CN1188142A - 清净齿轮的无硼齿轮润滑油添加剂和其生产方法 - Google Patents

清净齿轮的无硼齿轮润滑油添加剂和其生产方法 Download PDF

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CN1188142A
CN1188142A CN97120844A CN97120844A CN1188142A CN 1188142 A CN1188142 A CN 1188142A CN 97120844 A CN97120844 A CN 97120844A CN 97120844 A CN97120844 A CN 97120844A CN 1188142 A CN1188142 A CN 1188142A
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alkyl
carbon atom
oil
atom arranged
multifunctional additive
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CN1075109C (zh
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L·D·沙托夫
M·J·勒斯特尔
S·H·特尔思尼
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Afton Chemical Intangibles LLC
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Ethyl Corp
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Abstract

本发明涉及使用无硼无灰分散剂、硫源和磷源的清净齿轮的无硼齿轮润滑油添加剂。更特别的是,优选的无硼无灰分散剂是烃基琥珀酰亚胺。当该添加剂组合物与合适的基础油混合时满足MT－1和MIL－PRF－2105E的规格而不需要硼。MT－1是清净齿轮的手动传动机构润滑油的规格。MIL－PRF－2105E是后轴润滑油的规格。

Description

清净齿轮的无硼齿轮润滑油添加剂和其生产方法
本发明涉及使用无硼的无灰分散剂、硫源和磷源的清净齿轮的无硼齿轮润滑油添加剂。更具体地说，该优选的无硼无灰分散剂是烃基琥珀酰亚胺。
术语“清净齿轮润滑油”是润滑油领域的技术术语，其含有分散剂，以便使得用其润滑的齿轮在使用的过程中保持清净。通常，清净齿轮的手动传动机构润滑油和后轴润滑油都使用分散剂以保持齿轮清净。但是，满足严格的规格例如MT-1(清净齿轮的手动传动机构润滑油的SAE标准)以及MIL-PRF-2105E(用于后轴润滑油的，U.S.Army Tank Automotive and Armaments Command，Department of the Army颁布的标准)的这些公知的润滑油都使用硼化分散剂。使用非硼化的分散剂是合乎要求的，但是通常的知识认为，对于这样的润滑油硼是必要的。
Schwind等人的U.S.P.5,354,484公开了含有大量的润滑粘度的油和少量的至少一种可溶的取代膦酸的叔脂族伯胺盐和至少一种可溶的含氮组分的润滑油和功能液，该可溶的含氮组分是通过将产生烃取代的琥珀酸的化合物与相对每当量产生酸的化合物至少约1/2当量的含有至少一个连接到氮原子上的氢原子的胺进行反应制得的。优选地是，U.S.P.5,354,484也公开了用于不同的齿轮装配的润滑剂，其是由‘484’专利的组合物和大量的烃多硫化物组成的。但是，U.S.P.5,354,484专利没有提出是否它的润滑油满足严格的规格MT-1或MIL-PRF-2105E。
本发明的一个目的是提供一种能够清净齿轮的满足某L-60-1润滑剂标准的无硼齿轮润滑油添加剂。
本发明的另一个目的是提供一种制备无硼齿轮润滑油或后轴润滑油组合物的方法。
本发明的另一个目的是提供用于齿轮润滑油或后轴润滑油组合物的添加剂体系。
本发明涉及能够清净齿轮的无硼齿轮润滑油添加剂，其是一种用于齿轮润滑油或后轴润滑油组合物的添加剂，该添加剂含有：
含氮无硼无灰分散剂(组分1)、硫源(组分2)、磷源(组分3)与其它任选的组分。当该添加剂组合物与合适的基料油掺混时，未预计到的是在不需要硼的情况下能够满足MT-1和MIL-PRF-2105E规格。MT-1是用于清净齿轮的手动传动机械润滑油的规格，MIL-PRF-2105E是用于后轴润滑油的规格。相反，对于这种类型的清净齿轮的用途，常规的润滑油是用硼化的分散剂配制的。这种类型的分散剂特别与MT-1和MIL-PRF-2105E所共有的L-60-1试验有关。L-60-1试验性能标准包括％粘度增加、％戊烷不溶物、％甲苯不溶物、碳/漆膜率和淤渣率。
使用无硼分散剂的优点包括：(i)较低的费用，其是由于没有加硼或者由于不需要把硼加到该分散剂中的另外的加工，和(ii)没有与该分散剂分离的硼的沉淀问题。
组分1：含氮无硼无灰分散剂
在本发明的组合物中使用的组分1包括含氮无硼无灰分散剂。于是，该组合物含有至少一种含氮无灰分散剂例如烃基取代的琥珀酰亚胺、烃基取代的琥珀酸或烃基取代的琥珀酰胺。
烃基取代的琥珀酰亚胺是至少一种可溶的含氮的组分，该含氮组分是通过将产生烃取代的琥珀酸的化合物(在此有时叫做“琥珀酰化剂”)与相对于每当量产生酸的化合物至少约1/2当量的含有至少一个连接到氮原子上的氢原子的胺进行反应制得的。以这种方法得到的含氮组分通常是复杂的混合物，其精确的组成是不容易鉴别的。因此，该组分一般的是用制备方法描述的。在此，该含氮的组分有时叫做“酰胺”。该含氮的组分或者是油溶的，或者它们是在本发明的含油的润滑和功能液中可溶的。
可用于本发明的润滑组合物的可溶的含氮组分是本领域已知的，已经公开在很多美国专利中，包括U.S.P.3,172,892；3,215,707；3,272,746；3,316,177；3,341,542；3,444,170；3,454,607；3,541,012；3,630,904；3,632,511；3,787,374；4,234,435；和5,354,484。
上述的美国专利在此特别地列出，把它们对于含氮组分的制备引用作为参考。但是，任何这些参考文献中的含硼的组分特殊的不包括在本发明之内。
一般的，制备该可溶的含氮组分的方便的路线包括将产生烃取代的琥珀酸的化合物(“羧酸酰化剂”)与含有至少一个连接到氮原子上的氢原子(即H-N＝)的胺进行反应。产生烃取代的琥珀酸的化合物包括琥珀酸、琥珀酸酐、卤化物和酯。在产生琥珀酸的化合物上的烃取代基中的碳原子数可以在很宽的范围内变化，条件是该含氮的组分在本发明的润滑组合物中是可溶的。于是，该烃取代基一般可以含有平均至少约30个脂族碳原子，优选含有平均至少约50个脂族碳原子。除了油溶性的考虑之外，取代基中的平均碳原子数的下限也取决于在本发明的润滑油组合物中的这种化合物的效果。如果极性基团不是以大到足以明显地改变该基团的烃性质的比例存在的话，琥珀酸化合物的烃取代基可以含有极性基团。
大多数烃取代基源主要包括高分子量基本上饱和的石油馏分和基本上饱和的烯烃聚合物，特别是每个单烯烃有2-30个碳原子的单烯烃的聚合物。特别有用的聚合物是1-单烯烃的聚合物例如乙烯、丙烯、1-丁烯、异丁烯、1-己烯、1-辛烯、2-甲基-1-庚烯、3-环己基1-丁烯和2-甲基-5-丙基-1-己烯。中间烯烃的聚合物，即其中烯烃键不在端位的烯烃同样是有用的。它们通过2-丁烯、3-戊烯和4-辛烯来说明。
也可以用的是烯烃的共聚物例如上面用其它的可共聚的烯烃物质说明的那些例如芳族烯烃、环烯烃和聚烯烃。这样的共聚物包括例如通过聚合异丁烯与苯乙烯；异丁烯与丁二烯；丙烯与异戊二烯；乙烯与戊间二烯；异丁烯与氯丁二烯；异丁烯与对甲基苯乙烯；1-己烯与1，3-己二烯；1-辛烯与1-己烯；1-庚烯与1-戊烯；3-甲基-1-丁烯与1-辛烯；3，3-二甲基-1-戊烯与1-己烯；异丁烯与苯乙烯和戊间二烯等制备的那些。
在制备本发明的取代的琥珀酸酰化剂的过程中，一种或者多种上述的聚烯烃与一种或者多种选自马来酸或马来酸酐或者富马酸或富马酸酐的酸性反应物反应。通常，马来酸或者富马酸反应物是马来酸、富马酸、马来酸酐，或其两种或多种的混合物。马来酸反应物通常比富马酸反应物优选，因为前者较容易得到，并且一般是较容易与聚烯烃(或其衍生物)反应，来制备在本发明中可用的生产取代的琥珀酸的化合物。特别优选的反应物是马来酸、马来酸酐和它们的混合物。由于可得性和容易反应，通常将使用马来酸酐。
为了方便和简洁，后面常用术语“马来酸反应物”。当使用时，应该了解到该术语一般是指选自马来酸或富马酸反应物的酸性反应物。另外，此处所用的术语“琥珀酰化剂”是代表产生取代的琥珀酸的化合物。
制备本发明的取代的琥珀酰化剂的一种方法在U.S.P.3,219,666中有部分说明，其在此特别列出，其中关于制备琥珀酰化剂的介绍作为参考。该方法方便地称为“两步法”。其第一步是氯化聚烯烃，直到每分子重的聚烯烃平均至少约有一个氯基。对本发明来说，聚烯烃的分子量是相应于数均分子量(Mn)值的重量。氯化仅包括聚烯烃与氯气接触，直到所需要量的氯合并到氯化烯烃中。氯化一般在约75℃-约125℃的温度进行。
对本发明来说，两步氯化法的第二步通常是在约100℃-约200℃的温度范围内将氯化的聚烯烃与马来酸反应物反应。氯化聚烯烃与马来酸反应物摩尔比通常约1∶1。(对本发明来说，一摩尔氯化聚烯烃是相应于未氯化的聚烯烃的Mn值的氯化聚烯烃的重量。)但是，可以使用化学计量过量的马来酸反应物，例如摩尔比为1∶2。
如果在产物中不存在所需数目的琥珀基团，所得到的聚烯烃取代的琥珀酰化剂可任意地再氯化。
制备本发明的取代的琥珀酸酰化剂的另一个方法是用在U.S.P.3,912,764和U.K.P.1,440,219中所述的方法，二者在此特别列出，其关于该方法的介绍作为参考。按照该方法，在“直接酰化”过程中，聚烯烃和马来酸反应物通过一起加热首先进行反应。
与产生琥珀酸的化合物反应形成无硼含氮组分的胺可以是单胺和多胺。该单胺和/或多胺的特征必须是在它们的结构中存在至少一个伯(即H2N-)或仲(即H-N＝)氨基。该胺可以是脂族、环脂族、芳族或杂环的。而且，该胺可以是未取代的或者脂族取代的、环脂族取代的或芳族取代的。另外，该胺可以是饱和的或者不饱和的。该胺也可以含有非烃取代基或基团，只要这些基团不明显地影响胺与本发明的酰化剂的反应。这些非烃取代基或基团包括低级烷氧基、低级烷基氢硫基、硝基，中断基团例如-O-和-S-(例如象这样的基团-CH2CH2-X-CH2CH2，其中X是-O-或-S-)。
一般的，组分1的胺的特征可以是式子R1R2NH，其中R1和R2各自独立的是氢或烃、氨基取代的烃、羟基取代的烃、烷氧基取代的烃、氨基、氨基甲酰、硫代氨基甲酰、脒基和酰基亚氨基，条件是R1和R2中的仅一个可以是氢。
除了支链聚亚烷基多胺、聚氧亚烷基多胺和下面更详细的介绍的高分子量的烃基取代的胺之外，通常这些胺含有总数少于约40个碳原子，并且一般总数不多于20个碳原子。
脂族单胺包括单脂族和二脂族取代的胺，其中脂族基可以是饱和的或不饱和的和直链的或支链的。于是，它们是伯或仲脂族胺。这样胺包括例如单和二烷基取代的胺、单和二烯基取代的胺和具有一个N-烯基取代基和一个N-烷基取代基的胺等。如上所述，在这些脂族单胺中的碳原子总数通常要不超过约40，更好不超过约20个碳原子。这样的单胺的具体例子包括乙胺、二乙胺、正丁胺、二正丁胺、烯丙胺、异丁胺、椰子油胺、硬脂胺、月桂胺、甲基月桂胺、油胺、N-甲基辛胺、十二烷基胺、十八烷基胺等。
环脂族单胺是那些其中有一个环脂族取代基通过环结构中的一个碳原子直接连接到氨基氮原子上的单胺。
合适的芳族胺包括那些其中芳环结构的碳原子直接连接到氨基氮原子上的单胺。
从其衍生含氮无灰分散剂的多胺主要包括那些大部分与式I相符的亚烷基胺：
Figure A9712084400101
其中n优选是小于约10的整数，A是氢原子或者基本上优选具有多达约30个碳原子的烃基，亚烷基优选是具有少于约8个碳原子的低级亚烷基。该亚烷基胺主要包括亚甲基胺、亚乙基胺、亚丁基胺、亚丙基胺、亚戊基胺、亚己基胺、亚庚基胺、亚辛基胺、其它的多亚甲基胺。它们特殊的例子是亚乙基二胺、三亚乙基四胺、丙邻二胺、癸二胺、亚辛基二胺、二(七亚甲基)三胺、三亚丙基四胺、四亚乙基五胺、三亚甲基二胺、五亚乙基六胺、二(三亚甲基)三胺。例如通过缩合两种或者多种上述的亚烷基胺得到的高级的同系物同样是可以用的。
通过将产生琥珀酸的化合物与胺的反应得到的含氮组分可以是胺盐、酰胺、亚酰胺、咪唑啉及其混合物。为了制备含氮的组分，一般在约80℃直到该混合物或产物的分解温度的高温下，任意的在普通液体，基本上是惰性的有机溶剂/稀释剂的存在下，把一种或多种产生琥珀酸的化合物和一种或多种胺加热。通常使用的温度是约100℃到约300℃，条件是300℃不超过分解温度。
产生琥珀酸的化合物和胺进行反应，其量是每当量产生酸的化合物足以提供至少约1/2当量的胺。一般，胺存在的最大量应是每当量产生琥珀酸的化合物约2摩尔的胺。对于本发明来说，1当量的胺是胺的总重量除以存在的氮原子的总数所得的量。
本发明的优选的含氮无硼无灰分散剂是式子IIa和IIb的混合物：
Figure A9712084400111
其中，R是C2-C30聚亚烷基部分，优选聚乙烯、聚丙烯和聚丁烯(特别是聚异丁烯)。
R1是有1-40个碳原子，优选1-10个碳原子，更优选1-5个碳原子的烷基，最优选R1是(CH2)n，n是整数1-5，
R2是有1-40个碳原子，优选1-10个碳原子，更优选1-5个碳原子的烷基，最优选R2是(CH2)m，m是整数1-5，
R3选自氢和有1-40个碳原子的烷基，优选是氢和1-10个碳原子的烷基，
R4选自氢和有1-40个碳原子的烷基，优选是氢和1-10个碳原子的烷基，
参数X是整数0-12，优选2-8，更优选2-5，和
不存在其中单个氮原子连接到H和两个羰基的琥珀酰亚胺化合物。
优选的无灰分散剂是烃基琥珀酰亚胺，其中烃基取代基是氢化的或者未氢化的聚烯烃基，优选数均分子量(用凝胶渗透色谱法测定的)为700-10,000，更优选700-5,000，还更优选750-2,500，最优选950-1350的聚异丁烯基。
优选的无硼无灰分散剂的例子是式子IIIa和IIIb的聚异丁烯琥珀酰亚胺-聚乙烯多胺的混合物：
Figure A9712084400121
其中PIB是聚异丁烯，R3是H，R4是H。
组分2：含硫添加剂
很多种的含硫极压添加剂或抗磨添加剂可以用于本发明的实践。在这种用途的合适的组分中，包括硫化的动物或植物脂或油、硫化的动物或植物脂肪酸酯、磷的三价或五价酸的全或部分酯化的酯、硫化烯烃(见例如U.S.P.2,995,569；3,673,090；3,703,504；3,703,505；3,796,661；3,873,545；4,119,549；4,119,550；4,147,640；4.191,659；4,240,958；4,344,854；4,472,306；和4,711,736)，二烃基多硫化物(见例如U.S.P.2,237,625；2,237,627；2,527,948；2,695,316；3,022,351；3,308,166；3,392,201；4,564,709和G.B.1,162,334)，硫化Diels Alder加成物(见例如U.S.P.3,632,566；3,498,915和Re 27,331)，硫化二环戊二烯(见例如U.S.P.3,882,031和4,188,297)，脂肪酸酯和单不饱和烯烃的硫化或共硫化的混合物(见例如U.S.P.4,149,982；4,166,796；4,166,797；4,321,153；4,481,140)，脂肪酸、脂肪酸酯和α＝烯烃的共硫化混合物(见例如U.S.P.3,953,347)，官能团取代的二烃基多硫化物(见例如U.S.P.4,218,332)，硫代醛、硫代酮和其衍生物(例如酸、酯、亚胺或内酯)(见例如U.S.P.4,800,031；和PCT国际专利申请公开WO88/03552)，环硫化合物(见例如U.S.P.4,217,233)，含硫乙缩醛衍生物(见例如U.S.P.4,248,723)，萜烯和环烯烃的共硫化混合物(见例如U.S.P.4,584,113)，和多硫烯烃产物(见例如U.S.P.4,795,576)。
优选的用作组分(i)的材料是含硫的有机化合物，其中含硫部分直接键合到碳原子或者多个硫原子上。
一种特别优选类型的这种添加剂是通过烯烃例如异丁烯和硫反应制得的。该产物例如硫化异丁烯，优选硫化聚异丁烯，一般的硫含量为10-50％，优选30-50％(重)。许多其它的烯烃或者不饱和烃例如异丁烯二聚物或三聚物都可以用来形成这样的添加剂。
其它特别优选类型的这种添加剂是由式R6-Sx-R7表示的一种或多种化合物构成的多硫化物，其中R6和R7是烃基，其每一个优选含有3-18个碳原子，X优选2-8，更优选2-5，特别是3。烃基可以是很宽范围的类型，例如烷基、环烷基、链烯基、芳基或芳烷基。叔烷基多硫化物例如二叔丁基三硫化物和含有二叔丁基三硫化物的混合物(例如主要或者完全由三、四和五硫化物组成的混合物)是优选的。其它的可以用的二烃基多硫化物的例子包括二戊基多硫化物、二壬基多硫化物、二十二烷基多硫化物和二苄基多硫化物。
组分3：含磷的添加剂
组分3是由一种或多种含磷的酸的一种或多种偏酯，优选五价磷的一种或多种酸的一种或多种偏酯的一种或多种油溶的胺盐组成的，这样的化合物可以用式子IV，V和VI表示，或其混合物：
Figure A9712084400141
在式子IV，V和VI中，每一个R9-R15单独是烃基，每一个X1-X12单独是氧原子或硫原子。
有用的盐或加成物可以由一种或多种五价磷的酸和选自下面的胺制成的，所说的胺选自辛胺、壬胺、癸胺、十一烷胺、十二烷胺、十三烷胺、十四烷胺、十五烷胺、十六烷胺、十七烷胺、十八烷胺、环己胺、苯基胺、3，5-二甲基苯甲胺、油酰胺、椰子油胺、豆胺、C10-12叔烷基伯胺、和苯乙胺和任意这些化合物的混合物。仲烃基胺和叔烃基胺也可以使用，或者单独使用或者彼此混合使用或者与伯胺混合使用。于是，伯胺、仲胺和/或叔胺的任何混合物，不管单胺或多胺，都可以以盐或加成物的形式使用。优选使用伯胺。也许值得指出的是，为了方便起见，已使用“硫代-硫羧”系统命名，命名了上面所指的部分酯化的磷的五价酸。这样的化合物也可以用“硫代”系统命名。例如S，S-二烃基磷四硫代酸，(RS)2P(S)(SH)。同样，O，S-二烃基硫代磷酸也可以叫做O，S-二烃基磷二硫代酸，(RO)(RS)P(S)(OH)；S，S-二烃基二硫代磷酸也叫做S，S-二烃基磷二硫代酸，(RS)2P(O)(OH)。O，O-二烃基硫代磷酸也叫做O，O-二烃基磷硫代酸，(RO)2P(S)(OH)。
制备这样的胺盐的方法是公知的，并且在文献中已经报导。见例如U.S.P.2,063,629；2,224,695；2,447,288；2,616,905；3,984,448；4,431,522；Pesin等人的Zhumal Obshchei Khimii Vol，31，N0.8，pp.2508-2515(1961)；和PCT国际专利公开WO 87/07638。
组分3的一般的方案是由大约80∶20-20∶80，优选大约50∶50的下面的两个式子VII和VIII的化合物的混合物组成，其中R17是有4-10个碳原子的烃基，R18是8-22个碳原子的烃基：
在一般的含磷的添加剂中，R17是约5个碳原子的烃基(酸式磷酸戊酯)，约8个碳原子的烃基(2-乙基己基酸式磷酸酯)或酸式磷酸辛酯。
典型的R18是C18单不饱和和C11-C14支链烃基的混合物。在混合物中这些组分之间的一般比例是10-50％C18和50-90％C11-C14组分，优选20-30％C18和80-70％C11-C14组分，更优选25-30％C18和70-75％C11-C14。这样的胺的例子包括油酰胺(9-十八烯-1-胺)和C11-C14叔烷基伯胺。其它典型的胺是正辛胺。该C11-C14胺可以单独使用，但该混合物达到一个磨损和氧化性能的较好的平衡。
一般的反应包括大约50/50的二：单取代的式IX的酸式磷酸酯的混合物(二烷基-和单烷基磷酸)
Figure A9712084400152
与式X的胺反应：
                 R18-NH2    X上述的反应形成含磷的添加剂，其包括式XI的化合物的混合物：
Figure A9712084400153
稀释剂
本发明的添加剂浓缩物优选含有合适的稀释剂，最优选合适粘度的含油的稀释剂。这样的稀释剂可从天然或合成源衍生。在这当中，矿物(含烃的)油是石蜡基油、环烷基油、沥青基油和混合基油。其中，一般的合成基油包括聚烯烃油(特别是加氢的α-烯烃低聚物)、烷基化的芳族聚亚烷基氧化物、芳族酯和羧酸酯(特别是二酯油)。也可以使用天然油和合成油的混合物。优选的稀释剂是轻烃基油，天然的或合成的都行。一般的，稀释油应该具有的粘度是在40℃为13-35厘沲，优选在40℃为18.5-21.5厘沲。对于该用途，特别优选的是在40℃的粘度约为19厘沲、在15.6℃(60°F)比重(ASTM D 1298)为0.855或0.893(最优选约0.879)和ASTM颜色(D1500)最大2的100中性矿物油，或者在40℃的运动粘度约为4.5厘沲、比重为0.85-0.88和ASTM颜色最大2的45中性加氢的矿物油。
齿轮油基料
其中使用本发明的组合物的齿轮油可以是天然或者合成油，或其混合物，只要该润滑剂用于齿轮油中有合适的粘度。于是，该基料油通常应具有的粘度为SAE 50-SAE 250，更通常应为SAE 70W-SAE 140。合适的汽车齿轮油也包括交叉级油例如75W 140、80W-90、85W-140、85W-90等。对于该用途的基料油一般的是矿物油基本原料，例如常规的和溶剂精制的石蜡基中性光亮油料、氢处理的石蜡基中性光亮油料、环烷基油或者汽缸油，包括直馏油和混合油。在本发明的实践中也可以使用合成基础油料，例如聚α-烯烃油(PAO)、烷基化的芳香烃、聚丁烯、二酯、聚酯、聚乙二醇或聚苯醚，和其混合物。典型的这种类型的油是聚α-烯烃和合成二酯以重量比(PAO：酯)为95∶5-50∶50，一般为75∶25的混合物。对于满足L-60-1标准来说，某些基本原料比其它的原料工作的好。例如加氢的基本原料和合成基本原料是优选的。
比例
在形成本发明的齿轮油的过程中，润滑剂基础原料通常含有以下浓度(在本发明的齿轮油中活性组分的重量百分比)的上述组分1、2和3：
                     表1
    组分   优选的范围 更优选的范围 最优选的范围
(1)无灰分散剂     0.3-3.0     0.6-2     0.7-1.4
(2)含硫的添加剂     1-5.25     1.5-4.5     2-4
(3)含磷的添加剂     0.1-3     0.2-2     0.3-1.2
随意地，其它的组分例如稀释剂、消泡剂等，在该齿轮油中也存在。但是，本发明的优选的组合物基本上是没有含金属的组分。
本发明的组合物可以用作添加剂浓缩物。在含有稀释剂例如含油的液体的添加剂浓缩物中，按浓缩物的总重量计，在含油液体中该浓缩物的总含量通常应该为1-13％，优选1.5-10％，最优选2-9％(包括其它辅助组分，如果使用的话)。
在本发明的添加剂浓缩物中，组分(1)、(2)和(3)的重量比应该是这样一个值，即当该浓缩物以其合适的剂量用于含油液体中时，应使其满足表1的范围。其它的组分，例如如下所述的组分也可以包括在这样的添加剂浓缩物中。
其它组分
本发明的齿轮油和齿轮油添加剂浓缩物可以含有各种其它的常规添加剂，以提供它们附加的作用。这些包括例如下面的物质：
消泡剂-这种类型的说明性的物质包括合适粘度的硅油、一硬脂酸甘油酯、棕榈酸聚乙二醇酯、一硫代磷酸三烷基酯、磺化篦麻油酸酯、苯甲酰丙酮、水杨酸甲酯、一油酸甘油酯、二油酸甘油酯等。在该添加剂浓缩物中，一般以直到约1％的浓度使用消泡剂。
破乳剂-在齿轮油中可以用作破乳剂的一般的添加剂包括烷基苯磺酸盐、聚环氧乙烷、聚环氧丙烷、油溶的酸的酯等，在该添加剂浓缩物中，一般以直到约3％的浓度使用这样的添加剂。
硫清除剂-这种类型的添加剂包括象噻二唑、三唑这样的物质，一般的，在高温条件下含这部分的化合物与游离硫反应。见例如U.S.P.3,663,561和4,097,387。其在浓缩物中的浓度一般的是直到约3％。
抗氧化剂通常可以用于齿轮油配方的抗氧化剂包括酚化合物、胺、亚磷酸盐等。其在浓缩物中的量直到约5％一般就足够了。其它常用的添加剂或组分包括防锈剂、抗磨剂、清净剂、染料、金属钝化剂、倾点抑制剂和稀释剂。
于是，本发明包括所述类型的无硼无灰分散剂作为组分1、所述的含硫添加剂作为组分2和所述的含磷添加剂作为组分3以及其它任选的组分的组合物来生产添加剂，当其搀和在适合的基础油(在齿轮油基料中描述的)中时可以满足MT-1和MIL-PRF-2105E的规格。MT-1和MIL-PRF-2105E的规格是对于清净齿轮的手控传动机构润滑油(MT-1)和后轴润滑油(MIL-PRF-2105E)的要求。对于这种类型的清净齿轮的应用的添加剂通常是与硼化分散剂配制。
使用无硼分散剂的优点包括：
1.较低的费用，其是由于没有加硼或者由于不需要把硼加到该分散剂中的另外的加工；和
2.没有与该分散剂分离的硼的沉淀。
MIL-PRF-2105E标准
MIL-PRF-2105E标准(1995年8月22日泡括大量的必须通过的试验。MIL-PRF-2105E标准由U.S.Army Tank Automotive and ArmamentsCommand，Department of the Army颁布，其全部内容在此列为参考文献。齿轮润滑油有下面的等级：75W、80W-90和85W-140。
为了满足MIL-PRF-2105E，该齿轮润滑油有表2所规定的性能。
              表2
    性能1     等级75W     等级80W-90     等级85W-140
运动粘度，cSt，@100℃  最小最大@40℃2表观粘度cP，150,000最大@℃，温度成沟点，℃，最大闪点，℃，最小 4.1---40-45150 13.5＜24.0--26-35165 24.0＜41.0--12-20180
1应该报导所有的规格值2由用户提出
该齿轮润滑油也满足下面表3所列的标准。
                            表3
    试验     ASTM试验方法9 FED-STD-791方法号
运动粘度     D455
表观粘度     D2983
粘度指数     D2270
成沟点     3456
闪点     D92
重度，API     D287
倾点     D97
戊烷不溶物     D893
残碳     D524
颜色     D1500
总酸值     D664
皂化值     D94
沸点分布     D2887
硫3   D1552，D2622，D129，D4294，D4927，D4951，D5185
磷4     D1091，D4047，D4927，D4951，D5185
氯5     D808，D1317
氮     D3228，D4629
金属组分     D4628，D4927，D4951，D5185
起泡     D892
储存稳定性     3440
相容性6      3430
铜片腐蚀     D130
湿分腐蚀7     L-33
热和氧化稳定性     L-60-1(D-5704)
载荷、极压和沉淀性能齿轮伤痕7，8齿轮疲劳和沉积7 L-42L-37
循环周期     D-5579
弹性体相容性     D-5662
3D1552是优选的方法。D4294仅仅是与基础原料使用。4D1091是优选的方法。5D808是优选的方法，但是D1317可以用作替代方法。6见相容性参数。7根据ASTM STP 512A。8见齿轮伤痕参数。9所有的ASTM试验方法的拷贝应该委托the American Society for Testingand Materials，1916 Race Street，Philiadelphia，Pennsylvania 10103，U.S.A.
成沟点
当按照表3(方法3456 FED-STD-791)进行试验时，在表2所示的温度下该齿轮润滑油不成沟。
起泡
当按照表4(ASTM D892)中所列的方法进行试验时，该齿轮润滑油有下面的起泡性能。
a.在24±0.5℃开始试验。鼓泡5分钟之后，当即应该留有不超过20mL泡沫。
b.在93.5±0.5℃中期试验。鼓泡5分钟之后，当即应该留有不超过50mL泡沫。
c.在24±0.5℃最后试验。鼓泡5分钟之后，当即应该留有不超过20mL泡沫。
储存稳定性
当按照表3(方法3440，FED.-STD-791)进行试验时，该齿轮润滑油应该显示分离的固体物质、液体物质或这两种物质的混合物的性能。当分离的物质是固体时，每个离心管的重量平均增加和超过清净管的起始重量的残余物的量应该不超过样品中初始所含的添加剂物质的0.25％(质量)。当分离的物质是液体时，其应该不超过样品中初始所含的添加剂物质的0.50％(体积)。
相容性
当按照表3(方法3430，FED-STD-791)限制在MIL-PRF-2105E时，该齿轮润滑油与其它的齿轮润滑剂会是相容的。一般的，用该油的分离混合物与6种选择的参照油品进行该试验。
湿分腐蚀
在湿气的存在下，该油能防止对齿轮单元部件的腐蚀或者使得该腐蚀减少到最小。当该油按照表3(ASTM STP 512A，L-33试验)进行试验时，会显示满意的性能，并且显示的试验结果是在试验盖板上有1％或者少于1％的锈，并且在齿轮的齿、支承和功能部件上没有锈。
热稳定性和氧化稳定性
该油能耐热氧化和化学氧化。当该油按照表3(ASTM D-5704，L-60-1试验)进行5小时试验时，会显示满意的性能，并且满足表4中的标准。
                 表4
    参数     限度
运动粘度增加％，@100℃，cSt正戊烷不溶物，(重)％甲苯不溶物，(重)％碳/漆膜率淤渣率     100最大3.0最大2.0最大7.5最小9.4最小
如果进行一个以上的试验时，那么2个试验结果的平均值必须满足上面的限度。允许不超过3个试验。当进行3个试验时，3个试验之一可以废弃，留下的2个试验的平均值必须满足上面的限度。一般的，该油的正戊烷不溶物约为0-3％(重)，甲苯不溶物约为0-2.0％(重)，碳/漆膜率约为7.5-10，淤渣率约为9.4-10。该限度是对于MIL-PRF-2105E鉴定试验从军事角度上建立的。
极压载荷和沉积性能
在高速和冲击负载的条件和在高速、低转矩和低速、高转矩的条件下，该油能防止齿轮的损坏和润滑剂的沉积，或者使齿轮的损坏和润滑剂的沉积减少到最少。
齿轮伤痕
在高速和冲击负载的条件下，当该油按照表3(ASTM STP 512A，L-42试验)重复进行试验时，会显示满意的性能，并且显示伤痕少于或者等于ASTM参照油RGO114，或者由ASTM承认的最近的混合物。
对于等级75W油，应该改进L-42齿轮伤痕试验，以使试验的顺序II部分(高速)在79℃开始，顺序IV部分(冲击负载)在93℃通过喷水开始试验，最大的温升是5.5-8.3℃。
齿轮损坏和沉积
当该油按照表3(ASTM STP 512A，L-37试验)，使用未处理的和磷酸盐处理的齿轮组件进行试验，应显示满意的性能，并且在低速、高转矩的条件下能够防止齿轮-齿起皱、波动、点蚀、粘结、剥落，和过度的磨损或者其它表面损坏和有害的沉积，不产生轴承滚珠或轴承套的过度磨损、剥蚀或腐蚀。
铜片腐蚀
该油能够使铜片腐蚀减少到最少。当在121±1℃该油按照表3(ASTM D130)试验3小时应该显示满意的性能，当与ASTM铜片剥落腐蚀标准比较时，显示铜片剥落腐蚀不超过ASTM No.2。
循环周期
当该油按照表3(ASTM D-5579)进行试验时，会显示满意的性能。当进行高-低范围和高温循环操作时，该试验评价齿轮润滑剂的热稳定性。在相同的试验台，通过防止在等于或者低于现有的5次通过的标准油的结果的平均值所产生的两个不同步的转换，该油会避免损害同步测试器的性能。
弹性体相容性
该齿轮润滑剂会使弹性体材料的破坏减少到最少。当该油按照表3(ASTMD-5662)进行试验和评定时会显示满意的性能，并且在单一的弹性体批料中调整到适当的微小的变化时显示试验结果满足表5的通常的标准。
                  表5
    参数     最小     最大
聚丙烯酸酯@150℃，240小时：长度变化，％硬度变化，点体积变化，％ --25-5 -60+5.0+30
氟代弹性体@150℃，240小时：长度变化，％硬度变化，点体积变化，％ --5-5 -75+10+15
MT-1和GL-5标准
本说明书所公开的齿轮润滑剂满足American Petroleum Institute(API)Service Classification MT-1和GL-5，并且预期用于汽车齿轮机构、重负荷工业型封闭齿轮机构、重负荷非同步型7&8手动传动和汽车装备的液体润滑的万向节使用。
MT-1有下面如表6所列的规格。
                         表6
    最小     最大
ASTM D-5704L-60_1热稳定性和清净性能％粘度增加％戊烷不溶物％甲苯不溶物碳/漆膜率(大齿轮)淤渣率(4个面的平均值) ------7.59.4 100％3.0％2.0％----
ASTM D-5662齿轮油与密封材料的相容性
聚丙烯酸酯@150℃加长，％硬度点体积变化，％ -60-20-5 无+5.0+30
氟代弹性体@150℃加长，％硬度点体积变化，％ -75-5-5 无+10+15
ASTM D-5579在手动传动转换顺序中评价油的循环周期 比最后5次通过的参考值大 --
铜片腐蚀保护的试验方法ASTM D 130         --     2
评价耐磨损(FZG)的试验方法ASTM D1582 负荷阶段10次通过      --
试验方法ASTM D892测定润滑剂起泡的趋势顺序I，ml顺序II，ml顺序III，ml 20ml50ml20ml
齿轮润滑剂相容性特征的FTM 3400试验方法 与MIL-L-2105D油是相容的
通用的齿轮润滑剂的储存溶解度特性的试验方法FTM 3430   分离的固体物质0.25％/质量，0.25％/最大体积
10ASTM建立的标准。
L-60-1碳漆膜和淤渣率的试验包括使用润滑油润滑在试验装置中彼此咬合的大齿轮和小齿轮。对大齿轮前面、大齿轮后面、小齿轮前面和小齿轮后面进行碳/漆膜测定和淤渣测定。碳/漆膜率是大齿轮前面和大齿轮后面的碳/漆膜测定的平均值。淤渣率是所有4个面的淤渣测定的平均值。
GL-5有表7所列的规格。
                    表7
         MIL-L-2105D(GL-5)润滑剂的性能规格(1987.8)
SAE粘度等级   75W   80W90   85W140
CRC L-60热氧化稳定性 100℃粘度增加@50小时，最大％戊烷不溶物，％甲苯不溶物，％ 10032 10032 10032
CRC L-33，7天湿分腐蚀 齿轮齿轴承上的锈，最大％盖板上的锈，最大％ 01 01 01
CRCL-37高速-低转矩高转矩-低速 “Green”齿轮“Lubrited”齿轮 通过通过 通过通过 NRNR
CRC L-42高速-冲击负载轴试验 环&小齿轮齿伤痕，最大％ 等于或好于RGO 110-90 等于或好于RGO110-90     NR
ASTM D-130铜片腐蚀 剥离率，最大 3 3 3
注：
NR-不需要，如果在相同的基料中80W90通过的话。
对于75W油需要较低的L-37和L-42试验温度。
本发明用下面的非限定性的实施例进一步加以说明。
实施例
使用下面的组分制备按照L-60-1碳/漆膜率和L-60-1淤渣率进行试验的组合物。这些L-60-1试验是ASTM的标准试验。该L-60-1方法包括在ASTMSpecial Technical Publication STP 512A，“Laboratory Performence TestIntended for API GL-5Service”中，该文献在此列出作为参考文献。
下面的表8-13列出了试验添加剂浓缩物的组成和试验结果。在本说明书中的所有实施例中，在添加剂浓缩物中组分的量按无油基料为基准以重量％表示。除非另有说明，基础油的类型也列在合适的表中。除非另有说明，在所有表中用“X”表示基础油的存在。
所用的基础油是矿物油A、矿物油B、矿物油C或矿物油D。矿物油A是80W90基础油，其是2种精制基础油料(Pennzoil 150 Bright and Pennzoil140 Neutral)与少量(低于2％(重))的所加的倾点抑制剂的混合物。矿物油B是85W140基础油，其是2种精制基础油料(Pennzoil 150 Bright and Pennzoil140 Neutral)与少量(低于2％(重))的所加的倾点抑制剂的混合物。在矿物油A和B中所用的倾点抑制剂是丙烯酸聚合物在严格精制的矿物油中的溶液。矿物油C是80W-90基础油，其是3种溶剂精制基础油料(ExxOn 150 Bright、Exxon 600 Neutral和Exxon 150 Neutral)与少量(低于2％(重))的所加的HiTEC672(乙基公司)倾点抑制剂的混合物。矿物油D是85W140基础油，其也是3种溶剂精制基础油料(ExxOn 150 Bright、Exxon 600 Neutral和Exxon 150Neutral)与少量(低于2％(重))的所加的HiTEC 672(乙基公司)倾点抑制剂的混合物。
除非另有说明，按基础油和浓缩物的总重量计，浓缩物一般的存在量为约7.50％。在本说明书的实施例的所有的表中，相同的数字脚注表示相同的组分或参数。
实施例1-6
表8的实施例1-6表示增加分散剂的影响和使用不同的分子量的分散剂的影响。在这些实施例中，浓缩物在85W-140矿物油B中的浓度是7％(重)。
                     表8
    实施例号     1     2     3     4     5     6
    SIB1  47.14  47.14  47.14  47.14  47.14  47.14
    C11-14胺2  4.34  4.34  4.34  4.34  4.34  4.34
    油酰胺3  2.14  2.14  2.14  2.14  2.14  2.14
    酸式磷酸戊酯4  6.36  6.36  6.36  6.36  6.36  6.36
    HiTEC43135  0.64  0.64  0.64  0.64  0.64  0.64
    消泡剂6  0.54  0.54  0.54  0.54  0.54  0.54
    破乳剂7  0.16  0.16  0.16  0.16  0.16  0.16
  未硼化的琥珀酰亚胺A8  21.43  18.75  16.07  21.43  18.75
  未硼化的琥珀酰亚胺B9  21.43
    加工油#510  17.25  19.92  22.60  17.25  17.25  19.92
    碳/漆膜率11  8.40  8.90  7.50  8.50  8.95  9.15
    淤渣率12  9.41  9.50  9.41  9.36  9.48  9.40
    ％粘度增加13  76.00  163.40  67.10  64.70  111.90  110.10
    戊烷不溶物14  1.82  4.69  1.89  2.00  3.50  3.24
    甲苯不溶物15  0.84  0.20  0.12  0.87  0.31  1.42
    TAN16  6.00  7.70  7.40  7.80  6.90  8.10
    ％铜损失(重)17  11.00  7.90  11.00  11.20  10.97  10.00
注：
1数均分子量约310的硫化聚异丁烯。
2C11-C14叔烷基伯胺混合物，与磷源(酸式磷酸戊酯)反应形成抗磨添加剂。
3胺，与磷源(酸式磷酸戊酯)反应形成抗磨添加剂。
4酸式磷酸戊酯(AAP)，与C11-C14胺和油酰胺反应形成盐。
5HiTEC 4313无灰烷基噻二唑，Ethyl Corporation，Richmond，Virginia的产品，用作铜腐蚀抑制剂。
6聚甲基丙烯酸烷基酯，用作消泡剂。
7重均分子量2000的环氧乙烷和环氧丙烷的嵌段共聚物，用作破乳剂。
8未硼化的1300 MW聚丁烯基琥珀酰亚胺，其是由马来酸酐酰化聚异丁烯和将该酰化的烃与聚亚乙基胺反应而生产的。
9未硼化的900 MW聚丁烯基琥珀酰亚胺，其是由马来酸酐酰化聚异丁烯和将该酰化的烃与聚亚乙基胺反应而生产的。
10100中性矿物油(在100°F大约100 SUS)。
11L-60-1碳/漆膜率。
12L-60-1淤渣率。
13L-60-1粘度增加。
14L-60-1戊烷不溶物。
15L-60-1甲苯不溶物。
16总酸值。
17通过与试验前和后在油中的铜比较而测定的铜重量损失的％。
实施例7-8
实施例7-8使用添加剂，添加剂在矿物油B，85W-140基础油中的总浓度是7.5％(重)，如表9所示，表明增加未硼化的琥珀酰亚胺A和聚异丁烯的效果。
                   表9
    实施例号     7     8
    SIB1     48.000     48.000
    C11-14胺2     3.7000     3.700
    油酰胺3     2.000     2.000
    酸式磷酸戊酯4     5.963     5.963
    破乳剂7     0.150     0.150
    HiTEC 43135     1.000     1.000
    消泡剂6     0.500     0.500
未硼化的琥珀酰亚胺A8     20.000     24.000
    加工油#510     18.687     14.687
    碳/漆膜率11     8.80     8.75
    淤渣率12     9.44     9.38
    ％粘度增加13     140.64     71.91
    戊烷不溶物14     3.64     3.43
    甲苯不溶物15     0.40     0.27
    ％铜损失重17     11.63     12.27
注：见表8
这些试验表明增加未硼化的琥珀酰亚胺A的量在L-60-1性能方面的结果。所有的碳/漆膜率都通过。2个试验的淤渣率都是可以接受的。
实施例9-14
表10和11的实施例9-14说明在各种基础油中总添加剂浓度在7.5％(重)的本发明的效果。
                          表10
    实施例号     9     10     11     12
    SIB1  47.000  47.000  47.000  47.000
    C11-14胺2  4.050  4.050  4.050  4.050
    油酰胺3  2.000  2.000  2.000  2.000
    酸式磷酸戊酯4  5.936  5.936  5.936  5.936
    HiTEC 43135  0.600  0.600  0.600  0.600
    消泡剂6  0.500  0.500  0.500  0.500
    破乳剂7  0.150  0.150  0.150  0.150
  未硼化的琥珀酰亚胺A8  17.500  17.500  17.500  17.500
    加工油18  19.264  19.264  19.264  19.264
    加工油#510  3.000  3.000  3.000  3.000
    80W-90矿物油A     X     X
    85W-140矿物油B     X     X
    碳/漆膜率11  8.91  8.40  8.45  8.90
    淤渣率12  9.43  9.46  9.40  9.47
    ％粘度增加13  66.05  59.71  94.86  96.19
    戊烷不溶物14  3.22  2.33  3.53  2.28
    甲苯不溶物15  2.90  2.01  1.03  0.69
    TAN16  10.20  6.80  9.50  7.10
    ％铜损失重17  9.38  11.34  9.08  9.91
注：见表8
18用作稀释剂的加氢处理的45中性矿物油。
                    表11
    实施例号     13     14
    SIB1     47.000     47.000
    C11-14胺2     4.050     4.050
    油酰胺3     2.000     2.000
    酸式磷酸戊酯4     5.936     5.936
    HiTEC 43135     0.600     0.600
    消泡剂6     0.500     0.500
    破乳剂7     0.150     0.150
    未硼化的琥珀酰亚胺A8     17.500     17.500
    加工油18     19.264     19.264
    加工油#510     3.000     3.000
    80W-90矿物油C     X
    85W-140矿物油D     X
    碳/漆膜率11     8.75     8.80
    淤渣率12     9.47     9.44
    ％粘度增加13     46.27     47.50
    戊烷不溶物14     0.36     0.12
    甲苯不溶物15     0.31     0.13
    TAN16     9.60     6.00
    ％铜损失重17     12.40     11.27
表10和11中的数据说明当该添加剂搀混在几种基础原料中，通过了(用MIL-PRF-2105E和MT-1标准)使用未硼化的琥珀酰亚胺A的清净齿轮润滑油添加剂的L-60-1淤渣和碳/漆膜性能和粘度等级。
实施例15-16
表12中的实施例15-16使用用7.5％(重)的添加剂处理的油。
                     表12
    实施例号     15     16
    H-31321     40.000     40.000
    C11-14胺2     4.850     4.850
    油酰胺3     2.000     2.000
    AAP4     7.000     7.000
    辛酸     0.300     0.300
    HiTEC 43135     0.800     0.800
    消泡剂6     0.500     0.500
  未硼化的琥珀酰亚胺A8     10.000     20.000
  硼化的琥珀酰亚胺22     10.000
    加工油#510     24.550     24.550
    80W-90矿物油C     X     X
    ％粘度增加13     42.77     57.71
    戊烷不溶物14     0.19     0.17
    甲苯不溶物15     0.09     0.06
    TAN16     4.62     4.87
    碳/漆膜率11     8.80     8.70
    淤渣率12     9.56     9.50
    ％铜损失重17     9.60     9.65
    油损失重(gm)22     11.60     18.70
注：见表11。
20在该实施例的试验开始(约120ml)和结束时油的重量之差。
21TiTEC 313极压添加剂，可以从Ethyl Corporation，Richmond，Virgina买到，其是数均分子量大于约310的磺化的聚异丁烯。
22TiTEC 637性能添加剂，其是含有硼和其它组分的分散剂，由EthylCorporation，Richmond，Virgina制造。
表12的数据表明未硼化的分散剂和硼化的和未硼化的分散剂的混合物都有很好的碳/漆膜和淤渣性能。
实施例17-18
表13的数据表明对于包括未硼化的分散剂浓缩物在加入一定重量％的水的存在下有更好的稳定性。
                     表13
    实施例号     17     18
    SIB1     40.000     40.000
    C11-14胺2     4.850     4.850
    油酰胺3     2.-000     2.000
    AAP4     7.000     7.000
    未硼化的琥珀酰亚胺A8     20.000
    硼化的琥珀酰亚胺23     20.00
    加工油#510   26.150   26.150
浓缩物加1％重的蒸馏水的目测外观     清净     混浊
注：见表12
23硼化的1300 MW聚丁烯基琥珀酰亚胺，其是由马来酸酐酰化聚异丁烯和将该酰化的烃与聚亚乙基胺反应而生产的。该生成的琥珀酰亚胺与硼酸反应得到硼化的琥珀酰亚胺。
36天后，实施例17的产物仍是清净的，而实施例18的产物有很多沉淀。
很明显，上述的实施方案可以进行很多的改变，而仍在本发明的实质和范围内。因此，本发明不限于上述的实施方案，而由后面所附的权利要求来定义本发明。

Claims (25)

1.一种清净齿轮的无硼润滑油添加剂浓缩物，其包括：
一种无硼无灰分散剂，其选自烃基取代的琥珀酰亚胺、烃基取代的琥珀酸和烃基取代的琥珀酰胺中的至少一种；
不存在其中单个氮原子键合到H和2个羰基上的琥珀酰亚胺化合物；
选自硫化的聚异丁烯和多硫化物中的至少一种的硫源；和
选自式IV的油溶胺盐中的至少一种的磷源：
其中R6是有4-10个碳原子的烃基，每一个X单独是S或O，Y是+NH3R7或H，其中R7是有8-22个碳原子的烃基，Z是+NH3R8或H，其中R8是有8-22个碳原子的烃基；
其中选择分散剂、硫源和磷源的比例，使得当无灰分散剂、硫源和磷源的总重量是润滑油重的约1-10％时，含有齿轮油基料、分散剂、硫源和磷源的润滑油的L-60-1碳/漆膜率至少约7.5和L-60-1淤渣率至少约9.4。
2.根据权利要求1的添加剂浓缩物，其中无硼无灰分散剂选自式IIa和IIb所表示的化合物： 其中R是聚亚烷基部分，
R1是有1-40个碳原子的烷基，
R2是有1-40个碳原子的烷基，
R3选自H和有1-40个碳原子的烷基，
R4选自H和有1-40个碳原子的烷基，和
X是整数0-12。
3.根据权利要求1的添加剂浓缩物，其中该油的L-60-1碳/漆膜率是约7.5-10。
4.根据权利要求1的添加剂浓缩物，其中该油的L-60-1的淤渣率是约9.4-10。
5.根据权利要求2的添加剂浓缩物，其中R1是有1-10个碳原子的烷基，Ru是有1-10个碳原子的烷基，R3选自H和有1-10个碳原子的烷基，R4选自H和有1-10个碳原子的烷基，和X是整数2.8。
6.根据权利要求2的添加剂浓缩物，其中R是数均分子量约为750-2500的聚异丁烯部分。
7.根据权利要求2的添加剂浓缩物，其中
R1是(CH2)n，其中n是整数1-5，
R2是(CH2)m，其中m是整数1-5，
X是2-5，
R3是H或有1-5个碳原子的烷基，和
R4是H或有1-5个碳原子的烷基。
8.根据权利要求2的添加剂浓缩物，其中硫源是硫化聚异丁烯。
9.根据权利要求2的添加剂浓缩物，其中R是具有至少一种每单烯有2-30个碳原子的单烯的聚合物。
10.根据权利要求2的添加剂浓缩物，其中R是具有至少一种每单烯有2-8个碳原子的单烯的聚合物。
11.根据权利要求1的添加剂浓缩物，其中磷源有下面的结构式：
Figure A9712084400031
其中R6、X、Y和Z的定义同式子IV。
12.根据权利要求2的添加剂浓缩物，其中磷组分包括下面结构式VII和VIII二者的化合物的混合物：其中R17是有2-12个碳原子的烃基和R18单独是有4-30个碳原子的烃基。
13.根据权利要求12的添加剂浓缩物，其中结构式VII的化合物和结构式VIII的化合物的重量比是80∶20-20∶80。
14.根据权利要求12的添加剂浓缩物，其中R17是有约4-10个碳原子的烃基。
15.根据权利要求1的添加剂浓缩物，其中还含有消泡剂、破乳剂、硫脱除剂和抗氧化剂中的至少一种。
16.一种能够清净齿轮的润滑油，其包括
基料油；和
权利要求1的添加剂浓缩物。
17.根据权利要求16的润滑油，其中无硼无灰分散剂选自结构式IIa和IIb的化合物：
Figure A9712084400042
其中R是聚亚烷基部分，
R1是有1-40个碳原子的烷基，
R2是有1-40个碳原子的烷基，
R3选自H和有1-40个碳原子的烷基，
R4选自H和有1-40个碳原子的烷基，和
X是整数0-12。
18.根据权利要求16的润滑油，其中无灰分散剂、硫源和磷源总重是润滑油的约1-10％(重)。
19.根据权利要求17的润滑油，其中
R1是有1-10个碳原子的烷基，R2是有1-10个碳原子的烷基，R3选自H和有1-10个碳原子的烷基，R4选自H和有1-10个碳原子的烷基，和
X是整数2-8。
20.根据权利要求17的润滑油，其中R是数均分子量约为750-2500的聚异丁烯部分。
21.根据权利要求19的润滑油，其中该润滑油含有约0.26-3.0％(重)的无灰分散剂、约1-5.25％(重)的硫源和约0.1-3％(重)的磷源。
22.根据权利要求18的润滑油，其中磷组分包括下面的结构式VII和VIII二者的化合物的混合物：
Figure A9712084400051
其中R17是有4-10个碳原子的烃基和R18单独是有8-22个碳原子的烃基。
23.一种权利要求16的润滑油的制造方法，包括把基料油和添加剂浓缩物混合。
24.一种使用权利要求16的润滑油的方法，包括用该润滑油润滑机动车辆手动传动机构。
25.一种使用权利要求16的润滑油的方法，包括用该润滑油润滑机动车辆的后轴。
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CN114402058A (zh) * 2019-08-16 2022-04-26 路博润公司 用于润滑汽车齿轮、车轴和轴承的组合物和方法

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CN102268317B (zh) * 2002-06-28 2013-09-18 新日本石油株式会社 润滑油添加剂,包含这种添加剂的润滑油组合物,以及这种添加剂和组合物的生产方法
CN104334698A (zh) * 2012-04-04 2015-02-04 卢布里佐尔公司 用于粉碎设备的轴承润滑剂
CN114402058A (zh) * 2019-08-16 2022-04-26 路博润公司 用于润滑汽车齿轮、车轴和轴承的组合物和方法
CN114402058B (zh) * 2019-08-16 2023-06-23 路博润公司 用于润滑汽车齿轮、车轴和轴承的组合物和方法

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EP0848052A2 (en) 1998-06-17
SG53133A1 (en) 1998-09-28
AU725264B2 (en) 2000-10-12
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JP3332836B2 (ja) 2002-10-07
US5763372A (en) 1998-06-09
EP0848052A3 (en) 1998-06-24
JPH10176179A (ja) 1998-06-30
CN1075109C (zh) 2001-11-21
AU4684797A (en) 1998-06-18

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