CN101679899B - 润滑脂组合物 - Google Patents

润滑脂组合物 Download PDF

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Publication number
CN101679899B
CN101679899B CN2008800206524A CN200880020652A CN101679899B CN 101679899 B CN101679899 B CN 101679899B CN 2008800206524 A CN2008800206524 A CN 2008800206524A CN 200880020652 A CN200880020652 A CN 200880020652A CN 101679899 B CN101679899 B CN 101679899B
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weight
grease composition
fat
ionic liquid
oil
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CN101679899A (zh
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G·博德谢姆
M·施米特-阿梅伦克森
D·索恩
S·格伦戴
A·霍普克
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Klueber Lubrication Muenchen GmbH and Co KG
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Klueber Lubrication Muenchen GmbH and Co KG
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Abstract

本发明涉及一种润滑脂组合物，其含基于具有工业润滑剂通常粘度(ISO VG 2-ISO VG 1500)的油的基油混合物、离子液体、增稠剂如基于聚脲化合物的增稠剂以及通常的添加剂，该润滑脂组合物既可在高于120℃-260℃的常用使用温度，特别是在高于180℃-260℃的高使用温度的使用温度使用，也可在达-60℃的低温使用。本发明还涉及用于制备这种润滑脂组合物的方法。

Description

润滑脂组合物
本发明涉及润滑脂组合物，其含基于具有工业润滑剂用的通常粘度(ISO VG 2-ISO VG 1500)的油的基油混合物、离子液体、增稠剂如基于聚脲化合物的增稠剂以及通常的添加剂，该润滑脂组合物既可在高于120℃-260℃的常见使用温度，特别是在高于180℃-260℃的使用温度使用，也可在达-60℃的低温使用。本发明还涉及用于制备这种润滑脂组合物(Schmierfettzusammensetzung)的方法。
新润滑剂的研发需随工业的普遍进展而发展，这对润滑脂组合物提出新的和更高的要求。基于矿物油和/或合成油的已知润滑脂组合物已不再满足这些要求。
润滑剂用于汽车工业、输送技术、机器制造、办公技术以及在工业装置和机器中，以及还用于家用机器乐电子器件领域。
在滚动轴承(
Figure G2008800206524D00011
)和滑动轴承(Gleitlager)中，要使润滑剂在相互滑动或滚动的部件之间形成分离性的负荷转移的润滑膜。由此达到金属表面本身不发生接触和由此也无磨损。因此该润滑剂必需满足高的要求。其包括极端的运行条件如非常高或非常低的转数、由高转数或外来加热引起的高温、例如在低温环境下运行的轴承或在航空航天应用中出现的非常低的温度。现代的润滑剂也要能在所谓的净化室条件(Reinraumbedingung)下应用，以避免由于润滑剂的磨损或耗用产生的室内污染(Raumverschmutzung)。此外，在应用现代的润滑剂时要避免其挥发和由此“涂漆(verlacken)”，即在短时间使用后其变成固态并不再显示出润滑作用。在下面应用下也对润滑剂提出特殊要求，即轴承的滑动面不受低摩擦力的损害，轴承面以低噪声运行以及无后润滑下需长期运行。润滑剂还必须承受得住力作用如离心力、重力和振动。
在高温范围下脂润滑的滚动轴承的长期运行的重要特征除上述按DIN 51825的使用温度之外还有该润滑剂的噪声行为。润滑脂在参与旋转(Umlaufteilnahme)(滚动()、挤压(Walkung))下会在滚动轴承中激发振动，其作为“润滑剂噪声”处于频带的中频即300-1800Hz和高频即1800-10000Hz，而轴承噪声处于频带的低频即50-300Hz。该润滑剂噪声由在硬颗粒滚动通过滚动体在轴承环上以冲击脉冲形式产生的噪声峰所重叠。该噪声行为的评估按SKF-静音(Bequiet)-方法进行，该方法基于该噪声峰的统计求值和所归入的噪声等级BQ1-BQ4。该噪声行为和滚动轴承的使用寿命随噪声等级值的增加而恶化(H.Werries，E.Paland，FVA-Studie zum Thema″
Figure G2008800206524D00021
Schmierfette″，
Figure G2008800206524D00022
Hannover 1994)。如100％噪声等级BQ1表示非常好的噪声行为，仅在噪声等级BQ4中的低百分比值表示非常差的噪声行为。
润滑脂的噪声行为越好，则通过润滑剂强加的轴承振动越小。这与轴承的小负荷同等重要，并导致轴承的更长运行寿命。
近来对在润滑技术中使用离子液体(Ionisch Flüssigkeit)，也称为IL(＝离子液体(Ionic Liquid))进行了大量研究，因为通过阳离子或阴离子改性可提供宽的应用范围。离子液体是在室温下优选为液态或按定义熔点＜100℃的所谓的盐熔体。得到离子液体的已知阳离子/阴离子组合例如是二烷基咪唑鎓(Dialkylimidazolium)、吡啶鎓(Pyridinium)、铵和鏻(Phosphonium)等，与有机阴离子如磺酸根、酰亚胺、甲基化物(Methide)等，还有(als auch)无机阴离子如卤离子和磷酸根等，其中也可考虑阳离子和阴离子的任何其它组合，由此可实现低熔点。离子液体依其化学结构具有特别低的蒸气压、是不可燃的并常常直至大于260℃热稳定和还具有润滑性。
WO 2006/077082描述了一种在使用滑环密封条件下密封旋转轴的方法以及应用离子液体作为滑环密封的密封液体组分来密封旋转轴。该密封液体用于旋转轴的附加密封。该已知的密封液体是水或油，其行为应通过使用离子液体在与具有高密封要求的机器环境的相互作用方面得以改进。
DE 102004033021 A1描述了离子液体作为液压液体的应用，其中应降低液态传压介质(Druckübertragungsmittel)的可压缩性，并由此应改进液压***的传能效率(Energieubertragungseffizienz)。
由DE 102005007100 A1已知处理机(Prozeβmaschine)或工作机(Arbeitsmaschine)，其使用离子液体作为工作液体。该离子液体也可在工作液体应用范围内用作润滑液、密封液体(Sperrflüssigkeit)、密封液(Abdichtflüssigkeit)、压力传送液体等。
液态润滑剂的应用通常需使用昂贵的密封。润滑脂(Schmierfett)本身具有密封作用。这可不使用昂贵的密封，用简单的盖或密封板即可工作。
本发明的目的是提供一种润滑脂组合物，其满足上述要求，特别是可在高温条件和低温条件下应用，有小的蒸气压或无蒸气压，并由此在应用时不挥发，其显示出好的噪声行为，有长的运行时间和基本上无滚动轴承磨损现象。此外，该润滑脂组合物应产生适配于该应用的油分离
Figure G2008800206524D00031
根据本发明，该目的通过一种润滑脂组合物实现，该润滑脂组合物由基于具有针对工业润滑剂的通常粘度(ISO VG 2-ISO VG 1500)的油的基油混合物、离子液体或数种离子液体的混合物、增稠剂如基于聚脲化合物的增稠剂以及通常的添加剂组成，该润滑脂组合物既可在高于120℃-260℃的使用温度使用，也可在达-60℃的低温使用。
该基油混合物可以是合成油、矿物油和/或天然油。依应用不同这些油可单独地使用或组合使用。
该合成油选自脂族或芳香族的二-、三-或四-羧酸与一种或以混合物形式存在的C7-C22-醇的酯，选自聚苯醚或烷基化二苯醚，选自三羟甲基丙烷、季戊四醇或二季戊四醇与脂族C7-C22-羧酸的酯，选自C18-二聚酸与C7-C22-醇的酯，选自复合酯，作为单组分或以任意混合物的形式。此外，该合成油还可选自聚-α-烯烃、烷基化萘、烷基化苯、聚乙二醇、硅油、全氟聚醚。
矿物油可选自链烷烃基-、环烷烃基-、芳族的加氢裂化油
Figure G2008800206524D00032
气转液(Gas to Liquid)(GTL)-液体。GTL称为汽转液法，并描述了由天然气制备燃料的方法。天然气经蒸气重整转变成合成气，该合成气借助于催化剂经费托合成转变成燃料。该催化剂和工艺条件调制该燃料类型，即是否制成汽油、煤油、柴油或油。同样按煤转液法(CTL)可用煤作原料，在生物质转液(BTL)法中可用生物质作原料。
作为天然油可用来自动物来源/植物来源的甘油三酯，其按已知的方法如氢化法调质。特别优选的甘油三酯油是具有高油酸含量的基因改性的甘油三酯油。通常所用的和具有高油酸含量的基因改性的植物油是红花油、玉米油、菜籽油、葵花子油、大豆油、亚麻籽油、花生油、雷斯克懒勒属(Lesquerella)-油、绣线菊油
Figure G2008800206524D00033
和棕榈油。
在离子液体情况下，如上所述，通过合适选择阳离子和阴离子实现润滑剂组合物的各所需特性，如提高润滑剂的使用寿命和润滑作用、调节粘度以改进温度适应性、调节导电性以扩大应用领域。适于离子液体的阳离子是鏻阳离子、咪唑鎓阳离子、吡啶鎓阳离子或吡咯烷鎓阳离子，其可与阴离子组合，该阴离子含氟并选自双(三氟甲基磺酰基)酰亚胺、双(全氟烷基磺酰基)酰亚胺、全氟烷基磺酸根、三(全氟烷基)甲基化物、双(全氟烷基)酰亚胺、双(全氟芳基)酰亚胺、全氟芳基全氟烷基磺酰基酰亚胺和三(全氟烷基)三氟磷酸根或不含卤素的烷基硫酸根-阴离子。
特别优选是含高氟化的阴离子的离子液体，因为其通常具有高的热稳定性。也可通过这类阴离子明显降低吸水能力，例如在使用双(三氟甲基磺酰基)阴离子时。
这类离子液体(IL)的实例是：
丁基甲基吡咯烷鎓-双(三氟甲基磺酰基)酰亚胺(MBPimid)，
甲基丙基吡咯烷鎓-双(三氟甲基磺酰基)酰亚胺(MPPimid)，
1-己基-3-甲基咪唑鎓-三(全氟乙基)三氟磷酸根(HMIMPFET)，
1-己基-3-甲基咪唑鎓-双(三氟甲基磺酰基)酰亚胺(HMIMimid)，
己基甲基吡咯烷鎓-双(三氟甲基磺酰基)酰亚胺(HMP)，
四丁基鏻-三(全氟乙基)三氟磷酸根(BuPPFET)，
N-己基吡啶鎓-双(三氟甲基)磺酰基酰亚胺(Hpyimid)，
丁基甲基吡咯烷鎓-三(五氟乙基)三氟磷酸根(MBPPFET)，
三己基(十四烷基)鏻-双(三氟甲基磺酰基)酰亚胺(HPDimid)，
1-乙基-3-甲基咪唑鎓乙基硫酸根(EMIM乙基硫酸根)，
1-乙基-3-甲基咪唑鎓双(三氟甲基磺酰基)酰亚胺(EMIMimid)，
1-乙基-2，3-二甲基咪唑鎓-双(三氟甲基磺酰基)酰亚胺(EMMIMimid)，
N-乙基-3-甲基吡啶鎓-九氟丁烷磺酸根(EMPyflat)。
该增稠剂要么是由二异氰酸酯优选2，4-二异氰酸根合甲苯、2，6-二异氰酸根合甲苯、4，4’-二异氰酸根合二苯甲烷、2，4’-二异氰酸根合二苯甲烷、4，4’-二异氰酸根合二苯、4，4’-二异氰酸根合-3，3’-二甲基二苯、4，4’-二异氰酸根合-3，3’-二甲基苯甲烷(其可单独或组合使用)与通式为R’2N-R的胺或通式为R’2N-R-N-R’2的二胺或与胺和二胺混合物的反应产物，其中R是2-22碳原子的芳基、烷基或亚烷基，R’相同或不同地是氢、烷基、亚烷基或芳基，要么选自金属皂、金属磺酸盐、金属复合皂、膨润土、硅酸盐粉、聚四氟乙烯(PTFE)、聚酰胺、聚酰亚胺。
此外，本发明的润滑脂组合物还含通常的抗腐蚀、抗氧化和用于保护免受以螯合化合物、自由基捕获剂、UV-稳定剂、反应层形成剂存在的金属影响的添加剂以及无机或有机固态润滑剂如聚酰亚胺、聚四氟乙烯(PTFE)、石墨、金属氧化物、氮化硼、二硫化钼和磷酸盐。特别是使用含磷和含硫的化合物形式的添加剂例如二烷基二硫代磷酸锌、硼酸酯作为抗磨损/极端压力添加剂，使用芳族氨基、酚、含硫化合物作为抗氧化剂，使用金属盐、酯、含氮化合物、杂环化合物作为抑制腐蚀的试剂，使用甘油单酯或甘油二酯作为防摩擦剂以及使用聚异丁烯、聚甲基丙烯酸酯作为粘度改善剂。
本发明的润滑脂组合物含5-95重量％基油混合物、1-30重量％离子液体、3-50重量％增稠剂、0.1-10重量％添加剂。
在这类润滑脂组合物情况下，该基油粘度为1.98-1650mm2/s范围，离子液体的粘度为1.98-1650mm2/s范围。
此外，该润滑脂组合物的滴点根据DIN ISO 2176为＞180℃，且根据DIN 51825其适于达-60℃的使用温度。
根据DIN 51285，该润滑脂组合物适合用于高于120℃直至260℃的高使用温度和-60℃的低使用温度。根据DIN 51825，也可用于高于180℃
的高使用温度和低达-60℃的低使用温度。
令人意外的是，通过上述组分的组合得到这样的润滑剂组合物，其由于几乎不存在离子液体的挥发，所以由于延迟粘度增加并由此延迟润滑剂的涂漆/硬化而具有更长使用寿命。此外，通过使用离子液体可得到这样的润滑剂组合物，其可燃性下降，对氧化和热影响是稳定的，可在宽的范围呈液态使用，其有可忽略的蒸气压和可用合适的方法调节其粘度。
因为在高温占主导地位且达长的运行时间的滚动轴承中常使用脲基脂(Harnstofffett)，所以需使油脂适配这种应用，因为脲基脂在高温下易于硬化。这可导致内环直径为100mm或更大的滚子轴承(Rollenlager)或球轴承(Kugellager)无足够供油。该所述的硬化还可导致供再润滑用的导管不可通过，且由此不能加入新油脂或该硬化的油脂不再与新油脂混合。期望的是可应用在高温下具有较高油分离和较小硬化趋势的脲基脂。这种改进产品例如可用在瓦楞纸板制造业(Wellpappanlagenindustrie)、木材加工工业的滚动轴承和载重汽车的车轮轴承中应用。
相反，在金属皂油脂特别是锂皂脂和锂复合皂脂情况下，在较高温度下有过大的油放出
Figure G2008800206524D00061
以致尽管应用密封但所发生的油损失限制了轴承的使用寿命。
已发现，因为加入离子液体实现了上述缺点的改善。
下面的实施例表明，可使用这样的润滑脂组合物，其含脲作为增稠剂并可用于润滑具有直径至少为100mm的内环的滚子轴承或球轴承，其避免了已知的基于脲的润滑脂组合物的缺点。
这种润滑脂组合物也可用于对具有直径至少为100mm的内环的滚子轴承或球轴承的再润滑。
经证实，本发明的特别有利的润滑脂组合物实施方案是下列所述的组合物。
权利要求1的润滑脂组合物，其由79重量％的作为基油的聚-α-烯烃、17重量％的作为增稠剂的锂简单皂、4重量％的添加剂和1-30重量％的作为离子液体的丁基-甲基吡咯烷鎓-双(三氟甲基磺酰基)酰亚胺组成。
润滑脂组合物，其由73.5重量％的聚-α-烯烃、4.5重量％的脲增稠剂和15重量％的锂复合皂增稠剂、3重量％的添加剂和4重量％的固态润滑剂组成，向其中还加入1-5重量％的离子液体，该离子液体选自三己基(十四烷基)鏻-双(三氟甲基磺酰基)酰亚胺或N-乙基-3-甲基吡啶鎓-九氟丁烷磺酸盐。
在本发明应用中，由85重量％的酯混合物、7.5重量％的脲增稠剂、5重量％的添加剂混合物和2.5-10重量％的1-乙基-3-甲基咪唑鎓双-(三氟甲基磺酰基)酰亚胺组成的润滑脂组合物也是有利的。
根据本发明也可使用由84重量％的合成酯、14重量％的脲增稠剂、2重量％的添加剂和1-3重量％的1-乙基-3-甲基咪唑鎓-乙基硫酸盐组成的润滑脂组合物。
也可应用这样的润滑脂组合物，其由76重量％的合成酯和聚-α-烯烃的混合物、15重量％的脲增稠剂、9重量％的添加剂和另外的1-10重量％的丁基甲基吡咯烷鎓-双(三氟甲基磺酰基)酰亚胺组成。
本发明的润滑剂组合物要么由用双脲和/或聚脲增稠的基油与离子液体相混合并接着经高压均化器和/或三辊炼胶机均化而获得，要么由该基油与离子液体混合并在该混合物中通过原位合成聚脲或双脲化合物增稠，接着经高压均化器和/或三辊炼胶机均化而获得。
本发明将以下列实施例详述。
实施例
在实施例中只要没有另行说明，则％数据基于重量％。只要没有另行说明，剩余基油的百分比含量通过加入离子液体相应减少。
实施例1
为制备润滑脂组合物，将77重量％的作为基油的偏苯三酸酯/1，2，4，5-苯四酸酯的混合物、10重量％的作为离子液体的MPBimid、8重量％的作为增稠剂的聚脲或双脲以及5重量％的作为添加剂的防腐蚀剂、抗氧化剂和防磨损剂相混合。该离子液体在原位制备增稠剂后加到基油中，并且用高压均化器和/或三辊炼胶机或其它合适方法均化。
首先用如此制得的润滑脂组合物按DIN ISO 2137进行噪声检验，结果列于表1。
表1
SKF脂噪声检验静音+(BeQuiet+)
  静音+(BeQuiet+)检验
  脂等级：GN 1
  0％BQ1，26％BQ2，82％BQ3，99％BQ4
 静态针入度(Ruhepenetration)1/4锥，mm-1DIN ISO 2137   挤压针入度(Walkpenetration)60DT1/4锥，mm-1DIN ISO 2137   滴点℃DIN ISO 2176   流动压力-40℃DIN 51805
 64(264)   71(290)   190℃   475mbar
 耐水性3小时90℃DIN 51807第1部分   油分离7天40℃DIN 51817   油分离30小时150℃FTMS 791C 321   挥发损失24小时150℃DIN 58397T1   铜腐蚀24小时150℃DIN 51811
 0   195％   32％   3.8％   1b
上面的使用温度按DIN 51825在FAG FE-9滚动轴承检验机上，FAGFE-9检验在180℃，6000rpm，1500N，装置A进行：
L10＝73小时，
L50＝222小时，
β＝1.7，
结果表明，本发明的润滑脂组合物不仅满足滚动轴承脂的噪声检验要求和DIN-标准，而且远超过该值。
实施例2
为制备润滑脂组合物，在由79重量％和作为基油的聚-α-烯烃混合物、17重量％的作为增稠剂的锂简单皂、4重量％的添加剂组成的脂中另行加入10或30重量％的作为离子液体的MPBimid。该离子液体在原位制备锂皂脂后以低温形式混入基油中，并搅拌和均匀碾压。
表2
  试样   锂皂脂   含10％IL的锂皂脂   含30％1L的锂皂脂
  静态针入度，mm-1DIN ISO 2137   278   274   278
  挤压针入度60DT，mm-1DIN ISO 2137   286   278   298
  滴点℃DIN ISO 2176   198   197   199
  耐水性3小时，90℃   1   2   1
  油分离24小时，150℃FTMS 791C 321   6.09％   3.62％   2.45％
  挥发损失24小时，150℃   3.98％   4.15％   3.42％
表2表明，在保持其它检验参数下通过加入离子液体明显降低油分离。
分离的油(FTMS标准)经鉴定为基油，即无离子液体析出。
按上述实施例2的锂皂脂的基本配方，还进行了含较少量离子液体的其它试验，其结果列于表3。
表3
  试样   标准配方  含5％MBPimid  含2％MBPimid   含1％MBPimid
  静态针入度，mm-1DIN ISO 2137   278   264   264   274
  挤压针入度60DT，mm-1DIN ISO 2137   286   274   268   274
  油分离30小时，150℃FTMS 791C 321   10.1％   44％   46％   49％
  挥发损失24小时，150℃DIN 58397第1部分   398％   4.7％   4％   35％
在使用含1-5重量％的离子液体时，甚至当试验时间延长到30小时时也表现出降低的油分离。
实施例3
在该实施例中，按由合成烃、合成酯、芳族二异氰酸酯、脂族单胺组成的滚动轴承脂制有标准脂，其中加入10％的MBPimid在ROF-滚动轴承检验机中进行试验。用这种检验测定该受检润滑脂组合物的寿命，在滚动轴承中的润滑脂的上述使用温度在高转数和按标准在低的轴向和径向负荷下测定。使用槽形球轴承6204-2Z-C3/VM104作为检验轴承，经受轴向负荷为100N和径向负荷为200N的负荷，转数为18000min-1，温度为160℃，以及充填量为1.5cm3。已经表明，无IL的润滑脂组合物的L50值为186小时，而所述润滑脂组合物的L50为717小时。这表明用离子液体明显改进了润滑脂组合物的使用寿命。
实施例4
在此实施例中，按DIN 51350测定VKA-焊合力(Schweisskraft)。为此使用由合成酯、全氟聚醚(PFPE)、芳族二异氰酸酯以及脂族和芳族胺的混合物组成的滚动轴承脂。对下面的润滑脂组合物进行VKA-焊合力试验。
润滑脂组合物，其涉及NLGI 2-3的脂：
脂1：标准物，含全氟聚醚
脂2：标准物，不含全氟聚醚，含2.5％EMIMimid
脂3：标准物，不含全氟聚醚，含5％EMIMimid
脂4：标准物，不含全氟聚醚，含7.5％EMIMimid
脂5：标准物，不含全氟聚醚，含10％EMIMimid
表4
  润滑脂   VKA好的力(Gutkraft)/焊合力/球形帽直径
  脂1脂2脂3脂4脂5   1600N/1800N/2.6mm1500N/1600N/2.5mm2400N/2600N/3.2mm3600N/3800/3.5mm4400N/4600N/4.0mm
VKA-值的比较表明，在加入大于2.5％离子液体情况下，达到更好的VKA-值。
表5
  润滑脂   静音(BeQuiet)+   VKA好的力/焊合力/球形帽直径
  脂1脂5   GN4GN4   1600N/1800N/2.6mm4400N/4600N/4.0mm
此外还表明，在加入10％离子液体情况下，有更好的VKA值，同时有好的噪声值。
对该脂也进行FE 9滚动轴承脂-试验，在此试验中测定受检脂的寿命及在中等转数和中等轴向负荷下在滚动轴承中的润滑脂的高使用温度。使用FAG特种轴承529689H 109(对应于具有钢外壳的径向推力球轴承7206B)，具有JP2外壳，转数为6000min-1，轴向负荷1500N，温度200℃和充填量为2cm3。该受检润滑脂以及L10值和L50值的结果列于表6。
表6
  润滑脂   脂配方   FE 9 200℃
  脂1   标准物，含全氟聚醚   L10：10hL50：13h
  脂3   标准物，不含PFPE+5％EMIMimid   L10：8hL50：25h
  脂5   标准物，不含PFPE+10％EMIM imid   L10：63hL50：80h
  脂6   标准物，不含PFPE+10％MBPimid   L10：45hL50：55h
  脂7   标准物，不含PFPE+10％EMMIMimid   L10：16hL50：72h
该表表明，通过加入离子液体使该脂有较长的运行时间，如与含全氟聚醚但不含离子液体的脂1所得的值相比看出。
曾对另一润滑脂组合物进行FAG FE 9试验，在该不含PFPE的脂中加有10％的HDPimid(脂8)。得到下列的运行时间L10：66h，L50：101h和β：4.4。该结果表明，本发明的润滑脂组合物满足滚动轴承脂按DIN-标准对于达200℃的使用温度的要求。
实施例5
在此实施例中，VKA-焊合力按DIN 51350测定。为此使用由合成酯、芳族二异氰酸酯和脂族胺组成的滚动轴承脂作为标准组合物。对下面的润滑脂组合物进行VKA-焊合力试验。
润滑脂组合物，其涉及NLGI 2-3脂：
脂1：标准物，无IL
脂2：标准物，加有5％的EMIMimid，(油替代)
脂3：标准物，加有10％的EMIMimid，(油替代)
表7
  润滑脂   VKA好的力/焊合力/球形帽直径
  脂1脂2脂3   ＜1200N1400N/1600N/2.5mm3800N/4000N/3.5mm
表7表明，该焊合力有改进，在脂中使用IL得到更好的VKA-值。
表8
  润滑脂  静音+(BeQuiet+)   VKA好的力/焊合力/球形帽直径
  脂1脂3   GN4GN4   ＜1200N3800N/4000N/3.5mm
在同样好的噪声值下有更好的VKA-值(使用10％的IL)。
此检验，通过加入离子液体是否可在温度负荷下阻止脂硬化。
在160℃的温度负荷下使用所谓的“铝皿试验()”。为此首先测量尚未加负荷的脂的粘度。在直径约50mm，深约15mm的铝皿中，将待检脂尽可能均匀和平坦地涂抹到不大于皿深的3/4。接着用合适的盖封闭该皿。再将该封闭的皿置于炉口挡板上，并使其在炉中经受高温负荷。以周间隔测量该脂的粘度。
该表观动态粘度在300s-1；25℃测量。
对下列润滑脂组合物进行试验。
脂1：标准配方，无IL
脂5：加1％的EMIM乙基硫酸盐
脂6：加3％的EMIM乙基硫酸盐
脂7：加5％的EMIM乙基硫酸盐
表9
  新鲜的   1周   2周   3周
  脂1脂5脂6脂7   2794331233203348   55452000不可测不可测   45481842   46501425
该表观动态粘度值的单位为mPas。
加1％的EMIM乙基硫酸盐时该油脂较软，加3％的EMIM乙基硫酸盐时该油脂非常不均匀(不可测)，加5％时完全“相互分开沉降”(不可测)。
明显看出，通过加入1％的EMIM乙基硫酸盐时该材料在温度负荷下保持柔性。在加入大于1％的IL时，可证实在温度负荷方面无改进。
实施例6
在该实施例中试验了加入离子液体对车轮轴承脂的改进。特别是用于载重汽车的车轮轴承脂不仅在热负荷方面而且在载荷上均有高的要求。如果该汽车例如从山道驶离时总是必须不断制动时，会产生特别高的热负荷。为模拟这种要求，进行FE 8滚动轴承-试验，其特征是周期性的温度交替。
作为该试验的基础润滑脂，使用由聚-α-烯烃、芳族二异氰酸酯、由脂族和芳族胺得到的混合物和锂复合皂(标准物)组成的组合物。
使用下列润滑脂组合物：
脂1：标准配方
脂2：标准物加5％HDPimid
对这些润滑脂组合物进行下面表10中所示的检验。
表10
  润滑脂   静态针入度，mm-1   挤压针入度60DT，mm-1   耐水性   流动压力，mbar
  脂1脂2   223223   226223   00   11251075
  润滑脂   油分离7天40℃   油分离30小时150℃
  脂1脂2   0.54％0.57％   2.85％5.42％
其中加有5％HDPimid的脂有更高的油分离。
为检测硬化，进行了上述的封盖铝皿试验。
粘度测量在160℃进行，其值以mPas表示。
表11
  新鲜的   5天   12天   19天   25天   35天
 脂1脂2   99569395   80147522   86195492   87715717   10,2768817   12,2438508
对所有试样均可测量表观粘度，在表观图案中该标准脂比含IL的脂更干燥。
含IL的样品表现出粘度下降，并且比变得不含IL的样品更软，不含IL的样品是更硬的。
这导致在FE 8滚动轴承试验中的运行时间增长。在这些试验中，根据DIN 51819测定了在轴承中的摩擦力矩曲线和温度曲线以及滚动轴承组件的磨损。周期性的交变温度在对应于通常运行的130℃和对应于从山道驶离的170℃之间交变。
标记为脂1的不含IL的组合物表现出高的磨损和215小时的短运行时间，在170℃的第二温度阶段中必须中断检验过程，该材料产生如此大的固有热量，以致需接通风扇。
标记为脂2加有5％HDPimid的润滑脂组合物的试验表明有较少的磨损和377小时的较长运行时间，其可以170℃温度运行5个循环。该检验机曾故意关闭，继续运行是有可能的。该材料仅导致低的固有热量，其需要被加热。
用下列润滑脂组合物进行进一步的试验，结果列于表12和13。
脂1：标准配方(实施例6)，不含IL
脂3：标准物加1％HDPimid
脂4：标准物加2％HDPimid
脂5：标准物加3％HDPimid
脂6：标准物加1％N-乙基-3-甲基吡啶鎓-九氟丁烷磺酸盐
脂7：标准物加2％N-乙基-3-甲基吡啶鎓-九氟丁烷磺酸盐
脂8：标准物加3％N-乙基-3-甲基吡啶鎓-九氟丁烷磺酸盐
表12
  润滑脂   静态针入度，mm-1   挤压针入度60DT，mm-1   挥发损失24小时150℃   油分离30小时150℃
  脂1脂3脂4脂5脂6脂7脂8   223234219204208204211   226238219219211215208   2.2％2.67％2.44％2.14％3.26％3.4％3.18％   2.85％3.5％3.94％4.59％8.35％10.03％9.6％
含IL的样品表现出高的油分离。也可通过所用离子液体的类型和量调节油分离的程度。
表13
粘度测量，160℃负荷；值以mPas表示：
  新鲜的   1周   2周   3周
  脂1脂3脂4脂5脂6脂7脂8   995694689477942410,20697849637   7379697462836784685268326601   8561453257684294530465886734   14,920727669916240710975667639
该实施例表明，通过离子液体可明显提高用于载重汽车的车轮轴承脂的性能。
上面的这些实施例表明，在基于工业润滑剂的油中加入离子液体具有有利的作用。

Claims (12)

1.润滑脂组合物，其由下面组分的混合物组成：
(a)5-95重量％的基于具有针对工业润滑剂的通常粘度的油的基油，其由芳香族或脂族的二、三或四羧酸与一种或以混合物形式存在的C7-C22-醇的酯，由三羟甲基丙烷、季戊四醇或二季戊四醇与脂族C7-C22-羧酸的酯，由C18-二聚酸与C7-C22-醇的酯，由复合酯组成，作为单组分或以任意混合物的形式，或选自聚-α-烯烃，
(b)1-10重量％的离子液体或数种离子液体的混合物，所述离子液体选自
丁基甲基吡咯烷
Figure FSB00000955626600011
-双(三氟甲基磺酰基)酰亚胺，
三己基(十四烷基)
Figure FSB00000955626600012
-双(三氟甲基磺酰基)酰亚胺，
1-乙基-3-甲基咪唑-乙基硫酸盐，
1-乙基-3-甲基咪唑
Figure FSB00000955626600014
-双(三氟甲基磺酰基)酰亚胺，和
N-乙基-3-甲基吡啶
Figure FSB00000955626600015
-九氟丁烷磺酸盐
(c)3-50重量％的增稠剂，其选自由二异氰酸酯优选2，4-二异氰酸根合甲苯、2，6-二异氰酸根合甲苯、4，4’-二异氰酸根合二苯甲烷，其可单独地或以组合形式使用，与通式为R’2N-R的胺的反应产物，其中R是2-22个碳原子的芳基、烷基或亚烷基，R’相同或不同地是氢、烷基、亚烷基或芳基，或选自金属皂、金属复合皂，和
(d)0.1-10重量％的常规添加剂，单独地或以组合形式，选自防腐蚀剂、抗氧化剂、防磨损剂、降低摩擦的试剂、抗金属影响的试剂、UV-稳定剂、无机或有机固态润滑剂，选自聚酰亚胺、聚四氟乙烯(PTFE)、石墨、金属氧化物、氮化硼、二硫化钼和磷酸盐。
2.权利要求1或2的润滑脂组合物，其由79重量％的作为基油的聚-α-烯烃、17重量％的作为增稠剂的锂简单皂、4重量％的添加剂和另外1-30重量％的作为离子液体的丁基甲基吡咯烷
Figure FSB00000955626600016
-双(三氟甲基磺酰基)酰亚胺组成。
3.权利要求1的润滑脂组合物，其由73.5重量％的聚-α-烯烃、4.5重量％的脲增稠剂、15重量％的锂复合皂增稠剂、3重量％的添加剂、4重量％的固态润滑剂和1-5重量％的离子液体组成，其中该离子液体是三己基(十四烷基)
Figure FSB00000955626600017
-双(三氟甲基磺酰基)酰亚胺或N-乙基-3-甲基吡啶-九氟丁烷磺酸盐。
4.权利要求1的润滑脂组合物，其由85重量％的酯混合物、7.5重量％的脲增稠剂、5重量％的添加剂和2.5-10重量％的1-乙基-3-甲基咪唑-双(三氟甲基磺酰基)酰亚胺组成。
5.权利要求1的润滑脂组合物，其由84重量％的合成酯、14重量％的脲增稠剂、2重量％的添加剂和1-3重量％的1-乙基-3-甲基咪唑
Figure FSB00000955626600022
-乙基硫酸盐组成。
6.权利要求1的润滑脂组合物，其由76重量％的合成酯和聚-α-烯烃的混合物、15重量％的脲增稠剂、9重量％的添加剂和1-10重量％的丁基甲基吡咯烷
Figure FSB00000955626600023
-双(三氟甲基磺酰基)酰亚胺组成。
7.权利要求1-6之一的润滑脂组合物，其中该基油粘度为1.98-1650mm2/s，离子液体的粘度为1.98-1650mm2/s。
8.权利要求1-6之一的润滑脂组合物，其中按DIN ISO2176滴点为＞180℃，按DIN51825其适于达-60℃的使用温度。
9.权利要求1-8之一的润滑脂组合物，根据DIN51825，在高于120℃直至260℃的高使用温度和达-60℃的低使用温度使用。
10.权利要求1-9之一的润滑脂组合物，根据DIN51825，在高于180℃直至260℃的高使用温度和达-60℃的低使用温度使用。
11.权利要求1的润滑脂组合物，其含作为增稠剂的脲，并用于润滑内环直径至少为100mm的滚子轴承或球轴承。
12.权利要求1的润滑脂组合物，其含脲，并用于再润滑内环直径至少为100mm的滚子轴承或球轴承。
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CA2687149A1 (en) 2008-12-24
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