CN117887499A - High-temperature-resistant environment-friendly lubricating oil and preparation method thereof - Google Patents
High-temperature-resistant environment-friendly lubricating oil and preparation method thereof Download PDFInfo
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- 239000010687 lubricating oil Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 180
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 144
- 239000004005 microsphere Substances 0.000 claims abstract description 65
- -1 graphene compound Chemical class 0.000 claims abstract description 56
- 239000002199 base oil Substances 0.000 claims abstract description 36
- 239000002131 composite material Substances 0.000 claims abstract description 33
- 239000000654 additive Substances 0.000 claims abstract description 23
- 230000000996 additive effect Effects 0.000 claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 15
- 125000000217 alkyl group Chemical group 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- 238000001694 spray drying Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 11
- 239000003963 antioxidant agent Substances 0.000 claims description 10
- 230000003078 antioxidant effect Effects 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000003444 phase transfer catalyst Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000944 linseed oil Substances 0.000 claims description 7
- 235000021388 linseed oil Nutrition 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000006722 reduction reaction Methods 0.000 claims description 7
- 239000004359 castor oil Substances 0.000 claims description 6
- 235000019438 castor oil Nutrition 0.000 claims description 6
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 5
- HNTGIJLWHDPAFN-UHFFFAOYSA-N 1-bromohexadecane Chemical compound CCCCCCCCCCCCCCCCBr HNTGIJLWHDPAFN-UHFFFAOYSA-N 0.000 claims description 5
- WSULSMOGMLRGKU-UHFFFAOYSA-N 1-bromooctadecane Chemical compound CCCCCCCCCCCCCCCCCCBr WSULSMOGMLRGKU-UHFFFAOYSA-N 0.000 claims description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000005642 Oleic acid Substances 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- 239000003112 inhibitor Substances 0.000 claims description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 235000019482 Palm oil Nutrition 0.000 claims description 3
- 235000019483 Peanut oil Nutrition 0.000 claims description 3
- 235000019484 Rapeseed oil Nutrition 0.000 claims description 3
- 235000019486 Sunflower oil Nutrition 0.000 claims description 3
- 235000005687 corn oil Nutrition 0.000 claims description 3
- 239000002285 corn oil Substances 0.000 claims description 3
- 235000012343 cottonseed oil Nutrition 0.000 claims description 3
- 239000002385 cottonseed oil Substances 0.000 claims description 3
- 239000002540 palm oil Substances 0.000 claims description 3
- 239000000312 peanut oil Substances 0.000 claims description 3
- 239000003549 soybean oil Substances 0.000 claims description 3
- 235000012424 soybean oil Nutrition 0.000 claims description 3
- 239000002600 sunflower oil Substances 0.000 claims description 3
- 230000001050 lubricating effect Effects 0.000 abstract description 11
- 230000000052 comparative effect Effects 0.000 description 14
- 239000003921 oil Substances 0.000 description 12
- 235000019198 oils Nutrition 0.000 description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 7
- 238000001237 Raman spectrum Methods 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000013556 antirust agent Substances 0.000 description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 4
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical class CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920013639 polyalphaolefin Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical group [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 3
- QBVXKDJEZKEASM-UHFFFAOYSA-M tetraoctylammonium bromide Chemical compound [Br-].CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC QBVXKDJEZKEASM-UHFFFAOYSA-M 0.000 description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 238000006065 biodegradation reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940076810 beta sitosterol Drugs 0.000 description 1
- LGJMUZUPVCAVPU-UHFFFAOYSA-N beta-Sitostanol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CC)C(C)C)C1(C)CC2 LGJMUZUPVCAVPU-UHFFFAOYSA-N 0.000 description 1
- NJKOMDUNNDKEAI-UHFFFAOYSA-N beta-sitosterol Natural products CCC(CCC(C)C1CCC2(C)C3CC=C4CC(O)CCC4C3CCC12C)C(C)C NJKOMDUNNDKEAI-UHFFFAOYSA-N 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- WCLNGBQPTVENHV-MKQVXYPISA-N cholesteryl nonanoate Chemical compound C([C@@H]12)C[C@]3(C)[C@@H]([C@H](C)CCCC(C)C)CC[C@H]3[C@@H]1CC=C1[C@]2(C)CC[C@H](OC(=O)CCCCCCCC)C1 WCLNGBQPTVENHV-MKQVXYPISA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- RQVGZVZFVNMBGS-UHFFFAOYSA-N n-octyl-n-phenylaniline Chemical compound C=1C=CC=CC=1N(CCCCCCCC)C1=CC=CC=C1 RQVGZVZFVNMBGS-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- INFDPOAKFNIJBF-UHFFFAOYSA-N paraquat Chemical compound C1=C[N+](C)=CC=C1C1=CC=[N+](C)C=C1 INFDPOAKFNIJBF-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- 229950005143 sitosterol Drugs 0.000 description 1
- 150000003900 succinic acid esters Chemical class 0.000 description 1
- 235000020238 sunflower seed Nutrition 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
- C10M125/02—Carbon; Graphite
-
- 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
- C10M2201/04—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
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/283—Esters of polyhydroxy compounds
- C10M2207/2835—Esters of polyhydroxy compounds used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/401—Fatty vegetable or animal oils used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/402—Castor oils
-
- 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
-
- 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
- C10N2030/08—Resistance to extreme temperature
-
- 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
- C10N2030/64—Environmental friendly compositions
Landscapes
- 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
A high-temperature-resistant environment-friendly lubricating oil and a preparation method thereof belong to the technical field of lubricating oil. The high-temperature-resistant environment-friendly lubricating oil comprises the following components in percentage by mass: 90-98% of base oil, 0.01-0.05% of graphene compound and 1.99-9.95% of auxiliary additive; the graphene composite is a composite of modified flaky graphene and modified graphene microspheres, and the mass ratio of the modified flaky graphene to the modified graphene microspheres is 2:1-3:1. the lubricating oil disclosed by the invention is environment-friendly, has excellent lubricating property and extreme pressure bearing capacity, is stable in high-temperature performance, and is suitable for long-time use under high-temperature severe conditions.
Description
Technical Field
The invention belongs to the technical field of lubricating oil, and particularly relates to high-temperature-resistant environment-friendly lubricating oil and a preparation method thereof.
Background
Lubricating oils are liquid or semisolid lubricants used in various types of automobiles and mechanical equipment to reduce friction and protect machinery and workpieces, and mainly play roles in lubrication, cooling, rust prevention, cleaning, sealing, buffering and the like. In recent years, with the increasing enhancement of service conditions of various mechanical parts, new requirements are put on lubricating performance of lubricating oil, in particular high temperature resistance and extreme pressure bearing capacity. In addition, due to the improvement of environmental protection requirements, the lubricating oil needs to have good environmental protection performance.
At present, all finished lubricating oils are composed of base oil and additives, wherein the base oil is the main component of the lubricating oil and determines the basic properties of the lubricating oil, and the additives can make up for and improve the defects of the base oil in terms of performance and endow certain new performances. The base oil of the existing environment-friendly lubricating oil is mainly biological base oil, but the application of the base oil is limited due to the poor oxidation resistance and the compatibility of the base oil with additives. In addition, the addition of the additive has an influence on the biodegradability of the base oil itself, and in particular, has a detrimental effect on active microorganisms or enzymes in the degradation process of the base oil, thereby affecting the biodegradation rate of the base oil.
Patent CN105695065A discloses an energy-saving and environment-friendly gasoline engine lubricating oil, which comprises base oil and additives, wherein the base oil is total synthetic poly alpha-olefin base oil, and the additives comprise a viscosity index improver, a composite detergent, a composite dispersant, a composite antioxidant anticorrosive agent, a metal passivating agent, an antirust agent and an anti-foaming agent. The lubricating oil adopts single poly alpha-olefin, so that the environmental protection is limited; in addition, when the mechanical surfaces are in contact, a buffer effect cannot be formed in an oil film, so that the oil film is easy to break, and the lubrication protection effect is reduced. Patent CN106167730B discloses an environment-friendly antiwear lubricating oil, which is prepared from modified base oil, succinic acid ester, detergent, octyl diphenylamine, defoamer, antifriction antiwear synergist, dodecadiacid, beta-sitosterol, cholesterol nonanoate, castor oil and auxiliary additive, wherein the modified base oil is prepared by mixing poly alpha-olefin and sunflower seed oil, and the antifriction antiwear performance and extreme pressure performance of the lubricating oil are still to be further improved although the environment-friendly performance of the lubricating oil is improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide high-temperature-resistant environment-friendly lubricating oil and a preparation method thereof. The lubricating oil is environment-friendly, has excellent lubricating property and extreme pressure bearing capacity, has stable high-temperature performance, and is suitable for long-time use under high-temperature severe conditions.
In order to achieve the above object, according to one aspect of the present invention, there is provided a high temperature resistant environment friendly lubricating oil comprising the following components in mass percent: 90-98% of base oil, 0.01-0.05% of graphene compound and 1.99-9.95% of auxiliary additive; the graphene composite is a composite of modified flaky graphene and modified graphene microspheres, and the mass ratio of the modified flaky graphene to the modified graphene microspheres is 2:1-3:1.
In some embodiments, the base oil is a complex of a biobase oil, a low viscosity trimethylol propane ester, and a high viscosity trimethylol propane ester, the biobase oil, the low viscosity trimethylol propane ester, and the high viscosity trimethylol propane ester having a mass ratio of 7.5 to 8:1-1.5:1.
In some embodiments, the low viscosity trimethylolpropane esters have a kinematic viscosity of 3.9 to 4.0mm 2/s at 100 ℃ and a viscosity index of 132 to 135.
In some embodiments, the high viscosity trimethylolpropane esters have a kinematic viscosity of 9.0 to 9.5mm 2/s at 100 ℃ and a viscosity index of 185 to 190.
In some embodiments, the biobased oil comprises any one or more of linseed oil, soybean oil, sunflower oil, cottonseed oil, castor oil, corn oil, rapeseed oil, peanut oil, or palm oil.
In some embodiments, the modified graphene flakes are reduced graphene oxides modified with a brominated alkyl compound comprising any one or more of 1-bromohexadecane, 1-bromooctadecane, and 1-bromodocosyl.
In some embodiments, the modified graphene microspheres are long chain alkyl acid modified graphene microspheres, the long chain alkyl acid being oleic acid and/or stearic acid.
In some embodiments, the auxiliary additive includes any one or more of an antioxidant, a dispersant, a rust inhibitor.
According to another aspect of the invention, the invention also provides a preparation method of the high-temperature-resistant environment-friendly lubricating oil, which comprises the following steps:
(1) Preparing a graphene composite: dispersing graphene oxide in deionized water, carrying out ultrasonic and homogenizing treatment, adding a reducing agent, a brominated alkyl compound and a phase transfer catalyst, reacting for 12-24 hours at 80-90 ℃, filtering, and drying in an oven to obtain the modified flaky graphene; dispersing graphene oxide in deionized water, and carrying out ultrasonic and homogenizing treatment to obtain a dispersion liquid; spray drying the dispersion liquid, and carrying out high-temperature thermal reduction reaction at 300-350 ℃ to obtain reduced graphene microspheres; adding the reduced graphene microspheres into a solvent in which long-chain alkyl acid is dispersed, performing ultrasonic dispersion, then dropwise adding concentrated sulfuric acid, reacting for 6-12 hours at 80-90 ℃, filtering, and drying in an oven to obtain the modified graphene microspheres; the modified flaky graphene and the modified graphene microsphere are mixed according to the mass ratio of 2:1-3:1, mixing to obtain the graphene compound;
(2) Heating the base oil to 50-60 ℃, adding the graphene compound and the auxiliary additive while stirring, preserving heat for 1-2h, naturally cooling to room temperature, and stopping stirring to obtain the high-temperature-resistant environment-friendly lubricating oil.
In some embodiments, in step (1), the mass ratio of graphene oxide, reducing agent, brominated alkyl compound, and phase transfer catalyst is 1:0.2-0.5:1-2:1, a step of; the mass ratio of the reduced graphene microspheres to the long-chain alkyl acid to the concentrated sulfuric acid is 1:1-2:1-2.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention provides high-temperature-resistant environment-friendly lubricating oil, which is prepared by adding a specific content of a compound of modified flaky graphene and modified graphene microspheres into the lubricating oil, and the two substances are synergistic, so that the lubricating oil has excellent lubricating performance and extreme pressure bearing capacity, is stable in high-temperature performance and is suitable for long-time use under high-temperature harsh conditions.
(2) According to the invention, by selecting base oils with different types and viscosities for compounding, the lubricity of the lubricating oil, particularly the lubricating property under high temperature conditions, is further improved, so that the lubricating oil is environment-friendly and has excellent bearing capacity and oil film strength.
(3) The preparation method of the lubricating oil is simple, and the product is green and environment-friendly and has good application prospect.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
Herein, when embodiments or examples are described, it should be understood that they are not intended to limit the invention to these embodiments or examples. On the contrary, all alternatives, modifications, and equivalents of the methods and materials described herein are intended to be included within the scope of the invention as defined by the appended claims.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The invention provides high-temperature-resistant environment-friendly lubricating oil which comprises base oil, a graphene compound and an auxiliary additive, wherein the graphene compound is a modified flaky graphene and modified graphene microsphere compound.
In the present invention, the mass percentage of the base oil is 90-98% based on the total amount of the lubricating oil, and it is understood that the mass percentage may be any specific value of 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99% or any value in the range of 90-98%. In some embodiments, the base oil is a complex of a biobase oil, a low viscosity trimethylol propane ester, and a high viscosity trimethylol propane ester, the biobase oil, the low viscosity trimethylol propane ester, and the high viscosity trimethylol propane ester having a mass ratio of 7.5 to 8:1-1.5:1, preferably 7.5:1.5:1. in some embodiments, the biobased oil comprises any one or more of linseed oil, soybean oil, sunflower oil, cottonseed oil, castor oil, corn oil, rapeseed oil, peanut oil, or palm oil. In some embodiments, the low viscosity trimethylolpropane esters have a kinematic viscosity of 3.9 to 4.0mm 2/s at 100 ℃ and a viscosity index of 132 to 135. In some embodiments, the high viscosity trimethylolpropane esters have a kinematic viscosity of 9.0 to 9.5mm 2/s at 100 ℃ and a viscosity index of 185 to 190. The inventor discovers that the lubricating property of the lubricating oil, particularly the lubricating property after high-temperature (above 150 ℃) treatment can be further improved by selecting the compound base oil disclosed by the invention, so that the lubricating oil is environment-friendly and has excellent high-temperature resistance and extreme pressure bearing capacity.
In the invention, the mass percentage of the graphene composite is 0.01-0.05% based on the total weight of the lubricating oil, and it is understood that the mass percentage can be any specific value in 0.01%, 0.02%, 0.03%, 0.04%, 0.05% or any value in the range of 0.01-0.05%. In some embodiments, in the graphene composite, the mass ratio of the modified graphene flakes and modified graphene microspheres is 2:1-3:1, it will be appreciated that the mass ratio may be 2: 1. 2.1: 1. 2.2: 1. 2.3: 1. 2.4: 1. 2.5: 1. 2.6: 1. 2.7: 1. 2.8: 1. 2.9: 1. 3:1 or 2:1-3: any number within the range of 1. The inventor of the invention discovers that the quality ratio of the modified flaky graphene and the modified graphene microsphere can ensure that the comprehensive performance of the graphene composite is optimal, and the quality ratio is lower or higher, which leads to imperfect special structure of intercalation distribution between the flaky graphene and the graphene microsphere, and further leads to poor effect of sharing shearing force between two friction pairs through deformation and sliding, and poor antifriction and grinding performance.
In some embodiments, the modified graphene flakes are reduced graphene oxides modified with a brominated alkyl compound comprising any one or more of 1-bromohexadecane, 1-bromooctadecane, and 1-bromodocosyl. The brominated alkyl compound can be grafted onto graphene oxide by a simple and efficient method, so that the lipophilicity of the graphene oxide is improved, and the dispersion stability of the graphene oxide in lubricating oil is further improved. In some embodiments, the modified graphene flakes have an overall platelet size in the range of 400-700nm. The invention further controls the overall size of the modified flaky graphene to be in a nanometer level, so that the graphene compound can be stably dispersed in lubricating oil. In some embodiments, the modified graphene flakes satisfy the relationship: i D/IG is more than or equal to 0.96 and less than or equal to 0.98, wherein I D is the intensity of 1350cm -1 peak in the Raman spectrum, and I G is the intensity of 1590cm -1 peak in the Raman spectrum. Surprisingly, the inventor of the invention found that the modified flaky graphene can be ensured to have excellent dispersibility, high temperature resistance and antifriction and antiwear properties by controlling the I D/IG value of the modified flaky graphene, namely controlling the reduction degree and grafting amount of the modified flaky graphene. If the I D/IG value is too high, the defect degree of the modified flaky graphene is too high, and the high temperature resistance and antifriction and antiwear properties of the modified flaky graphene are reduced; if the I D/IG value is too low, the defect degree of the modified flaky graphene is low, the dispersibility of the modified flaky graphene is reduced, and the precipitation layering phenomenon can occur after long-time use.
In some embodiments, the modified graphene microspheres are long chain alkyl acid modified graphene microspheres, the long chain alkyl acid being oleic acid and/or stearic acid. In some embodiments, the modified graphene microspheres have an average particle size of 100-200nm.
In the invention, the mass percentage of the auxiliary additive is 1.99-9.95% based on the total weight of the lubricating oil. In some embodiments, the auxiliary additive includes any one or more of an antioxidant, a dispersant, a rust inhibitor. Specifically, the antioxidant, the dispersant and the rust inhibitor can be of conventional types in the field, and are preferably of green and environment-friendly types.
According to another aspect of the invention, the invention also provides a preparation method of the high-temperature-resistant environment-friendly lubricating oil, which comprises the following steps:
(1) Preparing a graphene composite: dispersing graphene oxide in deionized water, carrying out ultrasonic and homogenizing treatment, adding a reducing agent, a brominated alkyl compound and a phase transfer catalyst, reacting for 12-24 hours at 80-90 ℃, filtering, and drying in an oven to obtain the modified flaky graphene; dispersing graphene oxide in deionized water, and carrying out ultrasonic and homogenizing treatment to obtain a dispersion liquid; spray drying the dispersion liquid, and carrying out high-temperature thermal reduction reaction at 300-350 ℃ to obtain reduced graphene microspheres; adding the reduced graphene microspheres into a solvent in which long-chain alkyl acid is dispersed, performing ultrasonic dispersion, then dropwise adding concentrated sulfuric acid, reacting for 6-12 hours at 80-90 ℃, filtering, and drying in an oven to obtain the modified graphene microspheres; the modified flaky graphene and the modified graphene microsphere are mixed according to the mass ratio of 2:1-3:1, mixing to obtain the graphene compound;
(2) Heating the base oil to 50-60 ℃, adding the graphene compound and the auxiliary additive while stirring, preserving heat for 1-2h, naturally cooling to room temperature, and stopping stirring to obtain the high-temperature-resistant environment-friendly lubricating oil.
According to the preparation method provided by the invention, in some embodiments, the specific process for preparing the modified flaky graphene is as follows: dispersing graphene oxide in deionized water, carrying out ultrasonic and homogenizing treatment, adding a reducing agent, a brominated alkyl compound and a phase transfer catalyst, reacting for 12-24 hours at 80-90 ℃, filtering, and drying in an oven to obtain the modified flaky graphene. In some embodiments, in preparing the modified graphene flakes, the graphene oxide, reducing agent, brominated alkyl compound, and phase transfer catalyst are present in a mass ratio of 1:0.2-0.5:1-2:1. in some embodiments, the reducing agent is sodium hydroxide and/or potassium hydroxide; the phase transfer catalyst is tetrabutylammonium bromide and/or tetraoctylammonium bromide.
According to the preparation method provided by the invention, in some embodiments, the specific process for preparing the modified graphene microsphere is as follows: dispersing graphene oxide in deionized water, and carrying out ultrasonic and homogenizing treatment to obtain a dispersion liquid; spray drying the dispersion liquid, and carrying out high-temperature thermal reduction reaction at 300-350 ℃ to obtain reduced graphene microspheres; and adding the reduced graphene microspheres into a solvent in which long-chain alkyl acid is dispersed, performing ultrasonic dispersion, then dropwise adding concentrated sulfuric acid, reacting for 6-12 hours at 80-90 ℃, filtering, and drying in an oven to obtain the modified graphene microspheres. In some embodiments, the concentration of the dispersion is 1-5mg/mL. In some embodiments, the spray drying may be performed using a conventional spray dryer, the spray drying serving to obtain graphene oxide microspheres. The specific conditions of the spray drying may be: the inlet temperature of the spray dryer is 180-190 ℃, the temperature of the discharge outlet is 90-110 ℃, and the spray drying time is 2-3h. In some embodiments, the reduced graphene microspheres, long chain alkyl acid, and concentrated sulfuric acid have a mass ratio of 1:1-2:1-2, the concentrated sulfuric acid can be intercalated into the reduced graphene microsphere to provide a space for the full progress of the esterification reaction between the long-chain alkyl acid and the hydroxyl on the reduced graphene microsphere, and meanwhile, the introduced long-chain alkane generates steric hindrance and the fluffiness is increased. In some embodiments, the solvent comprises at least one or more of cyclohexane, n-hexane, n-pentane, and n-heptane, the solvent acting to disperse an amount of the long chain alkyl acid.
According to the preparation method provided by the invention, in some embodiments, the mass ratio of the modified flaky graphene to the modified graphene microsphere is 2:1-3:1, mixing to obtain the graphene compound. The mixing process is not particularly limited, and a mixing process conventional in the art can be adopted, so long as the modified flaky graphene and the modified graphene microsphere can be uniformly mixed.
In the invention, raw material graphene oxide can be purchased in a conventional market or self-made mode, and the sheet size of the raw material graphene oxide is 0.5-3 mu m. In the invention, a homogenizer is preferably used for homogenizing, and the homogenizing function is to crush the graphene oxide to obtain smaller-sized graphene oxide, so that the smaller-sized graphene oxide has larger specific surface area, a better foundation is provided for subsequent grafting modification, and meanwhile, the smaller-sized graphene oxide has better dispersion stability in lubricating oil. Preferably, the overall size of the smaller-sized graphene oxide obtained after homogenization may be 200-400nm. More preferably, the specific condition of homogenization may be high-speed dispersion at a rotation speed of 4000-5000r/min for 10-20min.
According to the preparation method provided by the invention, in some embodiments, the base oil is heated to 50-60 ℃, the graphene compound and the auxiliary additive are added while stirring, the temperature is kept for 1-2h, the mixture is naturally cooled to room temperature, and stirring is stopped, so that the high-temperature-resistant environment-friendly lubricating oil is obtained. Preferably, the biobase oil, the low viscosity trimethylolpropane ester and the high viscosity trimethylolpropane ester are uniformly mixed and then heated to 50-60 ℃.
The present invention will be described in detail by examples. It should be understood that the following examples are illustrative only and are not intended to limit the invention.
Unless otherwise specified, the raw materials in the examples and comparative examples of the present invention are all obtained from the general market, and specific information is as follows:
Graphene oxide, with a platelet size of 0.5-3 μm and a platelet thickness of 1nm, purchased from nanjing Jicang nanotechnology Co., ltd; 1-bromooctadecane, 1-bromohexadecane, available from Tianjin Bodi chemical Co., ltd; sodium hydroxide, potassium hydroxide, tetrabutylammonium bromide, tetraoctylammonium bromide, available from aladine; absolute ethanol, concentrated sulfuric acid, cyclohexane, available from national pharmaceutical reagent chemical company, ltd; oleic acid, stearic acid, purchased from tokyo chemical industry limited, mountain; low viscosity trimethylolpropane ester, with a kinematic viscosity of 4.0mm 2/s at 100deg.C, a viscosity index of 137, and a Yikou Starfire chemical Co., ltd; high viscosity trimethylolpropane ester with a kinematic viscosity of 9.5mm 2/s at 100deg.C and a viscosity index of 187, guangzhou Fufei chemical Co., ltd; linseed oil, castor oil, hubei Chengfengxiao Co., ltd; antioxidant ZDDP, ashless dispersant T154B, rust inhibitor T747, tin-free south petroleum additive Co.
Preparation example 1 of graphene composite
The graphene composite is a composite of modified flaky graphene and modified graphene microspheres, and the mass ratio of the modified flaky graphene to the modified graphene microspheres is 2:1.
The preparation method of the graphene composite comprises the following steps:
(1) Synthesizing modified flaky graphene: dispersing 5g of graphene oxide in 1000ml of deionized water, carrying out ultrasonic treatment for 1h, homogenizing for 20min at a rotating speed of 4000r/min by using a homogenizer, adding 1g of sodium hydroxide, 5g of 1-bromooctadecane and 5g of tetrabutylammonium bromide, reacting at 80 ℃ for 24h, filtering with absolute ethyl alcohol, and drying in a baking oven at 60 ℃ for 12h to obtain the modified flaky graphene;
(2) Synthesizing modified graphene microspheres: dispersing 5g of graphene oxide in 1000ml of deionized water, carrying out ultrasonic treatment for 1h, and homogenizing for 20min at the rotating speed of 4000r/min by using a homogenizer to obtain a dispersion liquid with the concentration of 5 mg/ml; spray drying the dispersion liquid by using a spray dryer, wherein the inlet temperature of the spray dryer is 180 ℃, the temperature of a discharge hole is 90 ℃, the spray drying time is 2 hours, and the graphene oxide microspheres obtained by spray drying are subjected to high-temperature thermal reduction reaction for 1 hour at 300 ℃ to obtain reduced graphene microspheres; adding 2g of the reduced graphene microsphere into 40ml of cyclohexane dispersed with 2g of oleic acid, performing ultrasonic dispersion, then dropwise adding 2g of concentrated sulfuric acid, reacting for 12 hours at 80 ℃, filtering with absolute ethyl alcohol, and drying for 12 hours in a 60 ℃ oven to obtain the modified graphene microsphere;
(3) And (2) mixing the modified flaky graphene and the modified graphene microsphere according to the mass ratio of 2: and 1, mixing to obtain the graphene composite A-1.
According to detection, in the Raman spectrum of the modified flaky graphene, the ratio I D/IG of the intensity I D of 1350cm -1 peak to the intensity I G of 1590cm -1 peak in the Raman spectrum is 0.96; the average particle size of the modified graphene microsphere is 130-190.
Preparation example 2 of graphene composite
The graphene composite is a composite of modified flaky graphene and modified graphene microspheres, and the mass ratio of the modified flaky graphene to the modified graphene microspheres is 3:1.
The preparation method of the graphene composite comprises the following steps:
(1) Synthesizing modified flaky graphene: dispersing 5g of graphene oxide in 1000ml of deionized water, carrying out ultrasonic treatment for 1h, homogenizing for 10min at a rotating speed of 5000r/min by using a homogenizer, adding 2.5g of potassium hydroxide, 10g of 1-bromohexadecane and 5g of tetraoctylammonium bromide, reacting for 12h at 90 ℃, filtering by using absolute ethyl alcohol, and drying in a baking oven at 60 ℃ for 24h to obtain the modified flaky graphene;
(2) Synthesizing modified graphene microspheres: dispersing 1g of graphene oxide in 1000ml of deionized water, carrying out ultrasonic treatment for 1h, and homogenizing for 10min at a rotating speed of 5000r/min by using a homogenizer to obtain a dispersion liquid with a concentration of 1 mg/ml; spray drying the dispersion liquid by using a spray dryer, wherein the inlet temperature of the spray dryer is 190 ℃, the temperature of a discharge hole is 110 ℃, the spray drying time is 3 hours, and the graphene oxide microspheres obtained by spray drying are subjected to high-temperature thermal reduction reaction for 2 hours at 350 ℃ to obtain reduced graphene microspheres; adding 1g of the reduced graphene microsphere into 50ml of cyclohexane dispersed with 2g of stearic acid, dropwise adding 2g of concentrated sulfuric acid after ultrasonic dispersion, reacting for 6 hours at 90 ℃, filtering with absolute ethyl alcohol, and drying in a baking oven at 60 ℃ for 12 hours to obtain the modified graphene microsphere;
(3) And (3) mixing the modified flaky graphene and the modified graphene microsphere according to a mass ratio of 3:1 to obtain the graphene composite A-2.
According to detection, in the Raman spectrum of the modified flaky graphene, the ratio I D/IG of the intensity I D of 1350cm -1 peak to the intensity I G of 1590cm -1 peak in the Raman spectrum is 0.98; the average particle size of the modified graphene microsphere is 100-160.
Preparation example 3 of graphene composite
The preparation method of the preparation example is the same as that of preparation example 1, and only the difference is that in the step (3), the mass ratio of the modified flaky graphene to the modified graphene microsphere is 1:1 to obtain the graphene composite A-3.
Preparation example 4 of graphene composite
The preparation method of the preparation example is the same as that of preparation example 1, and only the difference is that in the step (3), the mass ratio of the modified flaky graphene to the modified graphene microsphere is 4:1 to obtain the graphene compound A-4.
Example 1
The high-temperature-resistant environment-friendly lubricating oil comprises the following components in percentage by mass: 90% of base oil, 0.05% of graphene composite A-1 and 9.95% of auxiliary additive.
The preparation method of the high-temperature-resistant environment-friendly lubricating oil comprises the following steps:
Uniformly mixing 67.5g of linseed oil, 13.5g of low-viscosity trimethylolpropane ester and 9g of high-viscosity trimethylolpropane ester, heating to 50 ℃, adding 50mg of graphene compound A-1, 3g of antioxidant ZDDP, 3.95g of ashless dispersant T154B and 3g of antirust agent T747 while stirring, preserving heat for 1h, naturally cooling to room temperature, and stopping stirring to obtain the high-temperature-resistant environment-friendly lubricating oil.
Example 2
The high-temperature-resistant environment-friendly lubricating oil comprises the following components in percentage by mass: 95% of base oil, 0.05% of graphene composite A-2 and 4.95% of auxiliary additive.
The preparation method of the high-temperature-resistant environment-friendly lubricating oil comprises the following steps:
And uniformly mixing 76g of castor oil, 9.5g of low-viscosity trimethylolpropane ester and 9.5g of high-viscosity trimethylolpropane ester, heating to 60 ℃, adding 50mg of graphene compound A-2, 2g of antioxidant ZDDP, 1.5g of ashless dispersant T154B and 1.45g of antirust agent T747 while stirring, preserving heat for 2 hours, naturally cooling to room temperature, and stopping stirring to obtain the high-temperature-resistant environment-friendly lubricating oil.
Example 3
The high-temperature-resistant environment-friendly lubricating oil comprises the following components in percentage by mass: 98% of base oil, 0.01% of graphene composite A-1 and 1.99% of auxiliary additive.
The preparation method of the high-temperature-resistant environment-friendly lubricating oil comprises the following steps:
Uniformly mixing 76.4g of linseed oil, 11.8g of low-viscosity trimethylolpropane ester and 9.8g of high-viscosity trimethylolpropane ester, heating to 55 ℃, adding 10mg of graphene compound A-1 and 0.55g of antioxidant ZDDP, 1g of ashless dispersant T154B and 0.44g of antirust agent T747 while stirring, preserving heat for 1.5h, naturally cooling to room temperature, and stopping stirring to obtain the high-temperature-resistant environment-friendly lubricating oil.
Example 4
The high-temperature-resistant environment-friendly lubricating oil comprises the following components in percentage by mass: 90% of base oil, 0.05% of graphene composite A-1 and 9.95% of auxiliary additive.
The preparation method of the high-temperature-resistant environment-friendly lubricating oil comprises the following steps:
Uniformly mixing 67.5g of linseed oil and 22.5g of low-viscosity trimethylolpropane ester, heating to 50 ℃, adding 50mg of graphene compound A-1, 3g of antioxidant ZDDP, 3.95g of ashless dispersant T154B and 3g of antirust agent T747 while stirring, preserving heat for 1h, naturally cooling to room temperature, and stopping stirring to obtain the high-temperature-resistant environment-friendly lubricating oil.
Comparative example 1
The preparation method of this comparative example was the same as in example 1, except that graphene complex a-1 was replaced with an equal amount of graphene complex a-3.
Comparative example 2
The preparation method of this comparative example was the same as in example 1, except that graphene complex a-1 was replaced with an equal amount of graphene complex a-4.
Comparative example 3
The preparation method of this comparative example was the same as example 1, except that the mass percentage of the graphene composite a-1 was 0.1%.
Performance testing
The lubricating oils described in examples 1 to 4 and comparative examples 1 to 3 of the present invention were subjected to performance tests according to the following test methods, and specific performance indexes are shown in Table 1.
Plaque diameter: four-ball friction and wear test was performed according to SH/T0189-2017 four-ball method for determining wear resistance of lubricating oil. Specific test conditions: the rotation speed is 1200+/-60 rpm, the load is 392+/-2N, the temperature is 75+/-2 ℃, and the friction time is 60+/-1 min. The spots were observed with an optical microscope spot grinder, and the spot grinding diameters formed on 3 steel balls were measured from two directions perpendicular to each other, and the average value of these 6 spot grinding diameters was taken as the spot grinding diameter.
Average coefficient of friction: the friction coefficient of the lubricating oil was measured using a pin-disc frictional wear machine, the pin specimen was GCr15 steel, diameter 10mm, hardness HRC60, the disc specimen was HRC44 steel 45, and the surface roughness of the pin specimen and the disc specimen was 0.5 micrometers (Ra). The experimental conditions were a load of 100N and a linear velocity of 0.15m/s.
Dispersion stability: the lubricating oil was placed in an oven at 100℃for 10 days, and after removal, whether or not precipitation occurred was visually observed.
Maximum no bite load value: using a hydraulic four-ball friction tester to test, referring to GB/3142-82 lubricating oil extreme pressure performance measurement method, and respectively testing the extreme pressure bearing capacity of an original sample and a sample subjected to high temperature treatment; the larger this value, the greater the extreme pressure carrying capacity, the greater the oil film strength. High temperature treatment conditions: the sample was heated at 200℃for 200h for high temperature treatment.
Biodegradation rate: the test was performed according to CEC-L-33-A-93.
TABLE 1 Performance data for lubricating oils described in examples 1-3 and comparative examples 1-3
As can be seen from Table 1, the lubricating oils according to examples 1 to 3 of the present application have no occurrence of precipitation, and have small average friction coefficient and small average mill-spot diameter, which indicates that the lubricating oils of the present application have excellent high-temperature dispersion stability and lubricating properties; meanwhile, the maximum seizure-free load value after high-temperature treatment is still higher, which indicates that the lubricating oil provided by the application has better high-temperature resistance. The results of example 4, although inferior to example 1, are still significantly higher than those of comparative examples 1-3. As can be seen from example 1 and comparative examples 1-2, the mass ratio of the modified graphene flakes and the modified graphene microspheres in comparative example 1 is lower, and the abrasive spot diameter and the average friction coefficient are both obviously increased, which indicates that the lubricating performance is reduced; meanwhile, the maximum seizure-free load value is reduced, which indicates that the extreme pressure bearing capacity and the high temperature resistance are poor; the mass ratio of the modified flaky graphene to the modified graphene microsphere in the comparative example 2 is higher, and the abrasive spot diameter and the average friction coefficient are obviously increased, which indicates that the lubricating performance is reduced; meanwhile, the maximum seizure-free load value is reduced, which indicates that the extreme pressure bearing capacity and the high temperature resistance are deteriorated. As is clear from examples 1 and 3, the amount of graphene complex added to the lubricating oil of comparative example 3 was too high, and the occurrence of precipitation was observed, and the average friction coefficient and the average abrasion diameter were increased, so that the maximum seizure-free load value was decreased, indicating that the amount of graphene complex added to the lubricating oil was not as high as possible.
In summary, the lubricating oil provided by the invention has excellent lubricating performance and extreme pressure bearing capacity due to the synergistic effect of the two substances by adding the specific content of the compound of the modified flaky graphene and the modified graphene microsphere into the lubricating oil, and the lubricating oil has stable high-temperature performance and is suitable for long-time use under high-temperature severe conditions.
It should be understood that the foregoing examples of the present invention are provided for the purpose of illustration only and are not intended to limit the embodiments of the present invention, and that various other changes and modifications can be made by one skilled in the art based on the foregoing description, and it is not intended to be exhaustive of all the embodiments, and all obvious changes and modifications that come within the spirit of the invention are desired to be protected.
Claims (10)
1. The high-temperature-resistant environment-friendly lubricating oil is characterized by comprising the following components in percentage by mass: 90-98% of base oil, 0.01-0.05% of graphene compound and 1.99-9.95% of auxiliary additive; the graphene composite is a composite of modified flaky graphene and modified graphene microspheres, and the mass ratio of the modified flaky graphene to the modified graphene microspheres is 2:1-3:1.
2. The high temperature resistant environment friendly lubricating oil according to claim 1, wherein the base oil is a complex of biological base oil, low viscosity trimethylolpropane ester and high viscosity trimethylolpropane ester, and the mass ratio of the biological base oil, the low viscosity trimethylolpropane ester and the high viscosity trimethylolpropane ester is 7.5-8:1-1.5:1.
3. The high temperature resistant and environment friendly lubricating oil according to claim 2, wherein the low viscosity trimethylolpropane ester has a kinematic viscosity of 3.9-4.0mm 2/s at 100 ℃ and a viscosity index of 132-135.
4. The high temperature resistant and environment friendly lubricating oil according to claim 2, wherein the high viscosity trimethylolpropane ester has a kinematic viscosity of 9.0-9.5mm 2/s at 100 ℃ and a viscosity index of 185-190.
5. The high temperature resistant, environmentally friendly lubricating oil of claim 2 wherein the biological base oil comprises any one or more of linseed oil, soybean oil, sunflower oil, cottonseed oil, castor oil, corn oil, rapeseed oil, peanut oil, or palm oil.
6. The high temperature resistant and environment friendly lubricating oil according to claim 1, wherein the modified graphene flakes are reduced graphene oxide modified by a brominated alkyl compound, and the brominated alkyl compound comprises any one or more of 1-bromohexadecane, 1-bromooctadecane and 1-bromodocosyl.
7. The high temperature resistant environment friendly lubricating oil according to claim 1, wherein the modified graphene microsphere is a long chain alkyl acid modified graphene microsphere, and the long chain alkyl acid is oleic acid and/or stearic acid.
8. The high temperature resistant environment friendly lubricating oil according to claim 1, wherein the auxiliary additive comprises any one or more of an antioxidant, a dispersant and a rust inhibitor.
9. A method for preparing the high temperature resistant environment friendly lubricating oil according to any one of claims 1 to 8, comprising the steps of:
(1) Preparing a graphene composite: dispersing graphene oxide in deionized water, carrying out ultrasonic and homogenizing treatment, adding a reducing agent, a brominated alkyl compound and a phase transfer catalyst, reacting for 12-24 hours at 80-90 ℃, filtering, and drying in an oven to obtain the modified flaky graphene; dispersing graphene oxide in deionized water, and carrying out ultrasonic and homogenizing treatment to obtain a dispersion liquid; spray drying the dispersion liquid, and carrying out high-temperature thermal reduction reaction at 300-350 ℃ to obtain reduced graphene microspheres; adding the reduced graphene microspheres into a solvent in which long-chain alkyl acid is dispersed, performing ultrasonic dispersion, then dropwise adding concentrated sulfuric acid, reacting for 6-12 hours at 80-90 ℃, filtering, and drying in an oven to obtain the modified graphene microspheres; the modified flaky graphene and the modified graphene microsphere are mixed according to the mass ratio of 2:1-3:1, mixing to obtain the graphene compound;
(2) Heating the base oil to 50-60 ℃, adding the graphene compound and the auxiliary additive while stirring, preserving heat for 1-2h, naturally cooling to room temperature, and stopping stirring to obtain the high-temperature-resistant environment-friendly lubricating oil.
10. The method for preparing high temperature resistant environment friendly lubricating oil according to claim 9, wherein in step (1), the mass ratio of graphene oxide, reducing agent, brominated alkyl compound and phase transfer catalyst is 1:0.2-0.5:1-2:1, a step of; the mass ratio of the reduced graphene microspheres to the long-chain alkyl acid to the concentrated sulfuric acid is 1:1-2:1-2.
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