CN110295078B - A functional graphene/montmorillonite/modified molybdenum sulfide lubricant additive - Google Patents
A functional graphene/montmorillonite/modified molybdenum sulfide lubricant additive Download PDFInfo
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- CN110295078B CN110295078B CN201910650394.8A CN201910650394A CN110295078B CN 110295078 B CN110295078 B CN 110295078B CN 201910650394 A CN201910650394 A CN 201910650394A CN 110295078 B CN110295078 B CN 110295078B
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- lubricating oil
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- PTISTKLWEJDJID-UHFFFAOYSA-N sulfanylidenemolybdenum Chemical class [Mo]=S PTISTKLWEJDJID-UHFFFAOYSA-N 0.000 title claims abstract 8
- 239000003879 lubricant additive Substances 0.000 title description 5
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000010687 lubricating oil Substances 0.000 claims abstract description 50
- 239000000654 additive Substances 0.000 claims abstract description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 42
- 230000000996 additive effect Effects 0.000 claims abstract description 40
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 21
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000004140 cleaning Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002199 base oil Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- -1 A-1110 Chemical compound 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 claims 1
- 239000002689 soil Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000011056 performance test Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 24
- 239000002131 composite material Substances 0.000 description 15
- 238000002156 mixing Methods 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 241000239226 Scorpiones Species 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 230000001050 lubricating effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 231100000241 scar Toxicity 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 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
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
-
- 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
- C10M2201/10—Compounds containing silicon
- C10M2201/102—Silicates
- C10M2201/103—Clays; Mica; Zeolites
-
- 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
- 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
-
- 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)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
本发明公开了一种功能石墨烯/蒙脱土/改性硫化钼润滑油添加剂，该润滑油添加剂的原料为氧化石墨烯、硫化钼、蒙脱土和硅烷偶联剂，通过采用硅烷偶联剂处理氧化石墨烯和硫化钼，将二者与蒙脱土混合加热得到该润滑油添加剂，其中氧化石墨烯:硫化钼:蒙脱土的质量比例为1:(0.25‑4):(0.5‑8)。对该润滑油添加剂进行摩擦学性能测试，极少的添加量就能够明显降低摩擦系数，有着极为优异的减摩抗磨能力。
The invention discloses a functional graphene/montmorillonite/modified molybdenum sulfide lubricating oil additive. The raw materials of the lubricating oil additive are graphene oxide, molybdenum sulfide, montmorillonite and silane coupling agent. agent treatment graphene oxide and molybdenum sulfide, the two are mixed and heated with montmorillonite to obtain this lubricating oil additive, wherein graphene oxide: molybdenum sulfide: the mass ratio of montmorillonite is 1: (0.25-4): (0.5- 8). The tribological performance test of the lubricating oil additive shows that a very small amount of addition can significantly reduce the friction coefficient and has excellent anti-friction and anti-wear ability.
Description
Technical Field
The invention relates to the technical field of lubricating oil additives, in particular to a functional graphene/montmorillonite/modified molybdenum sulfide lubricating oil additive.
Background
Chinese patent CN201711383769 discloses a lubricating oil additive of functionalized graphene loaded montmorillonite, a preparation method and an application thereof, and although the lubricating oil additive has extremely excellent dispersion performance in lubricating oil and certain antifriction and repair capacity, the friction coefficient is not low enough to reduce.
Molybdenum disulfide (MoS)2) The transition metal sulfide is a typical transition metal sulfide, is composed of two layers of sulfur atoms and one layer of molybdenum atom in the middle to form a sandwich structure, is an excellent lubricating material, and is widely applied to the fields of lubricating liquid additives, self-lubricating coatings, solid lubricants and the like [ Beacon, Xifeng, tungsten disulfide lubricating additive tribological property research current situation, chemical man-hour journal, 2017,31(12):36-39.]Although molybdenum sulfide has excellent friction reducing properties, the reduction in the coefficient of friction is not sufficiently low, and it has not been reported that molybdenum sulfide has a repairing ability for friction surfaces. And the molybdenum sulfide composite material obtains technical attention due to the unique application advantages, not only maintains the excellent performance of the raw materials, but also effectively overcomes the defect of a single material. Functional graphene prepared by adopting methodThe montmorillonite/modified molybdenum sulfide composite lubricating oil additive integrates the excellent performances of three materials, and not only can effectively reduce the friction coefficient, but also can reduce the damage of a wear surface; and a self-repairing film is formed on the friction surface, particularly, due to the introduction of graphene, the hardness of the self-repairing film is remarkably improved compared with that of a friction pair, and the self-repairing film has further protection capability on the friction surface so that the friction surface is more wear-resistant.
Disclosure of Invention
The invention aims to provide a functional graphene/montmorillonite/modified molybdenum sulfide lubricating oil additive, a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme: a functional graphene/montmorillonite/modified molybdenum sulfide lubricant additive is prepared by mixing functional graphene oxide, modified molybdenum sulfide and montmorillonite in a mass ratio of 1 (0.25-4) to (0.5-8).
The lubricating oil additive is prepared by the following steps:
(1) preparing a dispersion solution of graphene oxide by taking graphene oxide as a raw material, adding a silane coupling agent, reacting for 1-6h at 25-100 ℃, and separating and cleaning to obtain functional graphene oxide;
(2) adding a silane coupling agent into the dispersion liquid of the molybdenum sulfide, reacting for 1-8h at 25-100 ℃, separating and cleaning to obtain modified molybdenum sulfide;
(3) mixing and stirring the modified molybdenum sulfide, the montmorillonite and the dispersion liquid of the functional graphene oxide for 0.5-2h, reacting for 1-5h at the temperature of 100-180 ℃, and separating and cleaning to obtain the lubricating oil additive.
Preferably, in the step (1) and the step (2), the silane coupling agent is any one of A-1100, A-1110, A-1120 and KBM-602.
Preferably, in the step (1), the mass ratio of the graphene oxide to the silane coupling agent is 1: 24-200.
Preferably, in the step (2), the mass ratio of the molybdenum sulfide to the silane coupling agent is 1: 50-200.
Preferably, the mass ratio of the graphene oxide to the molybdenum sulfide to the montmorillonite is 1 (0.25-4) to (0.5-8).
Preferably, in the step (1) to (3), the dispersion liquid of graphene oxide, the dispersion liquid of molybdenum sulfide and the dispersion liquid of functional graphene oxide are the same in each dispersion liquid, and include ethanol or water.
Preferably, in steps (1) to (3), the heating method is reflux heating or autoclave heating reaction.
The functional graphene/montmorillonite/molybdenum sulfide lubricating oil additive is applied, and the concentration of the additive in the lubricating oil is 0.011-0.133 wt%; the lubricating oil can be any brand of lubricating oil, such as Kunlun Scorpio F5000, SF15W-40 type lubricating oil and great wall SJ10W-40 lubricating oil, and can also be base oil such as mineral base oil or synthetic base oil.
By means of the technical scheme, the functional graphene/montmorillonite/modified molybdenum sulfide lubricating oil additive prepared by the invention has the following advantages:
1) simple operation, easily obtained raw materials and low cost.
2) The three components in the additive are chemically bonded and grown together, so that the aggregation in single use is inhibited, and the additive has excellent dispersion stability and strong mutual synergistic effect.
3) The three components in the additive have a certain anti-friction effect, and due to the excellent mechanical properties of the graphene component, the composite material has remarkable anti-wear and anti-friction effects and intelligent repair effects, and can effectively improve the hardness of a wear surface.
Drawings
FIG. 1 is a flow chart of the preparation of functional graphene/montmorillonite/modified molybdenum sulfide composite lubricant additive.
Detailed Description
The present invention will be described in detail below with reference to specific examples, but the present invention is not limited thereto in any way.
With reference to fig. 1, the preparation process of the functional graphene/montmorillonite/modified molybdenum sulfide composite lubricating oil additive according to the present invention is shown in the following example.
Example one
(1) First, 160g of an aqueous dispersion of graphene oxide having a concentration of 0.025 wt% was prepared. Then, 6mL of the silane coupling agent (A-1100) was added, and the mixture was magnetically stirred at room temperature for 1 hour. Finally, the mixture is transferred into a flask and is reacted for 2 hours in a water bath at 80 ℃. And after separation and cleaning, adding a proper amount of deionized water to obtain the aqueous dispersion of the functional graphene oxide.
(2) Weighing 0.04g of molybdenum sulfide, adding water, uniformly stirring to obtain a molybdenum sulfide water dispersion, adding 6mL of silane coupling agent (A-1100), stirring for 1h at room temperature, heating for 2h at 80 ℃, separating, and cleaning to obtain the modified molybdenum sulfide.
(3) Mixing and stirring the modified molybdenum sulfide, 0.16g of montmorillonite and the aqueous dispersion of the functional graphene oxide for 1 hour; transferring the mixture to a reaction kettle for hydrothermal reaction at 120 ℃ for 4 hours, standing and cooling; and separating, cleaning and drying to obtain the functional graphene/montmorillonite/modified molybdenum sulfide composite lubricating oil additive.
(4) Evaluation of tribological Properties
The prepared functional graphene/montmorillonite/modified molybdenum sulfide composite lubricating oil additive is mixed with Kunlun scorpion SF15W-40 lubricating oil according to different proportions. A friction and wear test is carried out by using an MRS-10G four-ball friction and wear testing machine, and a GCr steel ball with the hardness of 770HV and the diameter of 12.7mm is used for testing. And (3) testing conditions are as follows: load 197N, speed 600rpm, test time 3600 s. The friction coefficient and the wear-scar diameter of the lubricant additive at different concentrations in the example are shown in table 1, and the test results of the simple graphene oxide, montmorillonite and molybdenum sulfide at the concentration of 0.044 wt% are shown for comparison, so that the composite lubricant additive prepared by the single-component material has excellent lubricating performance, the friction coefficient can be reduced by about 62.50% and the wear-scar diameter can be reduced by about 18.18% compared with the simple lubricant. Meanwhile, microhardness test is carried out on the grinding spot surface, and the test result is shown in table 2, so that the use of the composite material lubricating oil additive can be seen, and the hardness of the grinding spot surface is improved by 16.88 percent compared with that of the steel ball.
Example two
(1) First, 160g of an aqueous dispersion of graphene oxide having a concentration of 0.025 wt% was prepared. Then, 1mL of a silane coupling agent (A-1110) was added and the reaction was carried out at 25 ℃ for 5 hours. And after separation and cleaning, adding a proper amount of deionized water to obtain the aqueous dispersion of the functional graphene oxide.
(2) 0.01g of molybdenum sulfide is weighed, added with water and stirred uniformly to obtain an aqueous dispersion of molybdenum sulfide, 0.5mL of silane coupling agent (A-1110) is added to react for 8h at 25 ℃, and the modified molybdenum sulfide is obtained after separation and cleaning.
(3) Mixing and stirring the modified molybdenum sulfide, 0.02g of montmorillonite and the aqueous dispersion of the functional graphene oxide for 0.5 h; transferring the mixture into a high-pressure kettle for hydrothermal reaction at 200 ℃ for 1h, standing and cooling; and separating, cleaning and drying to obtain the functional graphene/montmorillonite/modified molybdenum sulfide composite lubricating oil additive.
(4) Evaluation of tribological Properties
The prepared functional graphene/montmorillonite/modified molybdenum sulfide composite lubricating oil additive is mixed with 0.044 wt% of Kunlun scorpion SF15W-40 lubricating oil. A friction and wear test is carried out by using an MRS-10G four-ball friction and wear testing machine, and a GCr steel ball with the hardness of 770HV and the diameter of 12.7mm is used for testing. And (3) testing conditions are as follows: load 197N, speed 600rpm, time 3600 s. The test results are given in table 1.
EXAMPLE III
(1) First, 160g of an ethanol dispersion of graphene oxide having a concentration of 0.025 wt% was prepared. Then, 8mL of a silane coupling agent (A-1120) was added, and the reaction was refluxed at 80 ℃ for 1 hour. And separating, cleaning, and adding a proper amount of ethanol to obtain an ethanol dispersion liquid of the functional graphene oxide.
(2) Weighing 0.16g of molybdenum sulfide, adding ethanol, uniformly stirring to obtain ethanol dispersion of molybdenum sulfide, adding 16mL of silane coupling agent (A-1120), reacting at 60 ℃ for 3h, separating, and cleaning to obtain the modified molybdenum sulfide.
(3) Mixing and stirring the modified molybdenum sulfide, 0.32g of montmorillonite and the ethanol dispersion liquid of the functional graphene oxide for 2 hours; transferring the mixture into a flask, heating and refluxing the mixture at 100 ℃ for 5 hours, standing and cooling the mixture; and separating, cleaning and drying to obtain the functional graphene/montmorillonite/modified molybdenum sulfide composite lubricating oil additive.
(4) Evaluation of tribological Properties
The prepared functional graphene/montmorillonite/modified molybdenum sulfide composite lubricating oil additive is mixed with 0.044 wt% of Kunlun scorpion SF15W-40 lubricating oil. A friction and wear test is carried out by using an MRS-10G four-ball friction and wear testing machine, and a GCr steel ball with the hardness of 770HV and the diameter of 12.7mm is used for testing. And (3) testing conditions are as follows: load 197N, speed 600rpm, time 3600 s. The test results are given in table 1.
Example four
(1) First, 160g of an ethanol dispersion of graphene oxide having a concentration of 0.025 wt% was prepared. Then, 3mL of a silane coupling agent (KBM-602) was added, and the mixture was transferred to an autoclave at 95 ℃ for 4 hours. And separating, cleaning, separating and cleaning, and then adding a proper amount of ethanol to obtain the ethanol dispersion liquid of the functional graphene oxide.
(2) Weighing 0.08g of molybdenum sulfide, adding ethanol, stirring the mixture to be uniform, obtaining ethanol dispersion of the molybdenum sulfide, adding 16mL of silane coupling agent (KBM-602), transferring the mixture to a reaction kettle to react for 1 hour at 100 ℃, and separating and cleaning the mixture to obtain the modified molybdenum sulfide.
(3) Mixing and stirring the modified molybdenum sulfide, 0.24g of montmorillonite and the ethanol dispersion liquid of the functional graphene oxide for 2 hours; transferring to a high-pressure kettle, reacting for 5h at 150 ℃, standing and cooling; and separating, cleaning and drying to obtain the functional graphene/montmorillonite/modified molybdenum sulfide composite lubricating oil additive.
(4) Evaluation of tribological Properties
The prepared functional graphene/montmorillonite/modified molybdenum sulfide composite lubricating oil additive is mixed with 0.044 wt% of Kunlun scorpion SF15W-40 lubricating oil. A friction and wear test is carried out by using an MRS-10G four-ball friction and wear testing machine, and a GCr steel ball with the hardness of 770HV and the diameter of 12.7mm is used for testing. And (3) testing conditions are as follows: load 197N, speed 600rpm, time 3600 s. The test results are given in table 1.
TABLE 1 Friction coefficient and wear scar diameter of different additives in lubricating oil
TABLE 2 micro-hardness test results for the abraded surfaces
Claims (8)
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| Title |
|---|
| Synergistic lubricating behaviors of graphene and MoS2 dispersed;Yufu Xu;《Wear》;20150930;第342-343卷;第1-13页 * |
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| Publication number | Publication date |
|---|---|
| CN110295078A (en) | 2019-10-01 |
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