CN1216134C - 显示持久氧化稳定性的润滑剂组合物 - Google Patents

显示持久氧化稳定性的润滑剂组合物 Download PDF

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CN1216134C
CN1216134C CN991228529A CN99122852A CN1216134C CN 1216134 C CN1216134 C CN 1216134C CN 991228529 A CN991228529 A CN 991228529A CN 99122852 A CN99122852 A CN 99122852A CN 1216134 C CN1216134 C CN 1216134C
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oxidation inhibitor
base oil
oil
application
additive
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CN1255533A (zh
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H·T·赖安
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Afton Chemical Ltd
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Abstract

在包含液压抗磨耗组分与基油的润滑剂组合物中应用一种包含至少为一种的胺抗氧剂与至少为一种的选自无灰的二硫代甲氨酸酯、硫化烯烃和酚抗氧剂的另外抗氧剂的添加剂，以提供具有改进的热稳定性与氧化稳定性的润滑剂。

Description

显示持久氧化稳定性的润滑剂组合物
本发明涉及使用某些添加剂来延长润滑剂组合物的热稳定性与氧化稳定性，并涉及显示持久的热稳定性与氧化稳定性的润滑剂组合物。
适于抗磨的液压与工业应用的润滑剂组合物通常含有赋予其抗磨耗性的添加剂组分。就此而言通常使用液压级二烷基二硫代磷酸锌。该组合物常常还含有抗氧剂组分。该组合物按惯例是使用组I基油配制的。然而，使用加氢裂解和催化脱蜡的组II与组III基油的趋势正在增加。氢化与脱蜡过程涉及形成格外低的芳香性与硫含量。当与组I基油相比较时，现已发现组II与组III基油显示改进的抗氧剂组分效应。这已导致考虑使用组II与组III基油有可能减少所用的抗氧剂量，而不会损害最终使用者所要求的抗氧剂性能。然而，不是导致减少所用抗氧剂的量而是组II与组III基油的出现促使最终使用者提出对更高性能抗氧剂的需求，而不管事实上所用的基油之种类如何。例如，尽管ASTM D943热氧化试验的性能级为2000～4000小时在先前被认为是可以接受的，但是目前通常要求更持久的性能，例如在ASTM D943热氧化试验中为10000小时。
根据本发明现已发现，能将特定的抗氧剂组分及其组合掺入到含液压抗磨组分的润滑剂组合物中，以便在不会形成残渣的前提下达到持久的热与氧化稳定性。更具体地说。现已发现能获得具有改进的热稳定性的组合，并由此而导致在使用组I、II和III的基油时减少残渣的量和增加基油II或更高基油中的氧化稳定性。由此使有可能在配制润滑剂组合物时使用各种基油，从而使工业配方师获得更大的灵活性，同时还符合最终使用者当前的持久性要求。
因此，本发明提供在包含液压抗磨耗组分与基油的润滑剂组合物中使用一种包含至少为一种的胺抗氧剂与至少为另一种的选自无灰的二硫代甲氨酸酯、硫化烯烃和酚抗氧剂的另外添加剂以提供在所有类型基油中具有改进的热稳定性与氧化稳定性的润滑剂。
本发明中所用的抗氧剂组合的性能将随着，其中包括基油类型、所用添加剂的特定组合与浓度的变化而变化。由于本发明中所用添加剂之热稳定性，使有可能在使用组I基油的情况下配制出根据NOC试验测定能够在10天后避免形成过多残渣的润滑剂。在优选实施方案中，在该试验中10天后所产生的残渣量为不高于100毫克/100毫升，优选为不高于25毫克/100毫升。10天残渣量为10毫克/100毫升特别被优选。由于本发明中所用添加剂之氧化稳定性，通常使有可能在使用组II基油或更高基油的情况下配制出根据RBOT热稳定性试验测定结果至少为500分钟、优选至少为600分钟的润滑剂。于是，本发明涉及能在基油II或更高基油中使用而达到良好的氧化性能，同时在使用基油I或更高基油时不会损害热稳定性的抗氧剂组合，反之亦然。
本发明中所用的胺选自任选的烷基化的二苯胺、苯基-萘基胺及其混合物。在本发明中可被使用的这样组分之例子包括，但并不限于，二苯胺、苯基-α-萘基胺、苯基-β-萘基胺、丁基二苯胺、二丁基二苯胺、辛基二苯胺、二辛基二苯胺、壬基二苯胺、二壬基二苯胺、二辛基二苯胺、壬基二苯胺、二壬基二苯胺、庚基二苯胺、二庚基二苯胺、甲基苯乙烯基二苯胺、混合的丁基/辛基烷基化二苯胺、混合的丁基/苯乙烯基烷基化二苯胺、混合的壬基/乙基烷基化二苯胺、混合的辛基/苯乙烯基烷基化二苯胺、混合的乙基/甲基苯乙烯基烷基化二苯胺、辛基烷基化苯基-α-萘基胺、和混合的烷基化苯基-α-萘基胺。还可以使用2，6-二叔丁基-α-二甲基氨基对甲苯酚。
有用的胺抗氧剂一般特征为其氮含量和如ASTM D2896测定的TBN。最好的是，胺抗氧剂的氮含量为3.0～7.0wt％和TBN为100～250毫克KOH/克纯，即，未搀杂的组分。
在成品组合物中胺抗氧剂的浓度随所用的基油、消费者之要求与用途不同而变化。一般说，在成品组合物中胺抗氧剂的总量为0.04wt％～0.4wt％、优选为0.05wt％～0.2wt％。
本发明的含硫化合物选自硫化烯烃、硫化脂肪酸、无灰的二硫代甲氨酸酯、二硫化四烷基秋兰姆及其盐。适用于本发明的硫化烯烃可通过许多已知方法来制备。它们一般以其生产中所使用的烯烃类型与其最终的硫含量来表征。高分子量烯烃(例如那些具有重均分子量(Mn)为约112～约351克/摩尔)被优选。可被使用的烯烃之例子包括α-烯烃、异构α-烯烃、支化α-烯烃、环状α-烯烃、聚合烯烃和它们的混合物。可被使用的α-烯烃之例子包括1-丁烯、1-戊烯、1-己烯、1-庚烯、1-辛烯、1-壬烯、1-癸烯、1-十一碳烯、1-十二碳烯、1-十三碳烯、1-十四碳烯、1-十五碳烯、1-十六碳烯、1-十七碳烯、1-十八碳烯、1-十九碳烯、1-二十碳烯、1-二十一碳烯、1-二十二碳烯、1-二十三碳烯、1-二十四碳烯、1-二十五碳烯和它们的混合物。在硫化反应前或硫化反应期间α-烯烃可被异构化。还可以使用含有内双键或支化的α-烯烃的结构异构体和/或构象异构体。例如，异丁烯是α-烯烃1-丁烯的支化烯烃配对物可被用于硫化反应的硫源能够包括，例如，元素硫、一氯化硫、二氯化硫、硫化钠、多硫化钠、和被加在一起的或处于硫化过程不同阶段的它们的混合物。
不饱和的脂肪酸和油，由于其不饱和之故，也可被硫化与用于此发明中。可被使用的脂肪酸的例子包括月桂烯酸、肉豆蔻脑酸、棕榈油酸、油酸、反油酸、11-十八碳烯酸、亚油酸、亚麻酸、顺9-二十碳烯酸、花生四烯酸、芥酸、以及它们的混合物。可被使用的油或脂的例子包括玉米油、棉子油、葡萄子油、橄榄油、棕榈油、花生油、菜子油、红花油、芝麻子油、豆油、葵花油、葵花子油、以及它们的混合物。
可被使用的无灰的二硫代甲氨酸酯之例子包括，但并不限于，亚甲基-双(二烷基二硫代甲氨酸酯)、亚乙基-双(二烷基二硫代甲氨酸酯)、和二硫化异丁基-2，2′-双(二烷基二硫代甲氨酸酯)，此处二烷基二硫代甲氨酸酯的烷基能优选具有1～16个碳原子。优选的无灰的二烷基二硫代甲氨酸酯之例子为亚甲基-双(二丁基二硫代甲氨酸酯)、亚乙基-双(二丁基二硫代甲氨酸酯)、和二硫化异丁基-2，2′-双(二丁基二硫代甲氨酸酯)。可被使用的优选的二硫化四烷基秋兰姆之例子包括二硫化四丁基秋兰姆和二硫化四辛基秋兰姆。
在成品组合物中含硫化合物之浓度能随消费者的需要与用途的不同而变化。该化合物通常，以润滑剂组合物的总重量为基准计，以高达0.1wt％、优选以高达0.05wt％的量被使用的。选择该化合物浓度的一条重要准则是硫含量。该化合物通常应向成品组合物供给0.005wt％～0.07wt％的硫。例如，具有12wt％硫含量的硫化烯烃的被使用量应为0.04wt％～0.58wt％以便向成品组合物供给0.005wt％～0.07wt％的硫。具有30wt％硫含量的无灰的二硫代甲氨酸酯的被使用量应为0.02wt％～0.23wt％，以便向成品组合物供给0.005wt％～0.07wt％的硫。
选择含硫化合物的另一条有用准则是根据ASTM D1662确定的活性硫含量。高活性硫量的存在能导致成品组合物的严重腐蚀性与残渣问题。在本发明的优选的实施方案中，化合物中的活性硫含量根据ASTM D1662测定为低于1.5wt％。
可在本发明中使用的硫化烯烃的例子是含有约12wt％的总硫含量和小于1wt％的活性硫的硫化烯烃。可在本发明中使用的、商业上可得到的硫化脂肪油或硫化脂肪油与烯烃的混合物之例子包括含有约9.5wt％的硫含量和1wt％的活性硫、约12.5wt％的硫含量和1.5wt％的活性硫、和约10wt％的硫含量和小于1wt％的活性硫的那些。可在本发明中使用的无灰的二硫代甲氨酸酯的例子，从含硫化合物应含有最小为8.0wt％的硫以便将供给所需量硫所必不可少的添加剂之量缩减到最小的实用的观点考虑，为一种含有约30wt％硫的无灰的二硫代甲氨酸酯。
还可以使用各种比例的硫化烯烃、无灰的二硫代甲氨酸酯和二硫化四烷基秋兰姆的混合物，只要能满足希望的总硫含量与活性硫含量都行。
可被使用的酚抗氧剂之例子包括位阻酚例如2，6-二叔丁基苯酚、4-甲基-2，6-二叔丁基苯酚、2，4，6-三丁基苯酚、2-叔丁基苯酚、2，6-二异丙基苯酚、2-甲基-6-叔丁基苯酚、2，4-二甲基-6-叔丁基苯酚、4-(N，N-二甲基氨基甲基)-2，6-二叔丁基苯酚、4-乙基-2，6-二叔丁基苯酚、2-甲基-6-苯乙烯基苯酚、2，6-二苯乙烯基-壬基苯酚和它们的混合物。还有用的是亚甲桥的烷基苯酚并且它们可以单独或彼此相结合或与空间位阻的非桥酚一起使用。其例子包括4，4′-亚甲基-双(2，6-二叔丁基苯酚)、4，4′-亚甲基-双(6-叔丁基邻甲酚)、4，4′-亚甲基-双(2-叔戊基邻甲酚)、2，2′-亚甲基-双(4-甲基-6-叔丁基苯酚)、亚甲桥的叔丁基苯酚混合物、异辛基-3，5-二丁基-4-羟基氢化肉桂酸酯和硫二亚乙基-双(3，5-二丁基-4-羟基)氢化肉桂酸酯。还有用的是例如USP3211652中所述的亚甲桥的烷基苯酚的混合物。一般说，酚抗氧剂在成品润滑剂中的含量为高达0.4wt％、优选为高达0.15wt％。
本发明还提供如此处所述的润滑剂组合物，该组合物包括液压抗磨耗组分、基油、至少为一种的胺抗氧剂和至少为一种的另外抗氧剂。
本发明中有用的抗氧剂是可商购到的或可通过应用已知方法来制备。
通常，用于本发明组合物中的液压抗磨耗添加剂是液压级二烷基二硫代磷酸锌(ZDDP)。“液压级”意指该抗磨耗组分是适于在液压应用领域中使用的，特别是就其热稳定性而言。ZDDP类具有不充分的热稳定性而易于快速降解，从而破坏产品引起腐蚀性、特别是对铜。对作为由铜制成的某些液压系统的组件来说，这是个严重问题。此外，被破坏的产品能引起形成残渣，从而会堵塞过滤器。于是，并不是所有的ZDDP类均适用于本发明的。可被用于本发明的二烃基二硫代磷酸锌是在本技术领域中众所周知的(参见例如美国专利№4101429)。合适的二烃基二硫代磷酸锌是通常含有约4～约12个碳原子的二烷基二硫代磷酸锌，更常用的是每个烷基中含约6～约12个碳原子。优选为每个烷基中含约8～约12个碳原子。适用的烷基部分包括丁基、仲丁基、异丁基、叔丁基、戊基、正己基、仲己基、正辛基、2-乙基已基、癸基和十二烷基。每一烷基部分优选为2-乙基己基。此类二烷基二硫代磷酸锌被介绍于欧洲专利申请№ 95306722.0中并且是可商购到的。
ZDDP可以以广范围的重量比而被用于润滑剂中。然而，润滑剂通常含有约0.4～约0.9wt％的ZDDP。最好，润滑剂流体包含0.6wt％的ZDDP。
在本发明中有用的那些ZDDP通常能够根据其高碱性物与中性物的比率或根据其可滴定的碱值(TBN)来表征。有用的ZDDP类一般显示高碱性物与中性物的比率为0.3∶1～2∶1，优选为0.5∶1～2∶1。具有高碱性物与中性物的比率约为1∶1的ZDDP类是被更常用的。所讨论的比例是通过31Pnmr测定的。就TBN而言，有用的ZDDP一般显示约为10毫克KOH/克的最小值，且优选为约12毫克KOH/克。具有TBN约为15毫克KOH/克的ZDDP被更常用。TBN是根据ASTM D664测定的。
另外，通常还可以参考其中包含ZDDP的成品液压流体的热稳定性来表征ZDDP。此处所依据的参考数据是根据ASTM D2619和CCM“A”热稳定性试验得到的。为了符合ASTM D2619试验的要求，成品流体应达到最大的铜损失为0.2毫克。为了通过CCM“A”试验，成品流体应达到最大的铜棒级别为5和最大的残渣沉积为25毫克/100毫升。ASTMD2619和CCM“A”试验是本技术领域中所公知的。
有可能通过使用链烷酸锌对ZDDP组分进行后处理来进一步提高润滑剂组合物的热稳定性。链烷酸盐通常在其B-碳原子上被支化。这样的组分还被介绍于欧洲专利申请№95306722.0中。使用辛酸锌被优选，特别是使用高碱性的辛酸锌例如辛酸锌22％(可以以此标号从市场购到)。
在本发明的一个实施方案中胺抗氧剂是苯基-α-萘胺或2，6-二叔丁基-α-二甲基氨基对甲酚、它们的本身或各自与二苯基胺的混合物。基于苯基-α-萘胺和二苯基胺的混合物被优选。
优选的抗氧剂组合包括：苯基-α-萘胺、二苯基胺和无灰的二硫代甲氨酸酯，例如亚甲基-双(二丁基二硫代甲氨酸酯)；苯基-α-萘胺、二苯基胺和酚抗氧剂，例如2，6-二叔丁基苯酚；和苯基-α-萘胺、二苯基胺和硫化烯烃，例如由C16-18异构α-烯烃衍生的硫化烯烃。在这些组合中，苯基-α-萘胺可被2，6-二叔丁基-α-二甲基氨基对甲酚所取代。
被打算用于本发明中的润滑油包括天然润滑油、合成润滑油和它们的混合物。适用的润滑油还包括通过合成蜡与含油蜡的异构化而得到的基油，以及通过加氢裂化(而不是溶剂提取)原油的芳族与极性组分而生产的基油。一般说，天然与合成润滑油两者的每一种具有运动粘度范围在100℃为约1×106m2/s～约40×10-6m2/s(约1～约40cSt)，虽然一般应用仅要求每种油具有粘度范围在100℃为约2×10-6m2/s～约8×10-6m2/s(约2～约8cSt)。
天然基油包括动物油、植物油(例如，蓖麻油和猪油)、石油油料、矿物油、以及由煤或页岩衍生的油。优选的天然基油是矿物油。
在本发明中有用的矿物油包括所有普通的矿物油基原料。这将包括化学结构为环烷或链烷的油。它们是通过使用酸、碱、粘土或其他试剂例如氯化铝的惯用工艺进行提纯的提纯油，或者可以是，例如通过用溶剂如苯酚、二氧化硫、糠醛、二氯代二乙基醚等等而生产的提取油。它们可以是被加氢处理的或被加氢精制的、或通过冷却或催化脱蜡法而被脱蜡的、或被加氢裂化的。矿物油可以是由天然原油资源生产的，或者是由异构化的蜡原料或其他精制法的残余物组成的。
矿物油一般具有100℃的运动粘度为2×10-6m2/s～12×10-6m2/s(2～12cSt)。优选的矿物油具有100℃的运动粘度为3×10-6m2/s～10×10-6m2/s(3～10cSt)，而最优选的是那些具有100℃粘度为5×10-6m2/s～9×10-6m2/s(5～9cSt)的矿物油。
在本发明中有用的合成润滑油包括烃油和卤取代的烃油诸如低聚的、聚合的、和共聚的烯烃[例如，聚丁烯，聚丙烯，丙烯，异丁烯共聚物，氯化polylactenes，聚(1-已烯)，聚(1-辛烯)，以及它们的混合物]；烷基苯[例如，聚亚丁烯，聚亚丙烯，亚丙烯，异亚丁烯共聚物，氯化polylactenes，聚(1-己烯)，聚(1-辛烯)，以及它们的混合物]；烷基苯[例如，十二碳基苯，十四碳基苯，二壬基苯和二(2-乙基己基苯)]；聚苯[例如，联苯，三联苯，烷基化聚苯]；和烷基化二苯醚，烷基化二苯硫，以及它们的衍生物、类似物，及其同系物等等。优选的合成油是α-烯烃的低聚物，特别是1-癸烯的低聚物，也被称为聚α-烯烃或PAO类。
合成润滑油还包括烯化氧聚合物、共聚体、共聚物、及其端羟基已通过酯化或醚化而被改性的衍生物。此类合成油的例子是：通过环氧乙烷或环氧丙烷的聚合而制备的聚氧化烯聚合物；这些聚氧化烯聚合物的烷基和芳基醚(例如，具有平均分子量为1000的甲基-聚异丙二醇醚，具有平均分子量为100～1500的聚丙二醇二苯基醚)；及其单-和聚-羧酸酯(例如，乙酸酯，混合的C3～C8脂肪酸酯，四乙二醇的C12含氧酸二酯)。
另一类适用的合成润滑油包括二羧酸(例如，苯二甲酸，琥珀酸，烷基琥珀酸和链烯基琥珀酸，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，烷基丙二酸和链烯基丙二酸)与各种醇(例如，丁醇，己醇，癸醇，2-乙基己醇，乙二醇，二乙二醇单醚和丙二醇)的酯。这些酯的具体例子包括己二酸二丁酯，癸二酸二(2-乙基己基)酯，富马酸二(正己基)酯，癸二酸二辛酯，壬二酸二异辛酯，壬二酸二异癸酯，间苯二甲酸二辛酯，苯二甲酸二癸酯，癸二酸二十烷基酯，亚油酸二聚物的2-乙基己二酯，以及通过一摩尔癸二酸与二摩尔四乙二醇和二摩尔2-乙基己酸反应而形成的混合酯。此类合成油中的一类优选的油是C4～C12醇的己二酸酯。
作为合成润滑油的有用的酯还包括那些由C5～C12单羧酸和多元醇和多羟基化合物醚例如新戊二醇、三羟甲基丙烷季戊四醇、二季戊四醇和三季戊四醇制成的酯。
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)包括另一类有用的合成润滑油。这些油包括四乙基硅酸酯、四异丙基硅酸酯、四(2-乙基己基)硅酸酯、四(4-甲基-2-乙基己基)硅酸酯、四(4-对叔丁基苯基)硅酸酯、六(4-甲基-2-五氧基)二硅氧烷、聚(二甲基)-硅氧烷和聚(甲基苯基)-硅氧烷。其他的合成润滑油包括含硫酸的液态酯(例如，磷酸三羟甲苯酯，磷酸三辛酯，和癸基磷酸的二乙基酯)，聚合的四氢呋喃和聚-α-烯烃。
润滑基油可由精制的、再精制的油，或它们的混合物衍生。未精制油是在未进一步提纯或处理的情况下直接从天然来源或合成来源(例如，煤、页岩、或焦油砂沥青)得到的。未精制油的例子包括直接从干馏操作中得到的页岩油、直接从蒸馏操作中得到的石油油料、或直接从酯化操作中得到的酯油，然后在未经进一步处理的情况下使用它们中的每一种。精制油与未精制油相似，但它们已经过一种或多种的提纯步骤处理，以改进一种或多种性能。适用的提纯工艺包括蒸馏、加氢处理、脱蜡、溶剂提取、酸或碱提取、过滤、以及渗滤，所有的这些工艺是本技术领域熟练人员所熟知的。再精制油是通过类似于生产精制油所使用的方法处理使用过的油而得到的。再精制油也被称为再生油或后处理过的油，并且通常通过除去废添加剂和油废品的工艺进行另外的加工。如美国专利№ 5736490中所说的白油也可被用作基油，特别是汽轮机方面应用的基油。
在本发明的实施方案中，基油是组I、组II或组III基油。优选使用组II或组III基油。
美国石油协会已将这些不同类型的基油作如下的分类：基油I为＞0.03wt％硫，和/或∠90vol％饱和物(saturate)，粘度指数为80～120；基油II为≤0.03wt％硫，和≥90vol％饱和物，粘度指数为80～120；基油III为≤0.03wt％硫，和≥90vol％饱和物，粘度指数＞120；基油IV为全部聚α-烯烃。加氢处理的基油和催化脱蜡的基油，由于它们的低硫和芳香化合物含量之故，通常属于组II与组III类。聚α-烯烃(组IV基油)是由各种α-烯烃制备的合成基油，并且基本上不合硫与芳香化合物。
本发明的润滑剂组合物可以通过简单地掺合各种组分与合适的基油来制备。
为了方便起见，在本发明的另一种实施方案中，实施本发明所用的添加剂组分可以作为浓缩物被配制到准备使用的润滑剂组合物中。
除了流体组分外，浓缩物可以包括流体组分用的溶剂或稀释剂。溶剂或稀释剂应与添加浓缩物的基油相溶混的或能溶于基油中的。合适的溶剂或稀释剂是人们所熟知的。溶剂或稀释剂可以是润滑油组合物本身的基油。浓缩物可以适当地包括用于润滑油组合物中的任何添加剂。在浓缩物中每种组分的比例是根据预期的稀释度来控制的，虽然配制流体的顶级处理(top treatment)也是可能的。
常用于汽轮机、抗磨耗的液压与工业应用的润滑剂/流体中的其他添加剂可以被包括在本发明的组合物或浓缩物中。它们包括破乳剂、腐蚀抑止剂、分散剂、含硫或磷的抗磨剂和防锈剂。当这些添加剂存在时，其用量为在这样应用中的惯用量。某些添加剂可被包括在浓缩物中或者某些添加剂是在顶级处理时被添加到充分配制的润滑剂/流体中的。
现通过下列的实施例对本发明进行说明，但这些实施例并不是被用来对本发明的范围作任何限制的。
实施例
通过按下表中规定比例掺合各组分制备润滑剂组合物。
    组分     wt％
    腐蚀抑止剂     0.0085
    洗涤剂     0.050
    防锈剂     0.051
    酚抗氧剂     0.013
    破乳剂     0.0064
    加工油     0.0111
    *ZDDP     0.510
    基油     加至100％
ZDDP代表二(2-乙基己基)二硫代磷酸锌。
所使用的基油既可以是基油I也可以是基油II。有关些方面的更详细的资料见下表。
按下表中所列的浓度中向此润滑剂组合物掺入各种另外组分。然后对所得的润滑剂组合物进行CCM“A”、NOC和RBOT测试。其结果也被示于下表中。
                                               实            施           例
  组分(wt％)   1     2    3    4    5    6    7   8     9   10   11   12
  二苯胺   -     0.1    0.1    -    -    0.1    0.1   0.1   0.1   0.1   0.1   0.1
  苯基-α-萘胺   -     -    -    0.1    0.1    0.1    0.1   0.1   0.1   0.1   0.1   0.1
  硫化酚   -     -    -    -    -    -    -   0.1   0.1   0.05   0.05   0.1
  2，6-二叔丁基苯酚   -     -    -    -    -    -    -   -   -   -   -   -
  硫化烯烃   -     -    -    -    -    -    -   -   -   -   -   -
  无灰的二硫代甲氨酸酯   -     -    -    -    -    -    -   -   -   -   -   -
  基油类型   I     I    II    I    II    I    II   I   II   I   II   I
  CCM“A”铜棒等级   I     I    I    I    I    I    I   I   I   I   I   I
  10天后NOC残渣(毫克)   BF     4.4    2.0    313    2.8    BF    3.6   BF   12.1   BF   3.6   BF
  RBOT(分钟)   274     287    336    340    465    365    570   390   629   375   508   335
BF-堵塞过滤器
                                                      实    施    例
    组分(wt％)    13    14     15     16     17     18     19     20     21     22     23
    二苯胺    0.1    0.1     0.1     0.1     0.1     0.1     0.1     0.1     0.1     0.1     0.1
    苯基-α-萘胺    0.1    0.1     0.1     0.1     0.1     0.1     0.1     0.1     0.1     0.1     0.1
    硫化酚    0.1    0.05     0.05     -     -     -     -     -     -     -     -
    2，6-二叔丁基苯酚    -    -     -     -     -     -     -     0.1     0.1     -     -
    硫化烯烃    -    -     -     -     -     -     -     -     -     0.05     0.05
    无灰的二硫代甲氨酸酯    -    -     -     0.05     0.05     0.025     0.025     -     -     -     -
    基油类型    II    I     II     I     II     I     II     I     II     I     II
    CCM“A”铜棒等级    I    I     I     I     I     I     I     I     I     2     I
    10天后NOC残渣(毫克)    2.2    BF     4.7     82.4     14.3     93.4     6.7     4.0     4.3     48.2     16.0
    RBOT(分钟)    538    350     616     373     661     378     600     391     525     378     677
注解
组I基油是Texaco ISO 46。组II基油是RLOP ISO 46。在实施例8～11中硫化酚化合物是硫代亚乙烯-双(3，5-二叔丁基-4-羟基氢化肉桂酸酯)。在实施例12～15中使用不同的硫化酚化合物。硫化烯烃是一种商业上可购到的、由C16-18异构α-烯烃混合物衍生的硫化烯烃。无灰的二硫代甲氨酸酯是亚甲基-双(二丁基二硫代甲氨酸酯)。
NOC试验是如下进行的。向每组四个的50毫升烧杯注入45克试验油和用于ASTM D943的第八长度铜/铁线圈。将这些烧杯存放在140℃的炉中，且在4、6、8和10天后从炉中取出一个烧杯并分析试验油的颜色(ASTM D1500)和残渣含量(用0.8mm过滤器)。10天的残渣结果以每100毫升油的毫克残渣表示。
还使用Cincinnati Milacron热稳定性试验方法A(CCM“ A”)评估热稳定性，该试验是用铜和铁棒在135℃下进行168个小时。
RBQT是根据ASTM D2272进行的。该试验测量的氧化以分钟来表示寿命，并被用来作为ASTM D943(TOST)试验中氧化性能的标志。
在表中，在NOC试验中使用组I基油在10天后得到低的残渣值和使用组II基油在10天后得到高的RBOT(大于500分钟)，说明抗氧剂给予理想的热稳定性与氧化稳定性的组合。
在实施例I中在组I基油中使用添加剂组合物。大量残渣的形成导致在NOC试验中过滤器的堵塞。在实施例2～15中使用各种抗氧剂与抗氧剂的混合物。然而，在这些实施例中，当使用组I基油时发生过滤器的堵塞和/或当使用组II基油时RBOT的结果不是充分的低(少于500分钟)。
在实施例2～15中使用的抗氧剂不能提供理想的热稳定性(在组I的基油中)与氧化稳定性(在组II的基油中)的组合。
反之，实施例16～23为说明本发明的实施例。在这些实施例中，使用能获得基油II的持久氧化稳定性而当在使用基油I时不会形成过多残渣的抗氧剂组合。实施例16～19的结果显示，添加无灰的二硫代甲氨酸酯延长了二苯基胺与苯基-α-萘胺组合的氧化稳定性而不会形成过多的残渣。对于使用2，6-二叔丁基苯酚(实施例20和2 1)与硫化烯烃(实施例22和23)来说也一样。这些实施例的结果暗示，在所用的各别抗氧剂之间存在某种最佳协合作用。
这些结果证实，根据本发明选择抗氧剂能提供当在使用组II基油时获得持久氧化稳定性而当在使用组I或组II基油时不会形成过多残渣的抗氧剂体系。

Claims (11)

1.一种添加剂在含有0.4-0.9wt％的液压抗磨耗组分的润滑剂组合物中改进热稳定性和氧化稳定性的应用，其中在润滑剂组合物中所述添加剂含有0.04-0.4wt％的胺抗氧剂，以及选自至多0.1wt％的无灰的二硫代甲氨酸酯抗氧剂、至多0.1wt％的硫化烯烃抗氧剂以及至多0.4wt％的酚抗氧剂的至少一种抗氧剂或抗氧剂的混合物，其中所述添加剂通过将胺抗氧剂与至少一种另外的抗氧剂在标准温度和压力下以任何顺序混合而制得。
2.权利要求1的应用，其中抗磨耗组分是液压级二烷基二硫代磷酸锌。
3.权利要求1或2的应用，其中基油是美国石油协会定义的组I基油。
4.权利要求1或2的应用，其中基油是美国石油协会定义的组II或组III基油。
5.权利要求1～4中任一项权利要求的应用，其中添加剂包括二苯基胺和苯基-α-萘胺。
6.权利要求1～4中任一项权利要求的应用，其中添加剂包括二苯基胺和2，6-二叔丁基-α-二甲基氨基对甲酚。
7.权利要求1～6中任一项权利要求的应用，其中酚抗氧剂是2，6-二叔丁基苯酚。
8.权利要求1～6中任一项权利要求的应用，其中硫化烯烃是由C16-18异构α-烯烃衍生的。
9.权利要求1～6中任一项权利要求的应用，其中无灰的二硫代甲氨酸酯是亚甲基-双(二叔丁基二硫代甲氨酸酯)。
10.一种润滑剂组合物，其包含0.4-0.9wt％的液压抗磨耗组分、基油和添加剂，该添加剂包含0.04-0.4wt％的至少一种胺抗氧剂和选自至多0.1wt％的无灰的二硫代甲氨酸酯抗氧剂、至多0.1wt％的硫化烯烃抗氧剂和至多0.4wt％的酚抗氧剂的至少一种抗氧剂，其中所述添加剂通过将胺抗氧剂与至少一种另外的抗氧剂在标准温度和压力下以任何顺序混合而制得。
11.权利要求10的组合物，其中胺抗氧剂的总量，以组合物总重量为基准计，为0.04～0.4wt％。
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