CN1100859C - 具有优异的高温氧化稳定性的汽轮机油 - Google Patents

具有优异的高温氧化稳定性的汽轮机油 Download PDF

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CN1100859C
CN1100859C CN99121597A CN99121597A CN1100859C CN 1100859 C CN1100859 C CN 1100859C CN 99121597 A CN99121597 A CN 99121597A CN 99121597 A CN99121597 A CN 99121597A CN 1100859 C CN1100859 C CN 1100859C
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turbo
rust
preventive agent
oil
engine lube
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CN1251859A (zh
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V·J·加托
H·赖安
R·N·莱尔
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Afton Chemical Intangibles LLC
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Ethyl Corp
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Abstract

一种汽轮机润滑剂，其中包含(A)烷基化二苯胺和/或苯基萘胺，和(B)硫化烯烃和/或硫化脂肪酸和/或无灰二硫代氨基甲酸酯和/或二硫化四烷基秋兰姆，剩余物中含有(C)以很低的硫含量(＜0.03%重量)和高饱和物含量(＞90%体积)为特征的基础油，和任选的(D)中性防锈剂，该润滑剂显示出优越的氧化稳定性，并为汽轮机油和生锈及氧化油的使用提供了充分的腐蚀保护作用和控制淤渣作用。

Description

具有优异的高温氧化稳定性的汽轮机油
本发明涉及汽轮机，生锈和氧化(R&O)，以及具有优异高温氧化稳定性的无灰的液压油(以后统称为“汽轮机油”)。本发明的另一目的是提供这种水平的防氧化作用，而又不损害对淤渣的控制和不需要酚类抗氧化剂。
蒸汽轮机和燃气轮机油是最优质的防锈、防氧化油类。蒸汽轮机利用在高温和高压下进入汽轮机并穿过转动叶片和固定叶片膨胀的蒸汽。只有最高质量的润滑剂才能承受蒸汽轮机操作时的潮湿条件、高温及长的工作时间。在燃气轮机中，它们必须经得起与很热的表面接触，常常是间歇操作和停止使用。因此，两类油要想有效，都必须在良好的防腐蚀和可破乳的性能之外，还具有突出的抗氧化性，这包括在系统的关键部位形成沉积物的倾向极小。
为实现这些理想的性能，必须使用仔细平衡的添加剂组合物来配制这些油。这些流体的本性使其极易污染，特别是被其它润滑剂和添加剂污染。相当小程度的污染就会显著影响这些润滑剂的性质和预期的使用寿命。另外，为了维持有效的操作条件和避免损伤使用它们的设备，汽轮机油应当仔细地保持清洁和去除污染物。通过将汽轮机油过滤可将污染降至极低。为了保证汽轮机油基本上不含污染物，要使用很细的过滤器。
近几年来，汽轮机的输出功率和用油量之比已显著增大。这造成了汽轮机工作温度的大大升高。因此，必须保护润滑剂不发生氧化降解。使用更多的抗氧化剂是一种可能的解决办法，但是较高的用量有时会产生其它问题，例如形成淤渣和溶解困难。更好的办法是使用增放的抗氧化剂组合物，例如本发明中提取的那些，它们提供了改进的抗氧化性能而又不产生淤渣。
由于汽轮机油的要求，与其它类型的润滑组合物相比，只有少数几类添加剂可以与基础油混合。一般来说，成品汽轮机油中只含基础油、抗氧化剂、防锈剂、破乳剂、防腐蚀剂，以及需要时的稀释剂。
EP 0735128 A2公开了含有二硫代氨基甲酸酯和烷基苯基-α-萘胺的使用期延长的R&O润滑油。该文献未提及使用本发明所要求的第II级或更高级(即，第III或第IV级)基础油，或由此得到的好处。
本发明描叙了一种两组分抗氧化剂体系的使用，它在用第II组或更高组基础油配制的汽轮机油中提供了优异的防氧化作用和满意的淤渣控制作用。本发明的高度氧化稳定的润滑剂中含有(A)选自烷基化二苯胺、苯基萘胺及其混合物的一种胺类抗氧化剂，(B)选自硫化烯烃、硫化脂肪酸、无灰二硫代氨基甲酸酯、二硫化四烷基秋兰姆的含硫添加剂，和(C)一种基础油，其特征是硫含量很低(＜0.03％重量)，饱和物含量高(＞90％体积)。在本发明的另一实施方案中，这种高度氧化稳定的润滑剂还含有(D)至少一种防锈剂。
下面将参照附图详细说明本发明的某些特点，其中：
图1说明了在氢化处理的低硫II组油中使用硫化添加剂与胺类抗氧化剂组合物的好处；
图2显示了硫化的添加剂/胺类抗氧化剂组合物在不同类型基本油料中的性能。
本发明涉及汽轮机润滑油，其中含有(A)一种胺类抗氧化剂，选自烷基化二苯胺、苯基萘胺及其混合物，(B)含硫添加剂，选自硫化烯烃、硫化脂肪酸、无灰二硫代氨基甲酸酯、二硫化四烷基秋兰姆及它们的混合物，和(C)一种基础油，其特点是硫含量很低(＜0.03％重量)，饱和物含量高(＞90％体积)。
在本发明的另一实施方案中，该汽轮机润滑油还含有(D)至少一种防锈剂。
组分A-胺类抗氧化剂
适用于本发明的胺类抗氧化剂应当在汽轮机油组合物中溶解。这种胺类抗氧化剂选自烷基化二苯胺、苯基萘胺及其混合物。可用于本发明中的胺类抗氧化剂的实例包括但不限于：二苯胺、苯基-α-萘胺、苯基-β-萘胺、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、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-萘胺、混合烷基化的苯基-α-萘胺，以及具有石油工业中常用的各种纯度的这些物质混合物。商品二苯胺类的例子包括但不限于：Ciba Specialty Chemicals的IrganoxL06、IrganoxL57和IrgnaoxL67；Uniroyal Chemical Company的NaugalubeAMS，Naugalube438、Nau-galube438R、Naugalube438L、Naugalube500、Naugalube640、Nau-galube680和NaugardPANA；BF Goodrich Specialty Chemicals的Goodrite3123、Goodrite3190×36、Goodrite3127、Goodrite3128、Goodrite3185×1、Goodrite3190×29、Goodrite3190×40和Goodrite3191；Ethgl Corporation的HiTEC569抗氧化剂和HiTEC4793抗氧化剂；R.T.Vanderbilt Company，Inc.的VanlubeDND、VanlubeNA、VanlubePNA、VanlubeSL、VanlubeSLHP、VanlubeSS、Vanlube81、Vanlube848和Vanlube849。这些胺类抗氧化剂一般用其氮含量和按照ASTMD 2896测得的TBN来表征。胺类抗氧化剂的氮含量优选在3.0％至7.0％重量之间，TBN优选为每克纯净(即不稀释)添加剂浓缩物100-250mg KOH。
成品油中的胺类抗氧化剂的浓度可以随所用的基本油料，用户的要求及用途，以及特定的汽轮机油所需要的抗氧化剂保护作用的理想含量而变。通常，成品汽轮机油中胺类抗氧化剂的含量为0.04-0.5％重量，优选0.05-0.3％重量。组分B-含硫化合物
本发明的含硫化合物选自硫化稀烃、硫化脂肪酸、无灰二硫代氨基甲酸酯、二硫化四烷基秋兰姆及它们的混合物。适合用于本发明的硫化烯烃可以通过许多已知方法制备。它们以制备时使用的烯烃类型及其最终硫含量为特征。优选高分子量的烯烃(例如，平均分子量(Mn)从约112到约351g/mole的烯烃)。可以使用的烯烃的实例包括α-烯烃、异构的α-烯烃、支化的烯烃、环烯烃、聚合烯烃及它们的混合物。可以使用的α-烯烃的实例包括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、1-二十五碳烯及它们的混合物。可以在硫化反应之前或硫化反应期间将α-烯烃异构化。含有内部双键的或支化的α-烯烃的结构异构体和/或构象异构体也可以使用。例如，异丁烯和α-烯烃1-丁烯的支化的烯烃对应物。
可以用在硫化反应中的硫源包括例如元素硫、一氯化硫、二氯化硫、硫化钠、多硫化钠以及一起加入的或是硫化过程不同阶段加入的它们的混合物。
不饱和的脂肪酸和油因其不饱和性，也可以被硫化并用于本发明。可以使用的脂肪酸的实例包括9-十二烯酸、9-十四烯酸、9-十六烯酸、油酸、反油酸、11-十八烯酸、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。可以使用的油或脂肪的实例包括玉米油、棉籽油、葡萄籽油、橄榄油、棕榈油、花生油、油菜籽油、红花籽油、芝麻油、大豆油、向日葵油、向日葵籽油及它们的混合物。
适合在本发明中使用的无灰的二硫代氨基甲酸酯和二硫化四烷基秋兰姆最好是能溶于汽轮机油组合物中。可以使用的无灰二硫代氨基甲酸酯包括但不限于亚甲基双(二硫代氨基甲酸二烷基酯)，亚乙基双(二硫代氨基甲酸二烷基酯)和异丁基二硫化物-2，2’-双(二硫代氨基甲酸二烷基酯)，其中二硫代氨基甲酸二烷基酯的烷基优选有1-16个碳原子。优选的无灰二硫代氨基甲酸酯的实例是亚甲基双(二硫代氨基甲酸二丁酯)、亚乙基双(二硫代氨基甲酸二丁酯)和异丁基二硫化物-2，2’-双(二硫代氨基甲酸二丁酯)。可以使用的优选的二硫化四烷基秋兰姆包括二硫化四丁基秋兰姆和二硫化四辛基秋兰姆。
组分B在成品汽轮机油中的浓度可以随用户的要求及用途，以及对于特定的汽轮机油所要求的抗氧化剂保护程度而变。用来选定汽轮机油中组分B使用浓度的一个重要标准是硫含量。组分B应当向成品汽轮机油提供0.005-0.07％重量的硫。例如，为了向成品油提供0.005-0.07％重量的硫，含12％重量硫的硫化烯烃的使用浓度应为0.04-0.58％重量。而硫含量为30％重量的无灰二硫代氨基甲酸酯的使用浓度应为0.02-0.23％重量，以便向成品油提供0.005-0.07％重量的硫。
用来选择组分B的另一标准是按照ASTMD 1662测定的物质中的活性硫含量。高含量活性硫的存在会使成品汽轮机油产生严重的腐蚀和淤渣问题。在本发明的优选实施方案中，按照ASTMD 1662测得的组分B中活性硫的含量低于1.5％重量。
可以用于本发明的商品硫化烯烃的一个实例是HiTEC7188硫化烯烃，它可自Ethyl Corporation购得，含有约12％重量的总硫量和＜1％重量的活性硫。可用于本发明的商品硫化脂肪油或硫化脂肪油与烯烃的混合物包括约含9.5％重量的硫和1％重量活性硫的AdditinR4410，约含12.5％重量硫和1.5％重量活性硫的AdditinR 4412F，和约含10％重量硫和＜1％重量活性硫的AdditinRC 2810-A，它们全是Rhein Chemie Corporation的产品。可用在本发明中的商品无灰二硫代氨基甲酸酯的实例是R.T.Vanderb lit Company的Vanlube7723，其硫含量约为30％重量。从实用观点考虑，组分B应含有最少8.0％重量的硫，以便减小为提供所需硫量所必需的添加剂的数量。这是为控制汽轮机油组合物的成本所要求的。
也可以使用硫化烯烃、无灰二硫代氨基甲酸酯和二硫化四烷基秋兰姆的不同比例的混合物，只要它们满足所要求的总硫含量和活性硫含量。组分C——基础油
适合用于本发明的基础油的特征是很低的硫含量(＜0.03％重量)和高的饱和物含量(＞90％体积)。
第II和第III级基本油料特别适合用于本发明，它们通常用以下方法制备：用强氢化步骤处理常规的基本油料以减少芳香物、硫和氮含量，随后经脱蜡、加氢精制、抽提和/或蒸馏步骤，得到成品基础油。第II和第三级基本油料与常规的溶剂精制第I级基本油料的不同在于它们的硫、氮和芳香物含量很低。因此，这些基础油在成分上与常规的溶剂精制基本油料很不相同。美国石油研究所将这些不同的基本油料分类如下：第一级，硫含量＞0.03重量，和/或饱和物含量＜90％体积，粘度指数80-120；第二级，硫含量≤0.03％重量，饱和物含量≥90％，粘度指数80-120；第III级，硫含量≤0.03％重量，饱和物含量≥90％体积，粘度指数＞120；第IV级全是聚α-烯烃。经氢化处理的基本油料和催化脱蜡的基本油料，因其硫和芳香物含量低，通常属于第II和第III级范畴。聚α-烯烃(第IV级基本油料)是由各种α-烯烃制备的基本上不含硫和芳香物的合成基础油。聚α-烯烃也可以作为本发明的组分C使用。另外，也可以用第II级、第III级和/或第IV级基础油的掺混物作为本发明的组分C。再者，适合用于本发明的基础油可以含一些第I级基本油料，只要总的基础油组合物中硫含量＜0.03％重量，饱和物含量＞90％体积即可。
对于在组分C中使用的各种基本油料的化学成分没有限制。例如，在各种第II和第III级油中，芳香物、链烷烃和脂环烃之间的比例可以有很大的变化。此成分一般由精制程度和用来制造油的原料来源决定。最好是基本油料中的链烷烃含量高，即，＞60％体积。
本发明的基础油(C)占汽轮机润滑油总重量的约90-99.75％重量。组分D——防锈剂
如果存在防锈剂，则任何类型的防锈剂均可用于本发明。适合用于本发明的酸性防锈剂包括通过一元羧酸、聚亚烷基多胺和链烯基琥珀酸酐反应得到的反应产物，例如美国专利4,101,429中提到的那些，本文引用作为参考。当要求在水和污染物存在下具有混溶性时，使用中性防锈剂优于酸性防锈剂，因为发现它们能改进过滤性。防锈剂的浓度可以从0.02％至0.5％重量变化。在本发明中，术语“中性防锈剂”意味着防锈剂基本上不含-COOH官能基。
适合用于本发明的中性防锈剂包括任何基本上不含-COOH基的防锈剂。最好是，中性防锈剂是化学式为R(COOR’)n的烃基酯，其中R和R’是烃基或羟基烃基，含有1至约40个碳原子，优选含8-20个碳原子，n为1至约5。这些酯在分子中含有至少1个、优选1-5个羟基。它们可以全与R或全与R’连接，或者它们可以以不同的比例与R和R’连接。另外，这些羟基可以位于沿R或R’链的任何一个或多个位置。应该理解，在烃基或羟基烃基R上存在的COOR’基团数目最大值将随R中的碳原子数而变。
这些烃基酯可以由合适的醇和酸、酰基卤、酸酐或它们的混合物按照常规的酯化步骤制备。此外，本发明的酯可以用常规的酯交换方法制备。
通常，中性防锈剂的TAN小于10mg KOH/g。优选的酯包括但不限于：苹果酸辛基油基酯、苹果酸二油基酯、季戊四醇单油酸酯和甘油单油酸酯。
“基本上不含”是指，用来制备中性防锈剂的起始物酸、酰基卤、酸酐或它们的混合物是与数量足以在理论上将-COOH基转化为酯的醇反应。
另一类优选的中性防锈剂包括1-(2-羟基乙基)-2-十七碳烯基咪唑啉的天冬氨酸二酯。这种咪唑啉主要是基于油酸和氨基乙醇胺反应的L-天冬氨酸和咪唑啉的二酯的混合物。此类酯可自MonaIndestries，Inc.作为Monacor39购得。
式(I)表示的琥珀酰亚胺和琥珀酰胺也可以在本发明中作为防锈剂使用。这些化合物可以单独使用，或者与一种或多种上述中性或酸性防锈剂组合使用：
Figure C9912159700111
其中Z是基团R1R2CH-，其中的R1和R2彼此独立地是有1-34个碳原子的直链或支链烃基，且R1和R2基团中的总碳原子数为11-35。
在式(I)中，Z可以是例如1-甲基十五烷基、1-丙基十三碳烯基、1-戊基十三碳烯基、1-十三烷基十五碳烯基或1-十四烷基二十碳烯基。基团R1和R2中的碳原子数优选为16-28，更常见的是18-24。特别优选R1和R2中的碳原子总数为约20-22。优选的式(I)代表的化合物是所示的琥珀酰亚胺，优选的琥珀酰亚胺是3-C18-24链烯基-2，5-吡咯烷酮。这种琥珀酰亚胺的一种更优选的实施方案包含有18-24个碳原子的链烯基的混合物。
在本发明的一个方面，式(I)表示的化合物的可滴定酸值(TAN)为约8-140mg KOH/g，优选为约110mg KOH/g。TAN是按照ASTM D 664测定的。
这些化合物是市售商品，或是可以通过利用或修改已知方法来制得(例如见EP-A-0389237)。
通常，本发明的添加剂组分(A、B以及可能存在的D)是以添加剂组合物浓缩物的形式加到基础油(C)中。浓缩物中添加剂各组分的总量通常为20-95％重量或者更高，其余为稀释剂油。稀释剂油可以是本发明的第II级或更高级的油、如上所述的常规的第I级基础油，或是一种烃溶剂，优选芳烃溶剂，或它们的混合物。浓缩物中可以含其它添加剂。其它添加剂的实例包括破乳剂、防铜腐蚀剂、无灰抗磨添加剂和辅助的抗氧化剂，如位阻酚类。可以使用的位阻酚类抗氧化剂的实例包括2、6-二叔丁基苯酚、2，4，6-三叔丁基苯酚、4，4’-亚甲基双(2、6-二叔丁基苯酚)、亚甲基桥接的叔丁基苯酚混合物、3，5-二叔丁基-4-羟基氢化肉桂酸异辛酯和硫代二亚乙基双(3，5-二叔丁基-4-羟基)氢化肉桂酸酯。通常，添加剂组合物浓缩物在基础油(C)中的加入量足以向成品油提供0.25-2.0％重量的组分(A)、(B)和可能存在的(D)。
在本发明的一项优选实施方案中，制备了不加位阻酚抗氧化剂的汽轮机润滑油。使用位阻酚可能会带来很多问题。使用含低浓度游离酚的位阻酚会有毒性。另外，位阻酚在高温下会去烷基化并产生游离酚。某些水溶性酚的水可萃取性是另一个潜在的问题。因此无酚的制剂是理想的。
本发明还涉及一种改进基础油的氧化稳定性的方法，共中该方法包括向硫含量小于0.03％重量、饱和物含量大于90％体积的基础油中加入：(A)选自烷基化二苯胺、苯基萘胺及其混合物的一种胺；和(B)选自硫化烯烃、硫化脂肪酸、无灰二硫代氨基甲酸酯、二硫化四烷基秋兰姆及它们的混合物的一种含硫添加剂。
本发明的汽轮机油可以用于其它用途，包括循环系统、压缩机、无灰液压系统和氧化稳定性非常重要的其它设备。
实施例
必须指出，在成品汽轮机油中使用含硫添加剂(组分B中定义的那些)会由于腐蚀及在油氧化期间淤渣的显著增加而受到限制。适合用于汽轮机的油需要通过一定的试验以证实其合格的腐蚀性和淤渣控制性。
以下实施例表明了本发明的汽轮机油的优越的氧化稳定性及对淤渣和腐蚀的充分控制。
实施例I
用表1中所示的各组分、浓度和基本油料掺混成一系列32处油。掺混油时将所有组分与油混合并在50℃和充分搅拌下加热1小时。使用的各组分如下：
防腐蚀剂——衍生的甲苯基三唑防腐蚀剂。
无灰DTC——含约30％重量硫的亚甲基双(二硫代氨基甲酸二正丁酯)、此添加剂代表润滑剂组合物的组分B。
硫化烯烃——含约12％重量硫的C16-C18硫化烯烃。此添加剂代表润滑剂组合物的组分B。
酸性防锈剂-HiTEC536防锈剂，Ethyl Corporation销售的一种衍生的酸性防锈剂。
PANA——含约6.6％重量氮的苯基-α-萘胺。此添加剂代表润滑剂组合物的组分A。
2.6-DTBP——2.6-二叔丁基苯酚。
DPA——含约4.3％重量氮的一种苯乙烯基辛基烷基化的二苯胺。此添加剂代表本发明润滑剂组合物的组分A。
中性防锈剂-季戊四醇单油酸酯中性防锈剂。此添加剂代表润滑剂组合物的组分D。
100N II级——一种基本油料，含约0.01％重量硫，粘度指数99。它代表润滑剂组合物的组分C。
100N I级——一种含约0.15％重量硫、粘度指数为85的基本油料。
100N高VI II级——一种含硫量小于0.001％重量、粘度指数为110的基本油料。它代表润滑剂组合物的组分C。
150N I级——一种含0.33％重量硫、粘度指数94的基本油料。
表I中所有的配制油均按照ASTM D2272旋转弹氧化试验进行评价。旋转弹氧化试验(RBOT)是一种汽轮机油氧化试验，用来作为对已知成分的新的或用过的汽轮机油的质量控制，以及作为估计试验油氧化稳定性的研究手段。此试验对汽轮机油在升高的温度和氧气压力下及在铜线圈氧化催化剂和水存在下的氧化稳定性进行评价。一个旋转的玻璃弹提供了油-氧的最大接触。以时间报道了当氧压下降25psi时的结果。表I中列出了所有32种油的RBOT结果。
在表I的油1-16的结果中及图1中显示了烷基化二苯胺(DPA)和硫化烯烃及1或无灰二硫代氨基甲酸酯(无灰DTC)之间的协同作用。注意到只用硫化添加剂(油1至5)或只用DPA(油6)在对低硫的氢化处理的第II级油提供氧化保护作用方面均很差，即，诱导期很短。但是，当硫化添加剂与DPA组合使用时(油12-16)，显示出高度的氧化保护作用，即，诱导期很长。当硫化添加剂和DPA在防腐蚀剂和中性防锈剂存在下组合使用时，也显示出高度的氧化保护作用(油7-11)。
由比较表I中的油7、20、21和22和由图2都显示出这种硫化添加剂/DPA组合使氢化的第II级油具有优异的氧化稳定性。氢化的低硫II级油(7和21)比常规的含硫I级油(20和22)的氧化稳定性高得多。在图2中，所试验的基本油料如下：A是上述的100N I级基本油料，B是上述的150N I级基本油料，C是上述的100N II级基本油料，D是上述的100N高VI II级基本油料。
比较油7和19表明，酸性防锈剂(19)和中性防锈剂(7)均可与本发明的硫化添加剂及DPA组合使用。但是常常优选中性防锈剂，因其对控制成品汽轮机油的可过滤性有效。
油17和18表明，只用防腐蚀剂和防锈剂(17)或者用防腐蚀剂和防锈剂与硫化添加剂无灰DTC的组合(18)，在稳定低硫的加氢处理II级油方面均无效。
油23和24表明，防腐蚀剂和防锈剂的其它组合对于稳定低硫的加氢处理II级油也有效。在油23中，无灰DTC和DPA使用时只与中性防锈剂组合。在油24中，无灰DTC和DPA使用时只与一种防腐蚀剂组合。
油25-29显示了本发明在可使用的实际处理量的可能范围方面的有效性。无灰DTC由0.05％至0.15％重量变化。DPA由0.2％至0.4％重量变化。当然，成品油中无灰DTC和DPA含量较低时会造成油的氧化稳定性较低。但是，与I级基本油料相比，无灰DTC和DPA的组合在II级基本油料中能提供好得多的氧化保护作用。在需要达到相当于在I级基本油料中得到的氧化性能的情形下，在II级(或更高级)基本油料中可以使用较低含量的无灰DTC和DPA(比较油29与油20以及油25与油22)。另外，II级(或更高级)基本油料的氧化性能改进而又不产生淤渣，对于汽轮机应用是有利的。
比较油25与油30表明，可以使用一种辅助的抗氧化剂作为本发明的一部分，以进一步改进低硫、氢化处理的II级油的氧化稳定性。在油30中的辅助抗氧化剂是2，6-二叔丁基苯酚，这种抗氧化剂使油30的氧化稳定性比油25提高。
油31采用苯基-α-萘胺(PANA)与DPA组合作为本发明的一部分，而油32使用苯基-α-萘胺与DPA及一种酚类抗氧化剂代替含硫添加剂。注意到当使用PANA制备本发明的成品油时，得到了一种添加剂含量低(0.55％对0.7％重量)而氧化稳定性高(1554分钟对1300分钟)的油。
样品ID   防腐蚀剂(g)    无灰DTC(g)   硫化烯烃(g)     酸性防锈剂(g)     PANA(g)  2，6-DTBP(g)   DPA(g)   中性防锈剂(g)     100NII级(g)     100NI级(g)    100N高VIII级(g)     150NI级(g)    总量(g)    RBOT(分)
    1*     0.200     99.800     100     34
    2*     0.150     0.125     99.725     100     86
    3*     0.100     0.250     99.650     100     106
    4*     0.050     0.375     99.575     100     121
    5*     0.500     99.500     100     125
    6*   0.500     99.500     100     207
    7     0.050     0.200   0.250     0.200     99.300     100     2205
    8     0.050     0.150     0.125   0.250     0.200     99.225     100     1706
    9     0.050     0.100     0.250   0.250     0.200     99.150     100     1847
    10     0.050     0.050     0.375   0.250     0.200     99.075     100     1569
    11     0.050     0.500   0.250     0.200     99.000     100     1219
    12     0.200   0.250     99.550     100     1671
    13     0.150     0.125   0.250     99.475     100     2043
    14     0.100     0.250   0.250     99.400     100     1826
    15     0.050     0.375   0.250     99.325     100     1542
    16     0.500   0.250     99.250     100     1360
    17*     0.050     0.200     99.750     100     33
    18*     0.050     0.200     0.200     99.550     100     31
    19     0.050     0.200     0.200   0.250     99.300     100     2486
    20*     0.050     0.200   0.250     0 200   99.300     100     1052
    21     0.050     0.200   0.250     0.200     99.300     100     2638
    22*     0.050     0.200   0.250     0.200     99.300     100     731
    23     0.200   0.250     0.200     99.350     100     1720
    24     0.050     0.200   0.250     99.500     100     2990
    25     0.050     0.050   0.200     0.200     99.500     100     715
    26     0.050     0.050   0.400     0.200     99.300     100     709
    27     0.050     0.150   0.200     0.200     99.400     100     1542
    28     0.050     0.150   0.400     0.200     99.200     100     1758
    29     0.050     0.100   0.300     0.200     99.350     100     1050
    30     0.050     0.050     0.200   0.200     0.200     99.300     100     929
    31     0.050     0.050     0.050   0.200     0.200     99.450     100     1554
    32*     0.050     0.100     0.250   0.100     0.200     99.300     100     1300
*对照实施例实施例II
采用表II中所示的组分、浓度和基本油料掺混成一系列油。掺混时将所有组分与油混合，并在充分搅拌下于50℃加热1小时。所用的组分为实施例I中确定的组分及下列组分：
SBHHC-含约5％硫的硫代亚乙基双(3，5-二叔丁基-4-羟基氢化肉桂酸酯)。
Octyl BHHC-3，5-二叔丁基-4-羟基氢化肉桂酸异辛酯。
油33-44代表通常用在汽轮机油中的抗氧化剂组合物，而油12-16代表本发明的用于汽轮机油的抗氧化剂组合物。这些油按照实施例I中定义的RBOT ASTM D 2272评价。RBOT结果列在表II中。
可以看出，含通常使用的抗氧化剂体系的低硫氢化处理II级油(油34、36、38、41和44)与含同一抗氧化剂体系的含硫I级油的氧化稳定性无明显差别。在一些情形下低硫氢化处理II级油的氧化稳定性比含硫的I级油略差(34比33，38和37，41比39，44比42)，而另一些情形下它们的氧化稳定性稍强(36比35，41比40，44比43)。在低硫氢化处理II级油的氧化稳定性比含硫I级油高的情形下，它们的差别不大。
注意到油33到38含有与DPA组合使用的硫化抗氧化剂。抗氧化剂SBHHC含有约5％重量的硫。在油35和36中，0.019％重量的硫是由抗氧化剂SBHHC提供给油。这一硫含量处在本发明对组分B指定的范围。但是，SBHHC对于改进低硫氢化II级油的氧化稳定性不是有效的硫化添加剂，即，使用SBHHC时的RBOT诱导期在I级和II级油之间无显著差别。另外，SBHHC比本发明组分B中的硫化烯烃及无灰DTC贵得多。通过加入高含量的SBHHC来增加油的硫含量是不实际的，因为它的硫含量较低，需要的用量相当大。
油12和16代表本发明组合物。可以看出与油33-44相比，这些油具有优越的氧化稳定性。
表II
样品ID 抗氧化剂ID 抗氧化剂含量(wt％) DPA含量(wt％) 基本油料品种 RBOT两次结果平均值(分)
    33* SBHHC     0.25     0.25 100N  级  I     448
    34* SBHHC     0.25     0.25 100N  级  II     392
    35* SBHHC     0.375     0.125 100N  级  I     324
    36* SBHHC     0.375     0.125 100N  级  II     426
    37* SBHHC     0.125     0.375 100N  级  I     434
    38* SBHHC     0.125     0.375 100N  级  II     366
    39* 2，6-DTBP     0.25     0.25 100N  级  I     670
    40* 2，6-DTBP     0.25     0.25 150N  级  I     360
    41* 2，6-DTBP     0.25     0.25 100N  级  II     549
    42* Octyl BHHC     0.25     0.25 100N  级  I     461
    43* Octyl BHHC     0.25     0.25 150N  级  I     255
    44* Octyl BHHC     0.25     0.25 100N  级  II     286
    12 无灰DTC     0.2     0.25 100N  级  II     1671
    16 硫化烯烃     0.5     0.25 100N  级  II     1360
*对照实施例
实施例III
设计了许多试验以便对成品汽轮机油控制腐蚀和淤渣的能力进行筛选。一种很适用的试验是日本油色试验(NOC)。NOC方法进行如下：在四只50ml烧杯中装入45g要试验的油。在四只烧杯中各加入铁和铜线圈催化剂(用于ASTM D 943)。将烧杯在140℃下存放，4、6、8和10天后从烘箱中取出一只烧杯，分析颜色(ASTM D 1500)和淤渣含量。铜线圈按照ASTM D 130评级图定级。
油25-31按照NOC试验进行评价，用ASTM D 1500分析颜色形成，用生成的淤渣重量(毫克)表示淤渣形成。所有的油的颜色及淤渣结果均合格，即，油老化10天后，颜色小于8.0，淤渣小于10毫克。
本发明在其实施中易于做出相当大的变化。因此，本发明不限于此前所述的具体的实例，而是在所附权利要求的精神和范围内，在法律上包括它们可存在的等同物。
本专利权所有人不打算向公众奉献任何公开的实施方案，就任何公开的修改或变动在字面上可能不属于权利要求的范围来说，它们在等同论原则下被认为是本发明的一部分。

Claims (24)

1.一种汽轮机润滑油，其中含有：
(A)  0.04-0.5重量％选自烷基化二苯胺类、苯基萘胺
类及其混合物的一种胺类抗氧化剂；
(B)  其量足以为成品汽轮机油提供0.005-0.07重量％
硫的含硫添加剂，选自硫化烯烃类、硫化脂肪酸类、
无灰二硫代氨基甲酸酯类、二硫化四烷基秋兰姆类及
它们的混合物；
(C)  90-99.75重量％硫含量少于0.03重量％、饱和物
含量大于90％体积的一种基础油。
2.权利要求1的一种汽轮机润滑油，其中胺类抗氧化剂含有烷基化二苯胺。
3.权利要求1的一种汽轮机润滑油，其中胺类抗氧化剂含有苯基萘胺。
4.权利要求1的一种汽轮机润滑油，其中胺类抗氧化剂含有烷基化二苯胺和苯基萘胺的混合物。
5.权利要求1的一种汽轮机润滑油，其中含硫组分(B)含有硫化烯烃。
6.权利要求5的一种汽轮机润滑油，其中硫化烯烃的烯烃的平均分子量是从112到约351g/mole。
7.权利要求1的一种汽轮机润滑油，其中含硫化合物(B)含有硫化脂肪酸。
8.权利要求1的一种汽轮机润滑油，其中含硫化合物(B)含有无灰二硫代氨基甲酸酯。
9.权利要求1的一种汽轮机润滑油，其中含硫化合物(B)含有二硫化四烷基秋兰姆。
10.权利要求1的一种汽轮机润滑油，其中含硫化合物(B)含有由至少一种硫化烯烃和至少一种无灰二硫代氨基甲酸酯组成的混合物。
11.权利要求1的一种汽轮机润滑油，其中含硫化合物(B)按ASTM D 1662测定含有少于1.5％重量的活性硫。
12.权利要求1的一种汽轮机润滑油，其中还含有(D)至少一种防锈剂。
13.权利要求12的一种汽轮机润滑油，其中防锈剂含有至少一种酸性防锈剂。
14.权利要求12的一种汽轮机润滑油，其中防锈剂含有至少一种中性防锈剂。
15.权利要求12的一种汽轮机润滑油，其中防锈剂含有至少一种选自以下化学式的琥珀酰亚胺或琥珀酰胺化合物，
Figure C9912159700031
其中Z是基团R1R2CH-，其中的R1和R2各自独立地是含1-34个碳原子的直链或支链烃基，且R1和R2中总碳原子数11-35。
16.权利要求12的一种汽轮机润滑油，其中防锈剂含有至少一种酸性防锈剂和至少一种中性防锈剂的混合物。
17.权利要求12的一种汽轮机润滑油，其中防锈剂含有至少一种酸性防锈剂和至少一种琥珀酰亚胺或琥珀酰胺防锈剂的混合物。
18.权利要求12的一种汽轮机润滑油，其中防锈剂含有至少一种中性防锈剂和至少一种琥珀酰亚胺或琥珀酰胺防锈剂的混合物。
19.权利要求12的一种汽轮机润滑油，其中该汽轮机润滑油含0.02-0.5重量％的防锈剂。
20.权利要求1的一种汽轮机润滑油，其中还含有至少一种添加剂，选自破乳剂、铜腐蚀抑制剂、抗磨添加剂和辅助抗氧化剂。
21.权利要求20的一种汽轮机润滑油，其中还含有一种位阻酚抗氧化剂。
22.权利要求1的一种汽轮机润滑油，其中不含位阻酚抗氧化剂。
23.制备汽轮机润滑油的方法，该方法包括向硫含量小于0.03重量％、饱和物含量大于90％体积的基础油中加入(A)选自烷基化二苯胺、苯基萘胺和其混合物的一种胺类抗氧化剂；和(B)选自硫化烯烃、硫化脂肪酸、无灰二硫代氨基甲酸酯、二硫化四烷基秋兰姆及它们的混合物的一种含硫添加剂。
24.权利要求23的制备汽轮机润滑油的方法，其中还包括向基础油中加入(D)至少一种防锈剂。
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