CN105637073A - 由用铜处理的分散剂而减少的发动机沉积物 - Google Patents
由用铜处理的分散剂而减少的发动机沉积物 Download PDFInfo
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- CN105637073A CN105637073A CN201480054845.7A CN201480054845A CN105637073A CN 105637073 A CN105637073 A CN 105637073A CN 201480054845 A CN201480054845 A CN 201480054845A CN 105637073 A CN105637073 A CN 105637073A
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Classifications
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C10M169/04—Mixtures of base-materials and additives
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
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- C10M133/56—Amides; Imides
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C10M141/06—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 nitrogen-containing compound
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- C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
- C10M159/12—Reaction products
- C10M159/18—Complexes with metals
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
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- C10M2203/102—Aliphatic fractions
- C10M2203/1025—Aliphatic fractions used as base material
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- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/022—Ethene
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- C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
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- C10M2215/064—Di- and triaryl amines
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/28—Amides; Imides
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/30—Heterocyclic compounds
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/02—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds
- C10M2219/022—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds of hydrocarbons, e.g. olefines
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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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/046—Overbasedsulfonic acid salts
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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
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/045—Metal containing thio derivatives
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- C10M2227/09—Complexes with metals
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/02—Groups 1 or 11
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
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- C10N2030/04—Detergent property or dispersant property
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
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- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C10N2030/08—Resistance to extreme temperature
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Abstract
本发明提供包含具有润滑粘度的油和用铜试剂处理的分散剂的润滑组合物。本发明进一步涉及通过将所述润滑组合物供入内燃机中而润滑内燃机的方法。本发明进一步涉及用铜处理的分散剂减少发动机组件的内表面上的沉积物的用途。
Description
发明领域
本发明提供包含用铜处理的分散剂以减少组合物暴露于热期间形成的高温不溶性固体的形成的润滑组合物。本发明进一步涉及润滑组合物在内燃机中的用途。本发明进一步涉及使用所述用铜处理的分散剂和所述润滑组合物减少发动机中的不溶性沉积物的方法。
发明背景
已知润滑剂在其使用期间由于暴露于它们用于其中的装置的操作条件下，包括暴露于热、氧气和通过装置的操作产生的部分燃烧副产物下而变得较无效。例如，发动机油在其使用期间部分地由于油暴露于酸性和促氧化剂副产物下而变得较无效。润滑剂的这些氧化和酸性烃然后可继续导致腐蚀、磨损和沉积问题。
现代发动机设计倾向于结合与较高操作温度有关的比之前曾有的更小的油箱体积。这些设计规格导致润滑剂上较大的氧化应力和在关键发动机区如活塞环区上形成高温沉积物的提高倾向。
给定上述现代发动机设计对润滑剂的持续需求，现代发动机试验必然变得更加严苛。例如，工业标准高温沉积试验(SequenceIIIG)为以高油箱温度和高负载的非常严苛的活塞清洁性试验。存在多种台架试验，寻求在该发动机试验和其它发动机试验，包括Komatsu热管试验(KHT)中模拟润滑油的沉积物形成倾向。程序要求油循环通过热玻璃管(例如232-320℃，更通常270-290℃)指定的时间。在试验结束时，目测评定管的沉积物，其中10的评定值为完全干净管，0为黑色管。该试验测量润滑剂在不存在燃烧过程下形成沉积物的先天倾向。
目前和提议的曲轴箱润滑剂规格，例如关于客车机油的GF-5和关于重型柴油机的PC-10描述了越来越严格的标准或者极限以满足政府规定。特别的顾虑是硫和磷极限。来自润滑剂的硫和磷可能最终处于催化转化器中。广泛认为减低润滑剂中的这些极限可能对发动机性能、发动机磨损和发动机油氧化具有严重影响。这是因为历史上发动机油中的磷含量的主要贡献者为二烷基二硫代磷酸锌(ZDP)，且ZDP长期用于赋予发动机油抗磨和抗氧化性能。因此，当降低量的ZDP参与发动机油中时，需要可选方案赋予保护以防发动机性能、发动机磨损和发动机油氧化中的一种或多种性能劣化。该改进的保护是理想的，无论ZDP和相关材料是否包含在润滑剂中。理想的润滑剂可在磷和硫中的一种或多种方面是低的。
需要提供在高操作温度下的发动机沉积物控制以及发动机油添加剂的常规功能中的一种(例如煤烟分散)的双功能添加剂。另外，理想的是该双功能添加剂还可以与低含量的常规抗氧化剂和/或低含量的含金属或含硫添加剂一起在润滑剂中起作用。
发明概述
本发明涉及铜改性的分散剂。这些铜改性的分散剂倾向于使在玻璃管的壁和发动机组件上由于油不溶性氧化产物而形成的沉积物最小化。这些铜改性的分散剂在试验如SAECECL85中还提高配制的润滑剂的氧化诱导时间。
现在发现，例如以胺类(也称为无灰)分散剂和铜化合物的反应产物的形式提供的铜如Cu+1或Cu+2的存在对以上性能中的一种或多种提供有利影响。特别是，这类材料作为铜PIB-琥珀酰亚胺分散剂在一个或多个Komatsu热管沉积物筛分试验(KHT)中赋予有利影响。
所需金属可作为Cu改性的分散剂，例如琥珀酰亚胺分散剂、曼尼希碱或烃基聚合物分散剂提供。这类材料可通过在硫酸铜或乙酸铜与烃基取代琥珀酸酐如烯基-或烷基-琥珀酸酐之间形成铜混合酐而制备。所得铜-琥珀酸盐中间体可直接使用或者它可与大量材料中的任一种，例如(a)具有游离、可缩合–NH官能的多胺基琥珀酰亚胺/酰胺分散剂；(b)多胺基琥珀酰亚胺/酰胺分散剂的组分，即烯基-或烷基-琥珀酸酐和多胺，(c)通过取代琥珀酸酐与多元醇、氨基醇、多胺或其混合物反应而制备的含羟基聚酯分散剂反应。作为选择，铜-琥珀酸盐中间体可与其它试剂如醇、氨基醇、醚醇、聚醚醇或多元醇或者脂肪酸反应，且其产物直接用于赋予润滑剂铜，或者进一步与如上所述琥珀酸分散剂反应。作为用金属后处理的分散剂的实例，可使1份(摩尔计)硫酸铜、乙酸铜和/或氢氧化铜与2份(摩尔计)聚异丁烯取代琥珀酸酐在110-155℃或者在一个实施方案中，140-150℃下反应5-6小时以提供铜改性的分散剂或中间体。可使所得材料(30g)与来自聚异丁烯取代琥珀酸酐的琥珀酰亚胺分散剂和聚亚乙基多胺混合物(127g+稀释油)在155℃下进一步反应1.5小时以产生铜改性的琥珀酰亚胺分散剂。
分散剂是润滑剂领域中熟知的，主要包括称为无灰型分散剂和聚合物分散剂的。无灰型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含氮分散剂，例如N-取代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，通常具有500-5000的分子量的聚异丁基，且R2为亚烷基，通常亚乙基(C2H4)。这类分子通常衍生自烯基酰化剂与多胺的反应，并且除以上所示代表性酰亚胺结构外，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。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中。
本发明进一步提供润滑内燃机的方法，所述方法包括步骤：向内燃机供入本文所述润滑组合物。
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。
除非另外指出，存在于本文所述润滑组合物中的添加剂的量基于无油，即活性物质的量报出。
具有润滑粘度的油
本发明润滑组合物包含具有润滑粘度的油。合适的油包括天然和合成油、衍生自加氢裂化、氢化和加氢精制的油、未精炼、精炼和再精炼油或其混合物。
未精炼油为通常不经(或经很少)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善一种或多种性能。提纯技术是本领域中已知的，包括溶剂萃取、二次蒸馏、酸或碱萃取、过滤、渗滤等。
再精炼油也称作再生或再加工油，通过类似于用于得到精炼油的那些的方法得到并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。
用于制备本发明润滑剂的天然油包括动物油、植物油(例如蓖麻油)、矿物润滑油如液体石油或者链烷烃、环烷烃或混合链烷烃-环烷烃型的溶剂处理或酸处理的矿物润滑油，和衍生自煤或页岩的油，或其混合物。
合成润滑油是有用的，且包括烃油，例如聚合、低聚或共聚烯烃(例如聚丁烯、聚丙烯、丙烯异丁烯共聚物)；聚(1-己烯)、聚(1-辛烯)、1-癸烯的三聚物或低聚物，例如聚(1-癸烯)，这类材料通常称为聚α-烯烃，及其混合物；烷基苯(例如十二烷基苯、十四烷基苯、二壬基苯、二-(2-乙基己基)-苯)；聚苯(例如联苯、三联苯、烷基化聚苯)；二苯基烷烃、烷基化二苯基烷烃、烷基化二苯醚和烷基化二苯硫及其衍生物、类似物和同系物或其混合物。
其它合成润滑油包括含磷酸的多元醇酯(例如3970)、二酯、液体酯(例如磷酸三甲苯酯、磷酸三辛酯和癸烷膦酸的二乙基酯)，或聚四氢呋喃。合成油可通过费托反应制备，通常可以为加氢异构的费托合成烃或蜡。在一个实施方案中，油可通过费托气至液(gastoliquid)合成程序制备以及其它气至液油。
具有润滑粘度的油也可如“AppendixE-APIBaseOilInterchangeabilityGuidelinesforPassengerCarMotorOilsandDieselEngineOils”的2008年4月版本，第1.3部分，副标题1.3.“BaseStockCategories”中所述定义。在一个实施方案中，具有润滑粘度的油可以为APIII组或III组油。在一个实施方案中，具有润滑粘度的油可以为APII组油。
存在的具有润滑粘度的油的量通常为在由100重量％减去本发明化合物和其它性能添加剂的量之和以后的余数。
润滑组合物可以为浓缩物和/或完全配制润滑剂的形式。如果本发明润滑组合物(包含本文所述添加剂)为浓缩物的形式(其可与其它油组合以形成全部或部分最终润滑剂)，则这些添加剂与具有润滑粘度的油和/或与稀释油的比包括1:99-99:1重量计，或80:20-10:90重量计的范围。
用铜处理的分散剂
本发明提供包含具有润滑粘度的油和含有用铜处理的分散剂的添加剂的润滑组合物。
在一个实施方案中，与铜反应的无灰分散剂，在下文中，添加剂可以以基于润滑组合物的总重量为约0.5至约10重量％，更理想地约1至约5重量％，优选约1.5至约3.5重量％的浓度存在于润滑组合物中。理想地，由处理润滑组合物中的分散剂而结合到润滑剂中的铜的量为润滑组合物的约5、6或7至约500重量份每百万份(ppm)，更理想地约5、6、8或10至约50、100或350ppm，在一个实施方案中，约40或50至150或200ppm。
一般而言，无灰分散剂和铜化合物在至少100℃，更理想地至少140℃的温度下一起反应一段时间，理想地至少1小时，更理想地至少2或4小时，以形成其中显著部分的铜物理或化学地与分散剂缔合的反应产物。尽管反应产物为所需结果，已知一些铜和一些无灰分散剂可以保持为未转化成缔合材料的反应物的形式。
用于本发明组合物中的合适分散剂包括琥珀酰亚胺分散剂。在一个实施方案中，分散剂可作为单一分散剂存在。在一个实施方案中，分散剂可作为两种或三种不同分散剂的混合物存在，其中至少一种可以为琥珀酰亚胺分散剂。
琥珀酰亚胺分散剂可以为脂族多胺的衍生物或其混合物。脂族多胺可以为脂族多胺，例如亚乙基多胺、亚丙基多胺、亚丁基多胺或其混合物。在一个实施方案中，脂族多胺可以为亚乙基多胺。在一个实施方案中，脂族多胺可选自由乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺、多胺釜残及其混合物组成的组。
分散剂可以为N-取代长链烯基琥珀酰亚胺。N-取代长链烯基琥珀酰亚胺的实例包括聚异丁烯琥珀酰亚胺。通常，衍生出聚异丁烯琥珀酸酐的聚异丁烯具有350-5000，或者550-3000或750-2500的数均分子量。琥珀酰亚胺分散剂及其制备公开于例如美国专利3,172,892；3,219,666；3,316,177；3,340,281；3,351,552；3,381,022；3,433,744；3,444,170；3,467,668；3,501,405；3,542,680；3,576,743；3,632,511；4,234,435；Re26,433；6,165,235；7,238,650；和EP专利申请0355895A中。
另一类无灰分散剂为曼尼希碱类。这些为通过较高分子量烷基取代苯酚、亚烷基多胺和醛如甲醛缩合而形成的材料。这类材料可具有一般结构：
(包括多种异构体等)且更详细地描述于美国专利3,634,515中。
另一类无灰分散剂为高分子量酯类。这些材料类似于上述琥珀酰亚胺，不同的是它们可视为通过烃基酰化剂和多元脂族醇如甘油、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和3,306,908中。
其它分散剂包括聚合物分散剂添加剂，其通常为包含极性官能以赋予聚合物分散力特性的烃基聚合物。
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。详述该处理的参考列于美国专利4,654,403和3,305,905中。
其它性能添加剂
本发明组合物可任选包含一种或多种其它性能添加剂。这些其它性能添加剂可包括一种或多种金属减活剂、粘度改进剂、清净剂、摩擦改进剂、抗磨剂、腐蚀抑制剂、分散剂(不同于本发明化合物)、分散剂粘度改进剂、特压剂、抗氧化剂、抑泡剂、反乳化剂、倾点下降剂、密封溶胀剂及其任何组合或混合物。通常，完全配制润滑油包含这些性能添加剂中的一种或多种，以及通常多种性能添加剂的包。
在一个实施方案中，本发明提供进一步包含抗磨剂、分散剂粘度改进剂、摩擦改进剂、粘度改进剂、抗氧化剂、过碱性清净剂或其组合的润滑组合物，其中所列各添加剂可以为两种或更多种该类添加剂的混合物。在一个实施方案中，本发明提供进一步包含抗磨剂、分散剂粘度改进剂、摩擦改进剂、粘度改进剂(通常烯烃共聚物如乙烯-丙烯共聚物)、抗氧化剂(包括酚类和/或胺类抗氧化剂)、过碱性清净剂(包括过碱性磺酸盐和酚盐)或其组合的润滑组合物，其中所列各添加剂可以为两种或更多种该类添加剂的混合物。
在一个实施方案中，本发明润滑组合物进一步包含抗磨剂，例如含磷抗磨剂，例如二硫代磷酸盐试剂，例如金属二烃基二硫代磷酸盐(通常二烷基二硫代磷酸锌(ZDDP))，其中金属二烃基二硫代磷酸盐贡献给润滑组合物至少100ppm、至少200ppm，或者至少250ppm，或者200ppm至1000ppm，或者250或300ppm至800ppm，或者300或400ppm至600ppm磷。在一个实施方案中，润滑组合物不含或者基本不含(意指少于100、少于50或少于20ppm)的来自金属二烷基二硫代磷酸盐如二烷基二硫代磷酸锌的磷。
在一个实施方案中，本发明润滑组合物进一步包含分散剂粘度改进剂。分散剂粘度改进剂可以以润滑组合物的0重量％至5重量％，或者0重量％至4重量％，或者0.05重量％至2重量％存在。
合适的分散剂粘度改进剂包括官能化聚烯烃，例如用酰化剂如马来酸酐和胺官能化的乙烯-丙烯共聚物；用胺官能化的聚甲基丙烯酸酯，或与胺反应的酯化苯乙烯-马来酸酐共聚物。分散剂粘度改进剂的更详细描述公开于国际公开WO2006/015130或美国专利4,863,623；6,107,257；6,107,258；和6,117,825中。在一个实施方案中，分散剂粘度改进剂可包括美国专利4,863,623(参见第2栏第15行至第3栏第52行)或国际公开WO2006/015130(参见第2页第[0008]段和第[0065]-[0073]段所述制备实施例)所述那些。
在一个实施方案中，理想的是润滑剂组合物具有低含量或者不含选自由钼、钛和硼组成的组的金属。在一个实施方案中，润滑剂组合物具有基于润滑剂组合物的重量少于100、少于50、少于20、少于20或0ppm钼。ppm为重量份每百万重量份总组合物的缩写。在一个实施方案中，润滑剂组合物具有基于润滑剂组合物的重量少于50、少于30、少于10、少于5或0ppm钛。在一个实施方案中，润滑剂组合物具有基于润滑剂组合物的重量少于100、少于80、少于50、少于25、少于10或0ppm硼。在一个实施方案中，关于钼、钛和硼的限制都一起适用于组合物。
在一个实施方案中，本发明提供进一步包含过碱性清净剂的润滑组合物。过碱性清净剂可选自由无硫酚盐、含硫酚盐、磺酸盐、salixarate、水杨酸盐及其混合物组成的组。
过碱性清净剂也可包括由混合表面活性剂体系形成的“混杂”清净剂，所述体系包含酚盐和/或磺酸盐组分，例如酚盐/水杨酸盐、磺酸盐/酚盐、磺酸盐/水杨酸盐、磺酸盐/酚盐/水杨酸盐，例如如美国专利6,429,178；6,429,179；6,153,565；和6,281,179所述。如果例如使用混杂磺酸盐/酚盐清净剂，则认为该混杂清净剂等于分别引入类似量的酚盐和磺酸盐皂的单独酚盐和磺酸盐清净剂的量。
通常，过碱性清净剂可以为酚盐、含硫酚盐、磺酸盐、salixarate和水杨酸盐的钠盐、钙盐、镁盐或其混合物。过碱性酚盐和水杨酸盐通常具有180-450TBN的总碱值。过碱性磺酸盐通常具有250-600，或者300-500的总碱值。过碱性清净剂是本领域中已知的。在一个实施方案中，磺酸盐清净剂可主要是具有至少8的金属比的线性烷基苯磺酸盐清净剂，如美国专利公开2005065045(并授予US7,407,919)的第[0026]-[0037]段所述。线性烷基苯磺酸盐清净剂可特别用于帮助改进燃料经济性。线性烷基可在沿着烷基线性链的任何位置，但通常在线性链的2-、3-或4-位上与苯环连接。在一些情况下，线性烷基主要连接在2位上，产生线性烷基苯磺酸盐清净剂。过碱性清净剂可以以0重量％至15重量％、0.1重量％至10重量％、0.2重量％至8重量％，或者0.2重量％至3重量％存在。例如，在重型柴油机中，清净剂可以以润滑组合物的2重量％至3重量％存在。对于客车发动机，清净剂可以以润滑组合物的0.2重量％至1重量％存在。
在一个实施方案中，润滑组合物包含抗氧化剂或其混合物。抗氧化剂可以以润滑组合物的0重量％至15重量％、0.1重量％至10重量％，或者0.5重量％至5重量％存在。
抗氧化剂包括硫化烯烃、烷基化二芳基胺(通常烷基化苯基萘胺，例如作为L06由CIBA市购的那些，或者烷基化二苯胺，例如二壬基二苯胺、辛基二苯胺、二辛基二苯胺)、受阻酚、钼化合物(例如二硫代氨基甲酸钼)或其混合物。
受阻酚抗氧化剂通常含有仲丁基和/或叔丁基作为位阻基团。酚基可以进一步被烃基(通常为线性或支化烷基)和/或连接在第二个芳基上的桥联基团取代。合适的受阻酚抗氧化剂的实例包括2,6-二叔丁基苯酚、4-甲基-2,6-二叔丁基苯酚、4-乙基-2,6-二叔丁基苯酚、4-丙基-2,6-二叔丁基苯酚或4-丁基-2,6-二叔丁基苯酚或4-十二烷基-2,6-二叔丁基苯酚。在一个实施方案中，受阻酚抗氧化剂可以为酯，可包括例如来自Ciba的IrganoxTML-135。合适的含酯受阻酚抗氧化剂化学的更详细描述在美国专利6,559,105中找到。
摩擦改进剂的实例包括胺、脂肪酯或环氧化物的长链脂肪酸衍生物；脂肪咪唑啉，例如羧酸和聚亚烷基-多胺的缩合产物；烷基磷酸的胺盐；酒石酸脂肪烷基酯；脂肪烷基酒石酰亚胺；或脂肪烷基酒石酰胺。在一些实施方案中，如本文所用术语脂肪可意指具有C8-22线性烷基。
摩擦改进剂还可包括材料如硫化脂肪化合物和烯烃、二烷基二硫代磷酸钼、二硫代氨基甲酸钼、向日葵油或多元醇与脂族羧酸的单酯。
在一个实施方案中，摩擦改进剂可选自由胺的长链脂肪酸衍生物、长链脂肪酯或长链脂肪环氧化物；脂肪咪唑啉；烷基磷酸的胺盐；酒石酸脂肪烷基酯；脂肪烷基酒石酰亚胺；和脂肪烷基酒石酰胺组成的组。摩擦改进剂可以以润滑组合物的0重量％至6重量％，或者0.05重量％至4重量％，或者0.1重量％至2重量％存在。
在一个实施方案中，摩擦改进剂可以为长链脂肪酸酯。在另一实施方案中，长链脂肪酸酯可以为单酯或者二酯或其混合物，在另一实施方案中，长链脂肪酸酯可以为甘油三酯。
其它性能添加剂如腐蚀抑制剂包括作为WO2006/047486公开的美国申请US05/038319第5-8段所述那些、辛基辛酰胺、十二碳烯基琥珀酸或酐和脂肪酸如油酸与多胺的缩合产物。在一个实施方案中，腐蚀抑制剂包括腐蚀抑制剂。腐蚀抑制剂可以为氧化丙烯的均聚物或共聚物。腐蚀抑制剂更详细地描述于DowChemicalCompany出版的产品手册FormNo.118-01453-0702AMS中。该产品手册标题为“SYNALOXLubricants，High-PerformancePolyglycolsforDemandingApplications”。
可使用金属减活剂，包括苯并三唑(通常为甲苯基三唑)的衍生物、二巯基噻二唑衍生物、1,2,4-三唑、苯并咪唑、2-烷基二硫代苯并咪唑或2-烷基二硫代苯并噻唑；抑泡剂，包括丙烯酸乙酯和丙烯酸2-乙基己酯的共聚物，以及丙烯酸乙酯和丙烯酸2-乙基己酯和乙酸乙烯酯的共聚物；反乳化剂，包括磷酸三烷基酯、聚乙二醇、聚氧化乙烯、聚氧化丙烯和(氧化乙烯-氧化丙烯)聚合物；倾点下降剂，包括马来酸酐-苯乙烯的酯、聚甲基丙烯酸酯、聚丙烯酸酯或聚丙烯酰胺。
可用于本发明组合物中的倾点下降剂包括聚(α烯烃)、马来酸酐-苯乙烯的酯、聚(甲基)丙烯酸酯、聚丙烯酸酯或聚丙烯酰胺。
在不同的实施方案中，润滑组合物可具有如下表1中所述的组成：
表1
本发明简单地通过用几百ppm铜将分散剂改性而提供在KHT试验中减少反应器壁上的高温沉积物形成的惊讶能力。
工业应用
在一个实施方案中，本发明提供润滑内燃机的方法，所述方法包括向内燃机中供入如本文所述润滑组合物的步骤。一般而言，将润滑剂加入内燃机的润滑系统中，然后所述润滑系统在其操作期间将润滑组合物提供给需要润滑的发动机关键部件。
上述润滑组合物可用于内燃机中。发动机组件可具有钢或铝表面(通常钢表面)，并且还可例如涂有类金刚石碳(DLC)涂层。
铝表面可由铝合金组成，其可以为共晶或超共晶铝合金(例如衍生自硅酸铝、铝氧化物或其它陶瓷材料的那些)。铝表面可存在于具有铝合金或铝复合物的气缸筒、气缸柱或活塞环上。
内燃机可具有或不具有废气循环系统(EGR)。内燃机可安装有排放控制系统或涡轮增压器。排放控制系统的实例包括柴油颗粒物过滤器(DPF)，或使用选择性催化还原(SCR)的系统。
在一个实施方案中，内燃机可以为柴油燃料发动机或生物燃料发动机(通常重型柴油机)、汽油燃料发动机、天然气燃料发动机或混合汽油/醇燃料发动机。在一个实施方案中，内燃机可以为柴油燃料发动机，在另一实施方案中，为汽油燃料发动机。
内燃机可以为2冲程或4冲程发动机。合适的内燃机包括船用柴油机、航空用活塞式发动机、低载荷柴油机以及汽车和货车发动机。
本发明内燃机不同于燃气轮机。在内燃机中，单独的燃烧事件通过杆和曲轴由直线往复力转变成转动扭矩。相反，在燃气轮机(也可称为喷气发动机)中，它是连续产生转动扭矩而不平移的连续燃烧过程，而且还可在废气出口处发展推力。这些区别产生燃气轮机和内燃机不同操作环境和应力的操作条件。
用于内燃机的润滑剂组合物可适于任何发动机润滑剂而不管硫、磷和硫酸盐灰(ASTMD-874)含量。发动机油润滑剂的硫含量可以为1重量％或更少、0.8重量％或更少、0.5重量％或更少，或者0.3重量％或更少。在一个实施方案中，硫含量可以为0.001重量％至0.5重量％，或者0.01重量％至0.3重量％。磷含量可以为0.2重量％或更少、0.12重量％或更少、0.1重量％或更少、0.085重量％或更少、0.08重量％或更少、0.06重量％或更少、0.055重量％或更少，或者0.05重量％或更少。在一个实施方案中，磷含量可以为100ppm至1000ppm，或者200ppm至600ppm。总硫酸盐灰含量可以为2重量％或更少、1.5重量％或更少，或者1.1重量％或更少、1重量％或更少、0.8重量％或更少、0.5重量％或更少，或者0.4重量％或更少。在一个实施方案中，硫酸盐灰含量可以为0.05重量％至0.9重量％、0.1重量％至0.2重量％或者至0.45重量％。理想地，在一个实施方案中，来自所有含硫添加剂的硫的量基于润滑剂组合物的重量为约500或1000至约2500ppm硫，更理想地为约500至约1500ppm。
在一个实施方案中，润滑组合物可以为发动机油，其中润滑组合物的特征可以为具有以下至少一项：(i)0.5重量％或更少的硫含量，(ii)0.1重量％或更少的磷含量，和(iii)1.5重量％或更少的硫酸盐灰含量，或其组合。
实施例
通过以下实施例进一步阐述本发明，所述实施例阐述特别有利的实施方案。尽管提供实施例以阐述本发明，但它们不意欲限制它。
对比例1(CEX1)：由2000Mn常规聚异丁烯合成琥珀酰亚胺分散剂
将2升4颈圆底烧瓶装配搅拌器、滴液漏斗、液面下管(sub-surfacetube)、温度计套管、迪安斯达克分水器和Friedrick冷凝器，装入聚异丁烯琥珀酸酐(550g，2000Mn，常规PIBSA，TAN＝68)、稀释油(505g)并用氮气清洗。将聚乙烯胺釜残(25g，34重量％N)加入滴液漏斗中。随着搅拌将混合物加热至110℃。经35分钟将多胺逐滴加入液面下管中。将温度提高至155℃并将制剂搅拌5.25小时。在迪安斯达克分水器中收集2.2g水。将硅藻土(16g)加入混合物中，并将分散剂通过硅藻土(16g)补充垫过滤以得到作为清澈棕色油的琥珀酰亚胺分散剂(1013g，KV100＝548，％N＝0.79)。
对比例2(CEX2)：含Al分散剂的合成
将对比例1的分散剂(1400g)装入装配有搅拌器、温度计套管、液面下管、迪安斯达克分水器和Friedrick冷凝器的2升4颈圆底烧瓶中并将烧瓶用氮气清洗。随着搅拌将分散剂加热至90℃。以一等份装入Al(PrO)3(45g)，并将温度提高至155℃。将混合物搅拌5小时，通过硅藻土过滤并冷却以得到棕色油(1375g，KV100＝4626cSt，0.27％Al)。
对比例3(CEX3)：含La分散剂的合成
使用对比例2的程序，不同的是将对比例1的分散剂(1300g)用La(OH)3(7.1g)处理以得到棕色油(1178g，KV100＝487cSt)。
对比例4(CEX4)：含Ba分散剂的合成
使用对比例2的程序，不同的是将对比例1的分散剂(1300g)用Ba(OH)2·8H2O(12g)处理以得到棕色油(1187g，KV100＝478cSt，0.38％Ba)。对比例5(CEX5)：含Zn分散剂的合成
使用对比例2的程序，不同的是将对比例1的分散剂(1300g)用Zn(OAc)2(18g)处理以得到棕色油(1216g，KV100＝682cSt，0.39％Zn)。
实施例6(EX6)：含Cu分散剂1的合成
使用对比例2的程序，不同的是将对比例1的分散剂(1300g)用CuSO4(13g)处理以得到浅紫色油(1216g，KV100＝544cSt，0.08％Cu)。
实施例7(EX7)：含Cu分散剂2的合成
使用对比例2的程序，不同的是将对比例1的分散剂(1300g)用Cu(OAc)2·H2O(17g)处理以得到绿色油(1200g，KV100＝611cSt，0.39％Cu)。
实施例8(EX8)：将实施例7用对比例1稀释(50:50)
将分散剂2与对比例1以50:50重量计混合以观察金属处理分散剂的浓度的影响。
实施例9(EX9)：将实施例7用对比例1稀释(25:75)
将分散剂2与对比例1以50:50重量计混合以观察金属处理分散剂的浓度的影响。
制备实施例10(PEX10)：由2000Mn常规聚异丁烯制备合成高TBN琥珀酰亚胺分散剂
将2升4颈圆底烧瓶装配搅拌器、滴液漏斗、液面下管、温度计套管、迪安斯达克分水器和Friedrick冷凝器，装入聚异丁烯琥珀酸酐(600g，2000Mn，常规PIBSA，TAN＝73)、稀释油(635g)并用氮气清洗。将聚乙烯胺釜残(43g，34重量％N)加入滴液漏斗中。随着搅拌将混合物加热至110℃。经35分钟将多胺逐滴加入液面下管中。将温度提高至155℃并将制剂搅拌5.25小时。在迪安斯达克分水器中收集3.1g水。将硅藻土(18g)加入混合物中，并将分散剂通过硅藻土(18g)补充垫过滤以得到作为清澈棕色油的琥珀酰亚胺分散剂(1117g，KV100＝183，％N＝1.2)。
实施例11(EX11)：由Cu(OAc)2xH2O合成含Cu分散剂
使用对比例2的程序，不同的是将对比例10的分散剂(1300g)用Cu(OAc)2xH2O(16.6g)处理以得到棕色油(1200.0g，KV100＝611cSt)。
润滑油：
将来自实施例CEX1-EX11的材料如表2中详述混入II组基本油料中的APISN润滑油(5W-30)中。组分描述和处理率基于无稀释油列出。对比润滑剂1包含对比分散剂实施例1，其为不含用金属后处理的琥珀酰亚胺分散剂的基线。对比润滑剂2-5(CL2-CL5)分别包含相同处理率的含有Al、La、Ba和Zn后处理的对比分散剂实施例2-5。这些金属仅具有一个稳定的氧化态。润滑剂6-9和11(L6-L9和L11)具有不同类型或量的铜作为各实施例中所用分散剂的后处理。
表2.测试的配方(处理率基于无油)
1520TBN和690TBN过碱性磺酸钙清净剂的组合
2过碱性磺酸钠清净剂(650TBN)
3C3/C6仲二烷基二硫代磷酸锌(ZDDP)
4受阻酚、烷基化二苯胺和硫化烯烃的组合
5乙烯-丙烯共聚物
6其它添加剂包括摩擦改进剂、抑泡剂和/或倾点下降剂
性能试验：
在KHT试验中测试来自表1的润滑剂。简言之，将5mL试验油以0.31cc/h泵送通过热玻璃毛细管。将试样用空气以10cc/min的速率清洗。使试样循环通过玻璃管16小时，同时将管加热至280℃。在试验结束时，根据图1中找到的等级目测评定管(10＝干净管，0＝脏污管)。
表3显示来自表2的润滑剂的KHT性能。对比润滑剂(CL1-CL5)都得到脏污的黑色管(0)，而本发明润滑剂(L6-L8)都得到8.5-9的干净得多的管。
表3.来自表1的润滑剂的KHT性能
| 润滑剂 | CL1 | CL2 | CL3 | CL4 | CL5 | L6 | L7 | L8 |
| KHT评定值 | 0 | 0 | 0 | 0 | 0 | 8.5 | 9 | 8.5 |
已知一些上述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。由此形成的产品，包括经以其意欲用途使用本发明润滑剂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润滑剂组合物。
在此通过引用将以上提及的各文件并入本发明，如果有的话，如同是本申请要求其权益的优先权文件和所有相关申请。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。除非另有说明，本文提及的各个化学品或组合物应当理解为可含有异构体、副产物、衍生物和通常应当理解存在于商品级中的其它这类材料的商品级材料。然而，除非另有说明，各个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。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，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：
(i)烃取代基，即脂族(例如烷基或烯基)、脂环族(例如环烷基、环烯基)取代基，和芳族-、脂族-和脂环族取代的芳族取代基，以及其中环通过该分子的另一部分完成(例如两个取代基一起形成环)的环状取代基；
(ii)取代的烃取代基，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(例如卤素(尤其是氯和氟)、羟基、烷氧基、巯基、烷基巯基、硝基、亚硝基和亚硫酰基(sulphoxy))的取代基；
(iii)杂取代基，即在本发明上下文中，在具有主要烃性质的同时在由碳原子组成的环或链中含有不同于碳的取代基。
杂原子包括硫、氧、氮，并且包括取代基如吡啶基、呋喃基、噻吩基和咪唑基。一般而言，对于每10个碳原子，在烃基中存在不多于2，优选不多于1个非烃取代基；通常，烃基中不存在非烃取代基。
尽管已关于优选实施方案解释了本发明，应当理解经阅读本说明书，其各个改进会为本领域技术人员所了解。因此，应当理解此处公开的发明意欲涵盖属于所附权利要求范围的改进。
Claims (15)
1.内燃机润滑剂组合物，其包含：
a)具有润滑粘度的油,
b)基于所述发动机油润滑剂组合物的重量为约0.5至10重量％的金属取代的分散剂，
c)抗氧化剂，
d)抗磨添加剂，
其中金属分散剂的金属包含铜且金属取代的分散剂的量为使得提供给所述发动机润滑剂组合物约5至500ppm铜的量。
2.根据权利要求1的组合物，其中所述金属取代的分散剂以所述润滑剂组合物的约1至约6重量％存在。
3.根据权利要求1或2的组合物，其中所述铜以约5至约100ppm存在于所述发动机润滑剂组合物中。
4.根据权利要求1或2的组合物，其中所述铜以约40至约200ppm存在于所述发动机润滑剂组合物中。
5.根据权利要求1-4的组合物，其中所述金属取代的分散剂以约1.5至约3.5重量％存在于所述发动机润滑剂组合物中。
6.根据权利要求1-5的组合物，其中所述金属取代的分散剂为金属取代琥珀酰亚胺分散剂。
7.根据权利要求1-6的组合物，其进一步包含过碱性清净剂。
8.根据权利要求1-7的组合物，其中所述抗氧化剂包含胺类抗氧化剂和/或酚类抗氧化剂。
9.根据权利要求8的组合物，其中所述胺类抗氧化剂以基于所述润滑剂组合物为约0.1至约10重量％的量存在。
10.根据权利要求8的组合物，其中所述酚类抗氧化剂以基于所述润滑剂组合物为约0.1至约10重量％的量存在。
11.根据权利要求1-10的组合物，其中所述抗磨剂为金属二硫代磷酸盐抗磨剂。
12.根据前述权利要求中任一项的组合物，其中润滑剂组合物包含基于所述润滑剂组合物的重量少于1重量％，更理想地少于0.8重量％，优选少于0.3重量％的量的硫；和少于0.2重量％，更理想地少于0.1重量％，优选少于0.05重量％的量的磷。
13.根据前述权利要求中任一项的组合物，其中润滑剂组合物包含少于100份每百万份重量/重量(ppm)，更理想地少于50ppm，优选少于10ppm的量的钼；少于50ppm，更理想地少于30ppm，优选少于5ppm的量的钛；和少于100ppm，更理想地少于50ppm，优选少于10ppm的量的硼，都基于润滑剂组合物的重量。
14.使用与铜化合物反应的无灰分散剂作为润滑组合物中的添加剂以在所述润滑剂暴露于在150℃或更高的温度下使用时减少发动机沉积物的方法。
15.使用根据权利要求12的无灰分散剂的方法，其中所述温度为200℃或更高。
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| US201361863977P | 2013-08-09 | 2013-08-09 | |
| US61/863,977 | 2013-08-09 | ||
| PCT/US2014/049917 WO2015021135A1 (en) | 2013-08-09 | 2014-08-06 | Reduced engine deposits from dispersant treated with copper |
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| CN105637073A true CN105637073A (zh) | 2016-06-01 |
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| EP (1) | EP3030639A1 (zh) |
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| CA2920022A1 (en) | 2015-02-12 |
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