CN103003399B - 具有改进的密封和腐蚀性能的低灰分润滑剂 - Google Patents
具有改进的密封和腐蚀性能的低灰分润滑剂 Download PDFInfo
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- CN103003399B CN103003399B CN201180035171.2A CN201180035171A CN103003399B CN 103003399 B CN103003399 B CN 103003399B CN 201180035171 A CN201180035171 A CN 201180035171A CN 103003399 B CN103003399 B CN 103003399B
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Classifications
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- 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
- C10M165/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a compound of unknown or incompletely defined constitution, each of these compounds being essential
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- 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
- C10M141/08—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 sulfur-, selenium- or tellurium-containing compound
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- C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
- C10M103/02—Carbon; Graphite
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- C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
- C10M103/06—Metal compounds
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- C10M105/02—Well-defined hydrocarbons
- C10M105/04—Well-defined hydrocarbons aliphatic
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- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/02—Well-defined hydrocarbons
- C10M105/06—Well-defined hydrocarbons aromatic
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- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
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- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
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- C10M105/14—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms polyhydroxy
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- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
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- C10M105/16—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen having hydroxy groups bound to a carbon atom of a six-membered aromatic ring
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- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/18—Ethers, e.g. epoxides
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- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/20—Aldehydes; Ketones
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- C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
- C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
- C10M133/04—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M133/12—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to a carbon atom of a six-membered aromatic ring
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- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
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- C10M163/00—Lubricating compositions characterised by the additive being a mixture of a compound of unknown or incompletely defined constitution and a non-macromolecular compound, each of these compounds being essential
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
- C10M135/08—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium containing a sulfur-to-oxygen bond
- C10M135/10—Sulfonic acids or derivatives thereof
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- C10M149/00—Lubricating compositions characterised by the additive being a macromolecular compound containing nitrogen
- C10M149/12—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M149/14—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds a condensation reaction being involved
- C10M149/16—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds a condensation reaction being involved between the nitrogen-containing monomer and an aldehyde or ketone
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- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
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- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
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Abstract
具有如下组分的润滑剂组合物提供良好的密封和腐蚀性能：(a)具有润滑粘度的油；(b)包含羧酸官能化聚合物与具有至少3个芳环和至少一个伯或仲氨基的芳香胺的缩合产物的分散剂；和(c)包含油溶性中性金属盐组分和金属碳酸盐组分的过碱性金属清净剂。润滑剂组合物中中性金属盐组分的总量为至少约0.75重量%且润滑剂组合物的硫酸盐化灰分含量少于约1.1%。
Description
发明背景
所公开的技术涉及润滑剂，特别是用于内燃机，包括柴油机的润滑剂，其显示出低灰分配制剂中良好的密封性能和腐蚀性能。
用于内燃机的润滑剂是熟知的。例如，美国专利6,444,624，Walker等人，2002年9月3日公开了包含如下组分的润滑油组合物：0至小于10%的组I和/或组II基本油料(basestock)、提供给润滑剂不大于1000ppm钼的钼添加剂、提供10或更大毫摩尔表面活性剂/kg润滑剂的钙清净剂、一种或多种尤其选自无灰分散剂和粘度改进剂的其它润滑剂添加剂。
美国专利7,361,629，Loper等人，2008年4月22日公开了烃基取代的琥珀酸酰化剂与含有脂族多胺和芳族多胺的混合物的胺化产物。在芳族多胺中，公开了N-苯基-1,4-苯二胺。
美国专利4,863,623，Nalesnik，1989年9月5日公开了包含接枝共聚物和胺衍生的共聚物的添加剂组合物。它公开了尤其包括N-芳基苯二胺的氨基-芳族多胺化合物。还提供了包含它的润滑油组合物。
所公开的技术通过使用如本文所述的添加剂组合而解决了低灰分发动机润滑剂中的腐蚀和密封劣化的问题。
发明概述
所公开的技术提供了包含如下组分的润滑剂组合物：(a)具有润滑粘度的油；(b)包含羧酸官能化聚合物与具有至少3个芳环和至少一个伯或仲氨基的芳香胺的缩合产物的分散剂；和(c)包含油溶性中性金属盐组分和金属碳酸盐组分的过碱性金属清净剂；其中润滑剂组合物中的中性金属盐组分(来自过碱性清净剂)的总量为(组合物的)至少约0.75重量%且其中润滑剂组合物的硫酸盐化灰分含量少于约1.1%。
所公开的技术进一步提供了润滑内燃机的方法，其包括向内燃机提供以上润滑剂。
发明详述
下面通过非限定性阐述描述各个优选特征和实施方案。
除非另外说明，所述各化学组分的量表示为排除了通常可存在于商业材料中的任何溶剂或稀释油，即基于活性化学成分。然而，除非另外说明，本文提及的各个化学成分或组合物应当理解为可含有异构体、副产物、衍生物和通常理解存在于商品级中的其它这类材料的商品级材料。
如本文所用，术语“烃基取代基”或“烃基”以其本领域技术人员熟知的常用意义使用。具体而言，它指具有直接连接在分子其余部分上的碳原子且主要具有烃性质的基团。烃基的实例包括：烃基取代基，包括脂族、脂环族和芳族取代基；取代的烃基取代基，即含有在本发明上下文中不改变取代基的主要烃性质的非烃基团的取代基；和杂取代基，即具有主要烃性质但在环或链中含有不同于碳的取代基。“烃基取代基”或“烃基”的更详细定义在国际公开WO2008147704的第[0118]-[0119]段中找到。
所公开技术的一个组分为具有润滑粘度的油。本发明润滑油组合物中所用基油(baseoil)可选自如AmericanPetroleumInstitute(API)BaseOilInterchangeabilityGuidelines所述组I-V基油中的任一种。
五组基油如下：
组I、II和III为矿物油基本油料。则具有润滑粘度的油可包括天然或合成润滑油及其混合物。通常使用矿物油和合成油的混合物，特别是聚α烯烃油和聚酯油。
天然油包括动物油和植物油(例如蓖麻油、猪油和其它植物酸酯)以及矿物润滑油如液体石油及链烷烃、环烷烃和混合链烷烃-环烷烃型的溶剂处理或酸处理的矿物润滑油。加氢处理或加氢裂化油包含在有用的具有润滑粘度的油的范围内。
衍生自煤或页岩的具有润滑粘度的油也是有用的。合成润滑油包括烃油和卤素取代的烃油，例如聚合和共聚的烯烃及其混合物、烷基苯、聚苯(例如联苯、三联苯和烷基化聚苯)、烷基化二苯醚和烷基化二苯硫和它们的衍生物、其类似物和同系物。氧化烯聚合物和共聚物及其衍生物，和其中末端羟基已通过例如酯化或醚化改性的那些构成可使用的其它类已知合成润滑油。可使用的另一类合适的合成润滑油包括二羧酸的酯及由C5-C12单羧酸和多元醇或多元醇醚制备的那些。
其它合成润滑油包括含磷酸的液体酯、聚四氢呋喃、硅基油如聚烷基-、聚芳基-、聚烷氧基-或聚芳氧基-硅氧烷油和硅酸酯油(silicateoil)。
加氢处理的环烷烃油也是已知并可使用的。可使用合成油，例如通过费托反应制备的那些，且通常可为加氢异构化费托合成烃或蜡。在一个实施方案中，油可通过费托气至液合成程序制备，以及其它气至液油。
上文所述类型的天然或合成(以及任何这些中两种或更多种的混合物)的未精炼、精炼和再精炼油可用于本发明组合物中。未精炼油为不经进一步提纯处理，直接由天然或合成来源得到的那些。精炼油类似于未精炼油，不同的是已将它们在一个或多个提纯步骤中进一步处理以改进一种或多种性能。再精炼油通过将类似于用于得到精炼油的方法应用于已使用过的精炼油而得到。这类精炼油通常另外通过旨在除去废添加剂和油分解产物的技术加工。
完全配置润滑剂(fullyformulatedlubricant)中油的量通常为保持在考虑其余添加剂以后等于100%的量。通常这可以为60-99重量%，或70-97%，或80-95%，或85-93%。所公开技术也可作为浓缩物提供，在这种情况下，油的量通常降低且其它组分的浓度相应地提高。在这类情况下，油的量可以为30-70重量%或40-60%。
聚合物分散剂
本发明润滑组合物含有聚合物分散剂，所述聚合物分散剂包括用某些类型的胺官能化的聚合物。用于聚合物分散剂的胺通常为具有至少3或至少4个芳族基团，例如4-10或4-8或4-6个芳族基团，和至少一个伯或仲氨基的胺。在一些实施方案中，胺包含一个伯氨基和至少一个仲氨基。在某些实施方案中，胺包含至少4个芳族基团和至少2个仲氨基或叔氨基。一般性地理解缩合反应最容易与伯氨基发生，所以在一个实施方案中，胺包含至少一个伯氨基和至少两个仲氨基或叔氨基，即至少两个为非伯氨基的其它氨基，即仲氨基或叔氨基的任何组合。
如本文所用，术语“芳族基团”以该术语的普通含义使用且已知通过4n+2个π电子/环体系的Hückel理论定义。因此，本发明一个芳族基团可具有6或10或14个π电子。苯环具有6个π电子，萘环具有10个π电子，吖啶基团具有14个π电子。
具有至少3或4个芳族基团的胺的实例可由式(1)表示：
式1
其中各变量独立地如下：R1可以为氢或C1-5烷基(通常为氢)；R2可以为氢或C1-5烷基(通常为氢)；U可以为脂族、脂环族或芳族基团，条件是当U为脂族时，则脂族基团可以为含有1-5，或1-2个碳原子的线性或支化亚烷基；w可以为1-10，或1-4，或1-2(通常为1)。在一个实施方案中，当U为脂族基团时，则U特别是含有1-5个碳原子的亚烷基。
或者，具有至少3或4个芳族基团的胺的实例可由式(1a)表示：
式1a
其中各个变量U、R1和R2与上述相同，且w在该代表式中为0-9或0-3或0-1(通常为0)。
具有至少3或4个芳族基团的胺的其它实例可由以下式(2)和/或(3)中任一个表示：
式(2)
式(3)
具有氨基相对于亚烷基桥的各种置换的异构体也是可能的，包括式(2x)作为唯一的实例：
式(2x)
在一个实施方案中，具有至少3或4个芳族基团的胺可包括上述各式表示的化合物的混合物。本领域技术人员应当理解式(2)和(3)的化合物也可与以下所述醛反应而形成吖啶衍生物，包括下面式(2a)或(3a)-(3c)所示那些。除这些式表示的化合物外，其它吖啶结构也可以是可能的，其中醛与具有与>NH基团桥联的苄基的其它分子反应。
式(2a)
式(3a)
任何或所有N-桥联的芳环能够这样进一步缩合并可能芳构化。一种其它的许多可能结构显示于式(3b)中。
式(3b)
式(3c)
式(2)、(2a)、(3)或(3a)-(3c)中任一个也发生其它缩合反应，导致每分子形成一个或多个吖啶结构。
具有至少3或4个芳族基团的胺的实例包括双[对-(对-氨基苯胺基)苯基]-甲烷、2-(7-氨基-吖啶-2-基甲基)-N-4-{4-[4-(4-氨基-苯基氨基)-苄基]-苯基}-苯-1,4-二胺、N-4-{4-[4-(4-氨基-苯氨基)-苄基]-苯基}-2-[4-(4-氨基-苯氨基)-环己-1,5-二烯基甲基]-苯-1,4-二胺、N-[4-(7-氨基-吖啶-2-基甲基)-苯基]-苯-1,4-二胺及其混合物。在一个实施方案中，具有至少3或4个芳族基团的胺可以为双[对-(对-氨基苯胺基)苯基]-甲烷、2-(7-氨基-吖啶-2-基甲基)-N-4-{4-[4-(4-氨基-苯氨基)-苄基]-苯基}-苯-1,4-二胺或其混合物。
具有至少3或4个芳族基团的胺可通过包括使醛与胺(通常为4-氨基二苯胺)反应的方法制备。所得胺可描述为具有至少3或4个芳族基团、至少一个-NH2官能团和至少2个仲或叔氨基的亚烷基耦合胺。用于耦合的醛可以为脂族、脂环族或芳族的。脂族醛可以为线性或支化的。合适芳族醛的实例包括苯甲醛和邻香草醛。脂族醛的实例包括甲醛(或其反应性等价物如福尔马林或低聚甲醛)、乙醛和丙醛。通常醛可以为甲醛或苯甲醛。
或者，具有至少3或4个芳族基团的胺也可通过Berichteder DeutschenChemischenGesellschaft(1910)，43，728-39中所述的方法制备。
在一个实施方案中，具有至少3或4个芳族基团的胺可通过一种方法得到或可得到，所述方法包括使靛红酸酐或烷基取代的靛红酸酐与具有至少2个芳族基团和反应性伯或仲氨基的芳香胺反应。所得材料可以描述为邻氨基苯甲酸衍生物。
在一个实施方案中，邻氨基苯甲酸衍生物可通过使靛红酸酐或烷基取代的靛红酸酐与选自如下的芳香胺反应而制备：二甲苯二胺、4-氨基二苯胺、1,4-二甲基苯二胺及其混合物。在一个实施方案中，芳香胺可以为4-氨基二苯胺。
上述制备邻氨基苯甲酸衍生物的方法可在20-180℃，或40-110℃的反应温度下进行。该方法可(或不可)在溶剂的存在下进行。合适溶剂的实例包括水、稀释油、苯、叔丁基苯、甲苯、二甲苯、氯苯、己烷、四氢呋喃或其混合物。该反应可在空气或惰性气氛如氮气或氩气，通常氮气中进行。
羧酸官能化聚合物
胺官能化聚合物分散剂可以为上述具有至少3或4个芳族基团的胺与羧酸官能化聚合物的反应产物。所得产物可描述为胺官能化羧酸官能化聚合物。
羧酸官能化聚合物骨架可以为均聚物或共聚物，条件是它含有至少一个羧酸官能或羧酸官能的反应性等价物(例如酐或酯)。羧酸官能化聚合物可具有接枝于骨架上、在聚合物骨架内或作为端基在聚合物骨架上的羧酸官能(或羧酸官能的反应性等价物)。所有这些意欲包括在术语“羧酸官能化”内。
羧酸官能化聚合物可以为聚异丁烯取代的琥珀酸酐、马来酸酐-苯乙烯共聚物、马来酸酐-苯乙烯共聚物的酯、α烯烃-马来酸酐共聚物，或如下的马来酸酐接枝共聚物：(i)苯乙烯-乙烯-α烯烃聚合物，(ii)氢化链烯基芳基共轭二烯共聚物(即氢化链烯基芳烃共轭二烯共聚物，特别是苯乙烯-丁二烯的氢化共聚物)，(iii)与马来酸酐接枝的聚烯烃(特别是乙烯-丙烯共聚物)，或(iv)异戊二烯聚合物(特别是非氢化异丁烯-异戊二烯共聚物或氢化苯乙烯-异戊二烯聚合物)或其混合物。
本文所述羧酸官能化聚合物在润滑剂技术中是已知的。例如，马来酸酐和含苯乙烯聚合物的酯由美国专利6,544,935中已知。接枝的苯乙烯-乙烯-α烯烃聚合物教导于国际公开WO01/30947中。衍生自异丁烯和异戊二烯的共聚物用于制备分散剂且报告于国际公开WO01/98387中。接枝的苯乙烯-丁二烯和苯乙烯-异戊二烯共聚物描述于大量参考文献，包括DE3,106,959；和美国专利5,512,192和5,429,758中。聚异丁烯琥珀酸酐描述于大量出版物，包括美国专利4,234,435；3,172,892；3,215,707；3,361,673；和3,401,118中。接枝的乙烯-丙烯共聚物描述于美国专利4,632,769；4,517,104；和4,780,228中。(α-烯烃马来酸酐)共聚物的酯描述于美国专利5,670,462中。异丁烯和共轭二烯的共聚物(例如异丁烯-异戊二烯共聚物)描述于美国专利7,067,594和7,067,594和美国专利申请US2007/0293409中。乙烯、丙烯和非共轭二烯(例如二环戊二烯或丁二烯)的三聚物描述于美国专利5,798,420和5,538,651中。该段中提及的含有二烯单体(例如丁二烯或异戊二烯)的聚合物为部分或完全氢化的。许多聚合物骨架还描述于“ChemistryandTechnologyofLubricants”，第2版，R.M.Mortier和S.T.Orszulik编辑，BlackieAcademic&Professional出版中。特别是第144-180页讨论了许多聚合物骨架(i)-(iv)和(vi)-(viii)。
本发明聚合物骨架(不同于聚异丁烯)可具有可以具有至多150,000或更高，例如1,000或5,000至150,000或至120,000或至100,000的数均分子量(通过凝胶渗透色谱法，聚苯乙烯标准)。合适数均分子量范围的实例包括10,000-50,000，或6,000-15,000，或30,000-50,000。在一个实施方案中，聚合物骨架具有大于5,000，例如大于5000至150,000的数均分子量。还预期上述分子量极限的其它组合。当本发明聚合物骨架为聚异丁烯时，它的数均分子量(通过凝胶渗透色谱法，聚苯乙烯标准)可以为350-15,000，或550-10,000，或500-10,000，或750-5000或750-2500。(因此，聚异丁烯琥珀酸酐可衍生自具有前述分子量中任一种的聚异丁烯。)某些市售聚异丁烯聚合物具有550、750、950至1000、1550、2000或2250的数均分子量。一些市售聚异丁烯聚合物可通过将一种或多种具有不同分子量的聚异丁烯聚合物混合而得到以上所示数均分子量。在一个实施方案中，羧酸官能化聚合物包含带有至少一个琥珀酸基团(通常来自聚异丁烯与马来酸酐的反应)的数均分子量为约500至约10,000的聚异丁烯。
在一个实施方案中，产物可通过使羧酸官能化聚合物与具有至少3或4个芳族基团、至少一个-NH2官能团和至少2个仲或叔氨基的胺或胺官能化添加剂反应而得到或可得到。具有至少3或4个芳族基团的胺或胺官能化添加剂可在本领域技术人员已知用于形成羧酸官能化聚合物的酰亚胺和/或酰胺的反应条件下与羧酸官能化聚合物反应。
通过羧酸官能化聚合物与具有至少3或4个芳族基团、至少一个-NH2官能团和至少2个仲或叔氨基的胺反应而得到或可得到的胺官能化羧酸官能化聚合物在某些实施方案中可由式(4)和/或(5)表示：
式(4)
或
式(5)
其中各个变量R1、R2和U独立地如前文所述。BB表示聚合物骨架，并可以为聚异丁烯，或作为选择，如下的共聚物：(i)氢化链烯基芳基共轭二烯共聚物(特别是苯乙烯-丁二烯的氢化共聚物)，(ii)聚烯烃(特别是乙烯-α烯烃如乙烯-丙烯共聚物)，(iii)氢化异戊二烯聚合物(特别是氢化苯乙烯-异戊二烯聚合物)，或(iv)异戊二烯与异丁烯的共聚物。BB可以被一个琥珀酰亚胺基团取代，如式(4)和(5)所示，或它可被多个琥珀酰亚胺基团取代。在一个实施方案中，BB可以为异戊二烯与异丁烯的共聚物。式(4)和(5)中所示胺结构部分也可全部或部分地被式(2a)、(3)、(3a)、(3b)、(3c)的相应胺结构部分或其混合物取代。
当聚合物骨架BB为聚异丁烯时，所得羧酸官能化聚合物通常可以是聚异丁烯琥珀酸酐。通常，如式(1)中所定义，w可以为1-5，或1-3(或如式(1a)中所定义，w可以为0-4或0-2)。当BB不同于聚异丁烯且具有接枝于其上的马来酸酐(或其它羧酸官能)时，接枝的马来酸酐基团中的一个或多个可以为通过与上述胺中一种或多种反应而形成的琥珀酰亚胺。琥珀酰亚胺基团的数目可以为1-40，或2-40，或3-20。
胺官能化羧酸官能化聚合物可通过使衍生自马来酸酐-苯乙烯共聚物、马来酸酐-苯乙烯共聚物的酯、α-烯烃马来酸酐共聚物的羧酸官能化聚合物；或其混合物与具有至少3或4个芳族基团、至少一个-NH2官能团和至少2个仲或叔氨基的胺反应而得到或可得到。通常，这类产物可描述为交替共聚物。在交替共聚物中，马来酸酐衍生的基团中的一个或多个可具有式(6)表示的基团：
式(6)
其中R1、R2和U如前文所述，且式(6)的基团可通过如以上马来酸或琥珀酸环结构所示一个或两个波浪键结合在聚合物骨架的其它组分上。或者，仅一个波浪键可连接在聚合物上，第二个波浪键可连接在氢原子或其它非聚合物基团上。式(6)中胺衍生的基团也可被任何上述胺如式(3)中的胺或其混合物取代。
某些芳香胺也可描述为衍生自例如靛红酸酐的邻氨基苯甲酸衍生物。作为衍生自聚异丁烯(在式(7)中表示为“PIB”)的邻氨基苯甲酸衍生物的合适结构的实例，邻氨基苯甲酸衍生物和4-氨基二苯胺可由式(7)表示：
式(7)
应当指出此处，如在其它分散剂中，除简单单键外，存在琥珀酰亚胺结构部分在聚异丁烯上的多种类型的附着，包括各种环状附着结构，且所述结构不意欲为限定性的。
在一个实施方案中，胺官能化羧酸官能化聚合物可衍生自芳香胺和非聚异丁烯聚合物骨架。衍生自4-氨基二苯胺的邻氨基苯甲酸衍生物的合适结构的实例可由式(8)表示：
式(8)
其中如上文，BB表示聚合物骨架。通常BB可以为衍生自乙烯-丙烯共聚物的乙烯-丙烯共聚物。如所示，BB与马来酸酐接枝并官能化以形成酰亚胺基团，且u为方括号内所示的在各个位置上接枝于骨架上的接枝单元的数目。通常u可以为1-2000，或1-500，或1-250，或1-50、1-20、1-10，或1-4。
胺官能化羧酸官能化聚合物的更详细描述在国际申请PCT/US2008/082944中找到。特别参见第[0013]-[0021]、[0027]-[0091]段和第[0111]-[0135]段中公开的制备实施例1-25。
完全配制润滑剂中聚合物分散剂的量可以为至少0.6重量%，例如0.6或0.75或1.0至10%，或1.5-8%，或2-6重量%。或者，如果聚合物分散剂作为浓缩物提供，则浓缩物中存在的分散剂的量相应地更高，例如2-30%或5-20%。
所公开技术的另一组分是过碱性金属清净剂。过碱性金属清净剂可视为包含油溶性中性金属盐组分和金属碳酸盐组分。含金属清净剂通常为过碱性材料或过碱性清净剂。过碱性材料，另外称为过碱性或超碱性盐，一般为均匀牛顿体系，其特征是金属含量超过用于根据金属和与金属反应的特定酸性有机化合物的化学计量中和存在的量。过碱性材料通过酸性材料(通常为无机酸或低级羧酸，在一个实施方案中为二氧化碳)与包含酸性有机化合物、反应介质、化学计量过量的金属碱和促进剂如苯酚或醇和任选氨的混合物反应而制备，所述反应介质包含至少一种用于酸性有机材料的惰性有机溶剂(例如矿物油、石脑油、甲苯、二甲苯)。酸性有机材料通常具有足够的碳原子数，例如作为烃基取代基以提供在油中合理的溶解度。过量金属的量通常根据金属比表示。术语“金属比”为金属的总当量与酸性有机化合物的总当量之比。中性金属盐具有1的金属比。具有正盐中存在的4.5倍的金属的盐具有3.5当量的金属过量，或4.5的比。
过碱性清净剂通常通过总碱值(TBN，ASTMD4739或D974)表征。TBN为中和所有过碱性材料的碱度所需的强酸的量，表示为氢氧化钾当量(mgKOH/g试样)。由于过碱性清净剂通常以含有一定量的稀释油如40-50%油的形式提供，该清净剂的实际TBN值取决于存在的这类稀释油的量，而不管过碱性材料的“固有”碱度。就本发明而言，在无油的基础上再计算过碱性清净剂的TBN。用于本发明中的清净剂可具有100-800，在一个实施方案中150-750，在另一实施方案中400-700的TBN(无油基)。如果使用多种清净剂，清净剂组分的总TBN(即所有具体清净剂在一起的平均值)通常在以上范围内。
用于制备碱性金属盐的金属化合物一般为任何1族或2族金属化合物(CAS版本的元素周期表)。金属化合物的1族金属包括1a族碱金属如钠、钾和锂，以及1b族金属如铜。1族金属可以为钠、钾、锂和铜，在一个实施方案中为钠或钾，在另一实施方案中为钠。金属碱的2族金属包括2a族碱土金属如镁、钙和钡，以及2b族金属如锌或镉。在一个实施方案中，2族金属为镁、钙、钡或锌，在另一实施方案中为镁或钙。在某些实施方案中，金属为钙或钠或钙和钠的混合物。一般而言，金属化合物作为金属盐提供。盐的阴离子部分可以为氢氧根、氧、碳酸根、硼酸根或硝酸根。
在一个实施方案中，本发明润滑剂可含有过碱性磺酸盐清净剂。合适的磺酸包括磺酸和硫代磺酸。磺酸包括单-和多核芳族或脂环族化合物。油溶性磺酸盐可以大部分由下式中的一个表示：R2-T-(SO3-)a和R3-(SO3-)b，其中T为环状核，例如通常为苯；R2为脂族基团如烷基、烯基、烷氧基或烷氧基烷基；(R2)-T通常含有总计至少15个碳原子；且R3为通常含有至少15个碳原子的脂族烃基。R3的实例为烷基、烯基、烷氧基烷基和碳烷氧基烷基。基团T、R2和R3也可含有其它无机或有机取代基。在上式中，a和b为至少1。在一个实施方案中，磺酸盐清净剂可以为金属比为至少8的主要线性烷基苯磺酸盐清净剂，如美国专利申请2005065045的第[0026]-[0037]段所述。在一些实施方案中，线性烷基可在沿着烷基的线性链的任何位置连接在苯环上，但通常在线性链的2、3或4位上，在一些实施方案中主要在2位上。
可存在的另一过碱性材料为过碱性酚盐清净剂。用于制备酚盐清净剂的苯酚可由式(R1)a-Ar-(OH)b表示，其中R1为具有4-400个碳原子，或6-80或6-30或8-25或8-15个碳原子的脂族烃基；Ar为芳族基团(其可以为苯基或其它芳族基团如萘)；a和b独立地为至少1的数，a和b之和在2至Ar的一个或多个芳族核上的可取代氢的数目的范围内。在一个实施方案中，a和b独立地为1-4或1-2的数。R1和a通常使得对于各个苯酚化合物R1基团提供平均至少8个脂族碳原子。酚盐清净剂有时也作为硫桥联的物种提供。
在一个实施方案中，过碱性材料为过碱性水杨苷清净剂。过碱性水杨苷清净剂通常为基于水杨苷衍生物的过碱性镁盐。这类水杨苷衍生物的一般实例可以由下式表示：
其中X包括-CHO或-CH2OH，Y包括-CH2-或-CH2OCH2-，且其中这类-CHO基团通常包含至少10摩尔的X和Y基团；M为氢、铵，或金属离子的化合价(即在多价金属离子的情况下，化合价中的一个通过所示结构满足，其它化合价通过其它物种如阴离子满足，或通过相同结构的另一实例满足)，R1为含有1-60个碳原子的烃基，m为0至通常10，且各个p独立地为0、1、2或3，条件是至少一个芳环含有R1取代基，且所有R1基团中的碳原子总数为至少7。当m为1或更大时，X基团中的一个可以为氢。在一个实施方案中，M为Mg离子的化合价或Mg与氢的混合物。水杨苷清净剂更详细地公开于美国专利6,310,009中，具体参考它们的合成方法(第8栏和实施例1)及X和Y各物种的优选量(第6栏)。
Salixarate清净剂是过碱性材料，其可由包含至少一个式(I)或式(II)单元的基本线性化合物表示：
其中化合物的各端具有式(III)或(IV)的端基：
这类基团通过二价桥联基团A连接，所述桥联基团对于各个连接键而言可以是相同或不同的；其中在式(I)-(IV)中，R3为氢或烃基或金属离子的化合价；R2为羟基或烃基，j为0、1或2；R6为氢、烃基或杂取代的烃基；R4为羟基且R5和R7独立地为氢、烃基或杂取代的烃基，或者R5和R7都为羟基且R4为氢、烃基或杂取代的烃基；条件是R4、R5、R6和R7中至少一个为含有至少8个碳原子的烃基；且其中分子平均含有单元(I)或(III)中至少一个和单元(II)或(IV)中至少一个，且组合物中单元(I)和(III)的总数与单元(II)和(IV)的总数之比为约0.1:1至约2:1。二价桥联基团“A”每次出现时可以为相同或不同的，包括-CH2-(亚甲基桥)和-CH2OCH2-(醚桥)，其可衍生自甲醛或甲醛等价物(例如低聚甲醛、福尔马林)。
Salixarate衍生物及其制备方法更详细地描述于美国专利No.6,200,936和PCT公开WO01/56968中。认为salixarate衍生物具有主要线性而不是大环结构，但两种结构都意欲包含在术语“salixarate”中。
过碱性清净剂也可以为过碱性水杨酸盐，其可以为取代水杨酸的碱金属盐或碱土金属盐。水杨酸可以为烃基取代的水杨酸，其中各个取代基含有平均至少8个碳原子每取代基和1-3个取代基每分子。取代基可以为聚亚烷基取代基，其中聚亚烷基包括具有2-16，或2-6，或2-4个碳原子的可聚合烯烃单体的均聚物和共聚物。烯烃可以为单烯烃如乙烯、丙烯、1-丁烯、异丁烯和1-辛烯；或聚烯烃单体，例如二烯烃单体，例如1,3-丁二烯和异戊二烯。在一个实施方案中，水杨酸上的一个或多个烃基取代基含有7-300个碳原子并可以为分子量为150-2000的烷基。聚亚烷基和聚烷基通过常规程序制备，且这类基团在水杨酸上的取代可通过已知方法进行。烷基水杨酸盐可通过Kolbe-Schmitt反应由烷基苯酚制备；或者水杨酸钙可通过烷基苯酚的直接中和以及随后的碳化而制备。过碱性水杨酸盐清净剂和它们的制备方法公开于美国专利4,719,023和3,372,116中。
其它过碱性清净剂可包括具有曼尼希碱结构的过碱性清净剂，如美国专利6,569,818中所公开的。
过碱性材料是本领域技术人员熟知的。描述磺酸、羧酸、(烃基取代)苯酚、膦酸及这些中任何两种或更多种的混合物的碱性盐的制备技术的专利包括美国专利2,501,731；2,616,905；2,616,911；2,616,925；2,777,874；3,256,186；3,384,585；3,365,396；3,320,162；3,318,809；3,488,284；和3,629,109。
在所公开的技术中，过碱性金属清净剂包含油溶性中性金属盐组分和金属碳酸盐组分。“中性金属盐”意指表示为油溶性酸性材料的化学计量中和且具有1的金属比的盐，而不管该盐是严格地中性还是通过任何给定试验或滴定测量为稍微酸性或碱性的。“中性盐的量”意欲为依赖过碱化的酸性基质的量的尺度，其不同于中性盐的量之处是以可容易计算的方式得到的中和金属的质量。中性金属盐组分的量可容易地由本领域技术人员由存在的清净剂的总量和清净剂的过碱化程度或金属比或TBN的知识测定。在一个实施方案中，TBN测量用于计算或定义中性金属盐的量。例如，1g(无油)TBN(无油)为517的过碱性磺酸钙清净剂含有约0.46gCaCO3([517mgKOH/g]×[1eqKOH/56,100mgKOH]×[50gCaCO3/1eqKOH])。通过减法，中性皂的量为约0.54g或54%。(基质的任何固有残余碱度应在计算中性皂的量以前从测量TBN中减去，如本领域技术人员所知。)
对于本技术，润滑剂中清净剂的量应使得一种或多种中性金属盐组分的量为至少0.75重量%或作为选择至少1.0%，且至多3或2或1.8或1.5重量%。润滑剂中作为整体的过碱性清净剂的相应量，即包含金属碳酸盐组分但排除任何稀释油，可以为1-8%，或1.3-5%，或1.5-2.5重量%。在浓缩物中，该量可相应地更高。
配制本技术的润滑剂以具有少于1.1%，或者少于1.0或0.95或0.9或0.85重量%的硫酸盐化灰分含量(ASTMD874)。
并入所公开技术中的润滑剂还可含有已知用于润滑剂中的各种添加剂中的一种或多种。一种常用添加剂为分散剂，即不同于上述含有具有至少3个芳环和至少一个伯或仲氨基的芳香胺的那些的补充分散剂。分散剂是润滑剂领域中熟知的且主要包括称为无灰分散剂和聚合物分散剂的。之所以称为无灰分散剂，是因为当提供时，它们不含金属，因此在加入润滑剂中时通常不贡献硫酸盐化灰分。然而，它们在加入包含含金属物种的润滑剂中时当然可与环境金属相互作用。无灰分散剂的特征是连接在较高分子量烃链上的极性基团。典型的无灰分散剂包括N-取代的长链烯基琥珀酰亚胺，其具有多种化学结构，通常包括：
其中R1各自独立地为烷基，常常为基于聚异丁烯前体、分子量(Mn)为500-5000的聚异丁烯基团，且R2为亚烷基，通常为亚乙基(C2H4)。这类分子通常衍生自烯基酰化剂与多胺的反应，除以上所示简单的酰亚胺结构外，两个结构部分之间的多种键是可能的，包括多种酰胺和季铵盐。R1基团在酰亚胺结构上的多种键模式也是可能的，包括各种环键。酰化剂的羰基与胺的氮原子之比可以为1:0.5-1:3，在其它情况下为1:1-1:2.75或1:1.5-1:2.5。琥珀酰亚胺分散剂更完整地描述于美国专利4,234,435和3,172,892和EP0355895中。
另一类无灰分散剂是高分子量酯。这些材料类似于上述琥珀酰亚胺，不同之处在于它们可视为通过烃基酰化剂与多元脂族醇如甘油、季戊四醇或山梨糖醇反应而制备。这类材料更详细地描述于美国专利3,381,022中。另一类无灰分散剂为曼尼希碱。这些为通过较高分子量烷基取代的苯酚、亚烷基多胺与醛如甲醛缩合而形成的材料。这类材料更详细地描述于美国专利3,634,515中。又另外的分散剂包括聚合物分散剂添加剂，其一般为含有极性官能以赋予聚合物分散性的烃基聚合物。
也可将分散剂通过与多种试剂中的任一种反应而后处理。其中，这些为脲、硫脲、二巯基噻二唑、二硫化碳、醛、酮、羧酸、烃取代的琥珀酸酐、腈、环氧化物、硼化合物和磷化合物。详述该处理的参考文件列于美国专利4,654,403中。
润滑剂还可含有磷酸的金属盐。式[(R8O)(R9O)P(=S)-S]n-M(其中R8和R9独立地为含有3-30个碳原子的烃基)的金属盐可容易地通过加热五硫化二磷(P2S5)和醇或苯酚以形成O,O-二烃基二硫代磷酸而得到。反应以提供R8和R9基团的醇可以为醇的混合物，例如异丙醇与4-甲基-2-戊醇的混合物，在一些实施方案中，仲醇与伯醇的混合物，例如异丙醇与2-乙基己醇的混合物。所得酸可与碱金属化合物反应以形成盐。具有化合价n的金属M一般为铝、铅、锡、锰、钴、镍、锌或铜，在许多情况下为锌，以形成二烷基二硫代磷酸锌。这类材料是熟知的且润滑剂配制剂领域的技术人员可容易地得到。提供发动机中良好的磷保持力的合适变化方案例如公开于美国公开的申请2008-0015129中，例如参见权利要求书。
常用的另一组分是粘度改进剂。粘度改进剂(VM)和分散剂粘度改进剂(DVM)是熟知的。VM和DVM的实例可包括聚甲基丙烯酸酯、聚丙烯酸酯、聚烯烃、苯乙烯-马来酸酯共聚物，和类似的聚合物，包括均聚物、共聚物和接枝共聚物。DVM可包括含氮甲基丙烯酸酯聚合物，例如衍生自甲基丙烯酸甲酯和二甲基氨基丙胺的含氮甲基丙烯酸酯聚合物。
市售VM、DVM的实例和它们的化学类型可包括如下：聚异丁烯(例如来自BPAmoco的IndopolTM或来自ExxonMobil的ParapolTM)；烯烃共聚物(例如来自Lubrizol的LubrizolTM7060、7065和7067及来自Mitsui的LucantTMHC-2000L和HC-600)；氢化苯乙烯-丁二烯共聚物(例如来自Shell的ShellvisTM40和50和来自Lubrizol的7308和7318)；苯乙烯/马来酸酯共聚物，其为分散剂共聚物(例如来自Lubrizol的3702和3715)；聚甲基丙烯酸酯，其中一些具有分散剂性能(例如来自RohMax的ViscoplexTM系列、来自Afton的HitecTM系列中的那些及来自Lubrizol的LZ7702TM、LZ7727TM、LZ7725TM和LZ7720CTM中的那些)；烯烃接枝聚甲基丙烯酸酯聚合物(例如来自RohMax的ViscoplexTM2-500和2-600)；和氢化聚异戊二烯星形聚合物(例如来自Shell的ShellvisTM200和260)。可使用的粘度改进剂描述于美国专利5,157,088,5,256,752和5,395,539中。VM和/或DVM可以以至多20重量%的浓度用于官能流体中。可使用1-12%或3-10重量%的浓度。
另一组分为抗氧化剂。抗氧化剂包括酚类抗氧化剂，其可包括含有2或3个叔丁基的丁基取代苯酚。对位也可被烃基或桥联两个芳环的基团占据。后一类抗氧化剂更详细地描述于美国专利6,559,105中。抗氧化剂还包括芳香胺，例如壬基化二苯胺。其它抗氧化剂包括硫化烯烃、钛化合物和钼化合物。美国专利No.4,285,822例如公开了含有含钼和硫组合物的润滑油组合物。美国专利申请公开2006-0217271公开了多种钛化合物，包括钛醇盐和钛酸酯化分散剂，该材料还可赋予沉积物控制和过滤性的改进。抗氧化剂的典型量当然取决于具体抗氧化剂和它各自的效率，但说明性总量可以为0.01-5重量%或0.15-4.5%或0.2-4%。另外，可存在多于一种抗氧化剂，且这些中的某些组合在其组合总效果方面可以是协同增效的。
另一添加剂为抗磨剂。抗磨剂的实例包括含磷抗磨/特压剂如金属硫代磷酸盐(例如上述二烷基二硫代磷酸锌)、磷酸酯及其盐，含磷羧酸、酯、醚和酰胺；和亚磷酸盐。在某些实施方案中，磷抗磨剂可以以提供0.01-0.2或0.015-0.15或0.02-0.1或0.025-0.08%磷的量存在。不含磷的抗磨剂包括硼酸酯(包括硼酸化环氧化物)、二硫代氨基甲酸酯化合物、含钼化合物和硫化烯烃。其它类型的抗磨剂一般包括酒石酸酯、酒石酰胺和酒石酰亚胺，例如油基酒石酰亚胺，以及羟基聚羧酸的酯、酰胺和酰亚胺。除抗磨性能外，这些材料也可赋予润滑剂其它功能。这些材料更详细地描述于美国公开2006-0079413和2008年12月9日提交的美国临时申请61/120932中。
可任选用于润滑油中的其它添加剂包括倾点下降剂、特压剂、抗腐蚀剂、颜色稳定剂和消泡剂。
本技术可通过向其提供任何上述润滑剂而用于多种机械设备中任一种，包括内燃机的润滑。在某些实施方案中，发动机可以为柴油(压缩点火)发动机如重型柴油机。其它可能的发动机包括汽油(火花点火)发动机，和消耗醇、汽油-醇混合物、生物柴油燃料、各种混合燃料、合成燃料或气体燃料如天然气或氢气的发动机，二冲程循环发动机和船用柴油机。
已知上述一些材料在最终配制剂中可能相互作用，使得最终配制剂的组分可能与起初加入的那些不同。例如，金属离子(例如清净剂的)可迁移至其它分子的其它酸性或阴离子部位。由此形成的产品，包括经以其意欲用途使用本发明组合物而形成的产品可能不容易描述。然而，所有这类改进和反应产物均包括在本发明的范围内；本发明包括通过将上述组分混合而制备的组合物。
实施例
制备实施例1.部分(a).将500mL2M盐酸加入装配有顶入式搅拌器(overheadstirrer)、温度计套管、具有氮气管线的添加漏斗和冷凝器的1升四颈烧瓶中。加入184.2g的4-氨基二苯胺，并将烧瓶加热至75℃。然后将添加漏斗中装入40.5g的37%甲醛溶液并将该溶液经30分钟时间逐滴加入烧瓶中。将烧瓶保持在100℃下4小时。然后将烧瓶冷却至环境温度。经30分钟加入80g的50/50wt/wt氢氧化钠水溶液。在反应结束时，借助过滤得到固体产物。
部分(b).将装配有顶入式搅拌器、温度计套管、具有氮气管线的表面下入口和具有冷凝器的迪安-斯达克榻分水器的3L四颈烧瓶中装入聚异丁烯琥珀酸酐(1270.0g)(其中聚异丁烯具有2000的数均分子量)和稀释油(1400.1g)。将烧瓶加热至90℃。然后缓慢加入部分(a)的固体产物(442.0g)。然后将温度升高至110℃并保持直至除去水。然后将温度上升至160℃并保持10小时。向烧瓶中加入一部分硅藻土助滤剂，并将烧瓶内容物通过第二部分硅藻土助滤剂过滤。所得产物为具有0.65重量%的氮含量的暗色油。
润滑剂配制剂如下表所述制备。配制各配制剂为1.0%硫酸盐化灰分(ASTMD874)且具有10的总TBN。在包括在150℃下将碳氟密封试样浸入350g润滑剂试样中168小时的试验中，测试润滑剂在拉伸强度变化和断裂伸长变化方面的碳氟密封性能。较小百分比的拉伸强度和伸长的降低表明较好的结果。还根据ASTMD6594评估润滑剂的铜和铅腐蚀。
a所有分散剂和清净剂基于无油(活性化学物质)提供。报告的TBN还通过因式分解出稀释油的量而校准。
b.含有来自其它实施例的抗氧化剂的不同余量。
c.即清净剂的油溶性中性金属盐组分。
结果显示含有用氨基二苯胺和甲醛的2:1反应产物官能化的分散剂聚合物和更高量的清净剂基质的实施例1和2显示出比参比例更好的密封性能和更好的腐蚀性能。
将以上参考的各文件通过引用并入本发明。任何文件的提及不是承认该文件取得现有技术资格或以任何权限构成技术人员的一般知识。除实施例中，或另外明确说明外，在本说明书中描述材料的量、反应条件、分子量、碳原子数等的所有数量应当理解被措辞“约”修饰。应当理解本文所述量、范围和比的上限和下限可独立地组合。类似地，本发明各个元素的范围和量可以与任何其它元素的范围或量一起使用。如本文所用，表述“基本由…组成”容许包括不实质地影响所考虑的组合物的基本和新特性的物质。
Claims (18)
1.润滑剂组合物，其包含：
(a)具有润滑粘度的油；
(b)0.6-6重量％的分散剂，所述分散剂包含羧酸官能化聚合物与具有至少4个芳环以及至少一个伯或仲氨基和至少2个仲或叔氨基的芳香胺的缩合产物；和
(c)包含油溶性中性金属盐组分和金属碳酸盐组分的过碱性金属清净剂，其中润滑剂组合物中中性金属盐组分的总量为至少0.75重量％且润滑剂组合物的硫酸盐化灰分含量少于1.1％。
2.根据权利要求1的润滑剂组合物，其中润滑剂的硫酸盐化灰分含量少于1.0％。
3.根据权利要求1的润滑剂组合物，其中羧酸官能化聚合物包括数均分子量为500-10,000、带有至少一个琥珀酸酐基团的聚异丁烯。
4.根据权利要求1-3中任一项的润滑剂组合物，其中分散剂包括羧酸官能化聚合物与具有至少4个芳环、至少2个仲或叔氨基和至少一个氮官能团的芳香胺的缩合产物，所述氮官能团提供与羧酸官能化聚合物的连接键。
5.根据权利要求1-3中任一项的润滑剂组合物，其中芳香胺由以下结构表示：
其中各变量独立地为：
R1和R2为氢或C1-5烷基；
U为脂族、脂环族或芳族基团；且
w为0-9。
6.根据权利要求4的润滑剂组合物，其中芳香胺由以下结构表示：
其中各变量独立地为：
R1和R2为氢或C1-5烷基；
U为脂族、脂环族或芳族基团；且
w为0-9。
7.根据权利要求5的润滑剂组合物，其中U为脂族基团。
8.根据权利要求7的润滑剂组合物，其中U为含有1-5个碳原子的亚烷基。
9.根据权利要求6的润滑剂组合物，其中U为脂族基团。
10.根据权利要求9的润滑剂组合物，其中U为含有1-5个碳原子的亚烷基。
11.根据权利要求1-3、6-10中任一项的润滑剂组合物，其中芳香胺包括以下结构表示的材料：
12.根据权利要求1-3、6-10中任一项的润滑剂组合物，其中过碱性金属清净剂包括过碱性、碳酸化的钙或镁的磺酸盐、酚盐、水杨酸盐、水杨苷或salixarate清净剂。
13.根据权利要求1-3、6-10中任一项的组合物，其中过碱性金属清净剂包括过碱性碳酸化镁水杨苷清净剂。
14.根据权利要求1-3、6-10中任一项的组合物，其中过碱性金属清净剂的量为1.3-5重量％。
15.根据权利要求1-3、6-10中任一项的组合物，其中润滑剂组合物中中性金属盐组分的总量为至少1.0％。
16.通过将权利要求1-15中任一项的组分混合而制备的组合物。
17.润滑内燃机的方法，包括向其中供入权利要求1-16中任一项的润滑剂。
18.根据权利要求17的方法，其中内燃机为柴油机。
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| US34649710P | 2010-05-20 | 2010-05-20 | |
| US61/346,497 | 2010-05-20 | ||
| PCT/US2011/036776 WO2011146456A1 (en) | 2010-05-20 | 2011-05-17 | Low ash lubricants with improved seal and corrosion performance |
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| KR (1) | KR101807898B1 (zh) |
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| CN106459812B (zh) * | 2014-03-12 | 2020-02-18 | 路博润公司 | 润滑内燃机的方法 |
| EP3268456A1 (en) * | 2015-03-09 | 2018-01-17 | The Lubrizol Corporation | Method of lubricating an internal combustion engine |
| US20180201865A1 (en) | 2015-07-10 | 2018-07-19 | The Lubrizol Corporation | Viscosity Modifiers For Improved Fluoroelastomer Seal Performance |
| JP2022104376A (ja) * | 2020-12-28 | 2022-07-08 | 日本電産株式会社 | 流体軸受用潤滑油、流体軸受、モータ及び送風機 |
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| CN101389739A (zh) * | 2006-02-27 | 2009-03-18 | 卢布里佐尔公司 | 作为润滑剂的无灰tbn增进剂的含氮分散剂 |
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| CA2799921A1 (en) | 2011-11-24 |
| WO2011146456A1 (en) | 2011-11-24 |
| EP2571966A1 (en) | 2013-03-27 |
| US9399747B2 (en) | 2016-07-26 |
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| KR20130121694A (ko) | 2013-11-06 |
| US20140323372A1 (en) | 2014-10-30 |
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