CN101205496B - Grease additive, grease containing the same and preparation thereof - Google Patents
Grease additive, grease containing the same and preparation thereof Download PDFInfo
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- CN101205496B CN101205496B CN 200610165310 CN200610165310A CN101205496B CN 101205496 B CN101205496 B CN 101205496B CN 200610165310 CN200610165310 CN 200610165310 CN 200610165310 A CN200610165310 A CN 200610165310A CN 101205496 B CN101205496 B CN 101205496B
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- 239000004519 grease Substances 0.000 title claims abstract description 102
- 239000000654 additive Substances 0.000 title claims abstract description 57
- 230000000996 additive effect Effects 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 239000002105 nanoparticle Substances 0.000 claims abstract description 82
- 239000002131 composite material Substances 0.000 claims abstract description 73
- 150000001875 compounds Chemical class 0.000 claims abstract description 69
- 239000003112 inhibitor Substances 0.000 claims abstract description 31
- 230000001050 lubricating effect Effects 0.000 claims abstract description 28
- VFUXXFYLTHXJSF-UHFFFAOYSA-M lithium;octadecanoic acid;hydroxide Chemical compound [Li+].[OH-].CCCCCCCCCCCCCCCCCC(O)=O VFUXXFYLTHXJSF-UHFFFAOYSA-M 0.000 claims description 27
- 239000000047 product Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000002244 precipitate Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000012752 auxiliary agent Substances 0.000 claims description 8
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 claims description 7
- -1 alkenyl imidazoline dodecenylsuccinic acid Chemical compound 0.000 claims description 6
- QDCPNGVVOWVKJG-VAWYXSNFSA-N 2-[(e)-dodec-1-enyl]butanedioic acid Chemical group CCCCCCCCCC\C=C\C(C(O)=O)CC(O)=O QDCPNGVVOWVKJG-VAWYXSNFSA-N 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 150000001412 amines Chemical class 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910017464 nitrogen compound Inorganic materials 0.000 claims description 3
- 150000002830 nitrogen compounds Chemical class 0.000 claims description 3
- 125000003354 benzotriazolyl group Chemical class N1N=NC2=C1C=CC=C2* 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims 3
- 238000011010 flushing procedure Methods 0.000 claims 3
- 239000007789 gas Substances 0.000 claims 3
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 claims 2
- SKDGWNHUETZZCS-UHFFFAOYSA-N 2,3-ditert-butylphenol Chemical compound CC(C)(C)C1=CC=CC(O)=C1C(C)(C)C SKDGWNHUETZZCS-UHFFFAOYSA-N 0.000 claims 1
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N pentanoic acid group Chemical group C(CCCC)(=O)O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims 1
- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Substances CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims 1
- 239000003963 antioxidant agent Substances 0.000 abstract description 24
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 23
- 238000005260 corrosion Methods 0.000 abstract description 8
- 229910052802 copper Inorganic materials 0.000 abstract description 7
- 239000010949 copper Substances 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 7
- 230000003064 anti-oxidating effect Effects 0.000 abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 24
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 9
- FPLIHVCWSXLMPX-UHFFFAOYSA-M lithium 12-hydroxystearate Chemical compound [Li+].CCCCCCC(O)CCCCCCCCCCC([O-])=O FPLIHVCWSXLMPX-UHFFFAOYSA-M 0.000 description 9
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 7
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- COBPKKZHLDDMTB-UHFFFAOYSA-N 2-[2-(2-butoxyethoxy)ethoxy]ethanol Chemical compound CCCCOCCOCCOCCO COBPKKZHLDDMTB-UHFFFAOYSA-N 0.000 description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 239000012964 benzotriazole Substances 0.000 description 6
- 229950000688 phenothiazine Drugs 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 230000003078 antioxidant effect Effects 0.000 description 5
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 5
- 238000002329 infrared spectrum Methods 0.000 description 5
- 229940114072 12-hydroxystearic acid Drugs 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000013556 antirust agent Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 239000002199 base oil Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003925 fat Substances 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000005069 Extreme pressure additive Substances 0.000 description 2
- 239000007866 anti-wear additive Substances 0.000 description 2
- 239000005441 aurora Substances 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 125000005066 dodecenyl group Chemical group C(=CCCCCCCCCCC)* 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 229910052961 molybdenite Inorganic materials 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 2
- 231100000241 scar Toxicity 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 229940114069 12-hydroxystearate Drugs 0.000 description 1
- DTIWZILWCUSUSG-UHFFFAOYSA-N C(=CCCCCCCCCCC)C(C(=O)O)CC(=O)O.NCCC=1N(CCN1)C=CCCCCCCCCCCCCCCC Chemical compound C(=CCCCCCCCCCC)C(C(=O)O)CC(=O)O.NCCC=1N(CCN1)C=CCCCCCCCCCCCCCCC DTIWZILWCUSUSG-UHFFFAOYSA-N 0.000 description 1
- 229940126062 Compound A Drugs 0.000 description 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 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
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000002530 phenolic antioxidant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000004867 thiadiazoles Chemical class 0.000 description 1
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Abstract
本发明涉及一种润滑脂添加剂、含有该润滑脂添加剂的润滑脂以及它们的制备方法,所述润滑脂添加剂含有a.一种式A化合物/MoS2复合纳米微粒;b.至少一种选自下列物质的助剂:抗氧剂和防锈剂。本发明的润滑脂添加剂可以提高润滑脂产品的抗氧化性能和抑制铜腐蚀性能。
The present invention relates to a kind of lubricating grease additive, the lubricating grease containing this lubricating grease additive and their preparation method, described lubricating grease additive contains a. a kind of formula A compound/ MoS Composite nanoparticle; b. at least one selected from Auxiliary for the following substances: antioxidants and rust inhibitors. The lubricating grease additive of the invention can improve the anti-oxidation performance and inhibit copper corrosion performance of the lubricating grease product.
Description
技术领域 technical field
本发明涉及一种润滑脂添加剂、含有它的润滑脂及它们的制备方法。更具体而言,本发明涉及一种抗氧化和/或抑制铜腐蚀的润滑脂添加剂、含有它的润滑脂及它们的制备方法。 The present invention relates to a lubricating grease additive, lubricating grease containing it and their preparation method. More specifically, the present invention relates to an oxidation-resistant and/or copper-corrosion-inhibiting grease additive, greases containing it, and methods for their preparation. the
背景技术 Background technique
极压抗磨添加剂是润滑剂中非常重要的一类添加剂。近年来,噻二唑衍生物的极压抗磨作用得到了进一步的认识,作为润滑脂高性能极压抗磨剂开始崭露头角。这类极压抗磨剂不含磷和重金属元素,为无灰添加剂,而且还具有抗氧、金属钝化等功能,是环境友好、性能优异的多功能极压抗磨剂(参见美国专利USP 6,365,557)。其中,二硫代二唑硫酮与丁氧基三乙二醇的反应产物,同时具有极佳的四球极压性能和梯姆肯极压性能,且无灰、可生物降解,因此具有极强的应用背景。该物质虽然具有优秀的极压性能,但减摩抗磨性能不足,仍有改进的必要。 Extreme pressure and antiwear additives are a very important class of additives in lubricants. In recent years, the extreme pressure and antiwear effects of thiadiazole derivatives have been further understood, and they have begun to emerge as high-performance extreme pressure and antiwear agents for lubricating greases. This kind of extreme pressure antiwear agent does not contain phosphorus and heavy metal elements, it is an ash-free additive, and it also has functions such as anti-oxidation and metal passivation. It is an environmentally friendly and multifunctional extreme pressure antiwear agent with excellent performance (see US Patent USP 6,365,557). Among them, the reaction product of dithiooxadiazolethione and butoxytriethylene glycol has excellent four-ball extreme pressure performance and Timken extreme pressure performance, and is ashless and biodegradable, so it has extremely strong application background. Although the material has excellent extreme pressure properties, its anti-friction and anti-wear properties are insufficient, and there is still a need for improvement. the
发明内容 Contents of the invention
本发明人意外发现,如果合成二硫代二唑硫酮与丁氧基三乙二醇的反应产物/MoS2复合纳米微粒(简称复合纳米微粒,下同),用于基础润滑脂中,发现这样的复合纳米微粒克服了二硫代二唑硫酮与丁氧基三乙二醇的反应产物减摩抗磨性能不佳的问题。在此基础上,经进一步研究,发明人发现,如果在含有复合纳米微粒的润滑脂中加入抗氧剂和/或防锈剂制成润滑脂添加剂,可以使润滑脂产品具有进一步改善的抗氧化性能和/或抑制铜腐蚀的性能。 The present inventor unexpectedly finds that if the reaction product/MoS of dithiooxadiazolethione and butoxytriethylene glycol is synthesized Composite nanoparticles (composite nanoparticles for short, the same below) are used in base lubricating greases, and it is found that Such composite nanoparticles overcome the problem of poor anti-friction and anti-wear properties of the reaction product of dithiooxadiazolethione and butoxy triethylene glycol. On this basis, after further research, the inventors found that if an antioxidant and/or anti-rust agent is added to the grease containing composite nanoparticles to make a grease additive, the grease product can have further improved oxidation resistance performance and/or copper corrosion inhibition performance.
因此,本发明提供一种润滑脂添加剂,含有 Therefore, the present invention provides a kind of lubricating grease additive, contains
a.一种式A化合物/MoS2复合纳米微粒; A. a compound of formula A/ MoS Composite nanoparticles;
b.至少一种选自下列物质的助剂:抗氧剂和防锈剂。 b. At least one additive selected from the group consisting of antioxidants and rust inhibitors. the
本发明还提供一种制备润滑脂添加剂的方法,包括将一种式A化合物/MoS2复合纳米微粒与至少一种选自抗氧剂和防锈剂的助剂混合。 The present invention also provides a method for preparing a grease additive, comprising mixing a compound nanoparticle of formula A/MoS 2 with at least one additive selected from antioxidants and rust inhibitors.
本发明还提供一种润滑脂,含有 The present invention also provides a lubricating grease, containing
a.一种基础润滑脂; a. A basic grease;
b.一种式A化合物/MoS2复合纳米微粒; b. A compound of formula A/ MoS Composite nanoparticles;
c.至少一种选自下列物质的助剂:抗氧剂和防锈剂。 c. At least one additive selected from the group consisting of antioxidants and rust inhibitors. the
本发明还提供一种制备润滑脂的方法,包括混合一种基础润滑脂和一种包括下列组分的润滑脂添加剂: The present invention also provides a method of preparing grease comprising mixing a base grease and a grease additive comprising the following components:
a.一种式A化合物/MoS2复合纳米微粒; A. a compound of formula A/ MoS Composite nanoparticles;
b.至少一种选自下列物质的助剂:抗氧剂和防锈剂。 b. At least one additive selected from the group consisting of antioxidants and rust inhibitors. the
本发明还提供一种制备润滑脂的方法,包括混合下列组分: The present invention also provides a method for preparing lubricating grease, comprising mixing the following components:
a.一种基础润滑脂; a. A basic grease;
b.一种式A化合物/MoS2复合纳米微粒; b. A compound of formula A/ MoS Composite nanoparticles;
c.至少一种选自下列物质的助剂:抗氧剂和防锈剂。 c. At least one additive selected from the group consisting of antioxidants and rust inhibitors. the
在本发明中,“式A化合物/MoS2复合纳米微粒”为由式A化合物和MoS2构成的复合物的纳米级的粒子。可以采用下列方法获得:在加热至30-90℃的去离子水中,通惰性气体,然后加入硫代钼酸铵至完全溶解。搅拌下加入式A化合物和无水乙醇,然后加入盐酸羟胺反应,再加入浓盐酸继续反应,有沉淀生成;沉淀用去离子水及有机溶剂冲洗;将产物干燥,得到式A化合物/MoS2复合纳米微粒。 In the present invention, "the compound of formula A/MoS 2 composite nanoparticle" is a nanoscale particle of a composite composed of the compound of formula A and MoS 2 . It can be obtained by the following method: in deionized water heated to 30-90°C, pass an inert gas, and then add ammonium thiomolybdate until completely dissolved. Add the compound of formula A and absolute ethanol under stirring, then add hydroxylamine hydrochloride to react, then add concentrated hydrochloric acid to continue the reaction, and a precipitate is formed; the precipitate is washed with deionized water and an organic solvent; the product is dried to obtain a compound of formula A/MoS 2 nanoparticles.
附图说明Description of drawings
图1为式A化合物的红外光谱图。 Fig. 1 is the infrared spectrogram of formula A compound. the
图2为化合物A和MoS2构成的复合纳米微粒红外光谱。 Figure 2 is the infrared spectrum of composite nanoparticles composed of Compound A and MoS 2 .
图3为不同润滑脂产品的摩擦系数随时间的变化图(▲式A化合物; 12羟基润滑脂;■T321;●T351)。 Figure 3 is a graph of the friction coefficient of different grease products changing with time (▲Compound of formula A; 12 hydroxyl grease; ■ T 321 ; ● T 351 ).
具体实施方式Detailed ways
本发明的润滑脂添加剂中,含有 In the grease additive of the present invention, contain
a.一种式A化合物/MoS2复合纳米微粒; A. a compound of formula A/ MoS Composite nanoparticles;
b.至少一种选自下列物质的助剂:抗氧剂和防锈剂。 b. At least one additive selected from the group consisting of antioxidants and rust inhibitors. the
本发明的制备润滑脂添加剂的方法,包括将一种式A化合物/MoS2复合纳米微粒与至少一种选自抗氧剂和防锈剂的助剂混合。 The method for preparing grease additives of the present invention comprises mixing a compound nanoparticle of formula A/MoS 2 with at least one additive selected from antioxidants and rust inhibitors.
本发明的润滑脂中,含有 In the lubricating grease of the present invention, contain
a.一种基础润滑脂; a. A basic grease;
b.一种式A化合物/MoS2复合纳米微粒; b. A compound of formula A/ MoS Composite nanoparticles;
c.至少一种选自下列物质的助剂:抗氧剂和防锈剂。 c. At least one additive selected from the group consisting of antioxidants and rust inhibitors. the
本发明的制备润滑脂的方法,包括混合一种基础润滑脂和一种包括下列组分的润滑脂添加剂: The method for preparing lubricating grease of the present invention comprises mixing a kind of base lubricating grease and a kind of lubricating grease additive comprising following component:
a.一种式A化合物/MoS2复合纳米微粒; A. a compound of formula A/ MoS Composite nanoparticles;
b.至少一种选自下列物质的助剂:抗氧剂和防锈剂。 b. At least one additive selected from the group consisting of antioxidants and rust inhibitors. the
本发明还提供一种制备润滑脂的方法,包括混合下列组分: The present invention also provides a method for preparing lubricating grease, comprising mixing the following components:
a.一种基础润滑脂; a. A basic grease;
b.一种式A化合物/MoS2复合纳米微粒; b. A compound of formula A/ MoS Composite nanoparticles;
c.至少一种选自下列物质的助剂:抗氧剂和防锈剂。 c. At least one additive selected from the group consisting of antioxidants and rust inhibitors. the
在本发明的润滑脂添加剂、润滑脂以及它们的制备方法中,所使用的式A化合物/MoS2复合纳米微粒——即由式A化合物和MoS2构成的复合物的纳米级的粒子——可以采用下列方法获得:在加热至30-90℃的去离子水中,通惰性气体,然后加入硫代钼酸铵至完全溶解。搅拌下加入式A化合物(式A化合物与硫代钼酸铵的摩尔比优选为0.1∶10-10∶0.1,更优选0.2∶5-5∶0.2,进一步优选为0.5∶2-2∶0.5)和无水乙醇,然后加入盐酸羟胺反应,再加入浓盐酸继续反应,有沉淀生成;沉淀用去离子水及有机溶剂冲洗;将产物干燥,得到式A化合物/MoS2复合纳米微粒。该纳米微粒具有图2所示的红外光谱图。 In the grease additive, grease and their preparation methods of the present invention, the used formula A compound/ MoS Composite nanoparticles—that is, the nanoscale particles of the composite composed of the formula A compound and MoS— It can be obtained by the following method: in deionized water heated to 30-90°C, pass an inert gas, and then add ammonium thiomolybdate until completely dissolved. Add the compound of formula A under stirring (the molar ratio of compound of formula A to ammonium thiomolybdate is preferably 0.1:10-10:0.1, more preferably 0.2:5-5:0.2, further preferably 0.5:2-2:0.5) react with absolute ethanol, then add hydroxylamine hydrochloride, and then add concentrated hydrochloric acid to continue the reaction, and a precipitate is formed; the precipitate is washed with deionized water and an organic solvent; the product is dried to obtain a compound nanoparticle of formula A/MoS 2 . The nanoparticle has an infrared spectrum shown in FIG. 2 .
为本发明的目的,式A化合物/MoS2复合纳米微粒的粒径不高于100nm。 For the purposes of the present invention, the particle size of the compound of formula A/MoS 2 composite nanoparticles is not higher than 100 nm.
在本发明中,“式A化合物”指具有下列分子式的化合物: In the present invention, "compound of formula A" refers to a compound having the following molecular formula:
该化合物可以按下列方式制得:对二硫代二唑硫酮与丁氧基三乙二醇在90-150℃之间反应,然后过滤,得到产物。经表征,产物具有图1所 示的红外光谱图。二硫代二唑硫酮与丁氧基三乙二醇优选以0.1∶10-10∶0.1的摩尔比,更优选以0.2∶5-5∶0.2的摩尔比,最优选以0.2∶1-0.5∶1的摩尔比,在100-140℃,更优选在110-135℃之间反应;反应时间优选为0.5-5小时,更优选为1-3小时,最优选为1.5-2小时。 The compound can be prepared in the following manner: p-dithioxadiazolethione reacts with butoxytriethylene glycol at 90-150°C, and then filters to obtain the product. After characterization, the product has an infrared spectrogram shown in Figure 1. Dithiooxadiazolethione and butoxytriethylene glycol are preferably in a molar ratio of 0.1:10-10:0.1, more preferably in a molar ratio of 0.2:5-5:0.2, most preferably in a molar ratio of 0.2:1-0.5 : 1 molar ratio, react at 100-140°C, more preferably 110-135°C; the reaction time is preferably 0.5-5 hours, more preferably 1-3 hours, most preferably 1.5-2 hours. the
用于本发明的抗氧剂包含但不限于酚型、胺型、含硫、磷、氮化合物。在润滑脂添加剂中,抗氧剂的含量通常为1.0-40%,优选10-35%,更优选25-35%,以所采用的式A化合物/MoS2复合的的纳米微粒的重量为基准。其中,酚型抗氧剂优选2,6-二叔丁基对甲苯酚;胺型抗氧剂优选二苯胺;含硫、磷、氮化合物抗氧剂优选吩噻嗪。 Antioxidants used in the present invention include, but are not limited to, phenolic, amine, sulfur, phosphorus, and nitrogen compounds. In grease additives, the content of antioxidants is usually 1.0-40%, preferably 10-35%, more preferably 25-35%, based on the weight of the nanoparticles of the compound of formula A/ MoS2 . Among them, 2,6-di-tert-butyl-p-cresol is preferred as phenolic antioxidant; diphenylamine is preferred as amine antioxidant; phenothiazine is preferred as antioxidant containing sulfur, phosphorus and nitrogen compounds.
根据本发明的防锈剂包含但不限于有机羧酸类防锈剂、有机胺类防锈剂、硫、氮杂环类防锈剂。在润滑脂添加剂中,防锈剂的含量通常为0.1-40%,优选5.0-35%,更优选10.0-35%,以所采用的式A化合物/MoS2复合纳米微粒的重量为基准。其中,有机羧酸类防锈剂优选十二烯基丁二酸;有机胺类防锈剂优选十二烯基丁二胺,以及2-氨基乙基十七烯基咪唑啉十二烯基丁二酸;氮杂环类防锈剂优选苯并三氮唑。 The rust inhibitors according to the present invention include but not limited to organic carboxylic acid rust inhibitors, organic amine rust inhibitors, sulfur and nitrogen heterocycle rust inhibitors. In the grease additive, the content of the rust inhibitor is generally 0.1-40%, preferably 5.0-35%, more preferably 10.0-35%, based on the weight of the compound of formula A/MoS 2 composite nanoparticles used. Among them, the preferred dodecenyl succinic acid as the organic carboxylic acid rust inhibitor; Diacid; nitrogen heterocyclic rust inhibitor is preferably benzotriazole.
在本发明的润滑脂中,基础润滑脂可以是适于与式A化合物/MoS2复合纳米微粒结合使用的润滑脂,优选为12羟基硬脂酸锂基脂。12羟基硬脂酸锂基脂可以下列原料混合而成:12羟基硬脂酸、基础油(例如500SN的矿油)和氢氧化锂。 In the grease of the present invention, the base grease may be a grease suitable for use in combination with the compound of formula A/MoS 2 composite nanoparticles, preferably 12 hydroxy lithium stearate base grease. 12 hydroxy lithium stearate can be mixed with the following raw materials: 12 hydroxy stearic acid, base oil (such as 500SN mineral oil) and lithium hydroxide.
在本发明的润滑脂中,构成润滑脂添加剂的各组分-即构成润滑脂添加剂的两类物质:一种是式A化合物/MoS2复合纳米微粒;以及至少一种选自下列物质的助剂:抗氧剂和防锈剂——的含量为0.1-10%,优选1.0-8.0%,更优选为2.0-5.0%,以基础润滑脂的重量为基准。 In the grease of the present invention, each component that constitutes a grease additive—that is, two types of substances that constitute a grease additive: one is a compound of formula A/MoS 2 composite nanoparticles; and at least one auxiliary compound selected from the following materials Agents: antioxidants and rust inhibitors—the content is 0.1-10%, preferably 1.0-8.0%, more preferably 2.0-5.0%, based on the weight of the base grease.
为制备本发明的润滑脂添加剂的目的,在将一种式A化合物/MoS2复合纳米微粒与至少一种选自抗氧剂和防锈剂的助剂混合过程中,可以采用加热、搅拌等方法。 For the purpose of preparing the grease additive of the present invention, in the process of mixing a compound of formula A/ MoS2 composite nanoparticles with at least one auxiliary agent selected from antioxidants and rust inhibitors, heating, stirring, etc. can be used method.
为制备本发明的润滑脂的目的,可以先将一种式A化合物/MoS2复合纳米微粒与至少一种选自抗氧剂和防锈剂的助剂混合,制成润滑脂添加剂,然后再将润滑脂添加剂与基础润滑脂混合;也可以直接将一种基础润滑脂、一种式A化合物/MoS2复合纳米微粒与至少一种选自抗氧剂和防锈剂的助剂混合。在两种制备方法中,在各步骤中可以视需要采用加热、搅拌等。 For the purpose of preparing the lubricating grease of the present invention, a kind of formula A compound/ MoS Composite nanoparticles can be mixed with at least one auxiliary agent selected from antioxidants and rust inhibitors to make grease additives, and then The grease additive is mixed with the base grease; it is also possible to directly mix a base grease, a compound of formula A/MoS 2 composite nanoparticles and at least one additive selected from antioxidants and rust inhibitors. In both production methods, heating, stirring, etc. may be employed as necessary in each step.
本发明的润滑脂添加剂可以提高润滑脂产品的抗氧化性能和抑制铜 腐蚀性能。 The lubricating grease additive of the present invention can improve the anti-oxidation performance and inhibit copper corrosion performance of the lubricating grease product. the
实施例 Example
下面将通过实施例说明本发明。本发明包含但不限于以下实施例。在实施例中,12羟基硬脂酸锂基脂为以下列原料混合而成:12羟基硬脂酸,10%(重量百分含量,下同);基础油为500SN的矿油,90%;氢氧化锂,0.8%(以12羟基硬脂酸和基础油的重量总和为基准)。制备的12羟基硬脂酸锂基脂1/4锥入度为64,属2#脂。 The present invention will be illustrated by way of examples below. The present invention includes but is not limited to the following examples. In the embodiment, lithium 12 hydroxystearate is mixed with the following raw materials: 12 hydroxystearic acid, 10% (percentage by weight, the same below); base oil is 500SN mineral oil, 90%; Lithium hydroxide, 0.8% (based on the weight sum of 12 hydroxystearic acid and base oil). The 1/4 cone penetration of the prepared 12-hydroxy lithium stearate is 64, which belongs to 2# grease. the
制备实施例1 Preparation Example 1
式A化合物的制备The preparation of formula A compound
将对二硫代二唑硫酮与丁氧基三乙二醇(分别记为“酮”和“醇”)加入三颈烧瓶中,在一定温度反应若干时间,然后过滤,得到产物。 Add p-dithiooxadiazolethione and butoxytriethylene glycol (respectively denoted as "ketone" and "alcohol") into a three-necked flask, react at a certain temperature for several hours, and then filter to obtain the product. the
经表征,产物具有图1所示的红外光谱图。 After characterization, the product has the infrared spectrum shown in Figure 1. the
共进行16次制备,结果如表1所示: A total of 16 preparations were carried out, and the results are shown in Table 1:
表1式A化合物的制备The preparation of table 1 formula A compound
制备实施例2 Preparation Example 2
式A化合物/MoSFormula A compound/MoS 22 复合纳米微粒I(简称复合纳米微粒I)的制备Preparation of Composite Nanoparticle I (Composite Nanoparticle I for short)
在三口烧瓶中,加入150ml去离子水,加热至85℃,恒温。通氦气10分钟后,加入2.6g硫代钼酸铵至完全溶解。恒温,搅拌下加入1.8g的式A化合物和20ml无水乙醇,然后加入0.7g的盐酸羟胺,反应2小时,再逐渐加入浓盐酸1ml,继续反应6小时,有棕色沉淀生成。沉淀用去离子水、无水乙醇、丙酮大量冲洗。将产物放入真空干燥箱,干燥温度80℃,干燥48小时,得到式A化合物/MoS2复合纳米微粒3.3g。经透射电镜(TEM)表征,发现其粒径为45nm以下。 In a three-neck flask, add 150ml of deionized water, heat to 85°C, and keep the temperature constant. After passing helium for 10 minutes, add 2.6 g of ammonium thiomolybdate until completely dissolved. Constant temperature, add 1.8g of compound of formula A and 20ml of absolute ethanol under stirring, then add 0.7g of hydroxylamine hydrochloride, react for 2 hours, then gradually add 1ml of concentrated hydrochloric acid, continue to react for 6 hours, a brown precipitate is formed. The precipitate was washed with deionized water, absolute ethanol, and acetone in large quantities. The product was put into a vacuum drying oven at a drying temperature of 80° C. for 48 hours to obtain 3.3 g of compound nanoparticles of formula A/MoS 2 . Characterized by transmission electron microscopy (TEM), it was found that the particle size was below 45nm.
所得纳米微粒具有图2所示的红外光谱图。 The obtained nanoparticles have the infrared spectrum shown in FIG. 2 . the
制备实施例3 Preparation Example 3
式A化合物/MoSFormula A compound/MoS 22 复合纳米微粒II(简称复合纳米微粒II)的制备Preparation of Composite Nanoparticle II (abbreviated as Composite Nanoparticle II)
在三口烧瓶中,加入180ml去离子水,加热至70℃,恒温。通氦气35分钟后,加入4.0g硫代钼酸铵至完全溶解。恒温,搅拌下加入2.3g的式A化合物和30ml无水乙醇。然后加入1.2g的盐酸羟胺,反应2小时,再逐渐加入浓盐酸1ml,继续反应6小时,有棕色沉淀生成。沉淀用去离子水、无水乙醇、丙酮大量冲洗。将产物放入真空干燥箱,干燥温度80℃,干燥48小时,得到式A化合物/MoS2复合纳米微粒4.76g。经透射电镜(TEM)表征,发现其粒径为50nm以下。 In a three-necked flask, add 180ml of deionized water, heat to 70°C, and keep the temperature constant. After passing helium for 35 minutes, add 4.0 g of ammonium thiomolybdate until completely dissolved. At constant temperature, 2.3 g of the compound of formula A and 30 ml of absolute ethanol were added under stirring. Then add 1.2 g of hydroxylamine hydrochloride, react for 2 hours, then gradually add 1 ml of concentrated hydrochloric acid, continue to react for 6 hours, a brown precipitate is formed. The precipitate was washed with deionized water, absolute ethanol, and acetone in large quantities. The product was put into a vacuum drying oven at a drying temperature of 80° C. for 48 hours to obtain 4.76 g of compound nanoparticles of formula A/MoS 2 . Characterized by transmission electron microscopy (TEM), it was found that the particle size was below 50nm.
所得纳米微粒具有图2所示的红外光谱图。 The obtained nanoparticles have the infrared spectrum shown in FIG. 2 . the
对比实施例1 Comparative Example 1
含式A化合物的润滑脂的制备以及性能的测试Preparation of grease containing compound of formula A and performance test
采用3g式A化合物与100g 12羟基硬脂酸锂基脂在室温下进行混合,得到润滑脂产品(其中不加入抗氧剂和防锈剂),并根据ASTM D942和ASTM D4048分别进行抗氧化和抗铜腐蚀实验,结果如下所示。 Adopt 3g formula A compound and 100g 12 hydroxy lithium stearate base fats to mix at room temperature, obtain lubricating grease product (wherein do not add antioxidant and antirust agent), and according to ASTM D942 and ASTM D4048 respectively carry out anti-oxidation and ASTM D4048 Anti-copper corrosion test, the results are shown below. the
对比实施例2Comparative Example 2
式A化合物的减摩抗磨性能测试以及抗烧结性能实验Anti-friction and anti-wear performance test and anti-sintering performance experiment of the compound of formula A
1.减摩性能实验 1. Anti-friction performance experiment
分别采用3g的式A化合物、T321和T351(T321和T351是润滑脂常用的极压抗磨添加剂,市售产品,下同),与100g 12羟基硬脂酸锂基脂在室温混合,制得润滑脂产品。对所得产品进行减摩性能实验,实验按照SH/T0189-92进行,采用Serial 201-1284-VD Falex CorporationAurora.1L 60505U.S.A摩擦磨损试验机,电机转速为1200±50r/min,温度为室温,负荷392N,时间40min,评价润滑脂的减摩性能,结果如图3所示(摩擦系数越小越好,代表能有效减少因摩擦而产生的能量损耗)。 Respectively adopt 3g of formula A compound, T 321 and T 351 (T 321 and T 351 are extreme pressure and anti-wear additives commonly used in grease, commercially available products, the same below), and 100g of 12 hydroxy lithium stearate base fat at room temperature Mix to make a grease product. The anti-friction performance test of the obtained product was carried out in accordance with SH/T0189-92, using a Serial 201-1284-VD Falex Corporation Aurora.1L 60505U.SA friction and wear testing machine, the motor speed was 1200±50r/min, and the temperature was room temperature. Load 392N, time 40min, evaluate the anti-friction performance of the grease, the results are shown in Figure 3 (the smaller the friction coefficient, the better, which means that it can effectively reduce the energy loss caused by friction).
图3为采用各种添加剂(分别标示为式A化合物、T321和T351)制得 的润滑脂和12羟基硬脂酸锂基脂(空白脂,不加添加剂)的摩擦系数与时间关系图。从图3可以看出,含式A化合物的润滑脂具有高而不稳定的摩擦系数曲线,其减摩性能不好。 Fig. 3 is the graph of the friction coefficient versus time of lubricating grease and 12 hydroxystearate lithium base grease (blank grease, without additive) prepared by adopting various additives (respectively marked as formula A compound, T 321 and T 351 ) . It can be seen from Figure 3 that the grease containing the compound of formula A has a high and unstable friction coefficient curve, and its anti-friction performance is not good.
2.抗磨性能实验 2. Anti-wear performance experiment
分别采用不同重量比例(以12羟基硬脂酸锂基脂重量为基准)的添加剂,与100g 12羟基硬脂酸锂基脂在室温混合,制得润滑脂产品。对所得产品进行抗磨性能实验。实验按照SH/T0204-92进行,采用Serial201-1284-VD Falex Corporation Aurora.1L 60505U.S.A摩擦磨损试验机,电机转速为1200±50r/min,温度为室温,负荷392N,时间60min,结果如表2所示(磨斑越小,表明抗磨性能越好)。 The additives of different weight ratios (based on the weight of 12 hydroxy lithium stearate) were respectively mixed with 100g of 12 hydroxy lithium stearate at room temperature to prepare a grease product. The anti-wear property test was carried out on the obtained product. The experiment was carried out in accordance with SH/T0204-92, using Serial201-1284-VD Falex Corporation Aurora.1L 60505U.S.A friction and wear testing machine, the motor speed was 1200±50r/min, the temperature was room temperature, the load was 392N, and the time was 60min. The results are shown in the table 2 (the smaller the wear spot, the better the anti-wear performance). the
表2用不同添加剂制得的润滑脂的磨斑直径Table 2 Wear scar diameter of grease prepared with different additives
3.抗烧结性能实验 3. Anti-sintering performance experiment
分别采用不同重量比例(以12羟基硬脂酸锂基脂重量为基准)的添加剂,与100g 12羟基硬脂酸锂基脂在室温混合,制得润滑脂产品。对所得产品进行抗烧结性能实验。实验按照SH/T0202测定,电机转速为1770±60r/min,温度为室温,试验时间10s。以抗烧结性能评价润滑脂极压性能(烧结负荷值越大,极压性能越好)。结果如表3所示。 The additives of different weight ratios (based on the weight of 12 hydroxy lithium stearate) were respectively mixed with 100g of 12 hydroxy lithium stearate at room temperature to prepare a grease product. The anti-sintering performance test was carried out on the obtained product. The experiment is measured according to SH/T0202, the motor speed is 1770±60r/min, the temperature is room temperature, and the test time is 10s. The extreme pressure performance of grease is evaluated by anti-sintering performance (the larger the sintering load value, the better the extreme pressure performance). The results are shown in Table 3. the
表3极压性能实验结果Table 3 Experimental results of extreme pressure performance
对比实施例3Comparative Example 3
润滑脂的制备以及性能的测试Grease preparation and performance testing
将12羟基硬脂酸锂基脂100g与复合纳米微粒I 3g在室温下进行混合,得到润滑脂产品(其中不加入抗氧剂和防锈剂),并根据ASTM D942和ASTM D4048分别进行抗氧化和抗铜腐蚀实验,结果如下所示。 12 hydroxystearic acid lithium base grease 100g is mixed with composite nanoparticle 13g at room temperature, obtains grease product (wherein does not add antioxidant and antirust agent), and carry out oxidation resistance respectively according to ASTM D942 and ASTM D4048 And anti-copper corrosion experiment, the results are shown below. the
实施例1-13 Example 1-13
润滑脂添加剂的制备、润滑脂的制备以及性能的测试 Preparation of grease additives, grease preparation and performance testing
分别取不同重量的制备实施例1-2制备的复合纳米微粒I和II,与不同重量的抗氧剂和防锈剂在室温下混合,得到润滑脂添加剂1-13。 Different weights of composite nanoparticles I and II prepared in Preparation Examples 1-2 were mixed with different weights of antioxidants and antirust agents at room temperature to obtain grease additives 1-13. the
将所得到的润滑脂添加剂1-13分别与基础润滑脂在室温混合,得到润滑脂产品1-13,并根据ASTM D942和ASTM D4048分别进行抗氧化和抗 铜腐蚀实验,结果如下。 The obtained grease additives 1-13 were mixed with the base grease respectively at room temperature to obtain grease products 1-13, and anti-oxidation and copper corrosion tests were carried out according to ASTM D942 and ASTM D4048 respectively, and the results are as follows. the
实施例1 Example 1
原料:复合纳米微粒I 3g,十二烯基丁二酸0.01g,12羟基硬脂酸锂基脂100g。 Raw materials: composite nanoparticles 13g, dodecenyl succinic acid 0.01g, 12 hydroxy lithium stearate 100g. the
实施例2 Example 2
原料:复合纳米微粒II 3g,十二烯基丁二铵0.2g,12羟基硬脂酸锂基脂100g。 Raw materials: 3g of composite nanoparticles II, 0.2g of dodecenyl butanediammonium, 100g of lithium 12 hydroxystearate. the
实施例3 Example 3
原料:复合纳米微粒I 3g,十二烯基丁二胺1g,12羟基硬脂酸锂基脂100g。 Raw materials: composite nanoparticles 1 3g, dodecenyl butanediamine 1g, 12 hydroxy lithium stearate 100g. the
实施例4 Example 4
原料:复合纳米微粒I 3g,2-氨基乙基十七烯基咪唑啉十二烯基丁二酸0.2g,12羟基硬脂酸锂基脂100g。 Raw materials: composite nanoparticle 1 3g, 2-aminoethyl heptadecenyl imidazoline dodecenyl succinic acid 0.2g, 12 hydroxy lithium stearate 100g. the
实施例5 Example 5
原料:复合纳米微粒II 3g,二苯胺0.3g,12羟基硬脂酸锂基脂100g。 Raw materials: 3g of composite nanoparticles II, 0.3g of diphenylamine, 100g of lithium 12 hydroxystearate. the
实施例6 Example 6
原料:复合纳米微粒I 3g,二苯胺1.0g,12羟基硬脂酸锂基脂100g。 Raw materials: composite nanoparticles 1 3g, diphenylamine 1.0g, 12 hydroxy lithium stearate 100g. the
实施例7 Example 7
原料:复合纳米微粒II 3g,2,6-二叔丁基对甲苯酚0.05g,12羟基硬脂酸锂基脂100g。 Raw materials: 3g of composite nanoparticles II, 0.05g of 2,6-di-tert-butyl-p-cresol, and 100g of lithium 12-hydroxystearate. the
实施例8 Example 8
原料:复合纳米微粒I 3g,2,6-二叔丁基对甲苯酚1g,12羟基硬脂酸锂基脂100g。 Raw materials: composite nanoparticles I 3g, 2,6-di-tert-butyl-p-cresol 1g, 12 hydroxy lithium stearate 100g. the
实施例9 Example 9
原料:复合纳米微粒II 3g,二苯胺0.3g,十二烯基丁二酸0.01g,12羟基硬脂酸锂基脂100g。 Raw materials: 3g of composite nanoparticles II, 0.3g of diphenylamine, 0.01g of dodecenylsuccinic acid, 100g of lithium 12 hydroxystearate. the
实施例10 Example 10
原料:复合纳米微粒I 3g,二苯胺1.0g,十二烯基丁二酸0.01g,12羟基硬脂酸锂基脂100g。 Raw materials: composite nanoparticle 1 3g, diphenylamine 1.0g, dodecenyl succinic acid 0.01g, 12 hydroxy lithium stearate 100g. the
实施例11 Example 11
原料:复合纳米微粒II 3g,2,6-二叔丁基对甲苯酚0.05g,十二烯基丁二铵0.2g,12羟基硬脂酸锂基脂100g。 Raw materials: 3g of composite nanoparticles II, 0.05g of 2,6-di-tert-butyl-p-cresol, 0.2g of dodecenyl butanediammonium, and 100g of 12-hydroxy lithium stearate. the
实施例12 Example 12
原料:复合纳米微粒I 3g,2,6-二叔丁基对甲苯酚0.05g,十二烯基丁二胺1g,12羟基硬脂酸锂基脂100g。 Raw materials: composite nanoparticles 1 3g, 2,6-di-tert-butyl-p-cresol 0.05g, dodecenyl butanediamine 1g, 12 hydroxy lithium stearate 100g. the
实施例13 Example 13
原料:复合纳米微粒II 3g,2,6-二叔丁基对甲苯酚1g,2-氨基乙基十七烯基咪唑啉十二烯基丁二酸0.2g,12羟基硬脂酸锂基脂100g。 Raw materials: 3g of composite nanoparticles II, 1g of 2,6-di-tert-butyl-p-cresol, 0.2g of 2-aminoethyl heptadecenyl imidazolinium dodecenyl succinic acid, 12 hydroxy lithium stearate 100g. the
实施例14-22Examples 14-22
润滑脂的制备以及性能的测试Grease preparation and performance testing
分别取不同重量的制备实施例1-2制备的复合纳米微粒I和II,与不同重量的抗氧剂和防锈剂、以及基础润滑脂在室温下混合,得到润滑脂产品14-24,并根据ASTM D942和ASTM D4048分别进行抗氧化和抗铜腐蚀实验,结果如下。 Take different weights of composite nanoparticles I and II prepared in Preparation Example 1-2, mix with different weights of antioxidants and rust inhibitors, and base grease at room temperature to obtain grease products 14-24, and According to ASTM D942 and ASTM D4048, the anti-oxidation and anti-copper corrosion tests were carried out, and the results are as follows. the
实施例14 Example 14
原料:12羟基硬脂酸锂基脂90g,复合纳米微粒II 3g,2-氨基乙基十七烯基咪唑啉十二烯基丁二酸1g。 Raw materials: 90g of lithium 12 hydroxystearate, 3g of composite nanoparticles II, 1g of 2-aminoethylheptadecenylimidazolinium dodecenylsuccinic acid. the
实施例15 Example 15
原料:12羟基硬脂酸锂基脂100g,复合纳米微粒I 3g,苯并三氮唑0.05g。 Raw materials: 12 hydroxy lithium stearate 100g, composite nanoparticle 13g, benzotriazole 0.05g. the
实施例16 Example 16
原料:12羟基硬脂酸锂基脂100g,复合纳米微粒II 3g,苯并三氮唑0.1g。 Raw materials: 12 hydroxy lithium stearate 100g, composite nanoparticles II 3g, benzotriazole 0.1g. the
实施例17 Example 17
原料:12羟基硬脂酸锂基脂100g,复合纳米微粒II 3g,吩噻嗪0.5g。 Raw materials: 12 hydroxy lithium stearate 100g, composite nanoparticles II 3g, phenothiazine 0.5g. the
实施例18 Example 18
原料:12羟基硬脂酸锂基脂75g,复合纳米微粒I 3g,吩噻嗪1.0g。 Raw materials: 12 hydroxy lithium stearate 75g, composite nanoparticles 13g, phenothiazine 1.0g. the
实施例19 Example 19
原料:12羟基硬脂酸锂基脂83g,复合纳米微粒II 3g,2,6-二叔丁基对甲苯酚1g,2-氨基乙基十七烯基咪唑啉十二烯基丁二酸1g。 Raw materials: 83g of lithium 12 hydroxystearate, 3g of composite nanoparticles II, 1g of 2,6-di-tert-butyl-p-cresol, 1g of 2-aminoethylheptadecenyl imidazolinium dodecenylsuccinic acid . the
实施例20 Example 20
原料:12羟基硬脂酸锂基脂95g,复合纳米微粒I 3g,吩噻嗪0.3g,苯并三氮唑0.05g。 Raw materials: 12 hydroxy lithium stearate 95g, composite nanoparticle 13g, phenothiazine 0.3g, benzotriazole 0.05g. the
实施例21 Example 21
原料:12羟基硬脂酸锂基脂100g,复合纳米微粒II 3g,吩噻嗪0.5g,苯并三氮唑0.1g。 Raw materials: 100g of lithium 12 hydroxystearate, 3g of composite nanoparticles II, 0.5g of phenothiazine, and 0.1g of benzotriazole. the
实施例22 Example 22
原料:12羟基硬脂酸锂基脂95g,复合纳米微粒II 3g,吩噻嗪1.0g,苯并三氮唑0.1g。 Raw materials: 95g of lithium 12 hydroxystearate, 3g of composite nanoparticles II, 1.0g of phenothiazine, and 0.1g of benzotriazole. the
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| CN 200610165310 CN101205496B (en) | 2006-12-18 | 2006-12-18 | Grease additive, grease containing the same and preparation thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60202198A (en) | 1984-03-26 | 1985-10-12 | Tokai Rika Co Ltd | Additive for grease |
| CN1359416A (en) * | 1999-10-20 | 2002-07-17 | R·T·范德比尔特公司 | Thiadizole dimer additives and lubricating compositions containing the same |
| CN1796516A (en) * | 2004-12-28 | 2006-07-05 | 中国石油化工股份有限公司 | Lithium base grease in high drop point, and preparation method |
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2006
- 2006-12-18 CN CN 200610165310 patent/CN101205496B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60202198A (en) | 1984-03-26 | 1985-10-12 | Tokai Rika Co Ltd | Additive for grease |
| CN1359416A (en) * | 1999-10-20 | 2002-07-17 | R·T·范德比尔特公司 | Thiadizole dimer additives and lubricating compositions containing the same |
| CN1796516A (en) * | 2004-12-28 | 2006-07-05 | 中国石油化工股份有限公司 | Lithium base grease in high drop point, and preparation method |
Non-Patent Citations (2)
| Title |
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| 张治军等.表面修饰MoS2纳米微粒的XPS研究.河南大学学报25 4.1995,25(4),41-45. * |
| 王淮英等.表面修饰MoS2纳米微粒的合成及摩擦学性能.北京交通大学学报29 6.2005,29(6),55-57. * |
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