CN109563432A - 润滑脂组合物 - Google Patents

润滑脂组合物 Download PDF

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CN109563432A
CN109563432A CN201780048446.3A CN201780048446A CN109563432A CN 109563432 A CN109563432 A CN 109563432A CN 201780048446 A CN201780048446 A CN 201780048446A CN 109563432 A CN109563432 A CN 109563432A
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lubricant composition
quinoline
mass
system antioxidant
amine
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CN109563432B (zh
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广冈岩树
佐藤雄太
饭岛昌俊
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Kyodo Yushi Co Ltd
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Abstract

本发明提供一种润滑脂组合物，根据本发明，含有(a)基油、(b)含有脲系化合物的增稠剂、(c)以组合物的总质量为基准的0.5～5质量％的胺系抗氧剂以及(d)以组合物的总质量为基准的0.5～5质量％的喹啉系抗氧剂。

Description

润滑脂组合物
技术领域
本发明涉及适合滚动轴承中使用的润滑脂组合物，该滚动轴承支撑用于在各产业中使用的电力机械、机械部件中的电动机转子。
背景技术
由于各种产业机械中使用的电动机在从寒冷地带到如汽车发动机机舱内那样的高温气氛这样的各种环境中运转，因此，对于电动机中使用的轴承，要求能够在广泛的温度范围内长时间免维护地使用，并且对于耐久性也提高了要求。
作为机械部件等的润滑剂所使用的润滑脂组合物，一般的由增稠剂、基油以及添加剂这三者构成。
作为得到高温下长寿命的润滑脂的方法，需要提高润滑脂的耐氧化性。例如，提出了增稠剂中使用脲化合物、添加剂中使用规定量的过碱性金属磺酸盐的润滑脂，来作为能够用于在高温下使用的滚动轴承的润滑脂(专利文献1)。为了延长高温、高速等严苛条件下的咬死寿命，还提出了增稠剂中使用脂环式脂肪族二脲化合物、基油中使用作为高性能合成油的季戊四醇酯油的润滑脂(专利文献2)。
由于近年来的机械部件的高温、高速化，对滚动轴承的长寿命的要求也比以往进一步提高，为了更加能够用于通用用途，还要求不依赖于基油的耐氧化性(种类)而能够在广泛的温度范围内维持性能。
专利文献3中提出了一种生物分解性润滑脂组合物，其使用胺系的N-苯基-1-萘胺和喹啉系的聚(2,2,4-三甲基-1,2-二羟基喹啉)作为抗氧剂，但其终究是以赋予生物分解性为目的，作为轴承耐久性能的指标的轴承润滑寿命的评价是在100℃环境下进行的。
现有技术文献
专利文献
专利文献1:日本特开2010-77320号公报
专利文献2:日本特开2012-197401号公报
专利文献3:日本特开平11-222597号公报
发明内容
发明要解决的课题
因此，本发明的目的是提供一种润滑脂组合物，其在高温且高速环境下的耐久性优异，而且低温性能也优异，具有长寿命。
解决课题的方法
本发明提供如下的润滑脂组合物。
1.一种润滑脂组合物，含有：
(a)基油，
(b)含有脲系化合物的增稠剂，
(c)以组合物的总质量为基准，0.5～5质量％的胺系抗氧剂，以及
(d)以组合物的总质量为基准，0.5～5质量％的喹啉系抗氧剂。
2.如上述第1项记载的润滑脂组合物，上述(b)含有脲系化合物的增稠剂是由下述式(1)表示的二脲化合物。
[化1]
式中，R2是碳原子数6～15的2价芳香族烃基，R1和R3可相互相同也可以不同地是碳原子数6～30的饱和或不饱和烷基、碳原子数6或7的芳基或环己基。
3.如上述第1项或第2项记载的润滑脂组合物，其中，上述(a)基油含有从由矿物油和烃系合成油组成的组中选择的至少一种。
4.如上述第1项或第2项记载的润滑脂组合物，其中，上述(a)基油含有高精制矿物油。
5.如上述第1项～第4项中任一项记载的润滑脂组合物，其中，上述(a)基油的40℃时的运动粘度为50～150mm2/s。
6.如上述第1项～第5项中任一项记载的润滑脂组合物，其中，上述(c)胺系抗氧剂是从由苯基α萘胺、烷基苯基α萘胺和烷基二苯胺组成的组中选择的至少一种胺系抗氧剂。
7.如上述第1项～第6项中任一项记载的润滑脂组合物，其中，上述(d)喹啉系抗氧剂是从由2,2,4-三甲基-1,2-二羟基喹啉、2-甲基-2,4-二乙基-1,2-二羟基喹啉、2,2,4,6-四甲基-1,2-二羟基喹啉、2,2,4,7-四甲基-1,2-二羟基喹啉和6,6’-双(2,2,4-三甲基-1,2-二羟基喹啉)以及这些的衍生物或这些的高分子化物组成的组中选择的至少一种喹啉系抗氧剂。
8.如上述第1项～第7项中任一项记载的润滑脂组合物，其中，上述(c)胺系抗氧剂与上述(d)喹啉系抗氧剂的质量比为1：3～3：1。
9.如上述第1项～第8项中任一项记载的润滑脂组合物，其中，进一步含有(e)锌系防锈剂，以润滑脂组合物的总质量为基准，该锌系防锈剂的含量为0.5～10质量％。
10.如上述第1项～第9项中任一项记载的润滑脂组合物，用于在支持电动机转子的电动机用滚动轴承中使用。
发明效果
根据本发明，提供一种高温且高速环境下耐久性优异，而且低温性能也优异，具有长寿命的润滑脂组合物。
具体实施方式
＜基油＞
在本发明的润滑脂组合物中所使用的基油没有特别限制。例如，可以使用以矿物油为首的全部基油。基油优选含有从由矿物油和烃系合成油组成的组中选择的至少一种。基油可以单独使用，也可以并用二种以上。
作为矿物油，可以使用石蜡系矿物油、环烷系矿物油、这些的混合物。优选含有高精制矿物油。
高精制矿物油是指经过脱蜡处理降低低温时的蜡成分的析出，且因此与未精制的矿物油的流动点(-5℃～-20℃)相比流动点低的矿物油。通过含有流动点为-35℃以下的高精制矿物油，能够对低温时的低扭矩性不产生坏影响的情形下使用。此外，能够在耐蒸发性方面也没有问题的情形下使用。需说明的是，基油的流动点按照JISK2269来测定。
高精制矿物油的含有比例，以基油总量为100时，优选为5～30质量％，更优选为10～20质量％。通过以这样的比例含有高精制矿物油，低温性能优异。
作为合成油，可以使用以二酯、多元醇酯为代表的酯系合成油，以聚α烯烃、聚丁烯为代表的合成烃油，以烷基二苯醚、聚丙二醇为代表的醚系合成油，硅油、氟化油等各种合成油。其中，优选合成烃油、酯油、醚系合成油以及这些的混合油。更优选合成烃油、酯油以及这些的混合油。进而更加优选合成烃油以及合成烃油与其他油的混合油。
作为本发明的基油，特别优选单独使用矿物油。更加优选基油含有高精制矿物油。
本发明的基油的运动粘度没有特别限定。可以根据需要来选择基油运动粘度。优选40℃的基油运动粘度为10～200mm2/s，更优选为50～150mm2/s，进一步优选为70～100mm2/s。需说明的是，基油的运动粘度按照JIS K 2220 23.来测定。
本发明的润滑脂组合物中基油的含量优选为70～90质量％，更优选为80～90质量％。
＜增稠剂＞
本发明的润滑脂组合物中所使用的增稠剂为脲系增稠剂。脲系增稠剂中，优选由下述式(1)所表示的二脲化合物。
[化2]
式中，R2是碳原子数6～15的2价芳香族烃基，R1和R3可相互相同也可以不同地是碳原子数6～30的饱和或不饱和烷基、碳原子数6或7的芳基或环己基。
特别是，优选作为环己胺和脂肪族胺与二异氰酸酯的反应生成物的脂环式脂肪族二脲。其中，在R1和R3中任一个为环己基时，另一个优选为碳原子数12～22的饱和烷基，更优选为碳原子数16～18的饱和烷基，进一步优选包括碳原子数为18的饱和烷基的二脲化合物。尤其是，优选为R1和R3是环烷基的二脲化合物、R1和R3是碳原子数18的饱和烷基的二脲化合物以及R1和R3中的一方是环烷基且另一方是碳原子数18的饱和烷基的二脲化合物的混合物。脂环式脂肪族二脲中的环己基与烷基的摩尔比优选为10：90～50：50，更优选为20：80～40：60。如果摩尔比在这样的范围内，则润滑脂中所能够含有的基油的量会更多，耐久性变得良好，因而优选。
作为R2，优选为源自甲苯撑二异氰酸酯或二苯甲烷二异氰酸酯的基团，更优选为源自二苯甲烷二异氰酸酯的基团，进一步优选为源自二苯甲烷-4,4’-二异氰酸酯的基团。
式(1)的二脲化合物，例如，可以通过在基油中使规定的二异氰酸酯与规定的单胺反应来获得。作为二异氰酸酯的优选具体例，有二苯甲烷-4,4’-二异氰酸酯、甲苯撑二异氰酸酯。作为单胺，列举脂肪族胺、芳香族胺、脂环式胺或这些的混合物。作为脂肪族胺的具体例，可以举出辛胺、壬胺、癸胺、十一烷胺、十二烷胺、十三烷胺，十四烷胺、十五烷胺，十六烷胺，十七烷胺，十八烷胺，十九烷胺，二十烷胺和油胺等。作为芳香族胺的具体例，可以举出苯胺、对甲苯胺和萘胺等。作为脂环式胺的具体例，可以举出环己胺、二环己胺等。
本发明的润滑脂组合物中的增稠剂的含量根据增稠剂的种类而不同。本发明的润滑脂组合物的稠度适合为200～400，更优选为200～300，更加优选为240～280。增稠剂的含量优选为能够获得这样的稠度的量。本发明的润滑脂组合物中，增稠剂的含量通常为3～30质量％，优选为5～25质量％，更优选为5～15质量％。
＜添加剂＞
〔抗氧剂〕
本发明中所使用的抗氧剂含有(c)胺系抗氧剂、(d)喹啉系抗氧剂中的至少2种作为必须成分。
(c)胺系抗氧剂与(d)喹啉系抗氧剂的质量比优选为1：3～3：1。
作为(c)胺系抗氧剂，优选为苯基α萘胺、烷基苯基α萘胺、烷基二苯胺，更优选为烷基二苯胺。
作为(d)喹啉系抗氧剂，优选为2,2,4-三甲基-1,2-二羟基喹啉、2-甲基-2,4-二乙基-1,2-二羟基喹啉、2,2,4,6-四甲基-1,2-二羟基喹啉、2,2,4,7-四甲基-1,2-二羟基喹啉和6,6’-双(2,2,4-三甲基-1,2-二羟基喹啉)以及这些的衍生物或这些的高分子化物，可以举出具有下述式(2)的结构的各种化合物、其高分子化物。上述高分子化物可以举出聚(2,2,4-三甲基-1,2-二羟基喹啉)(与JIS K6211“橡胶用防老剂”中规定的防老剂TMDQ相当，比重为1.08～1.11，软化点为80～110℃，灰分为0.5％以下，加热减量为0.7％以下)或者6-乙氧基-2,2,4-三甲基-1,2-二羟基喹啉(相当于上述JIS K6211“橡胶用防老剂”中规定的防老剂ETMDQ)等。
其中，优选为聚(2,2,4-三甲基-1,2-二羟基喹啉)。需说明的是，下述式(2)中的n表示该化合物不仅为2,2,4-三甲基-1,2-二羟基喹啉的单体，还表示包括该化合物的2倍体以上的各种缩合物的混合物(也包括n＝1的单体)，但其具体的数值范围不清楚。
[化3]
尤其优选(c)胺系抗氧剂为烷基二苯胺，(d)喹啉系抗氧剂为聚(2,2,4-三甲基-1,2-二羟基喹啉)。
本发明的润滑脂组合物中的上述(c)的含量优选为0.5～5质量％，更优选为0.5～2.5质量％。上述(c)的含量如果为这样的范围，则对基油的溶解性优异。
本发明的润滑脂组合物中的上述(d)的含量优选为0.5～5质量％，更优选为0.5～2.5质量％。上述(d)的含量如果为这样的范围，则对基油的溶解性优异。
上述(c)与上述(d)的总量优选为组合物总量的1～10质量％，更优选为2～5质量％。上述(c)与上述(d)的总量如果为这样的范围，则不仅发挥充分的抗氧化效果来延长轴承润滑寿命，还能使得对基油的溶解为良好，不会对作为润滑脂的基本性能之一的轴承音响性能以及低温性能产生坏影响。
〔任意的添加剂〕
本发明的润滑脂组合物根据需要可以含有润滑脂组合物中通常使用的各种添加剂。作为这样的添加剂的例子，可以举出上述(c)和(d)以外的抗氧剂、防锈剂、金属减活剂、去垢分散剂、极压添加剂、消泡剂、抗乳化剂、油性提高剂、耐摩耗剂、固体润滑剂等。这些的添加量通常为0.01～10质量％。
优选含有防锈剂，更优选含有锌系防锈剂。特别优选防锈剂为环烷酸锌。对含量没有特别限定，但在为环烷酸锌时，以本发明的组合物的总质量为基准，优选为0.5～10质量％。通过含有如此量的环烷酸锌，即使在假定如Emcor防锈试验(IP220)这样的严苛条件的试验中，也能防止生锈。
本发明的润滑脂组合物可以用于支撑各产业中使用的电力机械、机械部件中所使用的电动机转子的滚动轴承中。
实施例
含有芳香族二脲(实施例6)作为增稠剂的润滑脂组合物，通过如下步骤来制造，即，在如下表中所示的基油中，以2摩尔原料胺(对甲苯胺)相对于1摩尔4.4'-二苯甲烷二异氰酸酯的比率使所定量进行反应，并添加规定量的胺系抗氧剂、喹啉系抗氧剂以及锌系防锈剂，由3辊研磨机来调整至规定稠度。
含有脂环式脂肪族二脲(实施例1～5、7～13、比较例4～9)作为增稠剂的润滑脂组合物，除了作为原料胺使用环己胺和十八酰胺代替对甲苯胺以外，与实施例6的润滑脂组合物同样地制造。
含有复合锂皂(比较例1～3)作为增稠剂的润滑脂组合物，通过如下步骤来制造，即，在基油中投入壬二酸和12羟基硬脂酸，加温后添加氢氧化锂水溶液，再度加热后，急冷，加入规定量的胺系抗氧剂、喹啉系抗氧剂以及锌系防锈剂，由3辊研磨机调整至规定稠度。
需说明的是，稠度(60次混和稠度)均调整至260(JIS K2220)。
(a)基油
矿物油A：粘度指数：95以上，运动粘度10.8mm2/s@100℃，运动粘度96.6mm2/s@40℃
矿物油B：粘度指数：95以上，运动粘度11.2mm2/s@100℃，运动粘度95.0mm2/s@40℃
矿物油C：粘度指数：95以上，运动粘度6.0mm2/s@100℃，运动粘度37.0mm2/s@40℃
矿物油D：粘度指数：95以上，运动粘度31.6mm2/s@100℃，运动粘度436mm2/s@40℃
高精制矿物油A：粘度指数：120以上，运动粘度7.80mm2/s@100℃，运动粘度46.0mm2/s@40℃
(c)胺系抗氧剂
·烷基二苯胺
·苯基α萘胺
(d)喹啉系抗氧剂
·2,2,4-三甲基-1,2-二羟基喹啉的高分子化物(上述式(2)表示的聚(2,2,4-三甲基-1,2-二羟基喹啉)，比重1.08～1.11，软化点80～110℃，灰分0.5％以下，加热减量0.7％以下)
·6-乙氧基-2,2,4-三甲基-1,2-二羟基喹啉(相当于上述JIS K6211“橡胶用防老剂”中规定的防老剂ETMDQ)
(e)锌系防锈剂
·环烷酸锌
(f)苯酚系抗氧剂
·十八烷基-3-(3,5-二叔丁基-4-羟基苯基)丙酸酯
＜试验方法和判定＞
〔耐久性(耐热性、轴承润滑寿命)〕
·评价方法
试验使用以ASTM D3336为基准的轴承润滑寿命试验机。
试验条件如下所示。需说明的是，以直至电动机产生过电流(4安培以上)的时间或轴承外轮温度上升至试验温度+15℃为止的时间中的任一个中较短的时间作为咬死寿命。
轴承形式：6204金属密封
试验温度：160℃
旋转数：10000rpm
润滑脂量：1.8g
试验负荷：轴向负荷66.7N径向负荷66.7N
·判定
轴承润滑寿命1000h以上···○(合格)
小于1000h···×(不合格)
〔低温性能(低扭矩性)〕
＜试验方法＞
低扭矩性以JIS K222018.中规定的低温扭矩试验为基准来进行。
轴承形式：6204
试验温度：-30℃
旋转数：1rpm
测量项目：
起动力矩(测定开始时的最大扭矩)
转矩(旋转10分钟的最后15秒中的平均扭矩)
评价基准
起动力矩(-30℃)小于1000mNm：合格(○)
1000mNm以上：不合格(×)
转矩(-30℃)小于100mNm：合格(○)
100mNm以上：不合格(×)
〔综合判定〕
耐久性评价、低扭矩性评价任一项均合格：○(合格)
任一项中有1项不合格：×(不合格)
[表1]
[表2]

Claims (10)

1.一种润滑脂组合物，含有：
(a)基油，
(b)含有脲系化合物的增稠剂，
(c)以组合物的总质量为基准，0.5～5质量％的胺系抗氧剂，以及
(d)以组合物的总质量为基准，0.5～5质量％的喹啉系抗氧剂。
2.如权利要求1所述的润滑脂组合物，其中，所述(b)含有脲系化合物的增稠剂是由下述式(1)表示的二脲化合物，
[化1]
式中，R2是碳原子数6～15的2价芳香族烃基，R1以及R3可相互相同也可以不同地是碳原子数6～30的饱和或不饱和烷基、碳原子数6或7的芳基或环己基。
3.如权利要求1或2所述的润滑脂组合物，其中，所述(a)基油含有从由矿物油和烃系合成油组成的组中选择的至少一种。
4.如权利要求1或2所述的润滑脂组合物，其中，所述(a)基油含有高精制矿物油。
5.如权利要求1～4中任一项所述的润滑脂组合物，其中，所述(a)基油的40℃时的运动粘度为50～150mm2/s。
6.如权利要求1～5中任一项所述的润滑脂组合物，其中，所述(c)胺系抗氧剂是从由苯基α萘胺、烷基苯基α萘胺和烷基二苯胺组成的组中选择的至少一种胺系抗氧剂。
7.如权利要求1～6中任一项所述的润滑脂组合物，其中，所述(d)喹啉系抗氧剂是从由2,2,4-三甲基-1,2-二羟基喹啉、2-甲基-2,4-二乙基-1,2-二羟基喹啉、2,2,4,6-四甲基-1,2-二羟基喹啉、2,2,4,7-四甲基-1,2-二羟基喹啉和6,6’-双(2,2,4-三甲基-1,2-二羟基喹啉)以及这些的衍生物或这些的高分子化物组成的组中选择的至少一种喹啉系抗氧剂。
8.如权利要求1～7中任一项所述的润滑脂组合物，其中，所述(c)胺系抗氧剂与所述(d)喹啉系抗氧剂的质量比为1：3～3：1。
9.如权利要求1～8中任一项所述的润滑脂组合物，其中，进一步含有(e)锌系防锈剂，以润滑脂组合物的总质量为基准，该锌系防锈剂的含量为0.5～10质量％。
10.如权利要求1～9中任一项所述的润滑脂组合物，用于在支撑电动机转子的电动机用滚动轴承中使用。
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