CN111534357B - Preparation method of nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive - Google Patents
Preparation method of nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive Download PDFInfo
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000002135 nanosheet Substances 0.000 title claims abstract description 81
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 239000000654 additive Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 230000000996 additive effect Effects 0.000 title claims abstract description 31
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000006228 supernatant Substances 0.000 claims abstract description 11
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 7
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 7
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 7
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 7
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000004729 solvothermal method Methods 0.000 claims abstract description 7
- 238000005119 centrifugation Methods 0.000 claims abstract 2
- 239000002243 precursor Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 10
- 239000002199 base oil Substances 0.000 claims description 9
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims 1
- 230000001050 lubricating effect Effects 0.000 abstract description 12
- 238000005461 lubrication Methods 0.000 abstract description 7
- 239000003921 oil Substances 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 238000000265 homogenisation Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 229910021389 graphene Inorganic materials 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 239000003879 lubricant additive Substances 0.000 description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 7
- 229910052750 molybdenum Inorganic materials 0.000 description 7
- 239000011733 molybdenum Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 229940057995 liquid paraffin Drugs 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 229910001069 Ti alloy Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005411 Van der Waals force Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000005069 Extreme pressure additive Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000007704 transition Effects 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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/24—Compounds containing phosphorus, arsenic or antimony
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
-
- 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
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Abstract
The invention discloses a preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive, which comprises the steps of preparing a black phosphorus nanosheet by adopting a liquid phase stripping method, uniformly dispersing black phosphorus powder into an N-methyl pyrrolidone solvent, carrying out ultrasonic treatment, centrifuging supernatant, repeating the centrifugation for several times, washing the centrifuged black phosphorus nanosheet, and drying; dispersing the black phosphorus nanosheets into a reaction solution containing ammonium molybdate and sodium sulfide, and obtaining the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive through a solvothermal method after ultrasonic homogenization. The composite lubricating oil additive has the advantages of easily obtained preparation raw materials and simple and convenient method, can effectively improve the antifriction lubricating property in the friction process, and can be applied to the fields of mechanical operation, oil lubrication of mechanical equipment and the like.
Description
Technical Field
The invention relates to a preparation method of a nano composite lubricating oil additive, in particular to a preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive.
Background
With the continuous progress of industrial technology, the working environment of various mechanical equipment and parts thereof becomes more complex and severe, and the traditional mineral-based lubricating oil is far from sufficient. In order to reduce friction and wear, various friction-reducing lubricant additives are widely used in extreme pressure additives for lubricating oils. The formation of an effective lubricating film through tribochemical reactions during the rubbing process is the key to the ability of the friction pair surface to resist gluing. Due to the importance of lubrication and the limited availability of existing lubrication methods, the development of lubricant additives with good performance is critical to achieving high reliability and long service life of mechanical equipment.
Molybdenum disulfide as an important transition group metal sulfide has the characteristic of a hexagonal system layered structure, and is bonded in a molecular layer through a strong chemical bond and bonded between layers through weak van der waals force, so that interlayer slippage can occur under low shear stress, and the molybdenum disulfide is widely used in the field of lubrication. Therefore, the molybdenum disulfide lubricating additive plays an important role in reducing friction and remarkably improving the anti-loading performance and performance.
In recent years, Black Phosphorus (BP), a novel two-dimensional material, has received much attention from researchers at home and abroad due to its special two-dimensional structure and thermodynamic stability. At present, the application of the nano molybdenum disulfide/black phosphorus nanosheet composite material in the field of lubricating additives does not exist.
Disclosure of Invention
The invention provides a preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive, which overcomes the defects of the existing traditional lubricating oil additive.
The technical scheme of the invention is as follows:
the invention provides a preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite material, which is prepared according to the following method, and comprises the following specific steps:
(1) preparation of black phosphorus nanosheet
Placing 5-10 parts of black phosphorus powder in 20000-plus 30000 parts of N-methylpyrrolidone solvent, carrying out ultrasonic treatment in a cold water bath for 8-10h, centrifuging at the rotating speed of 3000-plus 5000rpm for 20-30min after ultrasonic treatment, taking the supernatant, centrifuging at the rotating speed of 7000-plus 9000rpm for 20-30min, finally taking the supernatant, centrifuging at the rotating speed of 10000-plus 12000rpm for 20-30min, taking the precipitate, and drying at 40-60 ℃ in a vacuum environment to obtain black phosphorus nanosheets;
(2) preparation of precursor solution
Dispersing 5-8 parts of ammonium molybdate and 5-8 parts of sodium sulfide in 1000-2000 parts of deionized water to obtain a reaction solution, adding 3-5 parts of black phosphorus nanosheet into the reaction solution, and performing ultrasonic treatment for 0.5-1h to obtain a precursor solution.
(3) Preparation of composite materials
Pouring the precursor solution into a reaction kettle, adding 300 parts of 100-plus-one hydrazine hydrate solution into the reaction kettle, carrying out solvothermal reaction for 18-20h at the reaction temperature of 180-plus-one 210 ℃, after the reaction is finished and the sample is naturally cooled, centrifuging for 5-10min at the rotation speed of 10000-plus-one 12000rpm, taking the precipitate, drying at the temperature of 40-60 ℃ in a vacuum environment to obtain the nano molybdenum disulfide-black phosphorus alkene composite material,
the invention also provides a preparation method of the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive, which is prepared according to the following method, and the preparation method comprises the following specific steps:
(1) preparation of black phosphorus nanosheet
Placing 5-10 parts of black phosphorus powder in 20000-plus 30000 parts of N-methylpyrrolidone solvent, performing ultrasonic treatment in a cold water bath for 8-10h, centrifuging at the rotating speed of 3000-plus 5000rpm for 20-30min after ultrasonic treatment, taking the supernatant, centrifuging at the rotating speed of 7000-plus 9000rpm for 20-30min, finally taking the supernatant, centrifuging at the rotating speed of 10000-plus 12000rpm for 20-30min, taking the precipitate, and drying at 40-60 ℃ in a vacuum environment to obtain black phosphorus nanosheets;
(2) preparation of precursor solution
Dispersing 5-8 parts of ammonium molybdate and 5-8 parts of sodium sulfide in 1000-2000 parts of deionized water to obtain a reaction solution, adding 3-5 parts of black phosphorus nanosheet into the reaction solution, and performing ultrasonic treatment for 0.5-1h to obtain a precursor solution.
(3) Preparation of nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive
Pouring the precursor solution into a reaction kettle, adding 300 parts of 100-plus-material hydrazine hydrate solution into the reaction kettle, carrying out solvothermal reaction for 18-20h at the reaction temperature of 180-plus-material 210 ℃, after the reaction is finished and the sample is naturally cooled, centrifuging for 5-10min at the rotation speed of 10000-plus-material 12000rpm, taking the precipitate, drying at the temperature of 40-60 ℃ in a vacuum environment to obtain the nano molybdenum disulfide-black phosphorus alkene composite material, and dispersing the nano molybdenum disulfide-black phosphorus alkene composite material into base oil to obtain the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive.
Finally, the invention also discloses a composite lubricant additive prepared according to the method, wherein the nano molybdenum disulfide structure is a layered structure with the size of 200-400nm and the number of layers of 1-3; the size of the black phosphorus nanosheet structure is 30-500nm, and the number of layers is 3-5.
Compared with the prior art, the invention has the advantages that:
by adopting a solvothermal method, due to Van der Waals force between the molybdenum disulfide and the black phosphorus and full contact of reactants, the generated molybdenum disulfide is easier to load on the black phosphorus nanosheet, and the molybdenum disulfide and the black phosphorus can play a role in synergistic lubrication on a friction interface more efficiently, so that the antifriction lubrication performance under a high-load environment is ensured.
The black phosphorus is prepared by adopting a liquid phase stripping method, so that the black phosphorus is stripped in an N-methyl pyrrolidone solvent, the black phosphorus nanosheet is prevented from being oxidized, and the performance of the black phosphorus nanosheet is not influenced.
Drawings
FIG. 1(a) is a transmission electron microscope image of nano molybdenum disulfide prepared by the method of the present invention;
FIG. 1(b) is a transmission electron microscope image of nano molybdenum disulfide prepared by the method of the present invention;
FIG. 2(a) is a transmission electron microscope image of a black phosphorus nanosheet prepared by the method of the present invention;
FIG. 2(b) is a transmission electron microscope image of a black phosphorus nanosheet prepared by the method of the present invention;
fig. 3 is a friction coefficient diagram of the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive prepared in example 1 under different loads.
Detailed Description
The inventor of the application finds that the combination of the nano molybdenum disulfide and the black phosphorus nanosheet is not ideal enough in the process of research, and finally researches a hydrothermal method through multi-aspect research, which is different from the traditional hydrothermal method, so that the nano molybdenum disulfide and the black phosphorus nanosheet are combined in a hydrothermal reaction kettle under high pressure and high temperature, the intermolecular force can be overcome, and the performances of the nano molybdenum disulfide and the black phosphorus nanosheet are not influenced.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
The embodiment provides a preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive, which is implemented according to the following steps:
(1) preparation of black phosphorus nanosheet
Putting 50mg of black phosphorus powder into 200ml of N-methylpyrrolidone solvent, performing ultrasonic treatment in a cold water bath for 8 hours, centrifuging at the rotating speed of 3000rpm for 20 minutes after ultrasonic treatment, taking the supernatant fluid at the rotating speed of 7000rpm for 20 minutes, taking the supernatant fluid at the rotating speed of 11000rpm for 20 minutes, taking the precipitate, and drying at 60 ℃ in a vacuum environment to obtain black phosphorus nanosheets;
(2) preparation of precursor solution
Dispersing 50mg of ammonium molybdate and 50mg of sodium sulfide in 20ml of deionized water to obtain a reaction solution, adding 30mg of black phosphorus nanosheet into the reaction solution, and carrying out ultrasonic treatment for 1 hour to obtain a precursor solution.
(3) Preparation of nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive
Pouring the precursor solution into a reaction kettle, adding 2ml of hydrazine hydrate into the reaction kettle, carrying out solvothermal reaction for 20h at the reaction temperature of 210 ℃, after the reaction is finished and the sample is naturally cooled, centrifuging at 10000rpm for 8min, taking the precipitate, drying at 60 ℃ in a vacuum environment to obtain a nano molybdenum disulfide-black phosphorus alkene composite material, and dispersing the nano molybdenum disulfide-black phosphorus alkene composite material into base oil to obtain the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive.
Example 2
The embodiment provides a preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive, which is implemented according to the following steps:
(1) preparation of black phosphorus nanosheet
Putting 70mg of black phosphorus powder into 260ml of N-methylpyrrolidone solvent, performing ultrasonic treatment in a cold water bath for 10 hours, centrifuging for 20 minutes at the rotating speed of 4000rpm after ultrasonic treatment, taking the supernatant, centrifuging for 20 minutes at the rotating speed of 8000rpm, finally taking the supernatant, centrifuging for 20 minutes at the rotating speed of 12000rpm, taking the precipitate, and drying at 60 ℃ in a vacuum environment to obtain black phosphorus nanosheets;
(2) preparation of precursor solution
And dispersing 80mg of ammonium molybdate and 80mg of sodium sulfide in 15ml of deionized water to obtain a reaction solution, adding 20mg of black phosphorus nanosheet into the reaction solution, and carrying out ultrasonic treatment for 1 hour to obtain a precursor solution.
(3) Preparation of nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive
Pouring the precursor solution into a reaction kettle, adding 3ml of hydrazine hydrate into the reaction kettle, carrying out solvothermal reaction for 18h at the reaction temperature of 180 ℃, after the reaction is finished and the sample is naturally cooled, centrifuging for 10min at the rotating speed of 12000rpm, taking the precipitate, drying at the temperature of 50 ℃ in a vacuum environment to obtain a nano molybdenum disulfide-black phosphorus alkene composite material, and dispersing the nano molybdenum disulfide-black phosphorus alkene composite material into base oil to obtain the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive.
In order to detect the lubricating performance of the invention, the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive in example 1 adopts ball-disc rotation friction, the material of the small ball is GCr15, and the material of the sample disc is TC4The rotational speed of the testing machine is 150rpm, the load is 8, 11 and 15N, and the data of the antifriction lubricating performance of the composite lubricating oil additive under lubrication under different loads are shown in figure 3.
To test the lubricating performance of the present invention, the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive in example 2, molybdenum disulfide nanosheet (comparative example 2), black phosphorus nanosheet (comparative example 3), nano molybdenum disulfide/graphene oxide nanosheet (comparative example 4), nano graphene oxide/black phosphorus nanosheet (comparative example 5) were dispersed into a liquid paraffin base oil at a concentration of 0.5 wt% and subjected to a comparative friction experiment with the liquid paraffin in comparative example 1:
comparative example 1:
this comparative example presents liquid paraffin alone as a blank to test whether the friction effect was improved after adding the lubricant additive to the base oil.
Selecting a ball disk friction tester, wherein the small ball is a GCr15 bearing steel ball, and the disk is TC4And (4) a disc. The friction parameters are: the load was 8N, the rotational speed was 150rpm, and the rotational diameter was 4 mm. Before the experiment, the ball and the disc are cleaned by petroleum ether and ethanol in an ultrasonic way respectively, so that the surfaces of the ball and the disc are smooth. After the sample is loaded, a small amount of liquid paraffin is dripped on a TC4 disc, the test is stopped after the test time is 30min, and the average friction coefficient is recorded.
Comparative example 2:
the comparative example provides a preparation method of a black phosphorus nanosheet lubricant additive, which is the same as in example 2, to further test the effect of adding the lubricant additive alone.
Selecting a ball disk friction tester, wherein the small ball is a GCr15 bearing steel ball, and the disk is TC4And (4) a disc. The friction parameters are: the load was 8N, the rotational speed was 150rpm, and the rotational diameter was 4 mm. Before the experiment, the ball and the disc are cleaned by petroleum ether and ethanol in an ultrasonic way respectively, so that the surfaces of the ball and the disc are smooth. After the sample is loaded, it is sent to TC4And dripping a molybdenum disulfide oil-based lubricant with the concentration of 0.5 wt% on the disc, stopping the test after the test time is 30min, and recording the average friction coefficient.
Comparative example 3:
this comparative example presents a method of preparing a molybdenum disulfide lubricant additive, the method being the same as in example 2, to further examine the effect of adding the lubricant additive alone.
Selecting a ball disk friction tester, wherein the small ball is a GCr15 bearing steel ball, and the disk is TC4A titanium alloy disk. The friction parameters are: the load was 8N, the rotational speed was 150rpm, and the rotational diameter was 4 mm. Before the experiment, the ball and the disc are cleaned by petroleum ether and ethanol in an ultrasonic way respectively, so that the surfaces of the ball and the disc are smooth. After the sample is loaded, it is sent to TC4And (3) dropwise adding a black phosphorus oil-based lubricant with the concentration of 0.5 wt% on the disc, stopping the test after the test time is 30min, and recording the average friction coefficient.
Comparative example 4:
the method is the same as that in the embodiment 2, the black phosphorus nanosheet is replaced with the prepared graphene oxide nanosheet to prepare the nano molybdenum disulfide/graphene oxide nanosheet composite material, and the nano molybdenum disulfide/graphene oxide nanosheet composite material is dispersed into the base oil by 0.5 wt%, so that the nano molybdenum disulfide/graphene oxide nanosheet lubricating additive is obtained.
Selecting a ball disk friction tester, wherein the small ball is a GCr15 bearing steel ball, and the disk is TC4A titanium alloy disk. The friction parameters are: the load was 8N, the rotational speed was 150rpm, and the rotational diameter was 4 mm. Before the experiment, the ball and the disc are cleaned by petroleum ether and ethanol in an ultrasonic way respectively, so that the surfaces of the ball and the disc are smooth. After the sample is loaded, it is sent to TC4And (3) dropwise adding a nano molybdenum disulfide/graphene oxide nanosheet composite lubricant with the concentration of 0.5 wt% onto the disc, stopping the test after the test time is 30min, and recording the average friction coefficient.
Comparative example 5:
the preparation method comprises the steps of dispersing the prepared graphene oxide nanosheets and the prepared black phosphorus nanosheets into alcohol, mixing the graphene oxide nanosheets and the black phosphorus nanosheets, adding the mixture into a hydrothermal reaction kettle to prepare a nano black phosphorus/graphene oxide nanosheet composite material, and dispersing the nano black phosphorus/graphene oxide nanosheets into base oil by 0.5 wt% to obtain the nano molybdenum disulfide/graphene oxide nanosheet lubricating additive.
A ball disk friction tester is used, the small ball is a GCr15 bearing steel ball, and the disk is TC4A titanium alloy disk. The friction parameters are: the load was 8N, the rotational speed was 150rpm, and the rotational diameter was 4 mm. Before the experiment, the ball and the disc are cleaned by petroleum ether and ethanol in an ultrasonic way respectively, so that the surfaces of the ball and the disc are smooth. After the sample is loaded, it is sent to TC4And (3) dropwise adding the nano graphene oxide/black phosphorus nanosheet composite lubricant with the concentration of 0.5 wt% onto the disc, stopping the test after the test time is 30min, and recording the average friction coefficient.
TABLE-comparison of antifriction lubricating Properties of different lubricating oil additives
As can be seen from the table I, the friction performance of the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating additive prepared by the invention is superior to the independent action of the black phosphorus nanosheet, the base oil and the nano molybdenum disulfide nanosheet, and is superior to the condition that the molybdenum disulfide/graphene oxide nanosheet and the black phosphorus/graphene oxide nanosheet accord with the lubricating additive, so that the molybdenum disulfide and the black phosphorus nanosheet have good friction performance after being compounded.
Claims (2)
1. A preparation method of a nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) the nanometer molybdenum disulfide/black phosphorus nanosheet composite material is prepared according to the following method
Step (1) preparation of black phosphorus nanosheet
Putting the black phosphorus powder into an N-methyl pyrrolidone solvent, performing ultrasonic treatment in a cold water bath for multiple times, centrifuging, and drying in a vacuum environment to obtain black phosphorus nanosheets;
step (2) preparation of precursor solution
Dispersing ammonium molybdate and sodium sulfide in water to obtain a reaction solution, adding the black phosphorus nanosheet into the reaction solution, and performing ultrasonic treatment to obtain a precursor solution;
preparation of the composite Material in step (3)
Adding a reducing agent into the precursor solution, carrying out solvothermal reaction, centrifuging after the reaction is finished, taking out the precipitate, and drying to obtain the nano molybdenum disulfide/black phosphorus nanosheet composite material;
in the step (1), 5-10 parts of black phosphorus powder are placed in 20000-plus 30000 parts of N-methylpyrrolidone solvent, ultrasonic treatment is carried out for 8-10h in a cold water bath, centrifugation is carried out for 20-30min at the rotating speed of 3000-plus 5000rpm after ultrasonic treatment, the supernatant is taken and centrifuged for 20-30min at the rotating speed of 7000-plus 9000rpm, finally the supernatant is taken and centrifuged for 20-30min at the rotating speed of 10000-plus 12000rpm, precipitates are taken and dried at 40-60 ℃ in a vacuum environment, and black phosphorus nanosheets are obtained;
in the step (2), 5-8 parts of ammonium molybdate and 5-8 parts of sodium sulfide are dispersed in 2000 parts of deionized water of 1000-fold to obtain a reaction solution, 3-5 parts of black phosphorus nanosheet is added into the reaction solution, and a precursor solution is obtained after ultrasonic treatment for 0.5-1 h;
in the step (3), the precursor solution is poured into a reaction kettle, 300 parts of hydrazine hydrate solution with 100-;
(2) preparation of composite lubricating oil additive
And dispersing the nano molybdenum disulfide/black phosphorus nanosheet composite material into base oil to obtain the nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive.
2. The nano molybdenum disulfide/black phosphorus nanosheet composite lubricating oil additive prepared according to the preparation method of claim 1, which is characterized in that: the nano molybdenum disulfide structure is a layered structure with the size of 200-400nm and the number of layers of 1-3; the size of the black phosphorus nano-sheet structure is 300-500nm, and the number of layers is 3-5.
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| CN114479985A (en) * | 2022-01-27 | 2022-05-13 | 西安建筑科技大学 | Composite material coated with black phosphorus quantum dots and preparation method and application thereof |
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