CN107406793B - 润滑脂组合物 - Google Patents

润滑脂组合物 Download PDF

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CN107406793B
CN107406793B CN201680015980.XA CN201680015980A CN107406793B CN 107406793 B CN107406793 B CN 107406793B CN 201680015980 A CN201680015980 A CN 201680015980A CN 107406793 B CN107406793 B CN 107406793B
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oil
grease composition
grease
trimellitate
mass
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CN107406793A (zh
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井上正晴
渡边一弘
井筒智善
川村隆之
天利裕行
长谷川稔
中野康平
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NTN Corp
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Abstract

本发明的目的在于提供能够满足高温耐久性·低温性·耐剥离性·防锈性的全部特性的外轮旋转用的滚动轴承用润滑脂组合物。被封在汽车电装辅机中使用的外轮旋转用滚动轴承中的润滑脂组合物(7)，其特征在于，含有基油、增稠剂、耐剥离添加剂、耐磨损添加剂和防锈剂，基油为偏苯三酸酯油与合成烃油的比例为以质量比计偏苯三酸酯油：合成烃油＝(70：30)～(90：10)的混合油，增稠剂为由式(1)表示的二脲化合物。式中，R2表示碳数6～15的2价芳香族烃基，R1表示环己基。R1‑NHCONH‑R2‑NHCONH‑R1 (1)。

Description

润滑脂组合物
技术领域
本发明涉及在汽车电装辅机中使用的外轮旋转用的滚动轴承用润滑脂。
背景技术
近年来，就汽车部件而言，为了提高燃油效率、扩大室内空间，正在推进肃静化·小型化·轻质化。随着肃静化发动机室的密闭化推进，要求汽车电装辅机中使用的滚动轴承用润滑脂的高温耐久性。另外，由于通过高速旋转来弥补小型化导致的输出功率降低，因此在高速旋转并且高负荷下使用滚动轴承。随着这样的使用环境的严酷化，报道了在滚动面伴有白色纹理变化的轴承的剥离现象、所谓的氢脆性剥离，对于润滑脂要求氢脆性剥离的对策。另外，在俄罗斯、北美等寒冷地区，发动机起动时产生的异常声音、所谓的冷时异常声音成为了问题，对于润滑脂也要求低温性的进一步提高。进而，由于在行驶中也会遇到雨水，因此对于润滑脂也要求防锈性。从这样的背景出发，对于润滑脂要求满足高温耐久性·耐剥离性·低温性·防锈性的全部性能。
作为汽车电装辅机的轴承用润滑脂，使用了合成烃油·烷基二苯醚油·酯系合成油等基油的润滑脂是主流，但如果是以合成烃油作为主要成分的润滑脂，则高温耐久性不足。另外，如果是以烷基二苯醚油作为主要成分的润滑脂，则低温性不足。另外，如果是将酯系合成油用于基油的润滑脂，则有时耐热性和低温性的兼备变得困难。
作为高温耐久性优异的润滑脂，已知使用了酯系合成油的二脲润滑脂(专利文献1)。另外，作为低温性优异的润滑脂，已知使用了三羟甲基丙烷或季戊四醇酯系合成油与合成烃油的混合油的二脲润滑脂(专利文献2)。
作为耐氢脆性剥离性(以下也称为耐剥离性)优异的润滑脂，已知配合了钼酸盐的二脲润滑脂(专利文献3)。
作为防锈性和耐剥离性优异的润滑脂，已知配合了环烷酸锌和烯基琥珀酸半酯的二脲润滑脂(专利文献4)。
但是，专利文献1至专利文献4中记载的各润滑脂虽然高温耐久性、低温性、耐剥离性或者防锈性中的个别的特性优异，但没有得到满足这些全部性能的润滑脂。随着汽车部件的肃静化·小型化·轻质化推进，就这些汽车部件中所使用的轴承、特别是外轮旋转用的滚动轴承中使用的润滑脂组合物而言，需要不只是单一的性能而是同时满足全部性能的润滑脂组合物。
现有技术文献
专利文献
专利文献1：日本特开2013-253257号公报
专利文献2：日本专利第4427195号公报
专利文献3：日本特开2009-299897号公报
专利文献4：日本专利第4877343号公报
发明内容
发明要解决的课题
本发明的目的在于提供能够满足高温耐久性·低温性·耐剥离性·防锈性的全部特性的外轮旋转用的滚动轴承用润滑脂组合物。
用于解决课题的方案
本发明的润滑脂组合物是被封在汽车电装辅机中使用的外轮旋转用滚动轴承中的润滑脂组合物。其特征在于，该润滑脂组合物含有基油、增稠剂、耐剥离添加剂、耐磨损添加剂和防锈剂，上述基油为偏苯三酸酯油与合成烃油的比例为以质量比计上述偏苯三酸酯油：上述合成烃油＝(70：30)～(90：10)的混合油，上述增稠剂为由下述式(1)表示的二脲化合物。
[化1]
R1-NHCONH-R2-NHCONH-R1 (1)
式中，R2表示碳数6～15的2价芳香族烃基，R1表示环己基。
其特征在于，构成混合基油的上述偏苯三酸酯油在40℃下的运动粘度为40～140mm2/s，倾点为-35℃以下，上述合成烃油在40℃下的运动粘度为10～60mm2/s，倾点为-50℃以下。
另外，其特征在于，上述耐剥离添加剂为选自钼酸钠、钼酸钾和钼酸锂中的至少1种的钼酸碱金属盐，相对于润滑脂组合物总量，含有0.1～1.5质量％的上述耐剥离添加剂。
另外，其特征在于，上述耐磨损添加剂为二烷基二硫代磷酸锌，相对于润滑脂组合物总量，含有0.1～2.0质量％的上述耐磨损添加剂。
另外，其特征在于，上述防锈剂以环烷酸锌作为必要成分，相对于润滑脂组合物总量，含有0.5～5.0质量％的上述防锈剂。
发明效果
本发明的润滑脂组合物作为被封在汽车电装辅机中使用的外轮旋转用滚动轴承中的润滑脂组合物，以高水平满足高温耐久性·低温性·耐剥离性·防锈性的全部，即使在-40℃的低温环境下也抑制冷时异常声音的发生，即使在180℃的高温环境下也显示出优异的耐久性，并且即使在严酷的使用条件下也能够抑制氢脆性剥离。
附图说明
图1为表示封入了本发明的润滑脂组合物的滚动轴承的图。
具体实施方式
作为在汽车电装辅机中使用的轴承，可列举出在风扇耦合装置、交流发电机、空转轮、汽车空调用电磁离合器、电动风扇电机等中使用的滚动轴承。在这些轴承中有在外轮旋转下被使用的外轮旋转用滚动轴承，除了以往的电装辅机用轴承中所封入的润滑脂组合物所要求的高温耐久性·低温性·耐剥离性以外，对于在外轮旋转用滚动轴承中所封入的润滑脂组合物还要求防锈性。
对于构成本发明的润滑脂组合物的必要的成分，以下进行说明。
(1)基油
基油为偏苯三酸酯油与合成烃油的混合油。偏苯三酸酯油在高温下的蒸发损失少，氧化稳定性优异。另外，合成烃油的低温性优异。就偏苯三酸酯油与合成烃油的比例而言，以质量比计，为偏苯三酸酯油：合成烃油＝(70：30)～(90：10)。即，相对于混合油总量，偏苯三酸酯油为70～90质量％，余量为合成烃油，合成烃油为30～10质量％。如果混合油的比例在该范围外，则不能满足高温耐久性·低温性·耐剥离性·防锈性的全部特性。
偏苯三酸酯油优选为由下述式(2)表示、40℃下的运动粘度为40～140mm2/s、倾点为-35℃以下的偏苯三酸三酯油。
[化2]
Figure BDA0001408697670000041
式(2)中，R3、R4、R5可以相同也可以不同。优选相同。另外，R3、R4、R5优选为碳数7～10的脂肪族1元醇残基。该脂肪族1元醇残基可以为直链状烷基，也可为支链状烷基。具体地，可列举出偏苯三酸三(2-乙基己基)酯、偏苯三酸三(正辛基)酯、偏苯三酸三(异壬基)酯、偏苯三酸三(异癸基)酯等。
合成烃油为由碳和氢的化合物组成的烃化合物，可列举出聚α-烯烃油、α-烯烃与烯烃的共聚物、聚丁烯等脂肪族系烃油、烷基苯、烷基萘、聚苯、合成环烷烃等芳香族系烃油等。这些中，如果考虑低温性，则优选聚α-烯烃油。在聚α-烯烃油中特别优选的是40℃下的运动粘度为10～60mm2/s、倾点为-50℃以下的聚α-烯烃油。如果运动粘度超过60mm2/s，则低温性差，如果低于10mm2/s，则耐热性差。另外，如果倾点比-50℃高，则低温性差。
(2)增稠剂
增稠剂为剪切稳定性、高温耐久性优异的由上述式(1)表示的二脲化合物。R2为碳数6～15的2价芳香族烃基。如果碳数低于上述范围，则润滑脂的增稠性差，如果超过上述范围，则润滑脂变得容易固化。作为R2，例如可列举出芳香族单环、芳香族稠环、将这些单环或稠环用亚甲基链、氰脲酸环、异氰脲酸环等连接而成的基团等，作为优选的芳香族烃基，可列举出由以下的式(3)表示的各个基团。
[化3]
Figure BDA0001408697670000051
作为这些基团中优选的基团的具体例，可列举出由以下的式(4)表示的各个基团。
[化4]
Figure BDA0001408697670000052
二脲化合物可通过使二异氰酸酯化合物与单胺化合物反应而得到。就润滑脂而言，可在上述基油中使二异氰酸酯化合物与单胺化合物反应，另外，也可将预先合成的二脲化合物与基油混合。优选的制作方法为容易保持润滑脂的稳定性的前者的方法。
就增稠剂的配合量而言，相对于润滑脂总量，优选5～25质量％，如果低于5质量％，则润滑脂软，有可能从轴承泄漏，如果超过25质量％，则润滑脂硬，有可能发生冷时异常声音。
(3)耐剥离添加剂
耐剥离添加剂为选自钼酸钠、钼酸钾和钼酸锂中的至少1种的钼酸碱金属盐。优选为钼酸钾。
就耐剥离添加剂的配合量而言，相对于润滑脂组合物总量，优选0.1～1.5质量％。更优选为0.6～1.2质量％。如果耐剥离添加剂的配合量低于0.1质量％，则得不到充分的耐剥离性，如果超过1.5质量％，则有可能发生冷时异常声音。
(4)耐磨损添加剂
使高温耐久性提高的耐磨损添加剂为由下述式(5)表示的二烷基二硫代磷酸锌(ZnDTP)。
[化5]
Figure BDA0001408697670000061
式中的R6表示碳原子数1～24的伯或仲烷基、或者、碳原子数6～30的芳基。作为R6，例如可列举出甲基、乙基、丙基、异丙基、丁基、仲丁基、异丁基、戊基、4-甲基戊基、己基、2-乙基己基、庚基、辛基、壬基、癸基、异癸基、十二烷基、十四烷基、十六烷基、十八烷基、二十烷基、二十二烷基、二十四烷基、环戊基、环己基、甲基环己基、乙基环己基、二甲基环己基、环庚基、苯基、甲苯基、二甲苯基、乙基苯基、丙基苯基、丁基苯基、戊基苯基、己基苯基、庚基苯基、辛基苯基、壬基苯基、癸基苯基、十二烷基苯基、十四烷基苯基、十六烷基苯基、十八烷基苯基、苄基等。应予说明，这些的各R6可以相同，也可不同。
这些中，从稳定性优异、也有助于防止氢脆性导致的滚动面的剥离出发，优选R6为伯烷基。另外，在R6为烷基的情况下，碳原子数越多，耐热性越优异，另外，容易在基油中溶解。另一方面，碳原子数越少，耐磨损性越优异，难以在基油中溶解。作为适于本发明的市售品，例如可列举出Lubrizol公司制造：商品名BECROSAN9045等。
就配合量而言，相对于润滑脂组合物总量，优选为0.1～2.0质量％。如果低于0.1质量％，则得不到充分的效果，如果超过2.0质量％，则使防锈性、高温耐久性降低。
(5)防锈剂
防锈剂以环烷酸锌作为必要成分。优选相对于防锈剂总量，含有10质量％以上的环烷酸锌的防锈剂。更优选单独使用环烷酸锌。
就防锈剂的配合量而言，相对于润滑脂组合物总量，以环烷酸锌计，优选为0.5～5.0质量％。如果低于0.5质量％，则防锈性降低，如果超过5.0质量％，则使高温耐久性降低。
作为能够与环烷酸锌并用的防锈剂，例如能够例示以下的化合物。有机磺酸的铵盐、钡、锌、钙、镁等碱金属、碱土类金属的有机磺酸盐、有机羧酸盐、酚盐、膦酸酯(盐)、烷基或烯基琥珀酸酯等烷基、烯基琥珀酸衍生物、山梨糖醇酐单油酸酯等多元醇的部分酯、油酰肌氨酸等羟基脂肪酸类、1-巯基硬脂酸等巯基脂肪酸类或其金属盐、硬脂酸等高级脂肪酸类、异硬脂醇等高级醇类、高级醇与高级脂肪酸的酯、2,5-二巯基-1,3,4-噻二唑、2-巯基噻二唑等噻唑类、2-(癸基二硫代)-苯并咪唑、苯并咪唑等咪唑系化合物、或者2,5-双(十二烷基二硫代)苯并咪唑等二硫化物系化合物、或者亚磷酸三(壬基苯基)酯等磷酸酯类、二月桂基硫代丙酸酯等硫代羧酸酯系化合物。
另外，根据需要，能够使用抗氧化剂、极压剂、油性剂、增粘剂、金属钝化剂、表面活性剂等公知的添加剂作为其他添加剂。
作为本发明的润滑脂组合物的使用方式，对于封入了该润滑脂组合物的滚动轴承，根据图1进行说明。图1为润滑脂封入轴承(深沟球轴承)的截面图。就润滑脂封入轴承1而言，将在外周面具有内轮滚动面2a的内轮2与在内周面具有外轮滚动面3a的外轮3同心地配置，在内轮滚动面2a与外轮滚动面3a之间配置了多个滚动体4。设置了保持该多个滚动体4的保持器5。另外，被固定于外轮3等的密封构件6分别设置于内轮2和外轮3的轴方向两端开口部8a、8b。至少在滚动体4的周围封入上述的本发明的润滑脂组合物7。外轮旋转用的情况下，在内轮2固定的状态下外轮3旋转。
实施例
实施例1～3和比较例1～7
以表1中所示的配合比例制备了基油，该基油由作为偏苯三酸酯油的偏苯三酸三(异壬基)酯(40℃下的运动粘度：90mm2/s，倾点：-38℃)与作为合成烃油的聚α-烯烃油(40℃下的运动粘度：30mm2/s、倾点：-55℃)的混合油构成。应予说明，比较例5～7中所示的多元醇酯油使用了40℃下的运动粘度：71mm2/s、倾点：-48℃的特性的商品名ハトコールH3144。另外，二烷基二硫代磷酸锌使用了Lubrizol公司制、商品名BECROSAN9045，环烷酸锌系防锈剂使用了CHELEST公司制、商品名キレスガードC，酯系防锈剂使用了日油社制、商品名ノニオンOP-80R，磺酸盐系防锈剂使用了MORESCO公司制、商品名スルホールCa-45N，胺系抗氧化剂使用了VANDERBILT公司制、商品名VANLUBE81，酚系抗氧化剂使用了BASF公司制、商品名IRGANOX L101。
将上述混合基油分成两份液体，在其一半量中溶解4,4'-二苯基甲烷二异氰酸酯，在剩余的一半量的混合基油中溶解环己胺(以4,4'-二苯基甲烷二异氰酸酯的摩尔比计，为2倍当量)。予以说明，相对于混合基油总量，以成为表1中所示的配合比例的方式，溶解了作为脂环族二脲化合物的4,4'-二苯基甲烷二异氰酸酯和环己胺。边搅拌溶解了4,4'-二苯基甲烷二异氰酸酯的溶液，边加入了环己胺溶液，之后在100～120℃下持续搅拌30分钟，使其反应，向基油中配合了脂环族二脲化合物。以表1中所示的配合比例将表1中所示的配合剂加入其中，进而在100～120℃下搅拌了10分钟。然后冷却，用三联辊进行均质化，得到了润滑脂组合物。评价了该润滑脂组合物的各种性能。以下示出试验方法和试验条件。另外，将结果示于表1中。
(1)混和稠度
根据JIS K 2220测定。
(2)高温耐久性(按照ASTM D 3336)
如以下所示地，通过内轮旋转在高温环境下使封入了润滑脂的滚动轴承旋转，测定了直至滚动轴承达到寿命的时间。
Figure BDA0001408697670000081
(3)冷时异常声音性
如以下所示地，通过外轮旋转在低温环境下使封入了润滑脂的滚动轴承旋转，通过基于同一试验者的听觉来评价有无冷时异常声音的产生，将没有产生冷时异常声音的次数相对于全部试验次数的比例作为合格率进行了评价。
Figure BDA0001408697670000091
(4)低温扭矩
根据JIS K 2220，分别测定了-40℃下的起动扭矩、旋转扭矩。
(5)氢脆性剥离性
通过外轮旋转使封入了润滑脂的滚动轴承急加减速，将没有发生氢脆性剥离的次数相对于全部试验次数的比例作为合格率进行了评价。
Figure BDA0001408697670000092
(6)轴承防锈性
将涂布了润滑脂的圆锥滚子轴承在1质量％的盐水中浸渍10秒，在高湿环境下使其静置。试验后将轴承取出，通过目视观察外轮滚动面。就评价而言，将外轮滚动面分割为32个区块，根据其中哪些区块中生了锈算出了生锈率。
Figure BDA0001408697670000093
Figure BDA0001408697670000101
[表1]
Figure BDA0001408697670000102
实施例1～3满足了高温耐久性·低温性·耐剥离性·防锈性的全部性能。另一方面，比较例1～4由于没有使用合成烃油，因此低温性差，有发生冷时异常声音的风险。另外，比较例1的耐剥离添加剂的添加量少，氢脆性剥离的合格率低。比较例4的防锈剂不适当，防锈性差。进而，关于比较例5～7，由于大量包含合成烃油，因此高温耐久性差。
产业上的可利用性
本发明的润滑脂组合物由于满足高温耐久性·低温性·耐剥离性·防锈性的全部性能，因此能够适宜地作为要求更高的性能的汽车电装辅机中所使用的外轮旋转用滚动轴承用润滑脂组合物利用。
附图标记的说明
1 润滑脂封入轴承
2 内轮
3 外轮
4 滚动体
5 保持器
6 密封构件
7 润滑脂组合物
8a、8b 开口部

Claims (2)

1.润滑脂组合物，是被封在汽车电装辅机中使用的外轮旋转用滚动轴承中的润滑脂组合物，其特征在于，所述润滑脂组合物含有基油、增稠剂、耐剥离添加剂、耐磨损添加剂和防锈剂，所述基油是偏苯三酸酯油与合成烃油的比例为以质量比计所述偏苯三酸酯油：所述合成烃油＝(70：30)～(90：10)的混合油，所述增稠剂为由下述式(1)表示的二脲化合物，
所述偏苯三酸酯油在40℃下的运动粘度为40～140mm2/s，倾点为-35℃以下，所述合成烃油在40℃下的运动粘度为10～60mm2/s，倾点为-50℃以下，
所述耐剥离添加剂为选自钼酸钠、钼酸钾和钼酸锂中的至少1种的钼酸碱金属盐，相对于润滑脂组合物总量，含有0.1～1.5质量％，
所述耐磨损添加剂为二烷基二硫代磷酸锌，相对于润滑脂组合物总量，含有0.1～2.0质量％，
[化1]
R1-NHCONH-R2-NHCONH-R1 (1)
式中，R2表示碳数6～15的2价芳香族烃基，R1表示环己基。
2.权利要求1所述的润滑脂组合物，其特征在于，所述防锈剂以环烷酸锌作为必要成分，相对于润滑脂组合物总量，含有0.5～5.0质量％。
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