CN108517240A - A kind of high anti-friction wear-resistant lubricating oil and preparation method thereof - Google Patents
A kind of high anti-friction wear-resistant lubricating oil and preparation method thereof Download PDFInfo
- Publication number
- CN108517240A CN108517240A CN201810306693.5A CN201810306693A CN108517240A CN 108517240 A CN108517240 A CN 108517240A CN 201810306693 A CN201810306693 A CN 201810306693A CN 108517240 A CN108517240 A CN 108517240A
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- Prior art keywords
- graphene
- lubricating oil
- graphene oxide
- based additive
- concentration
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- 239000010687 lubricating oil Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 235
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 207
- 239000000654 additive Substances 0.000 claims abstract description 85
- 230000000996 additive effect Effects 0.000 claims abstract description 83
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 150000008282 halocarbons Chemical class 0.000 claims abstract description 17
- 238000012545 processing Methods 0.000 claims abstract description 11
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 5
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims abstract description 3
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims description 51
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 36
- 229910002804 graphite Inorganic materials 0.000 claims description 33
- 239000010439 graphite Substances 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- 230000029936 alkylation Effects 0.000 claims description 16
- 238000005804 alkylation reaction Methods 0.000 claims description 16
- 239000003960 organic solvent Substances 0.000 claims description 15
- -1 graphene oxide salt Chemical class 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 12
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 12
- 239000003638 chemical reducing agent Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- 241000446313 Lamella Species 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 239000012736 aqueous medium Substances 0.000 claims description 7
- 230000006837 decompression Effects 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 229930003268 Vitamin C Natural products 0.000 claims description 6
- 235000019154 vitamin C Nutrition 0.000 claims description 6
- 239000011718 vitamin C Substances 0.000 claims description 6
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 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 2
- DIIIISSCIXVANO-UHFFFAOYSA-N 1,2-Dimethylhydrazine Chemical compound CNNC DIIIISSCIXVANO-UHFFFAOYSA-N 0.000 claims description 2
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- 239000001263 FEMA 3042 Substances 0.000 claims description 2
- 229930091371 Fructose Natural products 0.000 claims description 2
- 239000005715 Fructose Substances 0.000 claims description 2
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 238000009775 high-speed stirring Methods 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000043 hydrogen iodide Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 229940079877 pyrogallol Drugs 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 2
- 229940033123 tannic acid Drugs 0.000 claims description 2
- 235000015523 tannic acid Nutrition 0.000 claims description 2
- 229920002258 tannic acid Polymers 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine group Chemical group NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims 1
- 239000004215 Carbon black (E152) Substances 0.000 claims 1
- 241001122767 Theaceae Species 0.000 claims 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims 1
- 229910052794 bromium Inorganic materials 0.000 claims 1
- 239000007810 chemical reaction solvent Substances 0.000 claims 1
- 229930195733 hydrocarbon Natural products 0.000 claims 1
- 150000002430 hydrocarbons Chemical class 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000003921 oil Substances 0.000 description 19
- 159000000000 sodium salts Chemical class 0.000 description 19
- 239000000314 lubricant Substances 0.000 description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 10
- 230000004048 modification Effects 0.000 description 8
- 238000012986 modification Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000007858 starting material Substances 0.000 description 7
- 125000003342 alkenyl group Chemical group 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 238000005461 lubrication Methods 0.000 description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 5
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 5
- 239000001103 potassium chloride Substances 0.000 description 5
- 235000011164 potassium chloride Nutrition 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 244000269722 Thea sinensis Species 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 150000008442 polyphenolic compounds Chemical class 0.000 description 3
- 235000013824 polyphenols Nutrition 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- PBLNBZIONSLZBU-UHFFFAOYSA-N 1-bromododecane Chemical class CCCCCCCCCCCCBr PBLNBZIONSLZBU-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- HNTGIJLWHDPAFN-UHFFFAOYSA-N 1-bromohexadecane Chemical compound CCCCCCCCCCCCCCCCBr HNTGIJLWHDPAFN-UHFFFAOYSA-N 0.000 description 1
- VUQPJRPDRDVQMN-UHFFFAOYSA-N 1-chlorooctadecane Chemical compound CCCCCCCCCCCCCCCCCCCl VUQPJRPDRDVQMN-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 239000003831 antifriction material Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000033001 locomotion Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- HKOOXMFOFWEVGF-UHFFFAOYSA-N phenylhydrazine Chemical compound NNC1=CC=CC=C1 HKOOXMFOFWEVGF-UHFFFAOYSA-N 0.000 description 1
- 229940067157 phenylhydrazine Drugs 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- RKHXQBLJXBGEKF-UHFFFAOYSA-M tetrabutylphosphanium;bromide Chemical compound [Br-].CCCC[P+](CCCC)(CCCC)CCCC RKHXQBLJXBGEKF-UHFFFAOYSA-M 0.000 description 1
- POOSGDOYLQNASK-UHFFFAOYSA-N tetracosane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCC POOSGDOYLQNASK-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- JTCWXISSLCZBQV-UHFFFAOYSA-N tribol Natural products CC(CO)CCC1OC2(O)CC3C4CC=C5CC(CCC5(C)C4CCC3(C)C2C1C)OC6OC(CO)C(OC7OC(C)C(O)C(O)C7O)C(O)C6OC8OC(C)C(O)C(O)C8O JTCWXISSLCZBQV-UHFFFAOYSA-N 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
- C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
- C10M141/04—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic halogen-containing compound
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/26—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon starting from organic compounds containing only halogen atoms as hetero-atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/11—Compounds covalently bound to a solid support
-
- 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
- C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2211/02—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen and halogen only
- C10M2211/022—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen and halogen only aliphatic
-
- 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
- C10N2030/40—Low content or no content compositions
- C10N2030/42—Phosphor free or low phosphor content compositions
-
- 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
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Abstract
The invention discloses a kind of high anti-friction wear-resistant lubricating oil and preparation method thereof.The composition of the lubricating oil is：100 mass parts of commercial lubricating oil, 0.001~0.10 mass parts of graphene-based additive.Graphene-based additive used in the lubricating oil is：Surface grafting has the redox graphene of chain alkyl.The preparation method of the lubricating oil is：Graphene-based additive is first gone out as Material synthesis using graphene oxide and halogenated hydrocarbons, commercial lubricating oil then is added in the graphene-based additive, product is made in last homogenized processing.The lubricating oil under low graphene-based additive amount (<0.10wt%) realize high anti-friction wear-resistant：Friction coefficient can be down to 0.060 (pure commercial lubricating oil be 0.073), and wear volume can be down to 9316 μm3(pure commercial lubricating oil is 18354 μm3).The product formula and simple production process of the lubricating oil are not necessarily to great number equipment investment, are very suitable for industrialized production, have broad mass market application prospect.
Description
Technical field
The present invention relates to lubricating oil field, more particularly to a kind of height based on commercial lubricating oil and graphene-based additive subtracts
Rub abrasion-proof lubricant oil and preparation method thereof.
Background technology
Friction is the physical phenomenon of generally existing in mechanical equipment operation process.Friction not only consumes energy, but also makes machine
Tool part is worn, and then leads to part failure.According to statistics, the industrial energy in 1/3 or more the whole world is consumed in various frictions
In loss, 80% failure part is as caused by wearing.Lubrication is to reduce the major measure of friction and wear, and use lubrication
It is oily then be to realize reasonable lubrication, decrease or even eliminate the effective means of friction and wear.However, with load, speed, temperature etc.
The continuous improvement of running parameter has been unable to meet modern mechanical based on the traditional lubrication oil that traditional anti-friction agent and anti-wear agent produce and sets
Standby properties of antifriction and wear resistance requirement.New additive agent is researched and developed, to realize the high anti-friction wear-resistant of lubricating oil, it has also become high-performance lubricates
One important development direction in oily field.
With the appearance and development of " Nanotribology "【Qian Linmao/Tian Yu/Wen Shizhu Nanotribology scientific publications
Society, 2013】, different nano materials are used as the attention that lube oil additive is increasingly subject to people.Due to large specific surface area,
The features such as diffusivity is good, hardness is high, easy-sintering, nano material not only can surface of friction pair formed one layer easily shear it is thin
Film effectively reduces friction coefficient, additionally it is possible to a degree of to the abrasions such as pit, the ditch dug with a plow of surface of friction pair progress to fill up and repair
Multiple, comprehensive advantage protrudes on promoting lubricating oil anti-friction wear-resistant【The vast solid lubricants Chemical Industry Press of Shi Miao,
2000】。
In recent years, emerging nano material-graphene is applied to great interest and the pass that lubricating oil field causes industry
Note.As a kind of ultra-thin two-dimension carbon nanomaterial, graphene has very excellent lubricity, anti-pressure and abrasion-proof and thermostabilization
Property, theoretically a small amount of addition is remarkably improved the greasy property of target lube product.However, in actual use but
Reunite in lubricating oil the challenges such as serious, evenly dispersed difficulty there are original graphite alkene.Use dispersing aid and progress
Surface chemical modification is to improve two the most frequently used solutions of graphene dispersion【Tribol.Lett.,2011,41,209；
US8222190B2】.Although dispersing aid can improve the dispersibility of graphene to a certain extent, it is in use
Easily withAntioxidant, foam in hibitors, other additives such as detersive interact, be unfavorable for graphene in lubricating oil
Dispersion steady in a long-term.In this regard, it is a kind of more preferably solution to carry out specific surface graft modification to graphene.It is sorry
, it is limited to the superpower chemical inertness of graphene, can directly carry out the embodiment party of graft modification on the surface of graphene at present
Method is also seldom, and these methods also all have the defects of reaction route and/or reaction time are long, grafting rate is low, of high cost, difficult
In industrialization【Chem Rev 2012,112,6156】.
As the ideal replacer of graphene, graphene oxide is just shown one's talent in terms of as lube oil additive.This
It is based primarily upon：1) graphene oxide is the important derivatives of graphene, has the microcosmic six-membered carbon ring structure similar to graphene
With macroscopical two-dimensional slice structure；2) graphene oxide mature production technology has realized industrialization, the cost of subsequent applications at present
Advantage protrudes；3) it is rich on the surface of graphene oxide there are many reactive oxygen-containing group, can be that further implementation grafting change
Property provide chemical fundamentals.But it is noted that graphene oxide is not appropriate for directly applying to lubrication oil systems, on surface
A large amount of polarity oxygen-containing groups can not only reduce the thermal stability of itself, can also reduce the dispersibility in non-polar lubricant oil
【Tribology,2014,34,93】.To improve dispersibility and target lube product of the graphene oxide in lubricating oil
Stability is used for a long time, reduction treatment is carried out to graphene oxide to improve its thermal stability, carry out surface graft modification to carry
Its high hydrophobic oleophilic oil, while lamella size is suitably reduced, it is to realize that graphene oxide based additive is successfully answered in lubricating oil
Main direction【J.Alloy.Compd.,2017,722,778】.
Invention content
In view of the foregoing, the purpose of the present invention is to provide a kind of high anti-friction wear-resistant lubricating oil and preparation method thereof.It should
The composition of lubricating oil is：100 mass parts of commercial lubricating oil, 0.001~0.10 mass parts of graphene-based additive.The lubricating oil institute
Graphene-based additive is：Surface grafting has the redox graphene of chain alkyl.The preparation method of the lubricating oil is：
Graphene-based additive is first gone out as Material synthesis using graphene oxide and halogenated hydrocarbons, quotient then is added in the graphene-based additive
Product is made in product lubricating oil, last homogenized processing.The core of this method is to improve graphene-based add using two kinds of strategy coordinations
Add dispersion stabilization of the agent in lubricating oil：Shearing-crushing is carried out to graphene oxide, to improve its point using small-size effect
The ability of dissipating；Graft modification and reduction treatment are carried out to graphene oxide, it is (i.e. long-term to improve its hydrophobic oleophilic oil and thermal stability
Stability in use).The invention solves graphene-based additive challenge of dispersibility and stability difference in lubricating oil and asks
Topic, realize under low graphene-based additive amount (<0.10wt%) the high anti-friction wear-resistant of target lube product.
In order to achieve the above objectives, graphene-based additive of the invention passes through shearing using graphene oxide as starting material
Broken, surface graft modification and reduction process are made.
Graphene oxide is stripping product of the graphite oxide in aqueous medium, and in stripping process, work is removed by regulation and control
Small size graphene oxide is made in skill parameter (i.e. high-speed stirred and ultrasonic processing technique parameter).Graphite oxide uses Hummers
It is prepared by method；A concentration of 1~15mg/ml of graphite oxide；High-speed stirred condition is 3000~12000rpm/30~120min；It is super
Sonication condition is 200~750W/25~500kHz/20~60min.The thickness of the small size graphene oxide is 0.4
~3.0nm, lamella size are 10~1000nm, and preferred thickness is 0.4~1.6nm, and preferably lamella size is 50~300nm.
The surface graft modification of graphene oxide is carried out using following steps：
1) sodium hydroxide or potassium hydroxide are added to the aqueous dispersions of above-mentioned small size graphene oxide, agitated reaction system
Obtain graphene oxide sodium (potassium) salt.A concentration of 1~15mg/ml of graphene oxide；Sodium hydroxide or potassium hydroxide it is a concentration of
0.1~10M；It is 100~1000rpm/25~50 DEG C/0.5~10h to be stirred to react condition；
2) tetrabutylammonium bromide and saturation unitary halogenated hydrocarbons are added to the organic solvent dispersion of graphene oxide sodium (potassium) salt
Alkylation graphene oxide is made in liquid, heated reaction.Organic solvent is methanol, ethyl alcohol, propyl alcohol, dimethylformamide, diformazan
One or more mixtures in base sulfoxide, acetone, pyridine；Saturation unitary halogenated hydrocarbons is in idohydrocarbon, bromo-hydrocarbons, chlorohydrocarbon
One or more mixtures；The alkyl chain length for being saturated unitary halogenated hydrocarbons is C8~C30, the preferably a length of C12~C18 of chain；Oxygen
A concentration of 1~the 10mg/ml of graphite alkene sodium (potassium) salt dispersion liquid；The matter of tetrabutylammonium bromide and graphene oxide sodium (potassium) salt
Amount is than being 0.5:1~5:1；The mass ratio for being saturated unitary halogenated hydrocarbons and graphene oxide sodium (potassium) salt is 0.5:1~5:1；Heating
Reaction condition be 40~100 DEG C/4~for 24 hours.
3) redox graphene is prepared using chemical reduction method.Abovementioned alkyl graphite oxide is added in chemical reducing agent
Alkylation redox graphene, i.e., graphene-based addition is made in the dimethylformamide dispersion liquid of alkene, then heated reaction
Agent.Chemical reducing agent be hydrazine hydrate, dimethylhydrazine, phenylhydrazine, to sulfonyloxy methyl hydrazine, hydrogen iodide, tannic acid, pyrogallol, vitamin
C, one kind in aniline, ethylenediamine, ammonium hydroxide, hydroquinone, tea polyphenols, sodium citrate, sodium borohydride, glucose, fructose, sucrose
Or a variety of mixture；It is alkylated a concentration of 1~10mg/ml of graphene oxide dispersion；Chemical reducing agent and graphite oxide
The mass ratio of alkene is 1:1~50:1；Heating reaction condition is 50~95 DEG C/1~48h.
The high anti-friction wear-resistant lubricating oil of the present invention is by the way that commercial lubricating oil is added then through even in graphene-based additive
Made from change processing.
Commercial lubricating oil is various types of vehicle lubricating oils of commercialization.
Commercial lubricating oil is added in graphene-based additive in the form of solid particle or dispersion in organic solvent, prepares dispersion liquid
Organic solvent be chloroform, dichloromethane, tetrahydrofuran, n-hexane, one or more mixtures in acetone, it is graphene-based
Add a concentration of 0.1~10mg/ml of agent dispersing liquid.
It is different according to the use form of graphene-based additive, it carries out homogenizing processing using different step.
When graphene-based additive is in solid particulate form in use, be specially：Graphene-based additive is added to quotient
In product lubricating oil, first high-speed stirred 1000rpm/1h is then ultrasonically treated 250W/40kHz/30min, is then centrifuged for handling
1000rpm/15min, it is product finally to take supernatant liquor；
When graphene-based additive with dispersion in use, be specially：Graphene-based additive is added to organic
It is uniformly mixed in solvent and forms graphene-based addition agent dispersing liquid, then above-mentioned dispersion liquid is added in commercial lubricating oil, first room
Temperature stirring 1000rpm/1h, then decompression remove organic solvent, product are made, reduced pressure process conditions are 0.1MPa/40 DEG C, used
Organic solvent is one or more mixtures in chloroform, dichloromethane, tetrahydrofuran, n-hexane, acetone, graphene-based to add
Add a concentration of 0.1~10mg/ml of agent dispersing liquid.
The invention has the advantages that：1) compared with other nano material additives, graphene-based additive has
Self lubricity and higher anti-pressure and abrasion-proof and thermal stability；2) compared to original graphite alkenyl additive, in of the invention
For graphene-based additive without additionally using dispersing aid, raw materials for production are plentiful, purchase cost is low, are easy to industrialization；3) phase
Dispersibility is improved than the graphene-based additive in graphene oxide additive, the present invention and stability is used for a long time；
4) graphene-based additive not sulfur-bearing, the P elements in the present invention, meet the low-sulfur of lube oil additive, low-phosphorous development trend；
5) the high anti-friction wear-resistant of target lube product can be realized under low graphene-based additive amount, it is cost-effective；6) this hair
The product formula and simple production process of bright high anti-friction wear-resistant lubricating oil are not necessarily to great number equipment investment, are very suitable for industrializing
Production has broad mass market application prospect.
Description of the drawings
Fig. 1 is that pure commercial lubricating oil and the lubricating oil containing graphene-based additive exist in comparative example 1-2 and embodiment 1-5
Photo after standing 30 days.
Fig. 2 is the 3D mill spot profiles (a) and wear track Elevation Analysis (b) of pure commercial lubricating oil in comparative example 1.
Fig. 3 is 3D mill spot profiles (a) and wear track height point containing graphene-based additive-treated oil in embodiment 1
It analyses (b).
Fig. 4 is 3D mill spot profiles (a) and wear track height point containing graphene-based additive-treated oil in embodiment 2
It analyses (b).
Fig. 5 is 3D mill spot profiles (a) and wear track height point containing graphene-based additive-treated oil in embodiment 3
It analyses (b).
Specific implementation mode
Below in conjunction with the accompanying drawings and by specific embodiment come present invention be described in more detail.It should be understood that following embodiments
It is to limit its protection domain for illustrating rather than.
Comparative example 1：
Use pure commercial lubricating oil A (trade mark is SM 10W30) as the Basal control group of embodiment in the present invention.Such as figure
Shown in 1a, which can keep uniform and stable after standing 30 days at room temperature.SRV fine motions are carried out to lubricating oil A to rub
Wear test is wiped, as a result shows that its friction coefficient and wear volume are respectively 0.073 and 18354 μm3.Wear track height simultaneously
Analysis (Fig. 2 b) shows that its greatest wear depth is 800nm.
Comparative example 2：
It is a kind of using redox graphene as the lubricating oil of additive, composition be commercial lubricating oil A (trade mark SM
10W30) it is 100 mass parts, 0.025 mass parts of redox graphene additive.The lubricating oil is prepared using following steps：
1) graphite oxide is prepared using Hummers methods, then in aqueous medium, is removed graphite oxide by being ultrasonically treated
And it is broken into small size graphene oxide；A concentration of 12mg/ml of graphite oxide；Supersound process condition is 300W/250kHz/
25min.The thickness of the small size graphene oxide is 0.9nm, and lamella average-size is 283nm.
2) chemical reducing agent vitamin C is added to the aqueous dispersions of graphene oxide, reduction-oxidation is made in heated reaction
Graphene；A concentration of 6mg/ml of graphene oxide dispersion；The mass ratio of chemical reducing agent and graphene oxide is 3:1；Add
Thermal rection condition is 60 DEG C/10h.
3) commercial lubricating oil A, room temperature is added in the tetrahydrofuran dispersion liquid of redox graphene (a concentration of 3mg/ml)
Under stir evenly 1000rpm/1h, then decompression removes 0.1MPa/40 DEG C of organic solvent, and target lube product is made.
As shown in Figure 1 b, there is apparent layering after standing 30 days in the lubricating oil containing redox graphene additive
A large amount of precipitations are arranged at phenomenon, bottom, show that carrying out simple modified with reduction to graphene oxide cannot achieve it in commercial lubricating oil
Long dispersion stability.
Embodiment 1：
A kind of high anti-friction wear-resistant lubricating oil, the additive of the lubricating oil are to use graphene oxide and unitary halogenated hydrocarbons for original
Expect that the graphene-based additive synthesized, composition are that commercial lubricating oil A (trade mark is SM 10W30) is 100 mass parts, graphite
0.025 mass parts of alkenyl additive.The efficient lubricant oil is prepared using following steps：
1) graphite oxide is prepared using Hummers methods, then in aqueous medium, is removed graphite oxide by being ultrasonically treated
And it is broken into small size graphene oxide；A concentration of 12mg/ml of graphite oxide；Supersound process condition is 300W/250kHz/
25min.The thickness of the small size graphene oxide is 0.8nm, and lamella average-size is 179nm.
2) graphene oxide aqueous dispersions are added in sodium hydroxide, graphene oxide sodium salt is made in agitated reaction, used
Graphene oxide a concentration of 6mg/ml；Naoh concentration is 3M；It is 800rpm/40 DEG C/1.0h to be stirred to react condition.
3) tetrabutylammonium bromide and 1- chlorine octadecanes are added to the dimethylformamide dispersion liquid of graphene oxide sodium salt, warp
Alkylation graphene oxide is made in heating reaction；A concentration of 5mg/ml of graphene oxide sodium salt dispersion liquid；Tetrabutylammonium bromide
Mass ratio with graphene oxide sodium salt is 2:1；The mass ratio of 1- chlorine octadecane and graphene oxide sodium salt is 3:1；Heating is anti-
It is 60 DEG C/8h to answer condition.
4) vitamin C is added to the dimethylformamide dispersion liquid of alkylation graphene oxide, alkane is made in heated reaction
Base redox graphene (i.e. graphene-based additive)；It is alkylated a concentration of 6mg/ml of graphene oxide dispersion；Dimension
The mass ratio of raw element C and graphene oxide is 3:1；Heating reaction condition is 60 DEG C/10h.
5) commercial lubricating oil A, room temperature is added in the tetrahydrofuran dispersion liquid of graphene-based additive (a concentration of 3mg/ml)
Under stir evenly 1000rpm/1h, then decompression removes 0.1MPa/40 DEG C of organic solvent, and target lube product is made.
The high anti-friction wear-resistant lubricating oil still maintains stable homogeneous (Fig. 1 c) after standing 30 days.Therefore, with 2 phase of comparative example
Than carrying out long chain alkane (chlorooctadecane) surface graft modification to graphene oxide and reduction treatment being remarkably improved graphene
Dispersibility and long-time stability of the based additive in lubricating oil.
The lubricating oil (0.025wt%) under low graphene-based additive amount realizes high anti-friction wear-resistant simultaneously：It rubs
Wiping coefficient can be down to 0.060 (pure commercial lubricating oil be 0.073, comparative example 1), and wear volume can be down to 9316 μm3(pure commodity profit
Lubricating oil is 18354 μm3, comparative example 1).In addition, wear track Elevation Analysis (Fig. 3 b) also confirms that its greatest wear depth is only
160nm。
Embodiment 2：
A kind of high anti-friction wear-resistant lubricating oil, the additive of the lubricating oil are to use graphene oxide and unitary halogenated hydrocarbons for original
Expect that the graphene-based additive synthesized, composition are that commercial lubricating oil B (trade mark is GL-5 80W90) is 100 mass parts, stone
0.050 mass parts of mertenyl additive.The efficient lubricant oil is prepared using step similar to Example 1, and difference is：
Step 1) prepares graphite oxide using Hummers methods, then in aqueous medium, by high-speed stirred by graphite oxide
It removes and is broken into small size graphene oxide；A concentration of 10mg/ml of graphite oxide；High-speed stirred condition is 8000rpm/
60min.The thickness of the small size graphene oxide is 0.9nm, and lamella average-size is 351nm.
Graphene oxide aqueous dispersions are added in potassium hydroxide by step 2), and graphene oxide sylvite is made in agitated reaction,
A concentration of 5mg/ml of graphene oxide used；Concentration of potassium hydroxide is 3M；Be stirred to react condition be 600rpm/30 DEG C/
3.0h。
The dimethyl sulfoxide (DMSO) dispersion liquid of graphene oxide sylvite is added in tetrabutylammonium bromide and 1- bromo-dodecanes by step 3),
Alkylation graphene oxide is made in heated reaction；A concentration of 6mg/ml of graphene oxide sylvite dispersion liquid；Tetrabutyl phosphonium bromide
The mass ratio of ammonium and graphene oxide sylvite is 3:1；The mass ratio of 1- bromo-dodecanes and graphene oxide sylvite is 2:1；Heating
Reaction condition is 70 DEG C/6h.
The lubricating oil still maintains stable homogeneous (Fig. 1 d) after standing 30 days, and friction coefficient and wear volume are respectively
0.068 and 11664 μm3, greatest wear depth is 460nm (Fig. 4 b).Therefore, bromohexadecane reductive modification graphite oxide alkenyl
Dispersibility and long-time stability of the additive in lubricating oil are more satisfactory, while the lubricating oil has high properties of antifriction and wear resistance.
Embodiment 3：
A kind of high anti-friction wear-resistant lubricating oil, the additive of the lubricating oil are to use graphene oxide and unitary halogenated hydrocarbons for original
Expect that the graphene-based additive synthesized, composition are that commercial lubricating oil C (trade mark is CD 15W-40) is 100 mass parts, graphite
0.075 mass parts of alkenyl additive.The efficient lubricant oil is prepared using step similar to Example 1, and difference is：
The dimethylformamide point of graphene oxide sodium salt is added in tetrabutylammonium bromide and 1- iodine lignoceranes by step 3)
Alkylation graphene oxide is made in dispersion liquid, heated reaction；A concentration of 8mg/ml of graphene oxide sodium salt dispersion liquid；The tetrabutyl
The mass ratio of ammonium bromide and graphene oxide sodium salt is 3:1；The mass ratio of 1- iodine lignocerane and graphene oxide sodium salt is 2:
1；Heating reaction condition is 70 DEG C/8h.
The dimethylformamide dispersion liquid of alkylation graphene oxide, heated reaction system is added in sodium borohydride by step 4)
Redox graphene (i.e. graphene-based additive) must be alkylated；It is alkylated a concentration of 5mg/ of graphene oxide dispersion
ml；The mass ratio of sodium borohydride and graphene oxide is 4:1；Heating reaction condition is 80 DEG C/8h.
The lubricating oil can still keep the stable homogeneous (Fig. 1 e), friction coefficient and wear volume to be respectively after standing 30 days
0.071 and 13239 μm3, greatest wear depth is 580nm (Fig. 5 b).It is indicated above：Iodo lignocerane redox graphene
Dispersibility and long-time stability of the based additive in lubricating oil are more satisfactory；Under low graphene-based additive amount (<
0.10wt%), lubricating oil can show excellent properties of antifriction and wear resistance.
Embodiment 4：
A kind of high anti-friction wear-resistant lubricating oil, the additive of the lubricating oil are to use graphene oxide and unitary halogenated hydrocarbons for original
Expect that the graphene-based additive synthesized, composition are that commercial lubricating oil A (trade mark is SM 10W30) is 100 mass parts, graphite
0.025 mass parts of alkenyl additive.The efficient lubricant oil is prepared using step similar to Example 1, and difference is:
Commercial lubricating oil A is added in graphene-based additive by step 5) in solid particulate form, homogenizes processing step：It is first high
Speed stirring 1000rpm/1h, is then ultrasonically treated 250W/40kHz/30min, is then centrifuged for processing 1000rpm/15min, finally
It is product to take supernatant liquor.
The efficient lubricant oil can keep stable homogeneous (Fig. 1 f), friction coefficient and wear volume difference after standing 30 days
It is 0.062 and 9624 μm3, show that lubrication oil systems for graphene-based additive to be added in solid particulate form, can equally make
Obtain lubricating oil that is whole uniform and stable and having high properties of antifriction and wear resistance.
Embodiment 5：
A kind of high anti-friction wear-resistant lubricating oil, the additive of the lubricating oil are to use graphene oxide and unitary halogenated hydrocarbons for original
Expect that the graphene-based additive synthesized, composition are that commercial lubricating oil B (trade mark is GL-5 80W90) is 100 mass parts, stone
0.005 mass parts of mertenyl additive.The efficient lubricant oil is prepared using step similar to Example 1, and difference is：
The dimethylformamide dispersion liquid of alkylation graphene oxide is added in chemical reducing agent tea polyphenols by step 4), through adding
Alkylation redox graphene (i.e. graphene-based additive) is made in thermal response；It is alkylated the concentration of graphene oxide dispersion
For 8mg/ml；The mass ratio of tea polyphenols and graphene oxide is 20:1；Heat reaction condition be 70 DEG C/for 24 hours.
Commercial lubricating oil B, room is added in the n-hexane dispersion liquid (a concentration of 6mg/ml) of graphene-based additive by step 5)
1000rpm/1h is stirred evenly under temperature, then decompression removes 0.1MPa/40 DEG C of organic solvent, and target lube product is made.
The lubricating oil keeps stable homogeneous (Fig. 1 g) after standing 30 days, and friction coefficient and wear volume are respectively
0.070 and 15396 μm3.It is therefore seen that under extremely low graphene-based additive amount (0.005wt%), the efficient lubricant oil is still
Excellent properties of antifriction and wear resistance can be achieved.
Embodiment 6：
A kind of high anti-friction wear-resistant lubricating oil, the additive of the lubricating oil are to use graphene oxide and unitary halogenated hydrocarbons for original
Expect that the graphene-based additive synthesized, composition are that commercial lubricating oil A (trade mark is SM 10W30) is 100 mass parts, graphite
0.001 mass parts of alkenyl additive.The efficient lubricant oil is prepared using following steps：
1) graphite oxide is prepared using Hummers methods, then in aqueous medium, is removed graphite oxide by being ultrasonically treated
And it is broken into small size graphene oxide；A concentration of 1mg/ml of graphite oxide；Supersound process condition is 200W/25kHz/
20min.The thickness of the small size graphene oxide is 0.7nm, and lamella average-size is 50nm.
2) graphene oxide aqueous dispersions are added in sodium hydroxide, graphene oxide sodium salt is made in agitated reaction, used
Graphene oxide a concentration of 1mg/ml；Naoh concentration is 0.1M；It is 100rpm/50 DEG C/10h to be stirred to react condition.
3) tetrabutylammonium bromide and 1- chlorine octadecanes are added to the dimethylformamide dispersion liquid of graphene oxide sodium salt, warp
Alkylation graphene oxide is made in heating reaction；A concentration of 1mg/ml of graphene oxide sodium salt dispersion liquid；Tetrabutylammonium bromide
Mass ratio with graphene oxide sodium salt is 0.5:1；The mass ratio of 1- chlorine octadecane and graphene oxide sodium salt is 0.5:1；Add
Thermal rection condition be 40 DEG C/for 24 hours.
4) vitamin C is added to the dimethylformamide dispersion liquid of alkylation graphene oxide, alkane is made in heated reaction
Base redox graphene (i.e. graphene-based additive)；It is alkylated a concentration of 1mg/ml of graphene oxide dispersion；Dimension
The mass ratio of raw element C and graphene oxide is 1:1；Heating reaction condition is 50 DEG C/48h.
5) commercial lubricating oil A, room is added in the tetrahydrofuran dispersion liquid of graphene-based additive (a concentration of 0.1mg/ml)
1000rpm/1h is stirred evenly under temperature, then decompression removes 0.1MPa/40 DEG C of organic solvent, and target lube product is made.
It is respectively 0.069 He that the lubricating oil keeps stable homogeneous, friction coefficient and wear volume after standing 30 days
16432μm3。
Embodiment 7：
A kind of high anti-friction wear-resistant lubricating oil, the additive of the lubricating oil are to use graphene oxide and unitary halogenated hydrocarbons for original
Expect that the graphene-based additive synthesized, composition are that commercial lubricating oil A (trade mark is SM 10W30) is 100 mass parts, graphite
0.10 mass parts of alkenyl additive.The efficient lubricant oil is prepared using following steps：
1) graphite oxide is prepared using Hummers methods, then in aqueous medium, is removed graphite oxide by being ultrasonically treated
And it is broken into small size graphene oxide；A concentration of 15mg/ml of graphite oxide；Supersound process condition is 750W/500kHz/
60min.The thickness of the small size graphene oxide is 3.0nm, and lamella average-size is 300nm.
2) graphene oxide aqueous dispersions are added in sodium hydroxide, graphene oxide sodium salt is made in agitated reaction, used
Graphene oxide a concentration of 15mg/ml；Naoh concentration is 10M；Be stirred to react condition be 1000rpm/25 DEG C/
0.5h。
3) tetrabutylammonium bromide and 1- chlorine octadecanes are added to the dimethylformamide dispersion liquid of graphene oxide sodium salt, warp
Alkylation graphene oxide is made in heating reaction；A concentration of 10mg/ml of graphene oxide sodium salt dispersion liquid；Tetrabutylammonium bromide
Mass ratio with graphene oxide sodium salt is 5:1；The mass ratio of 1- chlorine octadecane and graphene oxide sodium salt is 5:1；Heating is anti-
It is 100 DEG C/4h to answer condition.
4) vitamin C is added to the dimethylformamide dispersion liquid of alkylation graphene oxide, alkane is made in heated reaction
Base redox graphene (i.e. graphene-based additive)；It is alkylated a concentration of 10mg/ml of graphene oxide dispersion；Dimension
The mass ratio of raw element C and graphene oxide is 50:1；Heating reaction condition is 95 DEG C/1h.
5) commercial lubricating oil A is added in the acetone dispersion liquor of graphene-based additive (a concentration of 10mg/ml), stirred at room temperature
Uniform 1000rpm/1h is mixed, then decompression removes 0.1MPa/40 DEG C of organic solvent, and target lube product is made.
It is respectively 0.062 He that the lubricating oil keeps stable homogeneous, friction coefficient and wear volume after standing 30 days
14916μm3。
Finally, it is noted that preferred embodiment above is only used to illustrate the technical scheme of the present invention and unrestricted, although
The present invention is described in detail by above preferred embodiment, but should be appreciated that can be with by this field staff
Various changes are made to it in the form and details, without departing from claims of the present invention limited range.
Claims (7)
1. a kind of high anti-friction wear-resistant lubricating oil, which is characterized in that its composition is 100 mass parts of commercial lubricating oil, graphene-based
0.001~0.10 mass parts of additive.
2. high anti-friction wear-resistant lubricating oil according to claim 1, which is characterized in that commercial lubricating oil used is commodity
The various types of vehicle lubricating oils changed.
3. high anti-friction wear-resistant lubricating oil according to claim 1, which is characterized in that graphene-based additive used is table
Face is grafted with the redox graphene of chain alkyl.
4. a kind of preparation method of high anti-friction wear-resistant lubricating oil described in claim 1, which is characterized in that first with graphene oxide
It is that Material synthesis goes out graphene-based additive with unitary halogenated hydrocarbons, commercial lubricating oil then is added in graphene-based additive again,
Product is made in last homogenized processing.
5. the preparation method of high anti-friction wear-resistant lubricating oil according to claim 4, which is characterized in that graphene-based additive
It is synthesized using following steps：
(1) graphene oxide：In aqueous medium, graphite oxide is removed by high-speed stirred and supersound process and is broken into small ruler
Very little graphene oxide, graphite oxide used are prepared using Hummers methods；A concentration of 1~15mg/ml of graphite oxide；At a high speed
Stirring condition is 3000~12000rpm/30~120min；Supersound process condition be 200~750W/25~500kHz/20~
60min.The thickness of the small size graphene oxide is 0.4~3.0nm, and lamella size is 10~1000nm；
(2) graphene oxide salt：Graphene oxide aqueous dispersions are added in sodium hydroxide or potassium hydroxide, agitated reaction is made
Graphene oxide salt, a concentration of 1~15mg/ml of graphene oxide used；A concentration of the 0.1 of sodium hydroxide or potassium hydroxide
~10M；It is 100~1000rpm/25~50 DEG C/0.5~10h to be stirred to react condition；
(3) it is alkylated graphene oxide：The organic of graphene oxide salt is added in tetrabutylammonium bromide and saturation unitary halogenated hydrocarbons
Alkylation graphene oxide is made in solvent dispersions, heated reaction, and organic solvent used is methanol, ethyl alcohol, propyl alcohol, diformazan
One or more mixtures in base formamide, dimethyl sulfoxide (DMSO), acetone, pyridine；Saturation unitary halogenated hydrocarbons is idohydrocarbon, bromine
For one or more mixtures in hydrocarbon, chlorohydrocarbon, alkyl chain length is C8~C30；The concentration of graphite oxide salt dispersion liquid
For 1~10mg/ml；The mass ratio of tetrabutylammonium bromide and graphene oxide salt is 0.5:1~5:1；Be saturated unitary halogenated hydrocarbons with
The mass ratio of graphene oxide salt is 0.5:1~5:1；Heat reaction condition be 40~100 DEG C/4~for 24 hours；
(4) it is alkylated redox graphene：Chemical reducing agent is added to the dimethylformamide point of alkylation graphene oxide
Alkylation redox graphene is made in dispersion liquid, heated reaction, and chemical reducing agent used is hydrazine hydrate, dimethylhydrazine, benzene
It is hydrazine, more to sulfonyloxy methyl hydrazine, hydrogen iodide, tannic acid, pyrogallol, vitamin C, aniline, ethylenediamine, ammonium hydroxide, hydroquinone, tea
One or more mixtures in phenol, sodium citrate, sodium borohydride, glucose, fructose, sucrose；It is alkylated graphene oxide
A concentration of 1~10mg/ml of dispersion liquid；The mass ratio of chemical reducing agent and graphene oxide is 1:1~50:1；Heating reaction item
Part is 50~95 DEG C/1~48h.
6. the preparation method of high anti-friction wear-resistant lubricating oil according to claim 4, which is characterized in that graphene-based additive
Commercial lubricating oil is added in the form of solid particle or dispersion in organic solvent, organic solvent used is chloroform, dichloromethane, four
One or more mixtures in hydrogen furans, n-hexane, acetone；A concentration of the 0.1 of graphene-based addition agent dispersing liquid~
10mg/ml。
7. the preparation method of high anti-friction wear-resistant lubricating oil according to claim 4, which is characterized in that when graphene-based addition
Agent in solid particulate form in use, including homogenizing processing step as follows：First high-speed stirred 1000rpm/1h is then ultrasonically treated
250W/40kHz/30min is then centrifuged for processing 1000rpm/15min, and it is product finally to take supernatant liquor；Add when graphene-based
Add agent with dispersion in use, including homogenizing processing step as follows：1000rpm/1h is first stirred at room temperature, then decompression removes
Product is made in 0.1MPa/40 DEG C of organic solvent.
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