CN104053757A - 润滑脂组合物及轴承 - Google Patents
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Abstract
本发明提供一种润滑脂组合物,包含:(a)基油、(b)增稠剂、(c)由式(1)表示的具有烷基硫代氨基甲酰基的化合物、(d)受阻酚系抗氧化剂以及(e)金属钝化剂。式中,R1、R2、R3、R4表示独立且碳原子数为1~20的烷基,X表示S、S-S、S-CH2-S、S-CH2CH2-S或者S-CH2CH2CH2-S。
Description
技术领域
本发明涉及含有基油、增稠剂、特定抗氧化剂以及金属钝化剂的润滑脂组合物。更详细地,涉及适合使用于高温条件中的滚动轴承且润滑寿命提高的润滑脂组合物以及封入其的轴承。
背景技术
应对近年的高速化、节能化、低噪音化、低维护化的要求,在铁路车辆、汽车、电机、各种产业机械等中使用的发动机正推进小型轻量化、高旋转化、高效率化、长寿命化。伴随小型轻量化,润滑剂的使用量减少,而且高旋转化导致使用温度的上升等,使润滑剂的使用环境变得更加恶劣。特别在铁路车辆用主电动机中,由于噪音问题、维护周期延长的要求,正在推进发动机的全封闭化,与以往的开放型相比,由于冷却效率变差,因此需要更加耐热、长寿命的润滑脂。
因此,提出有关润滑脂组合物的性能提高的种种提案。
提案了一种润滑脂,其通过在基油、增稠剂中含有具有烷基硫代氨基甲酰基的化合物以及胺酮缩聚物系抗氧化剂,使高温条件下的滚动轴承的润滑寿命提高(专利文献1)。
提案了一种疲劳寿命改良润滑剂,其通过向润滑基材中添加具有烷基硫代氨基甲酰基的化合物以及钼化合物,或者进一步添加酯类化合物来改良疲劳寿命(专利文献2)。
此外,提案了一种改良抗氧化性的抗磨损性极压组合物,其由(a)亚甲基双(二正丁基二硫代氨基甲酸酯)以及(b)甲苯三唑或苯并三唑的二苯胺衍生物构成,且(a):(b)的质量%为约4:1~约50:1的范围,并提案了包含其的润滑剂(例如,参照专利文献3)。
进一步地,提案了一种锂润滑脂组合物,其含有(a)润滑油、(b)选自由含有至少1个羟基且碳原子数为12~24的脂肪族单羧酸的锂盐、碳原子数为2~12的脂肪族二羧酸的二锂盐以及碳原子数为12~24的脂肪族单羧酸锂盐组成的组中的至少1种的化合物以及(c)选自由3-(N-水杨酰基)氨基-1,2,4-三唑以及十亚甲基-二羧酸-二水杨酰肼(decamethylene-dicarboxylic acid-disalicyloylhydrazide)组成的组中的1种化合物(例如,专利文献4)。
然而,现状是即使将这些使用添加剂的润滑脂组合物用于高温条件中的滚动轴承,热氧化稳定性以及润滑寿命也不充分,还未能得到用户满意的产品。
现有技术文献
专利文献
专利文献1:日本特开2007-238755号公报
专利文献2:日本特公平03-31760号公报
专利文献3:日本特表2005-509732号公报
专利文献4:日本特许第2936084号公报
发明内容
发明所要解决的课题
作为热氧化稳定性优异的润滑脂,将分子内不含金属的脲类化合物作为增稠剂并将合成油作为基油的润滑脂通常用于主要使用深槽球轴承的汽车电装辅机中,在将其用于必须使用圆柱滚子轴承(roller bearing)的铁路车辆用主电动机的情况中,不能得到充分的润滑寿命。
本发明的目的是提供适合高温条件中的滚动轴承,而且长时间表现出稳定的润滑性的润滑脂组合物。即,提供热氧化稳定性以及润滑寿命优异的润滑脂组合物。
本发明的其他目的是提供封入上述润滑脂组合物的轴承。
解决课题的手段
为了实现上述目的,本发明人深入研究的结果是,通过使用基油、增稠剂、特定的抗氧化剂以及金属钝化剂,完成改善热氧化稳定性以及润滑寿命,适合高温下的滚动轴承,并且长时间表现出稳定润滑性的润滑脂组合物。
本发明提供如下所示的润滑脂组合物以及轴承。
[1]一种润滑脂组合物,其特征在于,含有(a)基油、(b)增稠剂、(c)由式(1)表示的具有烷基硫代氨基甲酰基的化合物、(d)受阻酚系抗氧化剂以及(e)金属钝化剂。
[化学式1]
式中R1、R2、R3、R4表示独立且碳原子数为1~20的烷基,X表示S、S-S、S-CH2-S、S-CH2CH2-S或者S-CH2CH2CH2-S。
[2]如[1]所述的润滑脂组合物,(d)受阻酚系抗氧化剂是2,6-二叔丁基-4-甲酚。
[3]如[1]或[2]所述的润滑脂组合物,(e)金属钝化剂是十亚甲基羧酸二水杨酰肼(decamethylenecarboxylic acid-disalicyloyl hydrazide)。
[4]如[1]~[3]中任一项所述的润滑脂组合物,(a)基油是多元醇酯油和烷基二苯醚油的混合油。
[5]如[1]~[4]中任一项所述的润滑脂组合物,(b)增稠剂选自由锂皂和复合锂皂组成的组中的至少一种。
[6]如[1]~[5]中任一项所述的润滑脂组合物,相对于润滑脂组合物整体,含有50质量%以上的(a)基油、1~30质量%的(b)增稠剂、0.1~10质量%的(c)由式(1)表示的具有烷基硫代氨基甲酰基的化合物、0.1~10质量%的(d)受阻酚系抗氧化剂、0.1~10质量%的(e)金属钝化剂。
[7]一种轴承,其封入如[1]~[6]中任一项所述的润滑脂组合物。
发明效果
本发明的润滑脂组合物由于具有改善的热氧化稳定性以及润滑寿命,适合用于高温条件中的滚动轴承,并且长时间表现出稳定的润滑性,因此非常有用。此外,本发明的润滑脂组合物即使在高温中长时间使用,也能够保持一定的稠度,不会明显硬化或软化。
具体实施方式
(a)基油
作为本发明的润滑脂组合物的基油,可以使用矿物油、合成油以及它们的混合油。作为合成油,可以举出双酯、多元醇酯为代表的酯系合成油,聚-α-烯烃、聚丁烯为代表的合成烃油,烷基二苯醚、聚丙二醇为代表的醚系合成油,硅油,氟化油等。
本发明中优选使用混合油,更优选2种以上合成油的混合油,进一步优选酯系合成油的混合油,特别优选耐热性优异的多元醇酯系合成油和烷基二苯醚系合成油的混合油。
基油在40℃时的运动粘度优选30~300mm2/s。如果40℃的运动粘度低于30mm2/s,则由于蒸发量的增加以及油膜厚度的减少会导致润滑性的降低而无法期待长寿命,因此不优选。另一方面,如果40℃的运动粘度高于300mm2/s,则由于粘性阻力增大并引起扭矩升高,因此不优选。
本发明的润滑脂组合物,相对于润滑脂组合物整体,优选含有50质量%以上、更优选60质量%以上的(a)基油。
(b)增稠剂
作为本发明的润滑脂组合物的增稠剂,可以使用所有增稠剂。具体可以举出锂皂、复合锂皂为代表的皂系增稠剂,双脲为代表的脲系增稠剂,有机粘土、二氧化硅为代表的无机系增稠剂,PTFE等有机系增稠剂等。
作为在本发明中能够使用的复合锂皂,优选由具有1个以上的羟基且碳原子数为12~24的羟基脂肪酸和碳原子数为2~12的脂肪族二羧酸的锂盐构成。作为上述羟基脂肪酸,可以举出12-羟基硬脂酸、12-羟基月桂酸、16-羟基棕榈酸等。其中,优选12-羟基硬脂酸。作为上述脂肪族二羧酸,可以举出壬二酸、癸二酸、草酸、丙二酸、丁二酸、戊二酸、己二酸、庚二酸、辛二酸、十一烷二酸、十二烷二酸。最优选壬二酸。
作为在本发明中使用的增稠剂,优选皂系增稠剂,由于锂皂及复合锂皂耐热性优异,因此更优选。在复合锂皂中,最优选12-羟基硬脂酸和壬二酸的锂盐。由于即使将锂皂以及复合锂皂用于必须设置圆柱滚子轴承的主电动机的情况中,也能够得到比脲类化合物更长的润滑寿命,因此优选。
本发明的润滑脂组合物,相对于润滑脂组合物整体,优选含有1~30质量%、更优选含有5~20质量%的(b)增稠剂。如果增稠剂过多,则润滑脂变硬,从而存在搅拌阻力变大的可能性。相反,如果增稠剂过少,则润滑脂变软,从而存在渗漏的可能性。
添加剂
本发明的润滑脂组合物含有(c)由式(1)表示的具有烷基硫代氨基甲酰基的化合物(ATC)以及(d)受阻酚系抗氧化剂来作为抗氧化剂。本发明的润滑脂组合物进一步含有金属钝化剂。
(c)在本发明中使用的具有烷基硫代氨基甲酰基的化合物由下述式(1)表示。
[化学式2]
式1中,R1、R2、R3、R4表示独立且碳原子数为1~20的直链或支链烷基,优选碳原子数为1~8的直链或支链烷基。优选R1、R2、R3、R4是全部相同的基。
X表示S、S-S、S-CH2-S、S-CH2CH2-S或者S-CH2CH2CH2-S。其中,优选S-CH2-S。
作为在式(1)中表示的化合物,可以举出双(二甲基硫代氨基甲酰基)单硫化物、双(二甲基硫代氨基甲酰基)二硫化物、亚甲基双(二甲基二硫代氨基甲酸酯)、亚甲基双(二正丁基二硫代氨基甲酸酯)等。其中,优选亚甲基双(二正丁基二硫代氨基甲酸酯)。
本发明的润滑脂组合物,相对于润滑脂组合物整体,优选含有0.1~10质量%、更优选含有0.5~5质量%的(c)由式(1)表示的具有烷基硫代氨基甲酰基的化合物。如果(c)的量大于10质量%,则抗氧化老化效果饱和,如果(c)的量小于0.1质量%,则不能得到添加效果。
作为(d)受阻酚系抗氧化剂,可以举出选自由2,6-二叔丁基-4-甲酚、季戊四醇四(3-(3,5-二叔丁基-4-羟苯基)丙酸酯)、苯丙酸,3,5-双(1,1-二甲基-乙基)-4-羟基C7-C9侧链烷基酯以及十八烷基-3-(3,5-二叔丁基-4-羟苯基)丙酸酯组成的组中的一种以上等。其中,优选2,6-二叔丁基-4-甲酚。
本发明的润滑脂组合物,相对于润滑脂组合物整体,优选含有0.1~10质量%、更优选含有0.5~5质量%的(d)受阻酚系抗氧化剂。如果(d)的量大于10质量%,则抗氧化老化效果饱和,如果(d)的量小于0.1质量%,则不能得到添加效果。
作为(e)金属钝化剂,可以举出草酸衍生物、水杨酸衍生物、肼衍生物等。具体可以举出由式(2)表示的3-(N-水杨酰基)氨基-1,2,4-三唑、由式(3)表示的十亚甲基羧酸二水杨酰肼(MCSH)、由式(4)表示的N,N-双[3-(3,5-二叔丁基-4-羟苯基)丙酰基]肼、间苯二甲酸双(2-苯氧基丙酰肼)、N-甲酰基-N’-水杨酰肼、2,2-草酰胺双-[乙基-3-(3,5-二叔丁基-4-羟苯基)丙酸酯]、草酰基-双-苯亚甲基-酰肼等。其中,优选由式(3)表示的十亚甲基羧酸二水杨酰肼(MCSH)。
3-(N-水杨酰基)氨基-1,2,4-三唑
[化学式3]
MCSH:十亚甲基羧酸二水杨酰肼
[化学式4]
N,N-双[3-(3,5-二叔丁基-4-羟苯基)丙酰基]肼
[化学式5]
本发明的润滑脂组合物,相对于润滑脂组合物整体,优选含有0.1~10质量%、更优选含有0.1~5质量%的(e)金属钝化剂。如果(e)的量大于10质量%,则金属钝化性的效果饱和,如果(e)的量小于0.1质量%,则不能得到添加效果。
根据其他需要,可以使用所有添加剂。具体可以举出除作为本发明必要成分的抗氧化基以外的抗氧化剂,例如,喹啉系抗氧化剂、胺系抗氧化剂,防锈剂,金属防蚀剂,油性剂,抗磨剂,极压剂以及固体润滑剂等。
本发明的润滑脂组合物,相对于润滑脂组合物整体,特别优选含有50质量%以上、优选60质量%以上的(a)基油,1~30质量%、优选5~20质量%的(b)增稠剂,0.1~10质量%、优选0.5~5质量%的(c)由式(1)表示的具有烷基硫代氨基甲酰基的化合物,0.1~10质量%、优选0.5~5质量%的(d)受阻酚系抗氧化剂,0.1~10质量%、优选0.1~5质量%的(e)金属钝化剂。
工作锥入度
本发明的润滑脂组合物的工作锥入度优选200~400,更优选250~350。如果工作锥入度高于400,则易于渗漏。另一方面,如果工作锥入度低于200,则搅拌阻力变大。
封入本发明的润滑脂组合物的轴承是滚动轴承,尤其是滚子轴承,其中适合圆柱滚子轴承。优选在全封闭型发动机中使用的轴承,尤其在全封闭型铁路车辆用主电动机中使用的轴承。轴承的材质没有特别限制,优选铜。
实施例
1.试验用润滑脂
根据表1以及表2所示的配方,调制了实施例1~7、比较例1~6的润滑脂组合物。各成分的量是基于润滑脂组合物的整体质量的质量%。
2.润滑脂的制造方法
向基油467.5g中加入82.5g12-羟基硬脂酸,并加热至使其变为完全透明的液体状态的温度(80~90℃)。向其中加入预先将11.9g一水氢氧化锂盐添加于60g水中并加热溶解的溶液,用力搅拌的同时进行12-羟基硬脂酸的皂化反应,从而形成12-羟基硬脂酸的锂盐。然后,加入26g壬二酸并持续搅拌直至变为均一的状态。向其中加入预先将11.9g一水氢氧化锂盐添加于60g水中并加热溶解的溶液,用力搅拌的同时进行壬二酸的皂化反应。在约60分钟后,用红外线分光分析确认看不到未反应脂肪酸的吸收后,终止了皂化反应。然后,将在加热工序中加入的内容物缓慢加热至200℃。在200℃时,添加余下的400.2g基油并冷却至室温,通过三重轧辊2次,从而得到复合锂基润滑脂。最终的内容物的量是1000g。
使用醚油(烷基二苯醚:运动粘度40℃100mm2/s,100℃12.5mm2/s)和酯油(季戊四醇酯:运动粘度40℃102mm2/s,100℃12.9mm2/s)的1:1混合物(质量比)作为基油(运动粘度40℃101mm2/s)。
3.分析方法以及评价试验方法
(1)稠度(JIS K22207)
稠度统一为280。
(2)高温薄膜试验
将润滑脂以2mm的厚度涂布于60×80×1mm的SPCC钢板上,测量试验前后的总酸值。
试验后的总酸值在规定温度(160℃)、规定时间(500h)后测量。总酸值依据JIS K25015.测量。
(3)轴承润滑寿命试验
将填充试验润滑脂(5.6g)的轴承放置于试验机中。对轴承施加径向载荷(100kgf),用加热器将轴承的外轮温度恒定控制在120℃,并使之以8000rpm的速度旋转。将轴承外轮温度到达130℃的时间作为寿命时间。
试验条件
轴承:圆柱滚子轴承(型号:NU214,内径70mm,外径125mm)
载荷:径向载荷:100kgf
旋转数:8000rpm
润滑脂封入量:5.6g
温度:控制在120℃
评价基准
总酸值的变化(mg KOH/g)○:0.20以下,×:大于0.20
轴承润滑寿命 ○:合格大于1000h,×:不合格1000h以下
综合评价 ○:总酸值变化及轴承润滑寿命全部合格
×:总酸值变化或/及轴承润滑寿命不合格
4.评价试验结果
在表1以及表2中表示实施例1~7、比较例1~6的润滑脂组合物的试验结果。
表1
*1醚油(烷基二苯醚:运动粘度40℃ 100mm2/s,100℃ 12.5mm2/s)和酯油(季戊四醇酯:运动粘度40℃ 102mm2/s,100℃ 12.9mm2/s)的1:1混合物(质量比)(运动粘度40℃ 101mm2/s)
*2亚甲基双(二正丁基二硫代氨基甲酸酯)
*3受阻酚系抗氧化剂:2,6-二叔丁基-4-甲酚
*4十亚甲基羧酸二水杨酰肼
*52,2,4-三甲基-1,2-二氢化喹啉聚合物
*6p,p’-二辛基二苯胺
表2
*1醚油(烷基二苯醚:运动粘度40℃ 100mm2/s,100℃ 12.5mm2/s)和酯油(季戊四醇酯:运动粘度40℃ 102mm2/s,100℃ 12.9mm2/s)的1:1混合物(质量比)(运动粘度40℃ 101mm2/s)
*2亚甲基双(二正丁基二硫代氨基甲酸酯)
*3受阻酚系抗氧化剂:2,6-二叔丁基-4-甲酚
*4十亚甲基羧酸二水杨酰肼
*52,2,4-三甲基-1,2-二氢化喹啉聚合物
*6p,p’-二辛基二苯胺
在含有成分(a)~(e)的实施例1~7中,总酸值变化小,热氧化稳定性优异,轴承润滑寿命也全部达到基准,综合评价合格。
另一方面,在分别不含有实施例1的(d)、(c)、(e)的比较例1、2、3中,总酸值变化大,热氧化稳定性差,轴承润滑寿命也短。
此外,在分别含有喹啉系抗氧化剂、胺系抗氧化剂来替代实施例1的(d)的比较例4、5中,总酸值变化大,热氧化稳定性差,轴承润滑寿命也短。
对于含有喹啉系抗氧化剂和胺系抗氧化剂来替代实施例1的(d)的比较例6,同样地,总酸值变化大,热氧化稳定性差,轴承润滑寿命也短。
Claims (7)
1.一种润滑脂组合物,其特征在于,含有(a)基油、(b)增稠剂、(c)由式(1)表示的具有烷基硫代氨基甲酰基的化合物、(d)受阻酚系抗氧化剂以及(e)金属钝化剂。
式中,R1、R2、R3、R4表示独立且碳原子数为1~20的烷基,X表示S、S-S、S-CH2-S、S-CH2CH2-S或者S-CH2CH2CH2-S。
2.如权利要求1所述的润滑脂组合物,所述(d)受阻酚系抗氧化剂是2,6-二叔丁基-4-甲酚。
3.如权利要求1或2所述的润滑脂组合物,所述(e)金属钝化剂是十亚甲基羧酸二水杨酰肼。
4.如权利要求1~3中任一项所述的润滑脂组合物,所述(a)基油是多元醇酯油和烷基二苯醚油的混合油。
5.如权利要求1~4中任一项所述的润滑脂组合物,所述(b)增稠剂选自由锂皂和复合锂皂组成的组中的至少一种。
6.如权利要求1~5中任一项所述的润滑脂组合物,相对于所述润滑脂组合物整体,含有50质量%以上的(a)基油、1~30质量%的(b)增稠剂、0.1~10质量%的(c)由式(1)表示的具有烷基硫代氨基甲酰基的化合物、0.1~10质量%的(d)受阻酚系抗氧化剂、0.1~10质量%的(e)金属钝化剂。
7.一种轴承,其封入如权利要求1~6中任一项所述的润滑脂组合物。
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DE112013000604T8 (de) | 2014-12-31 |
DE112013000604B4 (de) | 2022-03-24 |
JP2013147548A (ja) | 2013-08-01 |
JP5872300B2 (ja) | 2016-03-01 |
US20140336090A1 (en) | 2014-11-13 |
DE112013000604T5 (de) | 2014-10-23 |
WO2013108887A1 (ja) | 2013-07-25 |
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