil additive without surface treatment.
According to the embodiment of the present invention, the base oil includes at least one selected from the group consisting of liquid paraffin, synthetic oil, mineral oil, ester oil, vegetable oil and lubricating oil, so that the two-dimensional nano-flaky molybdenum disulfide modified with oleylamine molecules on the surface can be dispersed in the base oil of the above kind, thereby solving the problem that the lubricant is easily agglomerated in the lubricating oil.
According to the embodiment of the invention, the mass content of the two-dimensional nano flaky molybdenum disulfide is 1-4%, so that the two-dimensional nano flaky molybdenum disulfide added with the concentration can be uniformly dispersed in base oil and is not easy to agglomerate, and the nano molybdenum disulfide lubricating oil has long-term use stability. And if the mass content of the two-dimensional nano flaky molybdenum disulfide is lower than 1%, the friction reduction and wear resistance of the nano molybdenum disulfide lubricating oil are not obviously improved; if the mass content of the two-dimensional nano flaky molybdenum disulfide is higher than 5%, the friction reduction and wear resistance of the nano molybdenum disulfide lubricating oil can not be obviously improved, and the lubricating agent is easily wasted.
In summary, according to the embodiments of the present invention, the present invention provides a nano molybdenum disulfide lubricating oil, wherein two-dimensional nano flaky molybdenum disulfide can be stably dispersed in base oil, and the two-dimensional nano flaky molybdenum disulfide with an ultra-thin layered structure can timely enter a friction contact area during a friction process, and undergoes a tribochemical reaction with a friction surface to form a tribochemical reaction film, so as to effectively avoid direct contact of a roughness peak, and the reaction film can also fill and repair the wear surface, thereby greatly improving the anti-friction and anti-wear properties of the lubricating oil.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
In this example, two-dimensional nanosheet-shaped molybdenum disulfide was prepared. The method comprises the following specific steps:
(a) mixing 3mmol of sodium molybdate and 15mmol of thioacetamide with 10mL of hexadecylamine;
(b) continuously stirring the mixed solution under the protection of nitrogen with the purity of 99.9 percent, heating the mixture to 100 ℃ and keeping the temperature for 15 minutes to form a transparent orange-red solution, then increasing the temperature to 180 ℃ and keeping the temperature for 30 minutes, and then cooling to room temperature to obtain a black liquid;
(c) centrifuging the black liquid to obtain black precipitate, washing the black precipitate with cyclohexane for 1 time, washing with ethanol for 3 times, and oven drying in a vacuum drying oven at 40 deg.C for 6 hr to obtain oil soluble two-dimensional oil soluble oilNano-sheet MoS2。
Example 2
In this example, two-dimensional nanosheet-shaped molybdenum disulfide was prepared. The method comprises the following specific steps:
(a) mixing 2.5mmol ammonium molybdate and 50mmol L-cysteine with 30mL heptadecylamine;
(b) continuously stirring the mixed solution under the protection of nitrogen with the purity of 99.9 percent, heating the mixture to 120 ℃ and keeping the temperature for 30 minutes to form a transparent orange-red solution, then increasing the temperature to 200 ℃ and keeping the temperature for 120 minutes, and then cooling to room temperature to obtain a black liquid;
(c) centrifuging the black liquid to obtain black precipitate, washing the black precipitate with cyclohexane for 2 times, washing with ethanol for 2 times, and drying in a vacuum drying oven at 60 deg.C for 8 hr to obtain oil-soluble two-dimensional nano flaky MoS2。
Example 3
In this example, nano molybdenum disulfide lubricant was prepared. The method comprises the following specific steps:
(a) mixing 5mmol ammonium molybdate and 100mmol thioacetamide with 30mL octadecylamine;
(b) continuously stirring the mixed solution under the protection of nitrogen with the purity of 99.9 percent, heating the mixture to 100 ℃ and keeping the temperature for 20 minutes to form a transparent orange-red solution, then increasing the temperature to 200 ℃ and keeping the temperature for 60 minutes, and then cooling to room temperature to obtain a black liquid;
(c) centrifuging the black liquid to obtain black precipitate, washing the black precipitate with cyclohexane for 1 time, washing with ethanol for 3 times, and drying in a vacuum drying oven at 40 deg.C for 12 hr to obtain oil-soluble two-dimensional nano flaky MoS2；
(d) Two-dimensional nano flaky MoS2Adding the nano molybdenum disulfide lubricating oil serving as a lubricating additive into commercial engine lubricating oil according to the proportion of 3 wt%, and performing ultrasonic dispersion to obtain the nano molybdenum disulfide lubricating oil.
The two-dimensional nanosheet-shaped MoS of this example2A Scanning Electron Microscope (SEM) photograph of the sample is shown in FIG. 3. As can be seen in FIG. 3, MoS2Is shown as typicalThe transverse dimension of the layered structure is 20-30 nm, and the layers are in a highly disordered and low stacking state. Meanwhile, as can be seen from (c) of FIG. 3, MoS2Consists of a single layer or a plurality of atomic layers and has an ultrathin layer-shaped structure.
The two-dimensional nanosheet-shaped MoS of this example2The infrared spectrum of the sample is shown in curve 2 of fig. 4, while curve 1 of fig. 4 belongs to octadecylamine. As can be seen from FIG. 4, at 3460cm-1The broad peak is the stretching vibration peak of water molecule, and is at 2922, 2853, 1647, 1608, 1460 and 720cm-1The absorption peak appeared is the infrared characteristic peak of the octadecylamine molecule, which indicates that the prepared MoS2The surface of the lubricating oil is modified with octadecylamine molecules, so that the lubricating oil can be well dispersed in the lubricating oil.
The two-dimensional nanosheet-shaped MoS of this example2The thermogravimetric curve of the sample in a nitrogen atmosphere is shown in fig. 5, in which curve 1 of fig. 5 represents the rate of change of mass, and curve 2 minus 5 represents the mass fraction. As can be seen in FIG. 5, MoS2When the sample is heated to 900 ℃, the mass loss is 37.2 wt%, and the mass loss is caused by volatilization and decomposition of octadecylamine molecules in the sample; MoS2In the sample, the mass fraction of octadecylamine molecules is 37.2 wt%, so that MoS is obtained2Is 62.8 wt%.
The nano molybdenum disulfide lubricant of this example was tribologically tested on a SRV4 frictional wear test. The experimental conditions are as follows: 100N load, 50Hz frequency, 2mm stroke, 50-150 ℃ temperature, and the friction pair of the steel ball and the steel disc made of bearing steel material with the diameter of 10mm and the diameter of 24 multiplied by 7.88 mm. The tribology experiment was performed for 1h using the reciprocating mode. The tribological properties of pure engine oil were compared to the nano molybdenum disulfide lubricant of this example.
The results of the tribological performance test of the nano molybdenum disulfide lubricating oil of this example are shown in fig. 6 (a), and fig. 6 (b) are the results of the tribological performance test of the pure engine lubricating oil. As can be seen from fig. 6, the friction coefficient remained stable only around 0.125 at different test temperatures when lubricated with pure engine oil; while adding 3 wt% of two-dimensional nano flaky MoS2Then, the friction coefficient is reduced to a certain degree at the experimental temperatures of 50 ℃, 100 ℃ and 150 ℃, and meanwhile, the friction coefficient at the experimental temperature of 100 ℃ is minimum 0.08, and the friction coefficient is reduced by 36 percent compared with the friction coefficient under the lubrication of pure commercial engine lubricating oil.
The results of the anti-wear performance test of the nano molybdenum disulfide lubricating oil of this example are shown in table 1, and the results of the anti-wear performance test of pure engine lubricating oil are also included therein. As can be seen from table 1, the wear volume and the maximum wear scar depth were both greatly reduced when the nano molybdenum disulfide lubricating oil was used for lubrication at the experimental temperatures of 50 ℃, 100 ℃ and 150 ℃. Especially adding two-dimensional nano flaky MoS at high temperature of 150 DEG C2After that, the maximum wear scar depth was 28.53% under pure engine oil lubrication and the wear volume was only 22.45% under pure engine oil lubrication. Therefore, the two-dimensional nano flaky MoS prepared by the invention2The lubricating oil has good antifriction and antiwear performances when used as a lubricant, and has important positive effects on reducing energy loss and protecting friction pairs.
TABLE 1
In the description of the present invention, it is to be understood that reference throughout this specification to the word "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (7)
1. A method for preparing nano molybdenum disulfide lubricating oil is characterized by comprising the following steps:
(1) preparing a reaction liquid, wherein the reaction liquid consists of a molybdenum-containing compound, a sulfur-containing compound and an organic amine, and the molar ratio of the molybdenum-containing compound to the sulfur-containing compound is 1: (5-60), and the total mass concentration of the molybdenum-containing compound and the sulfur-containing compound is 0.01-1.5 g/mL based on the volume of the organic amine;
(2) stirring the reaction solution under the protection of inert gas, heating to 100-130 ℃, preserving heat for 15-60 minutes, continuously heating to 150-200 ℃, preserving heat for 30-180 minutes, cooling, carrying out centrifugal separation on the cooled reaction solution, washing the centrifugally separated precipitate, and drying to obtain the two-dimensional nano flaky molybdenum disulfide, wherein the washed organic solvent is selected from cyclohexane or ethanol;
(3) and dispersing the two-dimensional nano flaky molybdenum disulfide in base oil through ultrasonic dispersion to obtain the nano molybdenum disulfide lubricating oil.
2. The method according to claim 1, wherein the organic amine has a carbon chain length of C16-C22.
3. The method according to claim 1, wherein the molybdenum-containing compound is at least one selected from the group consisting of sodium molybdate, ammonium molybdate and molybdenum acetylacetonate, and the sulfur-containing compound is at least one selected from the group consisting of thioacetamide, L-cysteine, thiourea, guanylthiourea and thiosemicarbazide.
4. The method of claim 1, wherein the inert gas has a purity greater than 99.9%.
5. The nano molybdenum disulfide lubricating oil prepared by the method of any one of claims 1 to 4, which is characterized by comprising two-dimensional nano flaky molybdenum disulfide and base oil, wherein the mass content of the two-dimensional nano flaky molybdenum disulfide is 1-4%.
6. The nano molybdenum disulfide lubricating oil as claimed in claim 5, wherein the surface of the two-dimensional nano flaky molybdenum disulfide is modified with oleylamine molecules, and the chain length of the carbon chain of the oleylamine molecules is C16-C22.
7. The nano molybdenum disulfide lubricating oil of claim 5, wherein the base oil comprises at least one selected from synthetic oils and vegetable oils.
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