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CN1406270A - 用于恒速万向节的润滑脂组合物 - Google Patents

用于恒速万向节的润滑脂组合物 Download PDF

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CN1406270A
CN1406270A CN01805733A CN01805733A CN1406270A CN 1406270 A CN1406270 A CN 1406270A CN 01805733 A CN01805733 A CN 01805733A CN 01805733 A CN01805733 A CN 01805733A CN 1406270 A CN1406270 A CN 1406270A
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moly
sulfide
grease
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CN1222594C (zh
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Y·河村
K·仲泽
T·仁村
K·齐藤
N·筱田
K·田中
T·和田
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Shell Internationale Research Maatschappij BV
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Abstract

含有基油和脲基增稠剂的恒速万向节用润滑脂组合物，该润滑脂还含有(A)硫化钼二烷基二硫代氨基甲酸酯和(B)5，5’－二硫代双(1，3，4－噻二唑－2－硫醇)；包括用所述润滑脂填充万向节的恒速万向节的润滑方法；以及用所述润滑脂填充的恒速万向节。

Description

用于恒速万向节的润滑脂组合物
本发明涉及用于恒速万向节的润滑脂组合物，恒速万向节的润滑方法，以及填充了润滑脂的恒速万向节。特别是，本发明涉及可用于汽车驱动轴、动力输出万向传动轴和工业机械万向节的润滑脂组合物。
机械技术的进步不断要求减小机械的尺寸和重量，提高机械的精度，延长机械寿命等。
恒速万向节是能从最后减速齿轮向行走轮轴以恒定转速传输动力的特殊类型的万向接头。
由于用于汽车和工业机械的恒速万向节在高速和高表面压力条件下使用，因此要求用于润滑这些万向节的润滑脂具有更好的性能。以下将就汽车用恒速万向节(以下简称为CVJ)更详细地描述这种情况。
随着前轮驱动轿车和四轮驱动轿车等的发展，CVJ在汽车工业中的应用已显著增加。现代轿车输出功率更大，体积更小，重量更轻，这些都对CVJ的耐久性提出了更严格的要求。
用于CVJ润滑的润滑脂还要满足连接耐久性更好和寿命更长(抗损害，如抗剥落和抗咬合)的要求。
根据这些要求，商业上主要使用含有硫化脂肪/油脂和/或与二硫代磷酸锌结合的烯烃硫化物的硫-磷基特压剂，以及含有铅基添加剂和二硫化钼的锂润滑脂等。近年来，具有优异的耐热性的脲润滑脂的使用已超过锂润滑脂。
涉及硫化钼二烷基二硫代氨基甲酸酯的使用的现有技术的实例包括日本已审专利申请H4-34590和日本未审专利申请H6-57283、H6-330072和H10-273692。
日本已审专利公开H4-34590公开了含有：-(A)硫化钼二烷基二硫代氨基甲酸酯；和(B)选自硫化脂肪/油脂、烯烃硫化物、磷酸三甲苯酯、三烷基硫代磷酸酯和二烷基二硫代磷酸锌的至少一种硫-磷基特压添加剂的体系，该体系混和在脲润滑脂中。然而，这种体系在现行的恶劣CVJ工作条件下不能总认为是满意的。
日本未审专利申请H6-57283公开了含有硫化钼二烷基二硫代氨基甲酸酯、二硫化钼和硫化铅二烷基二硫代氨基甲酸酯的体系，该体系混和在脲润滑脂中。然而，由于该体系含有铅基添加剂，从环保角度不是理想的。
日本未审专利申请H6-330072公开了将(A)硫化钼二烷基二硫代氨基甲酸酯和(C)三苯基硫代磷酸酯都加入到脲润滑脂中的体系，但这些体系不能同时得到满意的耐损坏和耐磨损性能。
T.Sakurai的“Sekiyu Seihin Tenkazai”[石油产品添加剂](262页至结尾)介绍了作为润滑油添加剂的噻二唑化合物，226页上的表3建议加入噻二唑基化合物相对于铜和银得到了优异的硫化腐蚀保护。而且，日本已审专利公开H4-32880公开了向润滑脂中加入5，5’-二硫代双(1，3，4-噻二唑-2-硫醇)使得耐负载和特压性能提高，而不使金属腐蚀或褪色，但未提及耐损坏和耐磨损的平衡问题。
日本未审专利申请H11-131086公开了噻二唑基化合物在用磺酸钙配合物基增稠剂得到的润滑脂中作为添加剂的用法，但此处用噻二唑基化合物来钝化金属。
日本未审专利申H10-273692公开了用于恒速万向节的含有作为增稠剂的二脲的润滑脂组合物，其中二硫化钼、无磷的硫基特压添加剂和硫-氮基特压添加剂与(A)硫化钼二烷基二硫代氨基甲酸酯结合使用。然而，没有明确哪种具体的化合物可用作硫-氮基特压剂，只是在实施例中公开了例如R.T.Vanderbilt制造的“Vanlube 601”(商标)，且所述商品名只是证实了“Vanlube 601”是杂环硫-氮化合物。而且，根据该技术，二硫化钼与无磷的硫基特压添加剂结合使用是必不可少的。
在用于恒速万向节的润滑脂组合物领域中，满意的耐损坏性能和满意的耐磨损性能都是要求的。有很多润滑脂具有良好的耐磨损性能，但耐损坏性能很差。迫切要求发现在这些物理性能上都得到提高的恒速万向节用润滑脂组合物。
已发现可配制含有5，5’-二硫代双(1，3，4-噻二唑-2-硫醇)的恒速万向节用润滑脂，它具有有益的耐损坏和耐磨损性能。
本发明提供了含有基油和脲基增稠剂的恒速万向节用润滑脂组合物，该润滑脂还含有(A)硫化钼二烷基二硫代氨基甲酸酯；和(B)5，5’-二硫代双(1，3，4-噻二唑-2-硫醇)。
在优选实施方案中，本发明的润滑脂组合物还含有(C)三苯基硫代磷酸酯
硫化钼二烷基二硫代氨基甲酸酯(A)合适地可以是下式(1)所表示的化合物：
(R1R2N-CS-S)2-Mo2OmSn    (1)
其中R1和R2是独立地选自C1-C24烷基的基团，m+n＝4，m为0～3，n为1～4。
优选的烷基是C1-C18烷基，更优选的C1-C12烷基，再优选的C1-C6烷基，最优选的C1-C4烷基。所述烷基可以是直链或支化的。
适用于本发明的硫化钼二烷基二硫代氨基甲酸酯(A)的实例包括硫化钼二乙基二硫代氨基甲酸酯、硫化钼二丁基二硫代氨基甲酸酯、硫化钼二异丁基二硫代氨基甲酸酯、硫化钼二(2-乙基己基)二硫代氨基甲酸酯、硫化钼二戊基二硫代氨基甲酸酯、硫化钼二异戊基二硫代氨基甲酸酯、硫化钼二月桂基二硫代氨基甲酸酯、硫化钼二硬脂基二硫代氨基甲酸酯、硫化钼正丁基-2-乙基己基二硫代氨基甲酸酯和硫化钼2-乙基己基硬脂基二硫代氨基甲酸酯中的一种或多种
5，5’-二硫代双(1，3，4-噻二唑-2-硫醇)(B)可用下式(2)表示：
Figure A0180573300051
优选的本发明组合物具有一种或多种以下特征(相对于润滑脂总重而言)：(i)0.5～10％(重量)的A；(ii)0.5～5％(重量)的A；(iii)至少2％(重量)的A；(iv)最多3％(重量)的A；(v)0.1～10％(重量)的B；(vi)0.1～5％(重量)的B；(vii)至少0.5％(重量)的B；和(viii)最多2％(重量)的B。根据本发明，特别优选的组合物是具有特征(i)和(v)的那些；具有特征(i)和(vi)的那些；具有特征(i)和(vii)的那些；具有特征(i)和(viii)的那些；具有特征(i)、(vii)和(viii)的那些；具有特征(ii)和(v)的那些；具有特征(ii)和(vi)的那些；具有特征(ii)和(vii)的那些；具有特征(ii)和(viii)的那些；具有特征(ii)、(vii)和(viii)的那些；具有特征(iii)和(v)的那些；具有特征(iii)和(vi)的那些；具有特征(iii)和(vii)的那些；具有特征(iii)和(viii)的那些；具有特征(iii)、(vii)和(viii)的那些；具有特征(iv)和(v)的那些；具有特征(iv)和(vi)的那些；具有特征(iv)和(vii)的那些；具有特征(iv)和(viii)的那些；具有特征(iv)、(vii)和(viii)的那些；具有特征(iii)、(iv)和(v)的那些；具有特征(iii)、(iv)和(vi)的那些；具有特征(iii)、(iv)和(vii)的那些；具有特征(iii)、(iv)和(viii)的那些；以及具有特征(iii)、(iv)、(vii)和(viii)的那些。
如果A的用量少于0.5％(重量)，CVJ耐损坏的效果就变差，但不鼓励用10％(重量)以上的A，浓度限制如上所述，否则不会期望有更进一步的改进。
如果B的用量少于0.1％(重量)，CVJ耐损坏的效果就变差，但不鼓励用10％(重量)以上的B，浓度限制如上所述，否则不会有更进一步的改进。
三苯基硫代磷酸酯(C)是下式(3)表示的化合物：
(C6H5-O)3-P＝S    (3)
当加入三苯基硫代磷酸酯(C)时，优选的是以相对于润滑脂组合物总重为最多10％(重量)的浓度加入，如0.1～10％(重量)，更优选0.1～5％(重量)。
如果C的加入量少于0.1％(重量)，在耐磨损上的效果就变差，但不鼓励用10％(重量)以上的C，浓度限制如上所述，否则不会有更进一步的改进。
可用任何脲基增稠剂作为增稠剂用脲化合物，而对其类型没有具体限制。例如可方便地使用二脲、三脲和/或四脲。矿物油和/或合成油可用作基油。在本发明优选的实施方案中，相对于润滑脂组合物总重的脲基增稠剂的用量为2～35％(重量)。
也能向本发明的润滑脂组合物中加入诸如抗氧化剂、防锈剂和特压剂的各种添加剂。
此处具体描述的根据本发明用于恒速万向节的优选的润滑脂组合物的抗剥落和抗咬合(耐损坏)性能显著提高，还具有优异的耐磨损和温度控制性能。
本发明将通过以下实施例描述，这并不意味着以任何方式限制本发明的范围。
实施例
润滑脂组合物的制备
根据表1到3中所示的配方向基础润滑脂中加入添加剂，用三辊磨处理所得体系，得到实施例和比较例的润滑脂。应该指出的是用100℃下的运动粘度为15mm2/s的净化矿物油作为基油。
I二脲润滑脂
将1mol二苯基甲烷-4，4’-二异氰酸酯和2mol辛胺在基油中反应，均匀分散所得脲化合物，得到基础润滑脂。脲化合物的含量设定为10％(重量)。
II四脲化合物
使2mol二苯基甲烷-4，4’-二异氰酸酯、2mol辛胺和1mol乙二胺在基油中反应，均匀分散所得脲化合物，得到基础润滑脂。脲化合物的含量设定为15％(重量)。
表中所示的稠度、耐磨损性、万向节损坏和万向节耐久性是根据以下测试方法评估的。
(1)根据JIS K2220 5.3评价稠度
(2)根据ASTM D2266评价耐磨损性
(3)万向节损坏测试
将每种试样放入商用CVJ中，并在以下条件下运行系统，然后评价作为万向节内剥落标志的微细损坏的存在与否，运行期间万向节的最高温度也要评价。
CVJ型号：Barfield万向节
rpm：1500rpm
连接角：8°
力矩：300N.m.
时间：1小时
评价:(o)无损坏；×损坏；△轻微损坏
(4)万向节耐久性测试
将每种试样放入商用CVJ中，并在以下条件下运行系统，然后评价万向节中的球或内环、外环或定位圈的剥落或咬合存在与否。
CVJ型号：Barfield万向节
Ipm：1500rpm
连接角：8°
力矩：300N.m.
时间：150小时
评价：(o)无损坏；Δ轻微剥落；×剥落(不能继续使用)
表1
    实施例1     实施例2     实施例3
    基础润滑脂(％wt)     二脲润滑脂     95.0     95.0
    四脲润滑脂     95.0
    添加剂(％wt)     A-1    *1     3.0     2.0
    A-2    *2     2.0
    B      *3     2.O     0.5     0.5
    C      *4     1.0     1.0
    测试结果     稠度60W     320     316     318
    耐磨损性(mm)     0.47     0.40     0.39
    万向节损坏测试     (o)     (o)     (o)
    万向节温度(℃)     128     101     108
    万向节耐久睦测试     (o)     (o)
表2
   比较例1     比较例2     比较例3
    基础润滑脂(％wt)     二脲润滑脂     92.0     96.0     98.0
    四脲润滑脂
    添加剂(％wt)     A-1    *1     3.0     3.0
    A-2    *2
    B      *3     2.0
    C      *4     1.0     1.0
  2，5-双(叔辛基二硫代)-1，3，4-噻二唑     4.0
  二烷基二硫代磷酸锌
    二硫化钼
    测试结果     稠度60W     312     326     321
    耐磨损性(mm)     0.45     0.39     0.55
    万向节损坏测试     Δ     ×     ×
  万向节温度(℃)     120     107     154
  万向节耐久H劂试     Δ     ×
表3
  比较例4   比较例5   比较例6
  基础润滑脂(％wt)     二脲润滑脂    96.0     96.0     92.0
    四脲润滑脂    -     -     -
  添加剂(％wt)      A-1  *1    -     3.0     3.0
     A-2  *2    -     -     -
     B    *3    1.0     -     -
     C    *4    1.0     -     -
  2，5-双(叔辛基二硫代)-1，3，4-噻二唑    2.0     -     -
二烷基二硫代磷酸锌    -     1.0     -
    二硫化钼    -     -     5.0
  测试结果     稠度60W    322     318     316
  耐磨损性(mm)    0.48     0.41     0.65
  万向节损坏测试    ×     ×     ×
  万向节温度(℃)    106     108     118
  万向节耐久性测试    -     ×     -
*1：A-1是其中的烷基带有4个碳原子且n为2和3的硫化钼二烷基二硫代氨基甲酸酯化合物。
*2：A-2是其中的烷基带有4个碳原子且n为4的硫化钼二烷基二硫代氨基甲酸酯化合物。
*3：B是噻二唑化合物5，5’-二硫代双(1，3，4-噻二唑-2-硫醇)。
*4：C是三苯基硫代磷酸酯。

Claims (10)

1、恒速万向节用润滑脂组合物，含有基油和脲基增稠剂，该润滑脂还含有(A)硫化钼二烷基二硫代氨基甲酸酯和(B)5，5’-二硫代双(1，3，4-噻二唑-2-硫醇)。
2、根据权利要求1所述的润滑脂组合物，含有占润滑脂组合物总重0.5～10％(重量)的(A)硫化钼二烷基二硫代氨基甲酸酯和0.1～10％(重量)的(B)5，5’-二硫代双(1，3，4-噻二唑-2-硫醇)。
3、根据权利要求1或2所述的润滑脂组合物，其中所述润滑脂含有占润滑脂组合物总重0.5～5％(重量)的(A)硫化钼二烷基二硫代氨基甲酸酯和0.1～5％(重量)的(B)5，5’-二硫代双(1，3，4-噻二唑-2-硫醇)。
4、根据权利要求1-3任何一项所述的润滑脂组合物，其中所述润滑脂含有占润滑脂组合物总重2～35％(重量)的脲基增稠剂。
5、根据权利要求1到4任何一项所述的润滑脂组合物，其中(A)硫化钼二烷基二硫代氨基甲酸酯选自硫化钼二乙基二硫代氨基甲酸酯、硫化钼二丁基二硫代氨基甲酸酯、硫化钼二异丁基二硫代氨基甲酸酯、硫化钼二(2-乙基己基)二硫代氨基甲酸酯、硫化钼二戊基二硫代氨基甲酸酯、硫化钼二异戊基二硫代氨基甲酸酯、硫化钼二月桂基二硫代氨基甲酸酯、硫化钼二硬脂基二硫代氨基甲酸酯、硫化钼正丁基-2-乙基己基二硫代氨基甲酸酯和硫化钼2-乙基己基硬脂基二硫代氨基甲酸酯中的一种或多种。
6、根据权利要求1到5任何一项所述的润滑脂组合物，它还含有(C)三苯基硫代磷酸酯。
7、根据权利要求6所述的润滑脂组合物，它含有占润滑脂组合物总重0.1～10％(重量)的(C)三苯基硫代磷酸酯。
8、根据权利要求6或7所述的润滑脂组合物，其中所述润滑脂含有占润滑脂组合物总重0.1～5％(重量)的(C)三苯基硫代磷酸酯。
9、恒速万向节的润滑方法，包括用根据权利要求1到8任何一项所述的润滑脂填充万向节。
10、用根据权利要求1到8任何一项所述的润滑脂填充的恒速万向节。
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CN101107346B (zh) * 2004-12-27 2010-12-01 国际壳牌研究有限公司 脲基润滑脂组合物

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WO2005035700A1 (en) * 2003-10-10 2005-04-21 R.T. Vanderbilt Company, Inc. Lubricating compositions containing synthetic ester base oil, molybdenum compounds and thiadiazole-based compounds
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JP5258080B2 (ja) * 2007-05-30 2013-08-07 協同油脂株式会社 等速ジョイント用グリース組成物及びそれを封入した等速ジョイント
JP6292569B2 (ja) * 2013-12-04 2018-03-14 協同油脂株式会社 等速ジョイント用グリース組成物及びそのグリース組成物を封入した等速ジョイント
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CN100366712C (zh) * 2003-06-18 2008-02-06 国际壳牌研究有限公司 用于恒速接头的脲润滑脂组合物
CN101107346B (zh) * 2004-12-27 2010-12-01 国际壳牌研究有限公司 脲基润滑脂组合物

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