CN101889019B - 具有优异抗磨损和抗腐蚀特性的用于ep润滑脂的添加剂组合物 - Google Patents

具有优异抗磨损和抗腐蚀特性的用于ep润滑脂的添加剂组合物 Download PDF

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CN101889019B
CN101889019B CN200880119720.2A CN200880119720A CN101889019B CN 101889019 B CN101889019 B CN 101889019B CN 200880119720 A CN200880119720 A CN 200880119720A CN 101889019 B CN101889019 B CN 101889019B
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dmtd
dipolymer
molybdenum
thiadiazoles
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加斯顿·A·艾吉兰
罗纳德·J·赫泽
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Vanderbilt Minerals Ltd
Vanderbilt Chemicals LLC
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Abstract

本发明提供如下的润滑剂组合物：至少90％的基础润滑脂；(a)提供约1500ppm至3500ppm的硫的量的噻二唑聚(醚)乙二醇复合物；(b)提供约77ppm至450ppm的钼的量的二烃基二硫代磷酸钼；和(c)提供约600ppm至1000ppm的锌的量的二烃基二硫代磷酸锌。本发明还提供由组分(a)、(b)和(c)组成的用于润滑脂的添加剂组合物。

Description

具有优异抗磨损和抗腐蚀特性的用于EP润滑脂的添加剂组合物
发明领域
本发明涉及用于极端压力(“EP”)润滑脂组合物的添加剂组合物，其具有优异的抗磨损和抗腐蚀特性。更具体地，本发明涉及添加剂组合物，其包含(A)噻二唑聚(醚)乙二醇复合物、(B)二烃基二硫代磷酸钼和(C)二烃基二硫代磷酸锌。
发明背景
EP润滑脂在高负荷条件下润滑，并要求高效EP添加剂以防止刮伤和熔接。噻二唑是有效的EP添加剂化合物。美国专利6,365,557号公开了噻二唑/聚(醚)乙二醇复合物。尽管这些复合物是优异的润滑脂极端压力添加剂，但是它们对金属表面的高表面亲合力产生导致铜和其它有色金属不期望的变色并阻断抗磨损添加剂降低磨损的能力的涂层。本发明教导特定的润滑剂添加剂组合物，其中这些噻二唑聚(醚)乙二醇复合物不对磨损和腐蚀产生不良影响同时保持优异的极端压力特性。
美国专利6,541,427号(Dresel et al.)公开了具有添加剂系统的润滑脂配方，该添加剂系统含有2％的钼化合物(二烃基二硫代氨基甲酸盐MoDTC或二烃基二硫代磷酸盐MoDTP)、约2％的噻二唑添加剂并要求各种其它添加剂。
发明概述
本发明涉及润滑剂组合物，其包含均以重量％表示的下述组分：
(a)主要量(即，＞90％)的基础润滑脂，如锂、锂复合物、铝复合物、钙复合物有机粘土和聚脲；
(b)噻二唑聚(醚)乙二醇，其提供1500ppm至3500ppm的硫，优选2000ppm至2800ppm的S；
(c)二烃基二硫代磷酸钼，其提供77ppm至450ppm的钼(Mo)，优选192ppm至220ppm的Mo；
(d)二烃基二硫代磷酸锌，其提供600ppm至1000ppm的锌(Zn)，优选700ppm至900ppm的Zn。
本发明还公开了用于润滑脂的添加剂组合物。该添加剂组合物由下述化合物组成：
(a)噻二唑聚(醚)乙二醇复合物；
(b)二烃基二硫代磷酸钼；
(c)二烃基二硫代磷酸锌。
并且S∶Mo∶Zn的重量比为约150-350∶7.7-45∶60-100。在该比率中，S意指由噻二唑/聚(醚)乙二醇复合物提供的硫。
发明详述
本发明的噻二唑/聚(醚)乙二醇复合物描述于美国专利6,365,557号，其通过引用并入本文。优选的实施方案包含下述的复合物：
(a)一种或多种如下的噻二唑化合物：
(i)具有下述通式的2，5-二巯基-1，3，4-噻二唑(DMTD)的二聚物：
Figure GPA00001153329300021
其中n为1和/或2；和/或
(ii)具有下式的2-巯基-1，3，4-噻二唑(MTD)：
Figure GPA00001153329300022
以及(b)具有下述通式的聚(醚)乙二醇：
其中，R1为氢、支链或直链C1至C20烷基、苯基、C1至C8支化的直链酰基及上述的组合，并且m为1至300。优选的聚(醚)乙二醇是丁氧基三甘醇、聚乙二醇或上述的组合，并且后一种组合是最优选的。
如上文所示，
(a)噻二唑可以是DMTD的一硫化物二聚物(通式I，n＝1)、DMTD的二硫化物二聚物(通式I，n＝2)和MTD(通式II)中的一种或多种；并且该噻二唑可以与下述化合物复合：
(b)聚(醚)乙二醇(通式III)。
复合物可以包含约10％至60％重量比的噻二唑化合物和约40％至90％重量比的聚(醚)乙二醇化合物；优选约25％至50％重量比的噻二唑化合物和约50％至75％重量比的聚(醚)乙二醇化合物；并且最优选约30％至40％重量比的噻二唑和约60％至70％重量比的聚(醚)乙二醇。
复合物的最优实施方案如下：来自Norwalk，CT的R.T.范德比尔特公司的Vanlube972M添加剂。Vanlube 972M包含大约：(a)15％重量比的DMTD的一硫化物二聚物、10％重量比的DMTD的二硫化物二聚物、10％重量比的MTD；和(b)49％重量比的丁氧基三甘醇及16％重量比的聚乙二醇；并且平均分子量为每摩尔300克。
二烃基二硫代磷酸钼和二烃基二硫代磷酸锌化合物通常通过下述方法来制备：使P2S5与醇反应以形成二烃基二硫代磷酸化合物，然后将其用合适的钼化合物或锌化合物中和：
其中，R2和R3独立地是含有1至18个碳原子、优选2至12个碳原子的烃基，包括烷基、烯基、芳基、芳基烷基、烷基芳基和脂环基。烃基的实例是乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、异辛基、2-乙基己基和丁基苯基。对于二烃基二硫代磷酸钼，o为2和4，x为1至2，y为1至4，z为1至4。
测试方法
本发明中用于评价润滑脂组合物的极端压力、抗腐蚀性和磨损特性的测试方法如下：
1.铁姆肯(Timken)EP测试
2.铜带(Copper Strip)测试
3.4球磨损测试
铁姆肯测试是已知的标准化测试，并且描述于ASTM D 2509中。铁姆肯测试测量在旋转杯与固定块(stationary block)之间发生磨损，即擦伤时的负荷；因此，铁姆肯OK负荷越高，润滑脂的EP特性越好。下文提供了基于铁姆肯OK负荷性能的非正式EP排名；其中60-80(优良或优异)的任何值被认为对工业标准是可接受的：
  铁姆肯OK负荷(lb.)   EP性能排名
  80   优异
  60-70   优良
  50   良好
  40   一般
铜带测试方法ASTM D 4048用于评价润滑脂组合物的铜腐蚀特征。在该测试方法中，将抛光的铜带完全浸入润滑脂样品中，并于100℃下在炉中加热24小时。在该时间段的末尾，将带移除、洗涤并与ASTM铜带腐蚀标准进行比较。将铜带分级为1a至4b。1a的等级表示具有最少量腐蚀的带，而4c表示具有最大量腐蚀的带。商业润滑脂是不腐蚀的，并且获得不高于1b的等级。
根据ASTM D4172中所述的标准程序进行4球磨损测试。在该测试方法中，将1个球在3个均匀放置的静止球上转动，同时使4个球完全没入测试油中。于75℃下，以40kg的负荷和1200rpm的转速，将用于本发明的测试进行1小时。测量3个静止球的擦痕直径，结果是3个球的平均值。对于该测试，可接受的结果是直径小于0.5mm的平均擦痕。
实施例1
将含有噻二唑聚(醚)乙二醇复合物(来自Norwalk，CT的R.T.范德比尔特公司的Vanlube
Figure GPA00001153329300051
972M添加剂)、Vanlube 972M与二烷基二硫代磷酸钼(来自R.T.范德比尔特公司的Molyvan
Figure GPA00001153329300052
L添加剂)的组合、用10-20％的油稀释的Vanlube 972M与二烷基二硫代磷酸锌(来自Lubrizol Corp.的Lubrizol
Figure GPA00001153329300053
1395)的组合以及Vanlube 972M与MolyvanL和Lubrizol 1395的组合的锂润滑脂的磨损、EP和腐蚀特性。表1中汇总的数据表明，只有用全部三种组分和特定浓度处理的润滑脂具有优良至优异的铁姆肯OK负荷和可接受的擦痕及铜腐蚀等级。另外，配方10、11、12和13的数据表明，诸如二烷基二硫代氨基甲酸钼(Molyvan
Figure GPA00001153329300054
822)和有机钼酸盐(Molyvan
Figure GPA00001153329300055
855)的其它钼化合物并非MoDTP的有效替代选择。
表1
  1   2   3   4   5   6   7   8   9   10   11   12   13
  Vanlube 972M1   2.0   1.0   2.0   2.0   1.0   1.0   1.0   1.0   1.0   1.0   1.0   1.0   1.0
  Lubrizol 13952   ---   ---   1.0   ---   1.0   ---   ---   0.50   0.75   0.75   0.75   0.75   0.75
  Molyvan L3   ---   ---   ---   1.0   ---   1.0   0.5   0.25   0.25   ---   ---   ---   ---
  Molyvan 8224   ---   ---   ---   ---   ---   ---   ---   ---   ---   0.25   0.50   ---   ---
  Molyvan 8555   ---   ---   ---   ---   ---   ---   ---   ---   ---   ---   ---   0.25   0.50
  S含量，ppm   4800   2400   4800   4800   2400   2400   2400   2400   2400   2400   2400   2400   2400
  Mo含量，ppm   0   0   0   825   0   825   412   206   206   123   246   198   396
  Zn含量，ppm   0   0   1060   1060   0   0   530   795   795   795   795   795
  4球磨损，mm   0.64   0.58   0.61   0.52   0.53   0.46   0.44   0.47   0.46   0.52   0.51   0.48   0.53
  铁姆肯OK负荷，lb.   80   失败40   ---   ---   ---   ---   70   60   80   失败40   失败40   失败40   ---
  铜腐蚀   2e   2e   4a   2e   3a   4b   2e   3a   1b   1b   1b   1b   1b
1Vanlube 972M的硫含量为24％(重量比)。
3Lubrizol 1395的锌含量为10.6％。
3Molyvan L的钼含量为8.3％。
4Molyvan 822的钼含量为4.9％.
5Molyvan 855的钼含量为7.9％.
实施例2(比较实施例)
作为比较实施例，用其它基于磷酸和锌的抗磨损(AW)添加剂代替本发明的ZDDP组分，同时保持本发明的其它组分不变。如表2所汇总的，除了环烷酸锌以外，替代的选择均未提供令人满意的抗磨损性能。然而，含环烷酸锌的组合物的EP性能不令人满意。
表2(比较实施例)
  14   15   16   17   18   19
  Vanlube 972M   1.00   1.00   1.00   1.00   1.00   1.00
  Molyvan L   0.25   0.25   0.25   0.25   0.25   0.25
  Vanlube 7611M(无灰二烷基二硫代磷酸AW添加剂) 0.75 --- --- --- --- ---
  Vanlube 9123(磷酸胺盐AW添加剂) --- 0.75 --- --- --- ---
  Vanlube 727(无灰二烷基二硫代磷酸AW添加剂) --- --- 0.75 --- --- ---
  Vanlube 672(磷酸胺盐AW添加剂) --- --- --- 0.75 --- ---
  Vanlube AZ(50％二烷基二硫代氨基甲酸锌) --- --- --- --- 1.30 ---
  环烷酸锌   0.75
  4球磨损，mm   0.58   0.53   0.57   0.56   0.51   0.47
  铁姆肯OK负荷，lb   ---   ---   ---   ---   ---   失败40
  铜腐蚀   ---   ---   ---   ---   3a   1b
实施例3(比较实施例)
为了进行比较，用其它噻二唑衍生物代替本发明的噻二唑聚(醚)乙二醇复合物组分。如表3所汇总的，替代的选择均未提供令人满意的EP性能：
表3(比较实施例)
Figure GPA00001153329300061

Claims (2)

1.润滑剂组合物，包含以重量%表示的：
至少90%的基础润滑脂；以及
(a)提供2400ppm的硫的量的噻二唑聚(醚)乙二醇复合物；并且所述噻二唑聚(醚)乙二醇复合物包含：
(i)15%的DMTD的一硫化物二聚物、10%的DMTD的二硫化物二聚物、10%的MTD；以及
(ii)45%的丁氧基三甘醇及15%的聚乙二醇；
(b)提供206ppm的钼的量的二烃基二硫代磷酸钼；和
(c)提供795ppm的锌的量的二烃基二硫代磷酸锌，
其中所述DMTD的一硫化物二聚物具有
Figure FDA0000451202900000011
其中n为1；
所述DMTD的二硫化物二聚物具有
Figure FDA0000451202900000012
其中n为2；以及
所述MTD具有
Figure FDA0000451202900000013
2.用于润滑脂的添加剂，包含：
(a)噻二唑聚(醚)乙二醇复合物，并且所述噻二唑聚(醚)乙二醇复合物包含：
(i)15%的DMTD的一硫化物二聚物、10%的DMTD的二硫化物二聚物、10%的MTD；以及
(ii)45%的丁氧基三甘醇及15%的聚乙二醇；
(b)二烃基二硫代磷酸钼；和
(c)二烃基二硫代磷酸锌，
(a)所述噻二唑聚(醚)乙二醇复合物提供的硫的重量、(b)所述二烃基二硫代磷酸钼提供的钼的重量和(c)所述二烃基二硫代磷酸锌提供的锌的重量的(a):(b):(c)比率被计算为240:20.6:79.5，
其中所述DMTD的一硫化物二聚物具有
Figure FDA0000451202900000021
其中n为1；
所述DMTD的二硫化物二聚物具有
Figure FDA0000451202900000022
其中n为2；以及
所述MTD具有
CN200880119720.2A 2007-12-14 2008-12-11 具有优异抗磨损和抗腐蚀特性的用于ep润滑脂的添加剂组合物 Active CN101889019B (zh)

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