JP5516679B2 - Lubricating oil composition - Google Patents
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- JP5516679B2 JP5516679B2 JP2012202885A JP2012202885A JP5516679B2 JP 5516679 B2 JP5516679 B2 JP 5516679B2 JP 2012202885 A JP2012202885 A JP 2012202885A JP 2012202885 A JP2012202885 A JP 2012202885A JP 5516679 B2 JP5516679 B2 JP 5516679B2
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- 239000010687 lubricating oil Substances 0.000 title claims description 56
- 239000000203 mixture Substances 0.000 title claims description 56
- 239000000314 lubricant Substances 0.000 claims description 49
- 239000007787 solid Substances 0.000 claims description 25
- 239000003921 oil Substances 0.000 claims description 23
- 239000002199 base oil Substances 0.000 claims description 18
- 229910052744 lithium Inorganic materials 0.000 claims description 13
- 239000000344 soap Substances 0.000 claims description 13
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 11
- 239000004215 Carbon black (E152) Substances 0.000 claims description 9
- 229930195733 hydrocarbon Natural products 0.000 claims description 9
- 150000002430 hydrocarbons Chemical class 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 7
- 150000002148 esters Chemical class 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000012208 gear oil Substances 0.000 claims description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 4
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 29
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 25
- 239000004810 polytetrafluoroethylene Substances 0.000 description 25
- 230000000052 comparative effect Effects 0.000 description 17
- 239000003963 antioxidant agent Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 239000006185 dispersion Substances 0.000 description 11
- FPLIHVCWSXLMPX-UHFFFAOYSA-M lithium 12-hydroxystearate Chemical compound [Li+].CCCCCCC(O)CCCCCCCCCCC([O-])=O FPLIHVCWSXLMPX-UHFFFAOYSA-M 0.000 description 9
- 230000003078 antioxidant effect Effects 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 8
- 235000014113 dietary fatty acids Nutrition 0.000 description 8
- 239000000194 fatty acid Substances 0.000 description 8
- 229930195729 fatty acid Natural products 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 7
- 150000001412 amines Chemical class 0.000 description 7
- 150000001733 carboxylic acid esters Chemical class 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 125000004432 carbon atom Chemical group C* 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 229920013639 polyalphaolefin Polymers 0.000 description 6
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 5
- 239000012964 benzotriazole Substances 0.000 description 5
- 239000006078 metal deactivator Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 230000005484 gravity Effects 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 4
- 229910003002 lithium salt Inorganic materials 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 3
- XQVWYOYUZDUNRW-UHFFFAOYSA-N N-Phenyl-1-naphthylamine Chemical compound C=1C=CC2=CC=CC=C2C=1NC1=CC=CC=C1 XQVWYOYUZDUNRW-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 125000002029 aromatic hydrocarbon group Chemical group 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical class [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 2
- 150000003014 phosphoric acid esters Chemical class 0.000 description 2
- 229920001083 polybutene Polymers 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 150000003464 sulfur compounds Chemical class 0.000 description 2
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
- WMYJOZQKDZZHAC-UHFFFAOYSA-H trizinc;dioxido-sulfanylidene-sulfido-$l^{5}-phosphane Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([S-])=S.[O-]P([O-])([S-])=S WMYJOZQKDZZHAC-UHFFFAOYSA-H 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- XMKLTEGSALONPH-UHFFFAOYSA-N 1,2,4,5-tetrazinane-3,6-dione Chemical compound O=C1NNC(=O)NN1 XMKLTEGSALONPH-UHFFFAOYSA-N 0.000 description 1
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 description 1
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical class CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 1
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 description 1
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 1
- MDWVSAYEQPLWMX-UHFFFAOYSA-N 4,4'-Methylenebis(2,6-di-tert-butylphenol) Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 MDWVSAYEQPLWMX-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229920002367 Polyisobutene Polymers 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- 150000004651 carbonic acid esters Chemical class 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 150000002019 disulfides Chemical class 0.000 description 1
- LZJUZSYHFSVIGJ-UHFFFAOYSA-N ditridecyl hexanedioate Chemical compound CCCCCCCCCCCCCOC(=O)CCCCC(=O)OCCCCCCCCCCCCC LZJUZSYHFSVIGJ-UHFFFAOYSA-N 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 239000010696 ester oil Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- 239000012170 montan wax Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000002530 phenolic antioxidant Substances 0.000 description 1
- 229950000688 phenothiazine Drugs 0.000 description 1
- 150000002990 phenothiazines Chemical class 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000008301 phosphite esters Chemical class 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 description 1
- IKXFIBBKEARMLL-UHFFFAOYSA-N triphenoxy(sulfanylidene)-$l^{5}-phosphane Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=S)OC1=CC=CC=C1 IKXFIBBKEARMLL-UHFFFAOYSA-N 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Description
本発明は、潤滑油組成物に関する。さらに詳しくは、固体潤滑剤の良好な分散状態を長時間保持しうる潤滑油組成物に関する。 The present invention relates to a lubricating oil composition. More specifically, the present invention relates to a lubricating oil composition that can maintain a good dispersion state of a solid lubricant for a long time.
従来より、摺動部分に使用される潤滑油には、摩擦・摩耗特性の良好なことが要求されており、かかる要求に対して一般的には油性剤、摩耗防止剤、極圧剤を単独または複数配合することが行われている。これらの潤滑油組成物は、金属-金属、金属-樹脂、樹脂-樹脂間の摺動部に使用され、回転、往復動、揺動などの摺動に際し、焼付け、トルク上昇などの不具合なく円滑に行うことを目的に使用されるが、一方で金属、樹脂などの摺動部材に対して、金属の腐食やスラッジの発生や樹脂のクラックや割れの発生などの悪影響を及ぼすことが少なくないといった問題がある。 Conventionally, lubricating oils used for sliding parts have been required to have good friction and wear characteristics. In general, oil-based agents, antiwear agents, and extreme pressure agents are used alone to meet these requirements. Alternatively, a plurality of them are blended. These lubricating oil compositions are used for sliding parts between metal-metal, metal-resin, and resin-resin, and can smoothly run without problems such as seizure and torque increase during sliding such as rotation, reciprocation, and swing. On the other hand, there are many negative effects such as metal corrosion, sludge generation, resin cracking and cracking on sliding members such as metal and resin. There's a problem.
これに対して、潤滑油に、化学的に比較的安定で、層状構造により摩擦特性および極圧性能を発揮する固体潤滑剤として、例えばポリテトラフルオロエチレン樹脂(PTFE)を用いることが行われている。このPTFEは、金属あるいは樹脂を侵す心配がないものの、比重が約2.2と大きく、基油中に分散させた場合に、容易に沈降してしまうといった問題がある。 On the other hand, for example, polytetrafluoroethylene resin (PTFE) is used as a lubricant for a solid lubricant that is chemically relatively stable and exhibits friction characteristics and extreme pressure performance due to a layered structure. Yes. Although PTFE does not have a risk of corroding metal or resin, it has a large specific gravity of about 2.2 and has a problem that it easily settles when dispersed in a base oil.
かかる問題に対して、潤滑油、固体潤滑剤、有機溶剤にさらにワックスを添加することで、固体潤滑剤などの沈降・分離を防止もしくは軽減した、取り扱いやすく、経済性に優れた潤滑油組成物が提案されている。
しかるに、かかる潤滑油組成物は、基油およびPTFEを有機溶剤に分散させ、ディスパージョンの状態で適用部材に塗布し、その後有機溶剤を揮発させることによって潤滑性被膜を形成しなければならず、操作が煩雑であった。 However, such a lubricating oil composition has to form a lubricating film by dispersing base oil and PTFE in an organic solvent, applying the dispersion to an application member, and then volatilizing the organic solvent. The operation was complicated.
本発明の目的は、有機溶剤を用いることなく調製した場合にあっても、潤滑剤の流動性、耐荷重性、摩擦特性を損なうことなく、基油に分散させた固体潤滑剤の分散状態を良好に長時間保持することを可能とする潤滑油組成物を提供することにある。 The object of the present invention is to provide a dispersion state of a solid lubricant dispersed in a base oil without impairing the fluidity, load resistance, and friction characteristics of the lubricant even when prepared without using an organic solvent. An object of the present invention is to provide a lubricating oil composition that can be held well for a long time.
かかる本発明の目的は、合成炭化水素油およびエステル系合成油の少くとも一種からなる基油に、黒鉛、二硫化モリブデンまたはメラミンシアヌレートである固体潤滑剤を組成物中0.1〜5重量％の割合で含有させ、さらに固体潤滑剤量に対して重量比で0.10〜0.50となる量のリチウム系石けん、リチウム系複合石けんまたはウレア系化合物を配合してなり、軸受、ブッシュ、チェーンオイルまたはギヤオイル用途に用いられる潤滑油組成物によって達成される。 An object of the present invention is to add a solid lubricant that is graphite, molybdenum disulfide, or melamine cyanurate to a base oil that is at least one of a synthetic hydrocarbon oil and an ester-based synthetic oil in an amount of 0.1 to 5% by weight. In addition, it contains lithium-based soap, lithium-based composite soap or urea-based compound in an amount of 0.10 to 0.50 by weight with respect to the amount of solid lubricant, and is used for bearings, bushes, chain oil or gear oil. Achieved by the lubricating oil composition used in
本発明の潤滑油組成物は、有機溶剤を用いることなく調製したうえで、リチウム系(複合)石けんまたはウレア系化合物を添加することで、固体潤滑剤の分散状態を良好に長時間保持することが可能であり、さらには潤滑剤の流動性、耐荷重性、摩擦特性を損なうことがないといったすぐれた効果を奏する。かかる効果を奏する本発明の潤滑油組成物は、金属製あるいは樹脂製のいずれの摺動部材に対しても悪影響を及ぼすことが無く、これらの部材に対して有効に適用することができる。また、この潤滑油組成物は、有機溶剤に分散させてディスパージョンあるいはスプレーとしても使用することもできる。 The lubricating oil composition of the present invention can be prepared without using an organic solvent, and a lithium-based (composite) soap or urea-based compound can be added to keep the dispersed state of the solid lubricant well for a long time. In addition, there are excellent effects that the fluidity, load resistance, and friction characteristics of the lubricant are not impaired. The lubricating oil composition of the present invention exhibiting such effects does not adversely affect any of the metallic or resin sliding members and can be effectively applied to these members. The lubricating oil composition can also be used as a dispersion or spray by being dispersed in an organic solvent.
固体潤滑剤としては、黒鉛(比重約2.2)、二硫化モリブデン(比重約4.9)またはメラミンシアヌレート(MCA；比重約1.5)が用いられる。これらの固体潤滑剤は、組成物中0.1〜5重量％、好ましくは0.3〜3重量％を占めるような割合で用いられる。固体潤滑剤が、これ以下の割合で用いられると固体潤滑剤の効果が十分に発揮されず、一方これ以上の割合で用いられると潤滑油組成物の粘度が高くなりすぎてしまい、流動性が失われてしまうようになる。 As the solid lubricant, graphite (specific gravity about 2.2), molybdenum disulfide (specific gravity about 4.9) or melamine cyanurate (MCA; specific gravity about 1.5) is used. These solid lubricants are used in such a proportion that they occupy 0.1 to 5% by weight, preferably 0.3 to 3% by weight in the composition. If the solid lubricant is used at a ratio below this, the effect of the solid lubricant will not be sufficiently exerted. On the other hand, if it is used at a ratio above this, the viscosity of the lubricating oil composition will be too high, and the fluidity will be low. It will be lost.
基油としては、合成炭化水素油およびエステル系合成油の少くとも一種が、好ましくはこれらの混合油が用いられる。合成炭化水素油としては、ポリα-オレフィン、エチレン-α-オレフィンコオリゴマー、ポリブテンまたはこれらの水素化物、アルキルベンゼン、アルキルナフタレン等が、エステル系合成油としては、ポリオールエステル、二塩基性脂肪酸エステル、芳香族多価カルボン酸エステル、リン酸エステル、亜リン酸エステル、炭酸エステル等がそれぞれ例示される。これら二種の基油が混合して用いられる場合には、エステル系合成油が約60〜95重量％の割合で用いられることが好ましい。 As the base oil, at least one synthetic hydrocarbon oils and synthetic ester oils, preferably those mixtures oil is used. Synthetic hydrocarbon oils include poly α-olefins, ethylene-α-olefin co-oligomers, polybutenes or their hydrides, alkylbenzenes, alkyl naphthalenes, etc., and ester-based synthetic oils include polyol esters, dibasic fatty acid esters, Aromatic polyvalent carboxylic acid ester, phosphoric acid ester, phosphorous acid ester, carbonic acid ester and the like are exemplified. When these two types of base oils are used as a mixture, it is preferable to use an ester synthetic oil in a proportion of about 60 to 95% by weight.
これらの基油は、40℃における動粘度(JIS K2283準拠)が約20〜800mm2/秒のものが一般に用いられる。このうち軸受、ブッシュ用途にあっては、約20〜250mm2/秒、好ましくは約20〜100mm2/秒のものが用いられ、またチェーンオイル、ギヤオイルなどあまり低温性を必要とはせず、耐熱性を重視する用途にあっては、約100〜800mm2/秒、好ましくは約100〜400mm2/秒のものが用いられる。ここで、軸受用途としてこれ以上の動粘度の基油を用いると、低温流動性が悪化し、低温域でのトルクの上昇が生じるようになり、一方これ以下の動粘度の基油を用いると、揮発性の点で十分ではなく、さらに高温条件下において十分な油膜を保持することができない。また、あまり低温性を必要とはせず、耐熱性を重視する用途にあっては、これ以上の動粘度の基油を用いると、耐熱性の点では満足されるものの、広範な使用温度範囲内において良好な摺動特性を得るという観点からは好ましくなく、一方これ以下の動粘度の基油を用いると、耐熱性を十分に満足させることができない。 These base oils generally have a kinematic viscosity at 40 ° C. (based on JIS K2283) of about 20 to 800 mm 2 / sec. Of these, for bearings and bushes, those of about 20 to 250 mm 2 / sec, preferably about 20 to 100 mm 2 / sec are used, and chain oil, gear oil, etc. do not require low temperature properties, In applications in which heat resistance is important, a material having a temperature of about 100 to 800 mm 2 / second, preferably about 100 to 400 mm 2 / second is used. Here, if a base oil with a kinematic viscosity higher than this is used as a bearing application, the low temperature fluidity deteriorates and an increase in torque occurs at a low temperature range, while a base oil with a kinematic viscosity lower than this is used. It is not sufficient in terms of volatility, and a sufficient oil film cannot be maintained under high temperature conditions. Also, in applications that do not require low temperature resistance and place importance on heat resistance, using a base oil with a higher kinematic viscosity is satisfactory in terms of heat resistance, but a wide operating temperature range. On the other hand, it is not preferable from the viewpoint of obtaining good sliding characteristics. On the other hand, if a base oil having a kinematic viscosity lower than this is used, the heat resistance cannot be sufficiently satisfied.
固体潤滑剤を0.1〜5重量％で含有する潤滑油組成物中には、リチウム系(複合)石けんまたはウレア系化合物が、固体潤滑剤に対して重量比で0.10〜0.50となるような割合で用いられる。リチウム系(複合)石けんまたはウレア系化合物が、固体潤滑剤に対してこれ以下の割合で用いられると、十分な分散安定性を得ることができず、一方これ以上の割合で用いられると、固体潤滑剤の摩擦低減効果および耐荷重性向上効果が損なわれてしまうため、好ましくない。 In the lubricating oil composition containing 0.1 to 5% by weight of the solid lubricant, the ratio of the lithium (composite) soap or urea compound to the solid lubricant is 0.10 to 0.50 by weight. Used. When lithium-based (composite) soap or urea-based compound is used at a ratio below this relative to the solid lubricant, sufficient dispersion stability cannot be obtained, whereas when used at a ratio above this, solid This is not preferable because the effect of reducing the friction and improving the load resistance of the lubricant is impaired.
リチウム系石けんとしては、(a)炭素数12〜24の脂肪族モノカルボン酸および／または少くとも1個のヒドロキシル基を含む炭素数12〜24の脂肪族モノカルボン酸のリチウム塩、好ましくは12-ヒドロキシステアリン酸リチウム塩が、またリチウム系複合石けんとしては、(a)成分脂肪族モノカルボン酸2種以上のリチウム系複合石けんまたは(a)成分脂肪族モノカルボン酸と(b)炭素数2〜12の脂肪族ジカルボン酸またはそのジエステルおよび炭素数7〜24の芳香族モノカルボン酸またはそのエステルの少くとも一種とのリチウム系複合石けんが用いられる。また、ウレア系化合物としては、ジウレア、トリウレア、テトラウレア、ウレア樹脂等、好ましくはジウレア化合物が用いられる。ジウレア化合物としては、具体的には下記一般式で表されるものなどが挙げられる。
R1NHCONHR2NHCONHR1
R1：炭素数6〜24の1価の脂肪族炭化水素基または
炭素数6〜15の1価の芳香族炭化水素基
R2：炭素数6〜15の2価の芳香族炭化水素基
The lithium-based soap includes (a) a lithium salt of an aliphatic monocarboxylic acid having 12 to 24 carbon atoms and / or an aliphatic monocarboxylic acid having 12 to 24 carbon atoms containing at least one hydroxyl group, preferably 12 -Lithium hydroxystearate salt, and lithium-based composite soap, (a) two or more types of component aliphatic monocarboxylic acid lithium-based composite soap or (a) component aliphatic monocarboxylic acid and (b) 2 carbon atoms Lithium-based complex soaps with ˜12 aliphatic dicarboxylic acids or their diesters and at least one of C7-24 aromatic monocarboxylic acids or their esters are used. As the urea compound, diurea, triurea, tetraurea, urea resin, etc., preferably a diurea compound is used. Specific examples of the diurea compound include those represented by the following general formula.
R 1 NHCONHR 2 NHCONHR 1
R 1 : a monovalent aliphatic hydrocarbon group having 6 to 24 carbon atoms or
Monovalent aromatic hydrocarbon group having 6 to 15 carbon atoms
R 2 : a divalent aromatic hydrocarbon group having 6 to 15 carbon atoms
組成物中には、予め潤滑油に添加する形で、さらに従来潤滑油に添加されている酸化防止剤、防錆剤、腐食防止剤、極圧剤、油性剤、粘度指数向上剤等のその他の添加剤を必要に応じて添加し、潤滑油剤を形成させることができる。酸化防止剤としては、例えば2,6-ジ第3ブチル-4-メチルフェノール、4,4′-メチレンビス(2,6-ジ第3ブチルフェノール)等のフェノール系の酸化防止剤、アルキルジフェニルアミン、トリフェニルアミン、フェニル-α-ナフチルアミン、フェノチアジン、アルキル化フェニル-α-ナフチルアミン、アルキル化フェノチアジン等のアミン系の酸化防止剤、さらにはリン酸系酸化防止剤、イオウ系酸化防止剤などが挙げられる。 In the composition, other additives such as antioxidants, rust inhibitors, corrosion inhibitors, extreme pressure agents, oiliness agents, viscosity index improvers, etc., which have been added to the lubricating oil in advance, are added to the lubricating oil in the past. These additives can be added as necessary to form a lubricant. Examples of the antioxidant include phenolic antioxidants such as 2,6-ditertiarybutyl-4-methylphenol and 4,4′-methylenebis (2,6-ditertiarybutylphenol), alkyldiphenylamine, Examples include amine-based antioxidants such as phenylamine, phenyl-α-naphthylamine, phenothiazine, alkylated phenyl-α-naphthylamine, and alkylated phenothiazine, and phosphoric acid-based antioxidants and sulfur-based antioxidants.
防錆剤としては、例えば脂肪酸、脂肪酸アミン、アルキルスルホン酸金属塩、アルキルスルホン酸アミン塩、酸化パラフィン、ポリオキシエチレンアルキルエーテル等が挙げられ、また腐食防止剤としては、例えばベンゾトリアゾール、ベンゾイミダゾール、チアジアゾール等が挙げられる。 Examples of the rust preventive agent include fatty acids, fatty acid amines, alkyl sulfonic acid metal salts, alkyl sulfonic acid amine salts, oxidized paraffins, polyoxyethylene alkyl ethers, and the like, and corrosion inhibitors include, for example, benzotriazole and benzimidazole. , Thiadiazole and the like.
極圧剤としては、例えばリン酸エステル、亜リン酸エステル、リン酸エステルアミン塩等のリン系化合物、スルフィド類、ジスルフィド類等のイオウ系化合物、ジアルキルジチオリン酸金属塩、ジアルキルジチオカルバミン酸金属塩等のイオウ系化合物金属塩、塩素化パラフィン、塩素化ジフェニル等の塩素系化合物などが挙げられる。 Examples of extreme pressure agents include phosphorous compounds such as phosphate esters, phosphite esters, phosphate ester amine salts, sulfur compounds such as sulfides and disulfides, dialkyldithiophosphate metal salts, and dialkyldithiocarbamic acid metal salts. And sulfur-based compound metal salts, chlorinated paraffin, chlorinated diphenyl and other chlorinated compounds.
油性剤としては、例えば脂肪酸またはそのエステル、高級アルコール、多価アルコールまたはそのエステル、脂肪族アミン、脂肪酸モノグリセライド、モンタンワックス、アミド系ワックス等が挙げられる。また、他の固体潤滑剤としては、例えば窒化ホウ素、窒化シラン等が挙げられる。 Examples of the oily agent include fatty acids or esters thereof, higher alcohols, polyhydric alcohols or esters thereof, aliphatic amines, fatty acid monoglycerides, montan waxes, amide waxes, and the like. Examples of other solid lubricants include boron nitride and silane nitride.
粘度指数向上剤としては、ポリメタクリレート、エチレン-プロピレン共重合体、ポリイソブチレン、ポリアルキルスチレン、スチレン-イソプレン共重合体水素化物等が挙げられる。 Examples of the viscosity index improver include polymethacrylate, ethylene-propylene copolymer, polyisobutylene, polyalkylstyrene, styrene-isoprene copolymer hydride, and the like.
組成物の調製は、基油に予め他の必要な添加剤を添加した潤滑油剤に固体潤滑剤、リチウム系(複合)石けんまたはウレア系化合物を所定量添加し、ホモミキサ、3本ロールまたは高圧ホモジナイザで十分に混練する方法等によって行われる。 The composition is prepared by adding a predetermined amount of a solid lubricant, a lithium (composite) soap or a urea compound to a lubricant obtained by adding other necessary additives to the base oil in advance, and then adding a homomixer, three rolls or a high-pressure homogenizer. In the method of sufficiently kneading.
次に、実施例について本発明を説明する。 Next, the present invention will be described with reference to examples.
参考例１
ペンタエリスリトールC6〜C9カルボン酸エステル 87.1重量％
(コグニス製品、40℃動粘度；23mm2/秒)
合成炭化水素油(イノビーン製品PAO 6、40℃動粘度；31mm2/秒) 10.3重量％
合成炭化水素油(同社製品PAO 40、40℃動粘度；390mm2/秒) 2.6重量％
よりなる混合基油97.9重量部にペンタエリスリトールC6〜C9カルボン酸エステル中にて合成したPMA系粘度指数向上剤(Mw=250,000)1.0重量部、アミン系酸化防止剤(チバ・スペシャルティ・ケミカルズ社製品イルガノックスL57)1.0重量部およびベンゾトリアゾール系金属不活性化剤0.1重量部をホモミキサで配合して、潤滑油剤Aを調製した。この潤滑油剤Aの40℃動粘度は25.3mm2/秒、150℃、100時間の蒸発損失は、18.1重量％であった。
Reference example 1
Pentaerythritol C 6 -C 9 carboxylic acid ester 87.1% by weight
(Cognis product, 40 ° C kinematic viscosity; 23 mm 2 / sec)
Synthetic hydrocarbon oil (Inobean product PAO 6, kinematic viscosity at 40 ℃; 31mm 2 / sec) 10.3% by weight
Synthetic hydrocarbon oil (PAO 40, 40 ° C kinematic viscosity; 390mm 2 / sec) 2.6% by weight
PMA-based viscosity index improver (Mw = 250,000) synthesized in 97.9 parts by weight of a mixed base oil in pentaerythritol C 6 -C 9 carboxylic acid ester, amine antioxidant (Ciba Specialty Chemicals) Lubricant A was prepared by blending 1.0 part by weight of Irganox L57) and 0.1 part by weight of a benzotriazole metal deactivator with a homomixer. The lubricating oil A had a kinematic viscosity at 40 ° C. of 25.3 mm 2 / sec and an evaporation loss of 150 ° C. and 100 hours was 18.1% by weight.
この潤滑油剤A 98.5重量部に、固体潤滑剤としてのPTFE(乳化重合法ポリテトラフルオロエチレン；平均一次粒子径0.2μm；Mn約100,000〜200,000)1重量部および12-ヒドロキシステアリン酸リチウム塩0.5重量部(固体潤滑剤に対する重量比0.50)を混合して潤滑油組成物を調製した。なお、以下の各実施例および比較例でも、同じ粘度指数向上剤、酸化防止剤、金属不活性化剤およびPTFEが用いられた。 In 98.5 parts by weight of this lubricating oil A, 1 part by weight of PTFE (emulsion polymerization polytetrafluoroethylene; average primary particle size 0.2 μm; Mn of about 100,000 to 200,000) as a solid lubricant and 0.5 parts by weight of 12-hydroxystearic acid lithium salt A lubricating oil composition was prepared by mixing parts (weight ratio to solid lubricant 0.50). In the following Examples and Comparative Examples, the same viscosity index improver, antioxidant, metal deactivator and PTFE were used.
参考例２
参考例１において、潤滑油剤A量が98.9重量部に、また12-ヒドロキシステアリン酸リチウム塩量が0.1重量部(同重量比0.10)にそれぞれ変更されて潤滑油組成物が調製された。
Reference example 2
In Reference Example 1, the amount of lubricating oil A was changed to 98.9 parts by weight, and the amount of lithium 12-hydroxystearate was changed to 0.1 parts by weight (the same weight ratio of 0.10) to prepare a lubricating oil composition.
参考例３
参考例１において、潤滑油組成物として潤滑油剤A 93.0重量部、PTFE 5重量部および12-ヒドロキシステアリン酸リチウム塩2重量部(同重量比0.40)を混合したものが用いられた。
Reference example 3
In Reference Example 1, a mixture of 93.0 parts by weight of lubricant A, 5 parts by weight of PTFE, and 2 parts by weight of 12-hydroxylithium stearate (0.40) was used as the lubricating oil composition.
参考例４
トリメチロールプロパンC8〜C12カルボン酸エステル 72.9重量％
(コグニス製品、40℃動粘度；18mm2/秒)
合成炭化水素油(PAO 6、40℃動粘度；31mm2/秒) 20.8重量％
合成炭化水素油(PAO 40、40℃動粘度；390mm2/秒) 6.3重量％
よりなる混合基油90.9重量部にPMA系粘度指数向上剤8.0重量部、アミン系酸化防止剤1.0重量部およびベンゾトリアゾール系金属不活性化剤0.1重量部を配合して、潤滑油剤Bを調製した。この潤滑油剤Bの40℃動粘度は60.3mm2/秒、150℃、100時間の蒸発損失は、21.5重量％であった。
Reference example 4
Trimethylolpropane C 8 -C 12 carboxylic acid ester 72.9% by weight
(Cognis product, 40 ° C kinematic viscosity; 18 mm 2 / sec)
Synthetic hydrocarbon oil (PAO 6, 40 ° C kinematic viscosity; 31mm 2 / sec) 20.8% by weight
Synthetic hydrocarbon oil (PAO 40, 40 ° C kinematic viscosity; 390 mm 2 / sec) 6.3 wt%
Lubricant B was prepared by blending 8.0 parts by weight of PMA viscosity index improver, 1.0 parts by weight of amine antioxidant and 0.1 parts by weight of benzotriazole metal deactivator with 90.9 parts by weight of mixed base oil. . The lubricating oil B had a kinematic viscosity at 40 ° C. of 60.3 mm 2 / sec and an evaporation loss of 100 ° C. for 100 hours was 21.5% by weight.
この潤滑油剤B 96.7重量部に、PTFE 3重量部および12-ヒドロキシステアリン酸リチウム塩0.3重量部(同重量比0.10)を混合して潤滑油組成物を調製した。 A lubricating oil composition was prepared by mixing 36.7 parts by weight of PTFE and 0.3 part by weight of lithium 12-hydroxystearate (0.10 weight ratio) with 96.7 parts by weight of this lubricant B.
参考例５
合成炭化水素油(イノビーン製品PAO 10、40℃動粘度；68mm2/秒) 98.9重量％
アミン系酸化防止剤 1.0重量％
ベンゾトリアゾール系金属不活性化剤 0.1重量％
を配合して、潤滑油剤Cを調製した。この潤滑油剤Cの40℃動粘度は69.1mm2/秒、150℃、100時間の蒸発損失は、34.5重量％であった。
Reference Example 5
Synthetic hydrocarbon oil (Inobean product PAO 10, kinematic viscosity at 40 ℃; 68mm 2 / sec) 98.9wt%
Amine antioxidant 1.0% by weight
Benzotriazole metal deactivator 0.1% by weight
Was added to prepare Lubricant C. The lubricating oil C had a kinematic viscosity at 40 ° C. of 69.1 mm 2 / sec and an evaporation loss of 100 ° C. for 100 hours was 34.5% by weight.
この潤滑油剤C 98.5重量部に、PTFE 1重量部および12-ヒドロキシステアリン酸リチウム塩0.5重量部(同重量比0.50)を混合して潤滑油組成物を調製した。 A lubricating oil composition was prepared by mixing 18.5 parts by weight of PTFE and 0.5 parts by weight of 12-hydroxystearic acid lithium salt (same weight ratio of 0.50) with 98.5 parts by weight of this lubricant C.
参考例６
参考例１において、潤滑油組成物として潤滑油剤A 96.5重量部、PTFE 3重量部およびジウレア化合物(トリレンジイソシアネートとアニリンとの反応生成物)0.5重量部(同重量比0.17)を混合したものが用いられた。
Reference Example 6
In Reference Example 1, 96.5 parts by weight of lubricating oil A, 3 parts by weight of PTFE, and 0.5 parts by weight (reaction product of tolylene diisocyanate and aniline) (same weight ratio 0.17) were mixed as the lubricating oil composition. Used.
参考例７
参考例４において、潤滑油組成物として潤滑油剤B 94.0重量部、PTFE 5重量部および複合脂肪酸リチウム塩(12-ヒドロキシステアリン酸リチウムとアゼライン酸との複合石けん)1重量部(同重量比0.20)を混合したものが用いられた。
Reference Example 7
In Reference Example 4, 94.0 parts by weight of lubricant B as a lubricating oil composition, 5 parts by weight of PTFE, and 1 part by weight of a composite fatty acid lithium salt (composite soap of lithium 12-hydroxystearate and azelaic acid) (0.20 in the same weight ratio) A mixture of was used.
参考例８
アジピン酸ジトリデシル(大八化学製品、40℃動粘度；24mm2/秒) 98.9重量％
アミン系酸化防止剤 1.0重量％
ベンゾトリアゾール系金属不活性化剤 0.1重量％
を配合して、潤滑油剤Dを調製した。この潤滑油剤Dの40℃動粘度は24.9mm2/秒、150℃、100時間の蒸発損失は、25.0重量％であった。
Reference Example 8
Ditridecyl adipate (Daihachi Chemical Products, Kinematic viscosity at 40 ° C; 24mm 2 / sec) 98.9% by weight
Amine antioxidant 1.0% by weight
Benzotriazole metal deactivator 0.1% by weight
Was added to prepare Lubricant D. The lubricating oil D had a kinematic viscosity at 40 ° C. of 24.9 mm 2 / sec and an evaporation loss of 100 ° C. for 100 hours was 25.0% by weight.
この潤滑油剤D 98.9重量部に、PTFE 1重量部および12-ヒドロキシステアリン酸リチウム塩0.1重量部(同重量比0.10)を混合して潤滑油組成物を調製した。 A lubricating oil composition was prepared by mixing 18.9 parts by weight of PTFE and 0.1 parts by weight of lithium 12-hydroxystearate (same weight ratio of 0.10) with 98.9 parts by weight of this lubricant D.
参考例９
トリメチロールプロパンC8〜C12カルボン酸エステル 65.0重量％
(コグニス製品、40℃動粘度；18mm2/秒)
ポリブテン 30.0重量％
アミン系酸化防止剤 2.5重量％
C12ジチオリン酸亜鉛塩 2.5重量％
を配合して、潤滑油剤Eを調製した。この潤滑油剤Eの40℃動粘度は105mm2/秒、150℃、100時間の蒸発損失は、10.5重量％であった。
Reference Example 9
Trimethylolpropane C 8 -C 12 carboxylic acid ester 65.0 wt%
(Cognis product, 40 ° C kinematic viscosity; 18 mm 2 / sec)
Polybutene 30.0% by weight
Amine antioxidant 2.5% by weight
C 12 zinc dithiophosphate 2.5% by weight
Was added to prepare lubricating oil E. The lubricating oil E had a kinematic viscosity at 40 ° C. of 105 mm 2 / sec and an evaporation loss of 100 ° C. for 100 hours was 10.5% by weight.
この潤滑剤E 94重量部に、PTFE 5重量部および前記複合脂肪酸リチウム塩1重量部(同重量比0.20)を混合して潤滑油組成物を調製した。 A lubricating oil composition was prepared by mixing 94 parts by weight of this lubricant E with 5 parts by weight of PTFE and 1 part by weight of the above complex fatty acid lithium salt (same weight ratio: 0.20).
参考例１０
ジペンタエリスリトールC8〜C10カルボン酸エステル 70.0重量％
(コグニス製品、40℃動粘度；280mm2/秒)
トリメリット酸C8〜C10カルボン酸エステル 25.5重量％
(花王製品、40℃動粘度；46mm2/秒)
トリフェニルフォスフォロチオネート 1.0重量％
(チバ・スペシャルティ・ケミカルズ社製品；リン系摩耗防止剤)
C12ジチオリン酸亜鉛塩 1.0重量％
アミン系酸化防止剤 2.5重量％
を配合して、潤滑油剤Fを調製した。この潤滑油剤Fの40℃動粘度は300mm2/秒、150℃、100時間の蒸発損失は、4.7重量％であった。
Reference Example 10
Dipentaerythritol C 8 -C 10 carboxylic acid ester 70.0 wt%
(Cognis product, 40 ° C kinematic viscosity; 280mm 2 / sec)
Trimellitic acid C 8 to C 10 carboxylic acid ester 25.5% by weight
(Kao product, kinematic viscosity at 40 ℃; 46mm 2 / sec)
Triphenyl phosphorothioate 1.0% by weight
(Ciba Specialty Chemicals product; Phosphorous wear inhibitor)
C 12 zinc dithiophosphate 1.0% by weight
Amine antioxidant 2.5% by weight
Was added to prepare Lubricant F. The lubricating oil F had a kinematic viscosity at 40 ° C. of 300 mm 2 / sec, an evaporation loss at 150 ° C. for 100 hours of 4.7% by weight.
この潤滑剤F 96.5重量部に、PTFE 3重量部およびジウレア化合物(トリレンジイソシアネートとアニリンとの反応生成物)0.5重量部(同重量比0.17)を混合して潤滑油組成物を調製した。 A lubricating oil composition was prepared by mixing 96.5 parts by weight of this lubricant F with 3 parts by weight of PTFE and 0.5 part by weight (reaction product of tolylene diisocyanate and aniline) (same weight ratio of 0.17).
比較例１
参考例１において、潤滑油組成物として潤滑油剤A 96.95重量部、PTFE 3重量部および12-ヒドロキシステアリン酸リチウム塩0.05重量部(同重量比0.02)を混合したものが用いられた。
Comparative Example 1
In Reference Example 1, a mixture of 96.95 parts by weight of lubricant A, 3 parts by weight of PTFE and 0.05 parts by weight of 12-hydroxystearic acid lithium salt (0.02 in the same weight ratio) was used as the lubricating oil composition.
比較例２
参考例１において、潤滑油組成物として潤滑油剤A 85重量部、PTFE 10重量部および12-ヒドロキシステアリン酸リチウム塩5重量部(同重量比0.50)を混合したものが用いられた。
Comparative Example 2
In Reference Example 1, a mixture of 85 parts by weight of lubricant A, 10 parts by weight of PTFE, and 5 parts by weight of 12-hydroxylithium stearate (0.50 by weight) was used as the lubricant composition.
比較例３
参考例１において、潤滑油組成物として潤滑油剤A 82重量部、PTFE 10重量部およびジウレア化合物(トリレンジイソシアネートとアニリンとの反応生成物)8重量部(同重量比0.80)を混合したものが用いられた。
Comparative Example 3
In Reference Example 1, 82 parts by weight of lubricating oil A, 10 parts by weight of PTFE, and 8 parts by weight (reaction product of tolylene diisocyanate and aniline) (a weight ratio of 0.80) were mixed as a lubricating oil composition. Used.
比較例４
参考例４において、潤滑油組成物として潤滑油剤B 85重量部、PTFE 10重量部および複合脂肪酸リチウム塩5重量部(同重量比0.50)を混合したものが用いられた。
Comparative Example 4
In Reference Example 4, a mixture of 85 parts by weight of lubricant B, 10 parts by weight of PTFE, and 5 parts by weight of a composite fatty acid lithium salt (0.50 in the same weight ratio) was used as the lubricating oil composition.
比較例５
参考例１において、潤滑油組成物として潤滑油剤A 98重量部、PTFE 1重量部および12-ヒドロキシステアリン酸リチウム塩1重量部(同重量比1.00)を混合したものが用いられた。
Comparative Example 5
In Reference Example 1, as the lubricating oil composition, a mixture of 98 parts by weight of lubricating oil A, 1 part by weight of PTFE and 1 part by weight of 12-hydroxystearic acid lithium salt (1.00 weight ratio) was used.
比較例６
参考例５において、潤滑油組成物として潤滑油剤C 95重量部、PTFE 3重量部および12-ヒドロキシステアリン酸リチウム塩2重量部(同重量比0.67)を混合したものが用いられた。
Comparative Example 6
In Reference Example 5, a mixture of 95 parts by weight of lubricant C, 3 parts by weight of PTFE, and 2 parts by weight of 12-hydroxylithium stearate (0.67 in the same weight ratio) was used as the lubricating oil composition.
比較例７
参考例10において、潤滑油組成物として潤滑剤F92重量部、PTFE 5重量部および12-ヒドロキシステアリン酸リチウム塩3重量部(同重量比0.60)を混合したものが用いられた。
Comparative Example 7
In Reference Example 10, a mixture of 92 parts by weight of lubricant F, 5 parts by weight of PTFE and 3 parts by weight of 12-hydroxystearic acid lithium salt (same weight ratio: 0.60) was used as the lubricating oil composition.
実施例１〜８
参考例２、４〜１０において、それぞれPTFEの代わりに黒鉛(日本黒鉛製品J-CPB、平均粒径；5μm)が同量用いられた。
Examples 1-8
In Reference Examples 2 and 4 to 10 , the same amount of graphite (Japanese graphite product J-CPB, average particle size: 5 μm) was used instead of PTFE.
実施例９〜１３
参考例２、４〜７において、それぞれPTFEの代わりに二硫化モリブデン(大東潤滑製品LM13-SMパウダー、平均粒径；0.4μm)が同量用いられた。
Examples 9-13
In Reference Examples 2 and 4 to 7, the same amount of molybdenum disulfide (Daito Lubricated Product LM13-SM powder, average particle size: 0.4 μm) was used instead of PTFE.
実施例１４〜１８
参考例２、４〜７において、それぞれPTFEの代わりにMCA(日産化学製品MCA-6000、平均粒径；1〜5μm)が同量用いられた。
Examples 14-18
In Reference Examples 2 and 4 to 7, the same amount of MCA (Nissan Chemical Product MCA-6000, average particle size; 1 to 5 μm) was used instead of PTFE.
以上の各参考例、実施例および比較例で得られた潤滑油組成物について、流動性、分散安定性の検討を行った。
流動性：コーンプレート型レオメータを使用して、25℃、せん断速度300/秒の条件下における粘度を測定し、5,000mPa・秒以下のものを流動性良好と評価した
分散性：10ml目盛り付き沈降管に、合成油中に各実施例および比較例で得られた潤滑油組成物10mlを入れて撹拌後一週間静置し、分散した固体潤滑剤粒子の沈降状態を目視により確認することにより、粒子が凝集して沈降することなく、均一な分散液が得られたものを分散性良好と評価した
The fluidity and dispersion stability of the lubricating oil compositions obtained in the above Reference Examples, Examples and Comparative Examples were examined.
Fluidity: Viscosity was measured using a cone-plate rheometer at 25 ° C and a shear rate of 300 / sec, and 5,000 mPa · sec or less was evaluated as good fluidity. Dispersibility: Sedimentation with a 10 ml scale In the tube, put 10 ml of the lubricating oil composition obtained in each Example and Comparative Example in the synthetic oil, leave it for one week after stirring, and visually confirm the sedimentation state of the dispersed solid lubricant particles. The one in which a uniform dispersion was obtained without causing the particles to aggregate and settle was evaluated as having good dispersibility.
その結果、各参考例、各実施例および比較例５〜７で得られた潤滑油組成物では、流動性、分散安定性のいずれも良好であったが、比較例１で得られた潤滑油組成物では、流動性は良好なものの、分散安定性が不十分であり、比較例２〜４で得られた潤滑油組成物では、分散安定性は良好ではあるものの、流動性が悪く、潤滑油として機能しないものであった。 As a result, in the lubricating oil compositions obtained in the respective reference examples, the respective examples and the comparative examples 5 to 7, both the fluidity and the dispersion stability were good, but the lubricating oil obtained in the comparative example 1 In the composition, although the fluidity is good, the dispersion stability is insufficient. In the lubricating oil compositions obtained in Comparative Examples 2 to 4, although the dispersion stability is good, the fluidity is poor and lubrication is performed. It did not function as oil.
また、各潤滑油組成物を用いて摺動特性試験(耐荷重性の評価および摩擦係数を測定)が行われた。耐荷重性は、SRV摩擦試験機を用いて、下部試験片をSUJ2製ディスク、上部試験片を10mm径のSUJ2製球とし、これらを点接触させ、振動数50Hz、振幅1mm、温度100℃の条件下で、1分毎に荷重を50Nずつ増加させ、これを500Nに達するまで連続して行い、焼付きが発生しない最大荷重により評価を行い、また摩擦係数を各荷重毎に測定した。ここで試験温度を100℃としたのは、油膜を保持されにくくするためである。 In addition, a sliding property test (evaluation of load resistance and measurement of friction coefficient) was performed using each lubricating oil composition. Using a SRV friction tester, the load resistance was measured using a SUJ2 disk for the lower test piece and a SUJ2 ball of 10 mm diameter for the upper test piece, which were point-contacted, with a frequency of 50 Hz, an amplitude of 1 mm, and a temperature of 100 ° C. Under the conditions, the load was increased by 50N every minute, this was continuously performed until it reached 500N, the maximum load at which seizure did not occur was evaluated, and the friction coefficient was measured for each load. The reason for setting the test temperature to 100 ° C. is to make it difficult to hold the oil film.
得られた結果は、次の表に示される。流動性、分散安定性が良好であった比較例５〜６の潤滑油組成物は、それぞれ対応する参考例の数値に比べて摩擦係数が大きく、耐荷重性に劣っていることが示される。また、比較例７の潤滑油組成物は、参考例10に比べて摩擦係数の値が大きくなっている。
表
荷重(N)／接触面圧(N/mm 2 )
耐荷重 50/ 100/ 150/ 200/ 250/ 300/ 350/ 400/ 450/ 500/
例 性(N) 105 149 183 211 236 258 279 298 316 333
参考例１ ＞500 0.142 0.126 0.125 0.116 0.114 0.113 0.113 0.103 0.102 0.101
〃 ２ 450 0.131 0.115 0.112 0.107 0.107 0.099 0.105 0.102 0.102 -
〃 ３ 450 0.113 0.110 0.106 0.105 0.103 0.097 0.095 0.100 0.100 -
〃 ４ 450 0.135 0.130 0.115 0.109 0.105 0.103 0.100 0.099 0.098 -
〃 ５ 450 0.217 0.209 0.190 0.173 0.160 0.152 0.151 0.150 0.149 -
〃 ６ ＞500 0.149 0.124 0.119 0.116 0.114 0.110 0.108 0.107 0.106 0.104
〃 ７ ＞500 0.125 0.117 0.115 0.111 0.107 0.103 0.101 0.100 0.100 0.098
〃 ８ ＞500 0.130 0.112 0.107 0.105 0.102 0.100 0.099 0.098 0.098 0.098
〃 ９ 450 0.127 0.108 0.105 0.103 0.101 0.100 0.100 0.099 0.099 -
〃 10 ＞500 0.143 0.129 0.118 0.115 0.111 0.108 0.105 0.103 0.101 0.101
比較例５ 300 0.153 0.140 0.145 0.141 0.143 0.147 - - - -
〃 ６ 300 0.287 0.229 0.190 0.185 0.177 0.169 - - - -
〃 ７ ＞500 0.166 0.153 0.149 0.144 0.140 0.137 0.135 0.133 0.132 0.131
実施例１ 450 0.146 0.119 0.106 0.103 0.102 0.100 0.099 0.099 0.098 -
〃 ２ 450 0.135 0.116 0.108 0.105 0.102 0.101 0.100 0.100 0.100 -
〃 ３ 400 0.227 0.215 0.201 0.193 0.180 0.167 0.151 0.140 - -
〃 ４ ＞500 0.141 0.121 0.110 0.107 0.103 0.102 0.102 0.101 0.101 0.101
〃 ５ 450 0.132 0.112 0.108 0.105 0.102 0.100 0.099 0.098 0.098 -
〃 ６ 450 0.133 0.115 0.110 0.106 0.104 0.101 0.100 0.100 0.099 -
〃 ７ 450 0.130 0.113 0.108 0.105 0.104 0.102 0.101 0.101 0.100 -
〃 ８ ＞500 0.145 0.132 0.125 0.119 0.113 0.110 0.109 0.107 0.105 0.103
〃 ９ ＞500 0.136 0.129 0.130 0.131 0.126 0.119 0.114 0.106 0.103 0.103
〃 10 450 0.134 0.130 0.125 0.120 0.113 0.107 0.105 0.103 0.100 0.100
〃 11 450 0.222 0.217 0.209 0.200 0.185 0.177 0.169 0.160 0.155 -
〃 12 ＞500 0.137 0.132 0.125 0.121 0.116 0.110 0.107 0.105 0.104 0.103
〃 13 450 0.133 0.124 0.121 0.117 0.110 0.106 0.104 0.102 0.100 -
〃 14 450 0.151 0.117 0.108 0.107 0.105 0.103 0.101 0.100 0.100 -
〃 15 400 0.140 0.113 0.107 0.105 0.102 0.098 0.097 0.110 - -
〃 16 400 0.227 0.217 0.210 0.199 0.187 0.181 0.167 0.160 - -
〃 17 450 0.145 0.120 0.113 0.110 0.106 0.104 0.103 0.102 0.102 -
〃 18 400 0.141 0.110 0.107 0.103 0.100 0.099 0.099 0.098 - -
注） 比較例５〜７では、固体潤滑剤に対する12-ヒドロキシステアリン酸リチ ウム塩の比率が高く、固体潤滑剤の効果が発揮されなかった。
The results obtained are shown in the following table. It is shown that the lubricating oil compositions of Comparative Examples 5 to 6 having good fluidity and dispersion stability have large friction coefficients and inferior load resistance compared to the numerical values of the corresponding reference examples. In addition, the lubricating oil composition of Comparative Example 7 has a larger coefficient of friction than that of Reference Example 10.
table
Load (N) / Contact surface pressure (N / mm 2 )
Withstand load 50/100/150/200/250/300/350/400/450/500 /
Example (N) 105 149 183 211 236 258 279 298 316 333
Reference Example 1> 500 0.142 0.126 0.125 0.116 0.114 0.113 0.113 0.103 0.102 0.101
〃 2 450 0.131 0.115 0.112 0.107 0.107 0.099 0.105 0.102 0.102-
３ 3 450 0.113 0.110 0.106 0.105 0.103 0.097 0.095 0.100 0.100-
４ 4 450 0.135 0.130 0.115 0.109 0.105 0.103 0.100 0.099 0.098-
450 5 450 0.217 0.209 0.190 0.173 0.160 0.152 0.151 0.150 0.149-
６ 6> 500 0.149 0.124 0.119 0.116 0.114 0.110 0.108 0.107 0.106 0.104
〃 7> 500 0.125 0.117 0.115 0.111 0.107 0.103 0.101 0.100 0.100 0.098
８ 8> 500 0.130 0.112 0.107 0.105 0.102 0.100 0.099 0.098 0.098 0.098
９ 9 450 0.127 0.108 0.105 0.103 0.101 0.100 0.100 0.099 0.099-
〃 10> 500 0.143 0.129 0.118 0.115 0.111 0.108 0.105 0.103 0.101 0.101
Comparative Example 5 300 0.153 0.140 0.145 0.141 0.143 0.147----
〃 6 300 0.287 0.229 0.190 0.185 0.177 0.169----
〃 7> 500 0.166 0.153 0.149 0.144 0.140 0.137 0.135 0.133 0.132 0.131
Example 1 450 0.146 0.119 0.106 0.103 0.102 0.100 0.099 0.099 0.098-
〃 2 450 0.135 0.116 0.108 0.105 0.102 0.101 0.100 0.100 0.100-
〃 3 400 0.227 0.215 0.201 0.193 0.180 0.167 0.151 0.140--
４ 4 > 500 0.141 0.121 0.110 0.107 0.103 0.102 0.102 0.101 0.101 0.101
450 5 450 0.132 0.112 0.108 0.105 0.102 0.100 0.099 0.098 0.098-
６ 6 450 0.133 0.115 0.110 0.106 0.104 0.101 0.100 0.100 0.099-
450 7 450 0.130 0.113 0.108 0.105 0.104 0.102 0.101 0.101 0.100-
８ 8 > 500 0.145 0.132 0.125 0.119 0.113 0.110 0.109 0.107 0.105 0.103
〃 9 > 500 0.136 0.129 0.130 0.131 0.126 0.119 0.114 0.106 0.103 0.103
450 10 450 0.134 0.130 0.125 0.120 0.113 0.107 0.105 0.103 0.100 0.100
〃 11 450 0.222 0.217 0.209 0.200 0.185 0.177 0.169 0.160 0.155-
〃 12 > 500 0.137 0.132 0.125 0.121 0.116 0.110 0.107 0.105 0.104 0.103
〃 13 450 0.133 0.124 0.121 0.117 0.110 0.106 0.104 0.102 0.100-
〃 14 450 0.151 0.117 0.108 0.107 0.105 0.103 0.101 0.100 0.100-
〃 15 400 0.140 0.113 0.107 0.105 0.102 0.098 0.097 0.110--
〃 16 400 0.227 0.217 0.210 0.199 0.187 0.181 0.167 0.160--
450 17 450 0.145 0.120 0.113 0.110 0.106 0.104 0.103 0.102 0.102-
〃 18 400 0.141 0.110 0.107 0.103 0.100 0.099 0.099 0.098--
Note) In Comparative Examples 5 to 7, the ratio of 12-hydroxystearic acid salt to the solid lubricant was high, and the effect of the solid lubricant was not exhibited.
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| US10145417B2 (en) * | 2016-06-30 | 2018-12-04 | Minebea Mitsumi Inc. | Grease composition-filled ball bearing, pivot assembly bearing including the ball bearing, and hard disk drive including the pivot assembly bearing |
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| JP5808775B2 (en) * | 2013-07-05 | 2015-11-10 | 株式会社椿本チエイン | Lubricant composition for chain and chain |
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