CN102753663B - 改善氟烃弹性体密封相容性的方法 - Google Patents
改善氟烃弹性体密封相容性的方法 Download PDFInfo
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- CN102753663B CN102753663B CN201180008514.6A CN201180008514A CN102753663B CN 102753663 B CN102753663 B CN 102753663B CN 201180008514 A CN201180008514 A CN 201180008514A CN 102753663 B CN102753663 B CN 102753663B
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- lubricating oil
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- acid
- titanium
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- 125000001302 tertiary amino group Chemical group 0.000 description 1
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Abstract
公开了一种改善氟烃弹性体密封件与润滑油组合物的相容性的方法，所述润滑油组合物含有(a)主要量的润滑粘度基础油，和(b)一种或多种含有一个或多个碱性氮原子的分散剂。该方法涉及向润滑油组合物加入有效量的一种或多种包含一种或多种油溶性钛化合物的氟烃弹性体相容性改进剂。
Description
发明背景
1.技术领域
本发明总体上涉及改善氟烃(fluorocarbon)弹性体密封相容性的方法
2.相关技术描述
用于润滑内燃发动机和传动装置的润滑油组合物含有主要量的润滑粘度基础油、或此类油的混合物，以及一种或多种用于改善所述油的性能特性的润滑油添加剂。例如，使用润滑油添加剂来改善清净性，减少发动机磨损，提供抵抗热和氧化的稳定性，减少油耗，抑制腐性，充当分散剂，以及减少摩擦损失。一些添加剂可提供多重益处，例如分散剂-粘度改进剂。
其中最重要的添加剂是分散剂，如它们的名称所示，用于提供发动机清洁度和保持例如碳酸盐残余物、羧酸盐残余物、羰基残余物(carbonyl residue)、碳烟等处于悬浮。现今最广泛使用的分散剂是在α位被聚异丁烯(PIBSA)型烷基链取代的琥珀酸酐与聚亚烷基胺的反应产物，任选用硼衍生物、碳酸亚乙酯或专业文献中已知的其它后处理试剂后处理。
在所使用的多胺中，优选多亚烷基多胺，例如二亚乙基三胺(DETA)、三亚乙基四胺(TETA)、四亚乙基五胺(TEPA)、五亚乙基六胺(PEHA)和高级多亚烷基多胺(HPA)。
这些多亚烷基胺与聚异丁烯(PIBSA)型烷基取代的琥珀酸酐反应，按照这两种反应物的摩尔比，产生单琥珀酰亚胺、双琥珀酰亚胺或者单和双琥珀酰亚胺的混合物。
这样的反应产物，任选进行后处理，通常具有如通过总碱值或TBN所测量以每克样品的KOH的mg数计约5-50的非零碱性氮含量，这使它们能够保护发动机的金属件在使用时不受来源于润滑油或燃料氧化的酸性组分腐蚀，并同时保持所述氧化产物分散在润滑油中从而防止它们聚结和它们沉积到金属件上。
单琥珀酰亚胺或双琥珀酰亚胺型分散剂如果它们的相对碱性氮含量高，即只要多胺的氮原子数目大于聚异丁烯基团取代的琥珀酸酐基团的数目，则甚至更为有效。
然而，这些分散剂的碱性氮含量越高，则它们越加促进当今发动机中所用的氟烃弹性体密封件的侵蚀，这是因为碱性氮倾向于与这种类型密封件的酸性氢原子反应，这种侵蚀导致在弹性体表面形成裂纹并且损失这种类型材料所寻求的其它物理性能。
美国专利No.6,124,247(“‘247专利”)公开了单琥珀酰亚胺或双琥珀酰亚胺型分散剂如果它们的相对碱性氮含量高，即只要多胺的氮原子数目大于聚异丁烯基团取代的琥珀酸酐基团的数目，则甚至更为有效。然而，这些分散剂的碱性氮含量越高，则它们越加促进当今发动机中所用的氟烃弹性体密封件的侵蚀，这是因为碱性氮倾向于与这种类型密封件的酸性氢原子反应，这种侵蚀导致在弹性体表面形成裂纹并且损失这种类型材料所寻求的其它物理性能。‘247专利还公开了通过使用含有单琥珀酰亚胺或双琥珀酰亚胺型分散剂（后处理或不后处理）的润滑油组合物与硼酸化的甘油酯组合，获得了可与氟烃弹性体相容的组合物。
因此，将期望开发表现出改善的氟烃弹性体密封件相容性的润滑油组合物。
发明概述
根据本发明的一个实施方案，提供了改善氟烃弹性体密封件与润滑油组合物的相容性的方法，所述润滑油组合物包含(a)主要量的润滑粘度基础油，和(b)一种或多种含有一个或多个碱性氮原子的分散剂，该方法包括向所述润滑油组合物加入有效量的一种或多种包含一种或多种油溶性钛化合物的氟烃弹性体相容性改进剂。
根据本发明的第二实施方案，提供了改善氟烃弹性体密封件与润滑油组合物的相容性的方法，所述润滑油组合物包含(a)主要量的润滑粘度基础油，和(b)一种或多种含有一个或多个碱性氮原子的分散剂，该方法包括向所述润滑油组合物加入有效量的一种或多种如下通式的氟烃弹性体相容性改进剂。
其中R1、R2、R3和R4独立地为含烃氧基的基团。
根据本发明的第三实施方案，提供了维持或改善氟烃弹性体密封件与内燃发动机中的润滑油组合物的相容性的方法，该方法包括用润滑油组合物使发动机工作，所述润滑油组合物包含(a)主要量的润滑粘度基础油，(b)一种或多种含有一个或多个碱性氮原子的分散剂，和(c)有效量的一种或多种包含一种或多种油溶性钛化合物的氟烃弹性体相容性改进剂。
本发明方法有利地改善氟烃弹性体密封件与润滑油组合物的相容性的方法，所述润滑油组合物包含(a)主要量的润滑粘度基础油，和(b)一种或多种含有一个或多个碱性氮原子的分散剂，该方法是通过向所述润滑油组合物加入有效量的一种或多种包含一种或多种油溶性钛化合物的氟烃弹性体相容性改进剂。
优选实施方案的详述
本发明涉及改善氟烃弹性体密封件与润滑油组合物的相容性的方法，所述润滑油组合物包含(a)主要量的润滑粘度基础油，和(b)一种或多种含有一个或多个碱性氮原子的分散剂。一般而言，该方法涉及向润滑油组合物至少加入有效量的一种或多种包含一种或多种油溶性钛化合物的氟烃弹性体相容性改进剂。
总体上，所述一种或多种油溶性钛化合物由如下通式表示：
其中R1、R2、R3和R4独立地为含烃氧基的基团。这类含烃氧基的基团的实例包括但不限于C1-C20烷氧基、C6-C20芳氧基、C7-C20烷基芳氧基、C7-C20芳基烷氧基、C6-C20环烷氧基、C7-C20环烷基烷氧基、C7-C20烷基环烷氧基等和它们的混合物。在一个实施方案中，每个R1、R2、R3和R4独立地是C1-C20烷氧基、C6-C20芳氧基和C1-C6酰氧基。在另一个实施方案中，每个R1、R2、R3和R4独立地是C1-C20烷氧基或C3-C8烷氧基。在另一个实施方案中，R1、R2、R3和R4中的至少两个是相同的C1-C20烷氧基或C3-C8烷氧基。在另一个实施方案中，R1、R2、R3和R4中的至少三个是相同的C1-C20烷氧基或C3-C8烷氧基。在一个优选实施方案中，每个R1、R2、R3和R4是相同的C1-C20烷氧基或C3-C8烷氧基。
本文所使用的烷氧基的代表性实例以举例方式包括通过氧连接基与分子其余部分连接的本文所定义的烷基，即具有通式-OR5，其中R5是本文所定义的烷基、环烷基、环烷基烷基、环烯基、芳基或芳基烷基，例如-OCH3、-OC2H5或-OC6H5等。
本文所使用的烷基的代表性实例以举例方式包括1-约20个碳原子，优选1-约8个碳原子的含碳原子和氢原子的具有或不具有不饱和的连接到分子其余部分的直链或支链烷基，例如甲基、乙基、正丙基、异丙基、正丁基、正戊基等。
本文所使用的环烷基的代表性实例以举例方式包括约6-约20个碳原子的取代或未取代的非芳族单环或多环的环状体系，例如环丙基、环丁基、环戊基、环己基、任选含有一个或多个杂原子如O和N等的桥接环式基团或螺双环基团如螺-(4,4)-壬-2-基等。
本文所使用的环烷基烷基的代表性实例以举例方式包括含有约7-约20个碳原子的取代或未取代的含有环状环的基团，所述碳原子直接与烷基连接，所述烷基则在使得产生稳定结构的该烷基任意碳上连接到单体的主结构，例如环丙基甲基、环丁基乙基、环戊基乙基等，其中所述环状环可任选含有一个或多个杂原子，例如O和N等。
本文所使用的芳基的代表性实例以举例方式包括含有约6-约20个碳原子的取代或未取代的单环芳基(monoaromatic)或多环芳基，例如苯基、萘基、四氢萘基、茚基、联苯基等，任选含有一个或多个杂原子，例如O和N等。
本文所使用的芳基烷基的代表性实例以举例方式包括含有约7-约20个碳原子的取代或未取代的芳基，所述碳原子直接与烷基连接，所述烷基则在使得产生稳定结构的该烷基任意碳上连接到单体的主结构，例如-CH2C6H5、-C2H5C6H5等，其中所述芳基可任选含有一个或多个杂原子，例如O和N等。
在一个实施方案中，由式I的结构表示的合适的油溶性钛化合物的代表性实例包括钛(IV)醇盐例如甲醇钛、乙醇钛、丙醇钛、异丙醇钛、丁醇钛、2-乙基己醇钛、异丁醇钛、4-甲基-2-戊醇钛、己醇钛、戊醇钛、异戊醇钛、(三乙醇氨)异丙醇钛等和它们的混合物。
本文公开的油溶性钛化合物可商购或者可容易地通过对本领域技术人员而言将显而易见的适当合成技术来进行制备。此外，它们在室温下可以按固体或液体的形式存在，这取决于特定的化合物。或者，它们也可以以适当惰性溶剂中的溶液形式来提供。
通常，润滑油组合物中一种或多种氟烃弹性体相容性改进剂即所述一种或多种油溶性钛化合物的量基于润滑油组合物总重量可以为约0.01-约5wt.%。在另一个实施方案中，一种或多种氟烃弹性体相容性改进剂的量基于润滑油组合物总重量可以为约0.1-约2.5wt.%。
该润滑油组合物可用常规技术通过将适当量的一种或多种氟烃弹性体相容性改进剂与(a)主要量的润滑粘度基础油和(b)一种或多种含有一个或多个碱性氮原子的分散剂混合来进行制备。根据润滑油的预期用途和存在的其它添加剂来选择具体的基础油。用于本文公开的润滑油组合物的润滑粘度基础油通常以主要量，例如基于该组合物总重量计大于50wt.%，优选大于约70wt.%，更优选约80-约99.5wt.%，最优选约85-约98wt.%的量存在。本文所使用的表述“基础油”应该理解为是指作为润滑剂组分的基础料或基础料调合物，其由单一制造商按照相同规格生产（不依赖于进料来源或制造商的地点）；满足相同制造商的规格；并且由唯一配方(formula)、产品识别码或这两者加以识别。
用于本文的基础油可以是任何目前已知或后来发现的用于就任何和所有这类应用配制润滑油组合物的润滑粘度基础油，所述应用例如发动机油，船用气缸油，功能液如液压油、齿轮油、传动油等。另外，用于本文的基础油可任选含有粘度指数改进剂，例如聚合甲基丙烯酸烷基酯；烯属共聚物如乙烯-丙烯共聚物或苯乙烯-丁二烯共聚物；以及它们的类似物和混合物。
如本领域技术人员可容易地意识到的，基础油的粘度取决于应用。因此，用于本文的基础油的粘度可通常为在100摄氏度(℃)下约2-约2000厘沱(cSt)。通常地，用作机油的基础油可单独地具有在100℃下约2cSt-约30cSt，优选约3cSt-约16cSt，最优选约4cSt-约12cSt的运动粘度范围，并且可取决于所需的最终用途和成品油中产生所需机油等级的添加剂而进行选择或调合，所述等级例如SAE粘度等级为0W、0W-20、0W-30、0W-40、0W-50、0W-60、5W、5W-20、5W-30、5W-40、5W-50、5W-60、10W、10W-20、10W-30、10W-40、10W-50、15W、15W-20、15W-30或15W-40的润滑油组合物。用作齿轮油的油可具有在100℃下约2cSt-约2000cSt的粘度。
基础料可以使用包括但不限于蒸馏、溶剂精制、氢处理、低聚、酯化和再精制的各种不同方法进行制造。精制料应该基本上不含通过制造、污染或先前使用引入的物质。本发明润滑油组合物的基础油可以是任何天然或合成的润滑基础油。合适的烃合成油包括但不限于由乙烯聚合或由1-烯烃聚合以提供例如聚α烯烃或PAO油的聚合物制备的油，或者由使用一氧化碳和氢气的烃合成方法例如按费-托方法所制备的油。例如，合适的基础油是包含很少（如果有的话）的重馏分；例如很少（如果有的话）的在100℃下粘度为20cSt以上的润滑油馏分的基础油。
基础油可以衍生自天然润滑油、合成润滑油或它们的混合物。合适的基础油包括通过合成蜡和散蜡(slack wax)异构化获得的基础料，以及通过使粗产物的芳族和极性组分加氢裂化（而不是溶剂抽提）产生的加氢裂化基础料。合适的基础油包括如在API出版物1509,第14版,Addendum I,Dec.1998所定义的所有API类别即I、II、III、IV和V中的那些基础油。IV类基础油是聚α-烯烃(PAO)。V类基础油包括在I、II、III或IV类以外的所有其它基础油。虽然II、III和IV类基础油优选用于本发明，但是这些基础油可以通过将I、II、III、IV和V类基础料或基础油中的一种或多种合并进行制备。
有用的天然油包括矿物润滑油例如液体石油，溶剂处理的或酸处理的链烷属、环烷属或混合链烷属-环烷属型的矿物润滑油，衍生自煤或页岩的油，动物油，植物油（例如油菜籽油、蓖麻油和精制猪油）等。
有用的合成润滑油包括但不限于烃油和卤素取代的烃油，例如聚合和互聚的烯烃如聚丁烯、聚丙烯、丙烯-异丁烯共聚物、氯化聚丁烯、聚(1-己烯)、聚(1-辛烯)、聚(1-癸烯)以及它们的类似物和混合物；烷基苯如十二烷基苯、十四烷基苯、二壬基苯、二(2-乙基己基)-苯等；聚苯如联苯、三联苯、烷基化的聚苯等；烷基化的二苯醚和烷基化的二苯硫醚以及它们的衍生物、类似物和同系物等。
其它有用的合成润滑油包括但不限于通过使小于5个碳原子的烯烃例如乙烯、丙烯、丁烯、异丁烯、戊烯以及它们的混合物进行聚合制备的油。制备这类聚合物油的方法对于本领域技术人员而言是公知的。
另外的有用合成烃油包括具有适当粘度的α烯烃液体聚合物。特别有用的合成烃油是C6-C12α烯烃的氢化液体低聚物，例如1-癸烯三聚体。
另一类有用的合成润滑油包括但不限于其中末端羟基通过例如酯化或醚化加以改性的环氧烷聚合物，即其均聚物、共聚物和衍生物。这些油例示为通过环氧乙烷或环氧丙烷的聚合制备的油，聚氧亚烷基聚合物的烷基和苯基醚(例如具有1,000平均分子量的甲基聚丙二醇醚，具有500-1000分子量的聚乙二醇的二苯基醚，具有1,000-1,500分子量的聚丙二醇的二乙基醚，等等)或者它们的单-和多羧酸酯例如乙酸酯、混合的C3-C8脂肪酸酯、或四甘醇的C13含氧酸二酯。
又一类有用的合成润滑油包括但不限于二羧酸与各种醇的酯，所述二羧酸例如邻苯二甲酸、琥珀酸、烷基琥珀酸、烯基琥珀酸、马来酸、壬二酸、辛二酸、癸二酸、富马酸、己二酸、亚油酸二聚物、丙二酸、烷基丙二酸、烯基丙二酸等，所述醇例如丁醇、己醇、十二烷基醇、2-乙基己醇、乙二醇、二乙二醇单醚、丙二醇等。这些酯的具体实例包括己二酸二丁酯、癸二酸二(2-乙基己基)酯、富马酸二正己基酯、癸二酸二辛基酯、壬二酸二异辛基酯、壬二酸二异癸基酯、邻苯二甲酸二辛基酯、邻苯二甲酸二癸基酯、癸二酸双二十烷基酯、亚油酸二聚物的2-乙基己基二酯、由使1摩尔癸二酸与2摩尔四甘醇和2摩尔2-乙基己酸反应形成的复合酯等。
用作合成油的酯还包括但不限于由具有约5-约12个碳原子的羧酸与醇例如甲醇、乙醇等，多元醇和多元醇醚例如新戊二醇、三羟甲基丙烷、季戊四醇、二季戊四醇、三季戊四醇等制备的那些酯。
硅基油例如聚烷基-、聚芳基-、聚烷氧基-或聚芳氧基-硅氧烷油和硅酸酯油，构成另一类有用的合成润滑油。这些的具体实例包括但不限于硅酸四乙酯、硅酸四异丙酯、硅酸四(2-乙基己基)酯、硅酸四-(4-甲基-己基)酯、硅酸四(对叔丁基苯基)酯、己基-(4-甲基-2-戊氧基)二硅氧烷、聚(甲基)硅氧烷、聚(甲基苯基)硅氧烷等。还另外其它有用的合成润滑油包括但不限于含有磷的酸的液体酯例如磷酸三甲苯酯、磷酸三辛酯、癸烷膦酸(phosphionic acid)的二乙基酯等，聚合四氢呋喃等等。
润滑油可以衍生自未精制油、精制油和再精制油，可以是天然、合成或上文公开的这些类型中任意两种或更多种的混合物。未精制油是直接由天然或合成来源(例如煤、页岩或焦油砂沥青)而不进一步纯化或处理获得的那些。未精制油的实例包括但不限于直接由干馏操作获得的页岩油，直接由蒸馏获得的石油或直接由酯化工艺获得的酯油，然后它们中每一种在不进一步处理的情况下使用。精制油除了它们在一个或多个纯化步骤中进一步处理以改善一种或多种性能外与未精制油类似。这些纯化技术对于本领域技术人员是已知的，包括例如溶剂提取、二次蒸馏、酸或碱提取、过滤、渗滤、加氢处理、脱蜡等。再精制油通过将使用过的油按类似于用于获得精制油的那些方法进行处理来获得。这类再精制油还称作再生油或再加工油并且经常通过涉及除去废添加剂和油分解（breakdown）产物的技术进行另外处理。
衍生自蜡加氢异构化的润滑油基础料还可以单独使用或与上述天然和/或合成的基础料组合使用。这种蜡异构物通过将天然或合成的蜡或它们的混合物在加氢异构化催化剂上加氢异构化产生。
天然蜡典型地是通过矿物油的溶剂脱蜡回收的散蜡；合成蜡典型地是通过费-托方法产生的蜡。
该润滑油组合物还包含一种或多种含有一个或多个碱性氮原子的分散剂。用于本文的碱性氮化合物必需含有例如通过ASTM D664试验或D2896所测量的碱性氮。该碱性氮化合物选自琥珀酰亚胺类、聚琥珀酰亚胺、羧酸酰胺、烃基单胺、烃多胺、曼尼希碱、磷酰胺类、硫代磷酰胺类、膦酰胺类、分散剂粘度指数改进剂和它们的混合物。下文描述了这些含碱性氮的化合物(记住每一种必须具有至少一个碱性氮)。可以使用本领域公知的方法用例如硼和碳酸亚乙酯对任何含氮组合物进行后处理，只要该组合物仍含有碱性氮。
可用于制备本文所述的分散剂的单琥珀酰亚胺或聚琥珀酰亚胺公开在许多参考文献中并且是本领域中公知的。美国专利No.3,172,892；3,219,666和3,272,746（通过引用将它们的公开内容并入本文）中教导了由本领域的术语“琥珀酰亚胺”所包括的某些基本类型的琥珀酰亚胺和相关的物质。术语“琥珀酰亚胺”在本领域应理解为包括还可以形成的许多酰胺、酰亚胺和脒物质。然而主要产物是琥珀酰亚胺并且该术语通常公认为是指烯基取代的琥珀酸或酸酐与含氮化合物的反应产物。优选的琥珀酰亚胺由于它们的可商购性而为由烃基琥珀酸酐和亚乙基胺制备的那些琥珀酰亚胺，其中所述烃基含有约24-约350个碳原子，所述亚乙基胺中特别有代表的是乙二胺、二亚乙基三胺、三亚乙基四胺和四亚乙基五胺。在一个实施方案中，琥珀酰亚胺由约70-约128个碳原子的聚异丁烯琥珀酸酐和四亚乙基五胺或三亚乙基四胺及其混合物制备。
还包括在术语“琥珀酰亚胺”内的是烃基琥珀酸或酸酐和除含有两个或更多个仲氨基外还含有至少一个叔氨基氮的多仲胺的共低聚物。通常，该组合物具有约1,500-约50,000平均分子量。
羧酸酰胺组合物还是用于制备本发明中所用分散剂的合适起始材料。这类化合物的实例是公开于美国专利No.3,405,064（通过引用将其公开内容并入本文）中的那些。这些分散剂通常通过以下进行制备：使具有在主要脂族链中至少约12-约350个脂族碳原子并且如果需要时具有使分子呈油溶性的足够的侧链脂族基团的羧酸或酸酐或其酯，与胺或烃基多胺例如亚乙基胺反应以产生单或多羧酸酰胺。优选的是由(1)式R'COOH（其中R'为C12-C20烷基）的羧酸或者该酸与其中聚异丁烯基含有约72-约128个碳原子的聚异丁烯羧酸的混合物与(2)亚乙基胺、特别是三亚乙基四胺或四亚乙基五胺或其混合物制备的那些酰胺。
另一类用于本发明的化合物是优选为美国专利No.3,574,576（通过引用将其公开内容并入本文）中所公开类型的烃基一元胺和烃基多胺。烃基，优选烷基或者具有一个或两个不饱和位的烯属基，通常含有约9-约350个碳原子，优选约20-约200个碳原子。在一个实施方案中，烃基多胺可以是例如通过使聚异丁烯基氯和聚亚烷基多胺例如亚乙基胺如亚乙基二胺、二亚乙基三胺、四亚乙基五胺、2-氨乙基哌嗪、1,3-亚丙基二胺、1,2-亚丙基二胺等进行反应所衍生的那种。
用于提供碱性氮的另一类化合物为曼尼希碱组合物。这些组合物由酚或C9-C200烷基酚、醛例如甲醛或甲醛前体如多聚甲醛和胺化合物进行制备。所述胺可以是单胺或多胺并且典型的组合物由烷基胺例如甲胺或亚乙基胺如二亚乙基三胺或四亚乙基五胺等制备。酚类物质可以被硫化并且优选为十二烷基酚或C80-C100烷基酚。可用于本发明的典型曼尼希碱公开于美国专利No.3,368,972；3,539,663；3,649,229和4,157,309中，通过引用将它们的公开内容并入本文。美国专利No.3,539,663公开了曼尼希碱通过使具有至少50碳原子，优选50-200个碳原子的烷基酚与甲醛和亚烷基多胺HN(ANH)nH反应来进行制备，其中A为2-6个碳原子的饱和二价烷基烃，n为1-10并且其中可以进一步使所述亚烷基多胺的缩合产物与脲或硫脲反应。通过使用常规技术将硼引入到该组合物中来处理曼尼希碱通常可显著改善这些曼尼希碱作为用于制备润滑油添加剂的起始材料的有用性。
另一类用于制备本发明中所用的分散剂的组合物是磷酰胺类和膦酰胺类，例如在美国专利No.3,909,430和3,968,157中公开的那些化合物，通过引用将它们的公开内容并入本文。这些化合物可以通过形成具有至少一个P-N键的磷化合物来制备。它们例如可以通过使三氯氧磷与烃基二醇在单胺的存在下反应，或者通过使三氯氧磷与二官能仲胺和单官能胺反应来制备。硫代磷酰胺类可以通过使含有约2-约450个或更多碳原子的不饱和烃化合物，例如聚乙烯、聚异丁烯、聚丙烯、乙烯、1-己烯、1,3-己二烯、异丁烯、4-甲基-1-戊烯等与五硫化二磷和如上定义的含氮化合物，特别是烷基胺，烷基二胺，烷基多胺或亚烷基胺，例如乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺等反应来制备。
另一类用于制备本发明中所用的分散剂的含氮组合物包括所谓的分散剂粘度指数改进剂(VI改进剂)。这些VI改进剂通常通过将烃聚合物，尤其由乙烯和/或丙烯获得的聚合物（任选含有由一种或多种共聚单体例如脂环族或脂族烯烃或二烯烃衍生的其它单元）官能化来制备。所述官能化可以通过各种在聚合物上引入通常具有至少一个氧原子的一个或多个反应位的方法来进行。然后使聚合物与含氮源接触以在聚合物主链上引入含氮官能团。通常所用的氮源包括任何碱性氮化合物，特别是本文所述的那些含氮化合物和组合物。优选的氮源是亚烷基胺例如亚乙基胺、烷基胺、和曼尼希碱。
在一个优选实施方案，用于制备分散剂的碱性氮化合物是琥珀酰亚胺、羧酸酰胺和曼尼希碱。在另一个优选实施方案中，用于制备分散剂的碱性氮化合物是平均分子量为约1000或约1300或约2300的琥珀酰亚胺及其混合物。如本领域所已知的，这样的琥珀酰亚胺可用硼或碳酸亚乙酯进行后处理。
通常，润滑油组合物中一种或多种分散剂的量基于润滑油组合物总重量可以为约0.05-约15wt.%。在另一个实施方案中，一种或多种分散剂的量基于润滑油组合物总重量可以为约0.1-约9wt.%。
该润滑油组合物还可以含有用于提供辅助功能的其它常规润滑油添加剂以产生这些添加剂分散或溶解于其中的成品润滑油组合物。例如，可将润滑油组合物与以下物质调合：抗氧化剂、清净剂例如金属清净剂、防锈剂、去混浊剂、破乳剂、金属钝化剂、摩擦改性剂、抗磨损剂、倾点抑制剂、消泡剂、共溶剂、包相容剂(packagecompatibiliser)、腐蚀抑制剂、染料、极压剂以及它们的类似物和混合物。各种添加剂均为已知且可商购。可通过一般调合方法使用这些添加剂或它们的类似化合物制备本发明的润滑油组合物。
抗氧化剂的实例包括但不限于胺属(aminic)型抗氧剂例如二苯胺、苯基-α-萘基胺、N，N-二(烷基苯基)胺和烷基化苯二胺，酚类抗氧剂例如BHT、空间位阻酚型烷基酚如2,6-二叔丁基酚、2,6-二叔丁基对甲酚和2,6-二叔丁基-4-(2-辛基-3-丙酰)苯酚和它们的混合物。
金属清净剂的代表性实例包括磺酸盐、烷基酚盐、硫化的烷基酚盐、羧酸盐、水杨酸盐、膦酸盐和次磷酸盐。商购的产品通常是指中性或过碱性物质。通常通过对烃、清净剂酸如磺酸、烷基酚、羧酸酯等；金属氧化物或氢氧化物(例如氧化钙或氢氧化钙)和促进剂如二甲苯、甲醇和水的混合物进行碳酸化来制备过碱性金属清净剂。例如，为了制备过碱性磺酸钙，在碳酸化中，将钙的氧化物或氢氧化物与气态二氧化碳反应以形成碳酸钙。用过量的CaO或Ca(OH)2将磺酸进行中和，以形成磺酸盐。
含金属或形成灰分的清净剂同时起到清净剂来减少或除去沉积物的作用以及起到酸中和剂或防锈剂的作用，从而减少磨损和侵蚀并且延长发动机寿命。清净剂通常包含具有长疏水性尾部的极性头部。所述极性头部包含酸性有机化合物的金属盐。所述盐可包含基本上化学计量用量的金属，在这种情况下，它们通常被称为正盐或中性盐，并且该盐通常具有0-约80的总碱值或TBN（可通过ASTM D2896测量）。通过使过量金属化合物(例如氧化物或氢氧化物)与酸性气体(例如二氧化碳)反应可纳入大量金属碱。所得过碱性清净剂包含中和的清净剂以作为金属碱(例如碳酸盐)胶束的外层。这类过碱性清净剂可以具有约150或更大的TBN，典型地可具有约250-约450或更大的TBN。
可以使用的清净剂包括油溶性中性和过碱性磺酸盐、酚盐、硫化的酚盐、硫代磷酸盐、水杨酸盐和环烷酸盐以及金属、特别是碱金属或碱土金属如钡、钠、钾、锂、钙和镁的其它油溶性羧酸盐。最常用的金属是钙和镁，以及钙和/或镁与钠的混合物，它们可以同时存在于用于润滑剂的清净剂中。特别合宜的金属清净剂是TBN为约20-约450的中性和过碱性磺酸钙、TBN为约50-约450的中性和过碱性的钙的酚盐和硫化的酚盐、以及TBN为约20-约450的的中性和过碱性的镁或钙的水杨酸盐。清净剂的组合，无论是过碱性或中性或其两者，均可使用。
在一个实施方案中，所述清净剂可为烷基取代的羟基芳族羧酸的一种或多种碱金属或碱土金属盐。合适的羟基芳族化合物包括具有1-4、优选1-3个羟基的单核单羟基和多羟基芳烃。合适的羟基芳族化合物包括苯酚、儿茶酚、间苯二酚、对苯二酚、连苯三酚、甲酚等。优选的羟基芳族化合物是苯酚。
烷基取代的羟基芳族羧酸的碱金属或碱土金属盐的烷基取代部分衍生自具有约10-约80个碳原子的α烯烃。所用的烯烃可以是线性的、异构化线性的、支化的或部分支化的。烯烃可以是线性烯烃、异构化的线性烯烃的混合物、支化烯烃的混合物、部分支化的线性烯烃的混合物或任意前述的混合物。
在一个实施方案中，可以使用的线性烯烃混合物是选自每分子具有约12-约30个碳原子的烯烃的正构α烯烃的混合物。在一个实施方案中，正构α-烯烃使用至少一种固体或液体催化剂进行异构化。
在另一个实施方案中，所述烯烃为具有约20-约80个碳原子的支化烯属丙烯低聚物或其混合物，即衍生自丙烯聚合的支链烯烃。还可以用其它官能团如羟基、羧酸基团、杂原子等对所述烯烃进行取代。在一个实施方案中，支化的烯属丙烯低聚物或其混合物具有约20-约60个碳原子。在一个实施方案中，支化的烯属丙烯低聚物或其混合物具有约20-约40个碳原子。
在一个实施方案中，在烷基取代的羟基芳族羧酸的碱金属或碱土金属盐内的烷基（例如烷基取代的羟基苯甲酸清净剂的碱土金属盐的烷基）的至少约75mol%（例如至少约80mol%、至少约85mol%、至少约90mol%、至少约95mol%或至少约99mol%）为C20或以上。在另一个实施方案中，烷基取代的羟基芳族羧酸的碱金属或碱土金属盐是衍生自烷基取代的羟基苯甲酸的烷基取代的羟基苯甲酸的碱金属或碱土金属盐，其中所述烷基为含有至少75mol%C20以上正构α烯烃的正构α烯烃残基。
在一个实施方案中，在烷基取代的羟基芳族羧酸的碱金属或碱土金属盐内的烷基（例如烷基取代的羟基苯甲酸的碱金属或碱土金属盐的烷基）的至少约50mol%（例如至少约60mol%、至少约70mol%、至少约80mol%、至少约85mol%、至少约90mol%、至少约95mol%或至少约99mol%）为约C14-约C18。
所得的烷基取代的羟基芳族羧酸的碱金属或碱土金属盐是邻位和对位异构体的混合物。在一个实施方案中，所述产物可含有约1-99%邻位异构体和99-1%对位异构体。在另一个实施方案中，所述产物可含有约5-70%邻位异构体和95-30%对位异构体。
烷基取代的羟基芳族羧酸的碱金属或碱土金属盐可以为中性或过碱性。通常，烷基取代的羟基芳族羧酸的过碱性碱金属或碱土金属盐是其中通过例如加入碱源（如石灰）和酸性过碱化化合物（如二氧化碳）的方法而提高烷基取代的羟基芳族羧酸的碱金属或碱土金属盐的BN的物质。
过碱性盐可以呈低过碱性，例如BN低于约100的过碱性盐。在一个实施方案中，低过碱性盐的BN可以为约5-约50。在另一个实施方案中，低过碱性盐的BN可以为约10-约30。在又一个实施方案中，低过碱性盐的BN可以为约15-约20。
过碱性清净剂可以呈中过碱性，例如BN为约100-约250的过碱性盐。在一个实施方案中，中过碱性盐的BN可以为约100-约200。在另一个实施方案中，中过碱性盐的BN可以为约125-约175。
过碱性清净剂可以呈高过碱性，例如BN高于约250的过碱性盐。在一个实施方案中，高过碱性盐的BN可以为约250-约450。
磺酸盐可以由磺酸进行制备，所述磺酸典型地通过将烷基取代的芳烃例如得自石油分馏的那些物质进行磺化或者通过将芳烃进行烷基化获得。实例包括通过将苯、甲苯、二甲苯、萘、联苯或其卤素衍生物进行烷基化得到的那些物质。可在催化剂存在下用具有约3个至多于70个碳原子的烷化剂进行烷基化。烷芳基磺酸盐在每个烷基取代的芳族部分通常含有约9-约80个或更多碳原子，优选约16-约60个碳原子。
可以用金属的氧化物、氢氧化物、醇盐、碳酸盐、羧酸盐、硫化物、硫氢化物、硝酸盐、硼酸盐或醚将油溶性磺酸盐或烷芳基磺酸进行中和。根据期望的最终产物的TBN来选择金属化合物的量，但典型地为化学计量上所需量的约100-约220wt.%（优选至少约125wt.%）。
酚和硫化酚的金属盐通过与合适的金属化合物例如氧化物或氢氧化物反应来制备并且中性或过碱性产物可以通过本领域中熟知的方法获得。可以使酚与硫或含硫化合物例如硫化氢、一卤化硫或二卤化硫反应生成产物来制备硫化的酚类，所述产物通常是其中2个或更多个酚通过含硫的桥而桥接的化合物的混合物。
防锈剂的实例包括但不限于非离子聚氧乙烯试剂，例如聚氧乙烯月桂醇醚、聚氧乙烯高级醇醚、聚氧乙烯壬基苯基醚、聚氧乙烯辛基苯基醚、聚氧乙烯辛基硬酯基醚、聚氧乙烯油基醚、聚氧乙烯山梨糖醇单硬脂酸酯、聚氧乙烯山梨糖醇单油酸酯和聚乙二醇单油酸酯；硬脂酸和其它脂肪酸；二羧酸；金属皂；脂肪酸胺盐；重磺酸的金属盐；多羟基醇的偏羧酸酯；磷酸酯；(短链)烯基琥珀酸；其偏酯及其含氮衍生物；合成的烷芳基磺酸盐例如二壬基萘磺酸金属盐；以及它们的类似物和混合物。
摩擦改进剂的实例包括但不限于烷氧基化的脂肪胺；硼酸盐化的脂肪环氧化物；脂肪亚磷酸酯，脂肪环氧化物，脂肪胺，硼酸盐化的烷氧基化脂肪胺，脂肪酸的金属盐，脂肪酸酰胺，甘油酯，硼酸盐化的甘油酯；以及在美国专利No.6,372,696（通过引用将其内容并入本文）中公开的脂肪咪唑啉；摩擦改进剂由C4-C75，优选C6-C24，最优选C6-C20脂肪酸酯与选自氨、链烷醇胺以及它们的类似物和混合物的含氮化合物的反应产物获得。
抗磨损剂的实例包括但不限于二烷基二硫代磷酸锌和二芳基二硫代磷酸锌，例如描述于Born等发表于1992年1月的LubricationScience 4-2的题目为“Relationship between Chemical Structure andEffectiveness of Some Metallic Dialkyl-and Diaryl-dithiophosphatesin Different Lubricated Mechanisms”的文章中的那些（参见例如97-100页）；芳基磷酸盐和亚磷酸盐、含硫的酯、磷硫化合物、金属或无灰二硫代氨基甲酸盐类、黄原酸盐、烷基硫化物等和它们的混合物。
消泡剂的实例包括但不限于甲基丙烯酸烷基酯的聚合物；二甲基硅氧烷的聚合物及其类似物和混合物。
每种前述添加剂在使用时是以功能有效量使用以赋予润滑剂所需性能。因此，例如，如果添加剂是摩擦改性剂，则该摩擦改性剂的功能有效量将是足以赋予润滑剂所需摩擦改性特性的量。通常，这些添加剂在使用时各自的浓度基于润滑油组合物总重量计为约0.001重量%-约20重量%。在一个实施方案中，这些添加剂中每一种的浓度基于润滑油组合物总重量为约0.01-约10重量%。
本发明润滑油组合物的最终应用可以例如在于十字头柴油发动机中的船用汽缸滑润剂，内燃发动机和铁路机车中的曲轴箱滑润剂等等。润滑油组合物是流体还是固体通常将取决于是否存在增稠剂。典型的增稠剂包括聚脲乙酸盐、硬脂酸锂等。
在本发明的另一个实施方案中，本发明的一种或多种氟碳弹性体相容性改进剂可以作为添加剂包或浓缩物来提供，其中一种或多种氟碳弹性体相容性被纳入到基本上惰性的一般为液体的有机稀释剂例如矿物油、石脑油、苯、甲苯或二甲苯中以形成添加剂浓缩物。这些浓缩物通常含有约20%-约80重量%的这种稀释剂。典型地，可使用具有在100℃下约4-约8.5cSt和优选在100℃下约4-约6cSt的粘度的中性油作为稀释剂，尽管也可使用合成油，以及其它与添加剂和成品润滑油相容的有机液体。添加剂包还可典型地含有所需量和比率的一种或多种上文提及的各种其它添加剂以促进与所需量的基础油直接组合。
以下非限制性实施例说明本发明。
对比例A
通过将以下组分调合在一起获得SAE 15W-40粘度等级配方来制备基准润滑油组合物：
(a)4wt.%的硼酸化的由聚异丁烯基(PIB)琥珀酸酐（所述PIB具有1300的平均分子量）与重多胺制备的双琥珀酰亚胺；
(b)2wt.%的碳酸亚乙酯后处理的由PIB琥珀酸酐（所述PIB具有2300的平均分子量）与重多胺制备的双琥珀酰亚胺；
(c)3wt.%衍生自PIBSA、N-苯基苯二胺和平均分子量为900-1000的聚醚二胺的聚琥珀酰亚胺分散剂；
(d)硫化酚钙清净剂；
(e)二烷基二硫代磷酸锌；
(f)硼酸化的磺酸盐清净剂；
(g)磺酸镁清净剂；
(h)磺酸钙清净剂；
(i)琥珀酰亚胺钼络合物；
(j)一种或多种氧化抑制剂；
(k)泡沫抑制剂；
(l)粘度指数改进剂；和
(m)余量的II类基础油混合物。
实施例1
通过将1重量%异丙醇钛(IV)盐（可作为TPT得自DuPont）加入到对比例A的基准润滑油组合物来制备润滑油组合物。
氟烃弹性体密封件相容性的评价
将对比例A和实施例1的润滑油组合物就与氟烃弹性体密封件的相容性在Volkswagen(VW)台架试验(PV 3344)中通过将氟烃试样(AK6)悬浮在加热到150℃的基于油的溶液中168小时来进行测试。测量每个样品的体积改变百分数、点硬度(points hardness)改变(PH)、拉伸强度改变百分数(TS)和伸长率改变百分数(EL)的变化。结果汇总于表1中。
表1
结果证明，实施例1的润滑油组合物在所有类项中提供了改善的氟烃弹性体密封件相容性并且通过了每个密封试验。这些结果显示，通过将异丙醇钛(IV)加入到包含一种或多种含有一个或多个碱性氮原子的分散剂的润滑油组合物中，保护了氟烃弹性体密封件不遭受基准润滑油组合物（对比例A）中的其它组分。
应当理解可以对本文公开的实施方案作出各种修饰。因此上述描述内容不应该解释为具有限制性，而仅理解为优选实施方案的范例。例如，上文所述且作为实施本发明的最佳模式的功能仅出于说明目的。本领域技术人员采取其它配置和方法而不脱离本发明的范围和精神。此外，本领域技术人员可预想到在其所附权利要求的范围和精神内的其它修改。
Claims (14)
1.一种改善氟烃弹性体密封件与润滑油组合物的相容性的方法，所述润滑油组合物包含(a)主要量的润滑粘度基础油，和(b)一种或多种含有一个或多个碱性氮原子的分散剂，该方法包括向所述润滑油组合物加入有效量的一种或多种包含一种或多种油溶性钛化合物的氟烃弹性体相容性改进剂,其中所述一种或多种油溶性钛化合物由下面通式表示：
其中R1、R2、R3和R4独立地是含烃氧基的基团,其中基于润滑油组合物的总重量，所述润滑油组合物包含0.01-5wt.％的一种或多种氟烃弹性体相容性改进剂。
2.根据权利要求1的方法，其中所述润滑粘度基础油选自I类基础油、II类基础油、III类基础油、IV类基础油、V类基础油和它们的混合物。
3.根据权利要求1或权利要求2的方法，其中所述一种或多种分散剂选自琥珀酰亚胺、羧酸酰胺、烃基单胺、烃基多胺、曼尼希碱、膦酰胺、硫代膦酰胺和磷酰胺、噻唑、三唑、共聚物，其包含具有一个或多个另外极性官能团的羧酸酯、硼酸盐后处理的琥珀酰亚胺、碳酸亚乙酯后处理的琥珀酰亚胺、和它们的混合物。
4.根据权利要求1的方法，其中所述一种或多种分散剂是烯基琥珀酰亚胺。
5.根据权利要求3的方法，其中所述烯基琥珀酰亚胺是聚异丁烯基琥珀酰亚胺或聚异丁烯基双琥珀酰亚胺。
6.根据权利要求1的方法，其中每个R1，R2，R3和R4独立地是C1-C20烷氧基。
7.根据权利要求1的方法，所述油溶性钛化合物的R1、R2、R3和R4中的至少两个是相同的C1-C20烷氧基。
8.根据权利要求1的方法，其中所述油溶性钛化合物的R1、R2、R3和R4中的至少三个是相同的C1-C20烷氧基。
9.根据权利要求1的方法，其中所述油溶性钛化合物的R1、R2、R3和R4中的每一个是相同的C1-C20烷氧基。
10.根据权利要求1的方法，其中所述一种或多种油溶性钛化合物选自异丙醇钛(IV)，正丙醇钛(IV)，2-乙基己醇钛(IV)和它们的混合物。
11.根据权利要求1的方法，其中基于润滑油组合物的总重量，所述润滑油组合物包含0.05-15wt.％的一种或多种分散剂。
12.根据权利要求1的方法，该润滑油组合物还包含选自抗氧化剂、清净剂、防锈剂、去混浊剂、破乳剂、金属钝化剂、摩擦改进剂、抗磨损剂、倾点抑制剂、消泡剂、共溶剂、包相容剂、缓蚀剂、染料、极压剂和它们的混合物中的一种或多种润滑油添加剂。
13.根据权利要求1的方法，其中所述润滑油组合物是用于内燃发动机的曲轴箱润滑油组合物。
14.一种或多种油溶性钛化合物在包含(a)主要量的润滑粘度基础油和(b)一种或多种含有一个或多个碱性氮原子的分散剂的润滑油组合物中的用途，用以维持或改善氟烃弹性体密封件与内燃发动机中的润滑油组合物的相容性。
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