CN1069691C - 用于等速万向节的润滑脂组合物 - Google Patents

用于等速万向节的润滑脂组合物 Download PDF

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CN1069691C
CN1069691C CN97113570A CN97113570A CN1069691C CN 1069691 C CN1069691 C CN 1069691C CN 97113570 A CN97113570 A CN 97113570A CN 97113570 A CN97113570 A CN 97113570A CN 1069691 C CN1069691 C CN 1069691C
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calcium salt
constant velocity
grease composition
high alkaline
velocity cardan
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CN1168916A (zh
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畠山康
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Kyodo Yushi Co Ltd
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Kyodo Yushi Co Ltd
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Abstract

一种用于等速万向节的润滑脂组合物，主要由如下组分组成：(a)基础油；(b)脲增稠剂；(c)二硫化钼；(d)选自如下的钙盐或者高碱性钙盐：氧化蜡的钙盐或高碱性钙盐、石油磺酸的钙盐或高碱性钙盐、烷基芳基磺酸的钙盐或高碱性钙盐、水扬酸的钙盐或高碱性钙盐或者酚的钙盐或高碱性钙盐；(e)不含金属的硫-磷极压剂；和(f)二硫代氨基甲酸钼。该润滑脂组合物显示出极好的耐磨性能和耐点蚀作用。

Description

用于等速万向节的润滑脂组合物
本发明涉及用于等速万向节的润滑脂组合物，更具体地说，本发明涉及用于球形固定的和滑叉式等速万向节的润滑脂组合物。要润滑的等速万向节的部件之间会产生非常高的接触压力，并且这些连接部件经受复杂的滚动和滑动运动。这就常常导致不正常的磨损和金属疲劳，然后，就导致碎裂现象，即连接部件的点蚀。更特别的是，本发明涉及用于等速万向节的润滑脂组合物，该润滑脂组合物可以有效地润滑这些等速万向节，有效地降低万向节的磨损，并且有效地降低部件的任何点蚀的发生。
通常用于这样的等速万向节的润滑脂的例子包括含有二硫化钼的锂皂增稠极压润滑脂和含有二硫化钼和极压剂例如硫-磷或者环烷酸铅的锂皂增稠极压润滑脂。但是，这些用于等速万向节的润滑脂在目前的高性能汽车所产生的苛刻的工况条件下不总是那么令人满意的。
最近，四轮驱动(FF-型)汽车的数量迅速增加，为了用于这些汽车，等速万向节需要做的尽可能的轻和尽可能的小。用作滑叉式万向节的双效补偿型等速万向节和交错沟槽型(cross groove type)等速万向节以及用作固定万向节的Birfield万向节有一种其中通过6个球传送的扭转结构。在高接触压力的情况下旋转的过程中这些万向节发生复杂的往复运动例如复杂的滚动和滑动运动，应力重复的施加到球上和金属的表面上，使金属表面与球接触，因此，由于金属的疲劳，在这些部位往往产生点蚀现象。与常规的发动机比较，近期的发动机功率方面的改善就伴随着接触压力的增加。为了改善燃料的消耗，汽车造的更小了，因此万向节的大小相应的变小。这就使得接触压力相对的增加，因此常规的润滑脂是无效的，因为在其中它们不能有效地降低点蚀现象。另外，润滑脂的耐热性能方面也必须改善。
因此，本发明的一个目的是提供一种新的用于等速万向节的润滑脂组合物，该润滑脂组合物有很好的耐点蚀性能和耐热性能。
本发明的发明人已进行了很多研究，以开发出一种润滑脂组合物，该组合物能够使等速万向节有最适宜的磨损，并且消除由于非正常的磨损和金属疲劳而产生的点蚀的问题，并且该组合物改善了耐热性。本发人已经使用叫做振荡摩擦和磨损试验机的SRV(SchwingungReibung und Verschleiss)试验机，在如上述的高接触压力下，在伴随复杂的往复运动例如复杂的滚动和滑动的润滑条件下，进行了所用润滑脂的质量评定试验，来测定各种类型的极压剂、固体润滑剂或者添加剂混合物的润滑性能(例如摩擦系数和磨耗)。结果，发明人发现含有基础油、脲增稠剂、二硫化钼、特殊化合物的钙盐或高碱性钙盐、不含金属的硫-磷极压剂和二硫代氨基甲酸钼的混合物显示出所需要的润滑性能例如很好的摩擦系数和低的磨损，并且已通过使用实际的等速万向节进行的耐久性试验证实，该润滑脂可以防止任何的点蚀现象的产生，其不像用于等速万向节的那些常规润滑脂，因此就完成了本发明。
通过提供用于等速万向节的主要由下列组分组成的润滑脂组合物可以有效地达到本发明的上述目的：
(a)基础油；
(b)脲增稠剂；
(c)二硫化钼；
(d)选自下述的钙盐或者高碱性钙盐：氧化蜡的钙盐、石油磺酸的钙盐、烷基芳基磺酸的钙盐、水扬酸的钙盐、酚的钙盐、氧化蜡的高碱性钙盐、石油磺酸的高碱性钙盐、烷基芳基磺酸的高碱性钙盐、水扬酸的高碱性钙盐、酚的高碱性钙盐；
(e)不含金属的硫-磷极压剂；和
(f)二硫代氨基甲酸钼。
下面要对本发明进行更详细的解释。
作为组分(a)的基础油并不被限制到具体的某几种，其可以是例如通常所用的润滑油如矿物油、酯型合成油、醚型合成油、烃型合成油或其混合物。
作为组分(b)的脲增稠剂并不被限制到具体的某几种，其可以是例如双脲化合物和聚脲化合物。
双脲化合物的例子包括那些通过单胺与二异氰酸酯化合物反应得到的化合物。二异氰酸酯化合物的例子包括二异氰酸亚苯酯、二异氰酸二苯酯、二异氰酸苯酯、二苯基甲烷二异氰酸酯、十八烷二异氰酸酯、癸烷二异氰酸酯和己烷二异氰酸酯。单胺的例子包括辛胺、十二胺、十六胺、十八胺、油胺、苯胺、对甲苯胺和环己胺。
聚脲化合物的例子包括那些通过二胺与二异氰酸酯化合物反应得到的化合物。二异氰酯化合物的例子包括用来生成如上所述的双脲化合物的那些二异氰酸酯。二胺的例子包括乙二胺、丙二胺、丁二胺、己二胺、辛二胺、苯二胺、甲苯二胺和二甲苯二胺。
优选的脲增稠剂的例子包括那些通过芳胺例如苯胺或对甲苯胺、环己胺或其混合物与二异氰酸酯反应得到的化合物。在双脲化合物中的芳基优选是具有6个或者7个碳原子的那些，并且在双脲化合物中的芳基的比率，以在双脲化合物中的芳基和环己基的总摩尔数计，为100-0摩尔％。
作为(c)组分的二硫化钼已广泛地用作极压剂。关于其润滑机理，在滑动的情况下通过形成一薄层，因为其具有层格结构，所以二硫化钼很容易剪切，并且其表现出有减少摩擦力的作用和防止万向节卡住的作用。已经知道有具有不同粒度的二硫化钼产品，但是在本发明中优选的是使用以平均粒度表示的粒度为0.25-10μm的那些产品，特别是平均粒度为0.55-0.85μm的那些产品，平均粒度是用叫做Fisher法(通过使用Fisher亚筛粒度分析仪)的方法测定的。
作为组分(d)的钙盐或者高碱性钙盐选自用在润滑剂如发动机油中的叫做金属清净分散剂或者防锈剂的那些，例如氧化蜡的钙盐、通过润滑油馏分中的芳烃的磺化得到的石油磺酸的钙盐、合成磺酸的钙盐例如二壬基萘磺酸和烷基苯磺酸的钙盐、水扬酸的钙盐、酚的钙盐、氧化蜡的高碱性钙盐、石油磺酸的高碱性钙盐、烷基芳基磺酸的高碱性钙盐、水扬酸的高碱性钙盐和酚的高碱性钙盐。
作为组分(e)的优选的不含金属的硫-磷极压剂，其硫含量为15-35％(重)，磷含量为0.5-3％(重)，并且通过很好建立的硫和磷含量之间的平衡，其显示出很好的耐磨作用和防止万向节卡住的作用。更特别的是，如果硫含量超过上述规定的上限，万向节就很容易腐蚀，而如果磷含量超过上述规定的上限，就不能达到其预期的耐磨效果。另一方面，如果硫和磷的含量都低于相应的下限，同样不能达到本发明的任何所需要的效果。
作为组分(f)的二硫代氨基甲酸钼优选的是由下面的式子表示：
           (R1R2N-CS-S)2-Mo2OmSn其中，R1和R2独立地代表具有1-24个碳原子，优选3-18个碳原子的烷基，m是0-3，n是4-1，并且m+n＝4。
根据本发明的用于等速万向节的润滑脂组合物除了含有上述的基本组分之外，还可以含有抗氧化剂、防腐剂、防锈剂。
根据本发明的用于等速万向节的润滑脂组合物，以润滑脂组合物的总重量计，优选的是含有52.0-97.8％(重)的基础油(a)；1-25％(重)的脲增稠剂(b)；0.5-5.0％(重)的二硫化钼(c)；0.5-15％(重)的钙盐或者高碱性钙盐(d)；0.1-3％(重)的不含金属的硫-磷极压剂(e)；和0.1-5％(重)的二硫代氨基甲酸钼(f)。
如果脲增稠剂(b)的量少于1％(重)，其增稠效果往往变的太低，以致于不能转化该组合物成为润滑脂，而如果其量超过25％(重)，所生成的组合物往往变的太硬，以致于不能保证所需要的本发明的效果。此外，如果二硫化钼(c)的量低于0.5％(重)，钙盐或者高碱性钙盐(d)的量低于0.5％(重)，不含金属的硫-磷极压剂(e)的量低于0.1％(重)，或者二硫代氨基甲酸钼(f)的量低于0.1％(重)，就变的难以得到所需要的本发明的效果。另一方面，如果二硫化钼(c)的量超过5％(重)，钙盐或者高碱性钙盐(d)的量超过15％(重)，不含金属的硫-磷极压剂(e)的量超过3％(重)，或者二硫代氨基甲酸钼(f)的量超过5％(重)，就不能期望效果上有任何进一步的改善，并且这些组分相反的影响本发明的抑制点蚀的效果。
下面将根据下述的非限定的操作实施例和比较实施例更详细地描述本发明。
实施例1-9和比较实施例1-3
在一个容器中，加入4100g基础油和1012g二苯基甲烷4，4＇-二异氰酸酯，把该混合物加热到70-80℃。在另外一个容器中加入4100g基础油、563g环己胺和225g苯胺，接着在70-80℃的温度下加热，并且把其加到上述的容器中。然后，在充分搅拌的情况下使该混合物反应30分钟，在搅拌下反应体系的温度升到160℃，使反应体系冷却，得到一种基础脲润滑脂。向该基础润滑脂中加入下面的表1中所列量的所列添加剂和任意的附加量的基础油，用三级辊压机调节生成的混合物的针入度到No.1级。
实施例10
在一个容器中，加入440g基础油和58.9g 4，4＇-二异氰酸二苯基甲烷，把该混合物加热到70-80℃。在另外一个容器中加入440g基础油、61.1g辛胺，接着在70-80℃的温度下加热，并且把其加到上述的容器中。然后，在充分搅拌的情况下使该混合物反应30分钟，在搅拌下反应体系的温度升到160℃，使反应体系冷却，得到一种基础脂肪胺脲润滑脂。向该基础润滑脂中加入下面的表1中所列量的所列添加剂和任意的另外量的基础油，用三级辊压机调整生成的混合物的针入度到No.1级。
在所有的上述的实施例和比较例中，使用具有下面的性能的矿物油作为基础油。
         粘度：        在40℃     157mm2/s
                       在100℃    14mm2/s
         粘度指数：    88
另外，从市场上可以买到的含有二硫化钼、硫-磷极压剂和环烷酸铅的锂基润滑脂用作比较实施例4的润滑脂。
这些润滑脂的物理性能按照下面所述的方法进行评价。这样得到的结果也汇总于表1。
[针入度]      按照ISO 2137。
[滴点]        按照ISO 2176。
[SRV试验]
试验件：球：  直径10mm          (SUJ-2)
    柱面板：  直径24mm×7.85mm  (SUJ-2)
评价条件：
负载：        500N
频率：        15Hz
振幅：        3000μm
时间：        10分钟
试验温度：    25℃
评价的项目：  最大摩擦系数
              在球上观察到的磨损伤痕的平均直径(mm)
              在板上观察到的磨损的最大深度(μm)
[使用真实万向节的耐久性台架试验]
在下面的条件下，通过使用真实万向节的耐久性台架试验，观察润滑脂发生点蚀的情况。
试验条件：
转速：                1000rpm
转矩：                392N·m
万向节的角度：        8°
操作时间：            100小时
所用的万向节的类型：  Birfield万向节
                      交错沟槽型万向节
评价的项目：操作之后每个部件发生点蚀的情况。
                         表1
                                         实施例 组分                       1       2       3       4       5  1)双脲润滑脂①             94.0    94.0    93.5    93.5    94.02)双脲润滑脂②              -       -       -       -       -3)二硫化钼                 3.0     3.0     3.0     3.0     3.04)氧化蜡的钙盐             2.0      -       -       -       -5)石油磺酸钙                -      2.0      -       -       -6)萘磺酸钙                  -       -      2.0      -       -7)水扬酸钙                  -       -       -      2.0      -8)苯酚钙                    -       -       -       -      2.09)磺酸钙①                  -       -       -       -       -10)磺酸钙②                 -       -       -       -       -11)S-P极压剂               0.5     0.5     0.5     0.5     0.512)二硫代氨基甲酸钼①      0.5     0.5      -       -      0.513)二硫代氨基甲酸钼②       -       -      1.0     1.0      -评价试验14)针入度(60W)             321     327     335     326     32915)滴点(℃)                260＜   260＜   260＜   260＜   260＜16)SRV试验 最大摩擦系数    0.06    0.06    0.06    0.06    0.0617)磨损伤痕的直径(mm)      0.62    0.63    0.59    0.61    0.6118)磨损深度(μm)           0.4     0.4     0.4     0.4     0.4耐久性试验19)Birfield万向节          ○      ○      ○      ○      ○20)交错沟槽型万向节        ○      ○      ○      ○      ○
                          表1(续)
                                            实施例 组分                           6       7       8       9       10  1)双脲润滑脂①                 94.0    93.5    94.0    92.5     -2)双脲润滑脂②                  -       -       -       -      93.53)二硫化钼                     3.0     3.0     3.0     3.0     3.04)氧化蜡的钙盐                  -       -       -       -       -5)石油磺酸钙                    -       -       -       -       -6)萘磺酸钙                      -       -      2.0     2.0     2.07)水扬酸钙                      -       -       -       -       -8)苯酚钙                        -       -       -       -       -9)磺酸钙①                     2.0      -       -       -       -10)磺酸钙②                     -      2.0      -       -       -11)S-P极压剂                   0.5     0.5     0.5     0.5     0.512)二硫代氨基甲酸钼①          0.5      -       -       -       -13)二硫代氨基甲酸钼②           -      1.0     0.5     2.0     1.0评价试验14)针入度(60W)                 332     325     328     324     31715)滴点(℃)                    260＜   260＜   260＜   260＜   260＜16)SRV试验最大摩擦系数         0.06    0.06    0.06    0.06    0.0617)磨损伤痕的直径(mm)          0.60    0.60    0.61    0.61    0.6218)磨损深度(μm)               0.4     0.4     0.4     0.4     0.4耐久性试验19)Birfield万向节               ○      ○      ○      ○      ○20)交错沟槽型万向节             ○      ○      ○      ○      ○
                           表1(续)
                                       比较实施例 组分                            1          2         3         4  1)双脲润滑脂①                  97.0       98.0      98.02)双脲润滑脂②                   -          -         -3)二硫化钼                      3.0         -         -4)氧化蜡的钙盐                   -          -         -5)石油磺酸钙                     -          -         -6)萘磺酸钙                       -         2.0        -7)水扬酸钙                       -          -         -8)苯酚钙                         -          -         -9)磺酸钙①                       -          -        2.010)磺酸钙②                      -          -         -11)S-P极压剂                     -          -         -12)二硫代氨基甲酸钼①            -          -         -13)二硫代氨基甲酸钼②            -          -         -评价试验14)针入度(60W)                  324        321       321         28015)滴点(℃)                     260＜      260＜     260＜       19016)SRV试验最大摩擦系数          0.15＜     0.09      0.15＜      0.15＜17)磨损伤痕的直径(mm)           I.M.*     0.63      I.M.        I.M.18)磨损深度(μm)                I.M.       0.6       I.M.        I.M.耐久性试验19)Birfield万向节               ×                    ×                  ×                      ×20)交错沟槽型万向节             ×                    ×                  ×                      ×
*：I.M.＝不能测量
1)使用其中环己胺和苯胺用作单胺的双脲化合物的双脲润滑脂。
2)使用其中辛胺用作单胺的双脲化合物的双脲润滑脂。
3)从Climax Molybdenum Company买到的商品名为Molysulfide的二硫化钼，平均粒度：0.7μm。
4)从Alox corporation买到的商品名为Alox 165的氧化蜡的钙盐。
5)从Matsumura Petroleum Laboratory Co.，Ltd.买到的商品名为Sulfol Ca-45的石油磺酸钙盐。
6)从King Industries Co.，Ltd.买到的商品名为NA-SUL 729的二壬基萘磺酸钙盐。
7)从Osca Chemical Co.，Ltd.买到的商品名为OSCA 423的水扬酸钙。
8)从Oronite Japan Co.，Ltd.买到的商品名为OLOA 218A的苯酚钙。
9)从Lubrizol Japan买到的商品名为Lubrizol 5283的高碱性磺酸钙①。
10)从Witco Corporation买到的商品名为Bryton C-400C的高碱性磺酸钙②。
11)从Lubrizol Japan买到的商品名为Anglamol 99的硫-磷极压剂。
12)从R.T.Vanderbilt买到的商品名为Molyvan A的二硫代氨基甲酸钼①。
13)从R.T.Vanderbilt买到的商品名为Molyvan 822的二硫代氨基甲酸钼②。
14)根据ISO 2137的针入度。
15)根据ISO 2176的滴点(℃)。
16)最大的摩擦系数。
17)在球上观察到的磨损伤痕的平均直径(mm)。
18)在板上观察到的磨损的最大深度(μm)。
19)用真实万向节的耐久性台架试验
         Birfield万向节。
20)用真实万向节的耐久性台架试验
交错沟槽型万向节。
在耐久性试验中，根据下面的标准评价这些润滑脂：
○：没有观察到点蚀；
×：观察到点蚀；
如上面所详细讨论的，按照本发明的用于等速万向节的润滑脂组合物基本上由(a)基础油；(b)脲增稠剂；(c)二硫化钼；(d)特殊的钙盐或者特殊的高碱性钙盐；(e)不含金属的硫-磷极压剂；和(f)二硫代氨基甲酸钼组成，因此由实施例的结果和比较实施例的结果比较可以看出，本发明的润滑脂组合物呈现出极好的耐磨作用和极好的耐点蚀作用。

Claims (4)

1.一种用于等速万向节的润滑脂组合物，按组合物的总重量计，其主要组成如下：
(a)52.0-97.8％的基础油；
(b)1-25％的脲增稠剂；
(c)0.5-5.0％的二硫化钼；
(d)0.5-15％的选自如下的钙盐或者高碱性钙盐：氧化蜡的钙盐、石油磺酸的钙盐、烷基芳基磺酸的钙盐、水扬酸的钙盐、酚的钙盐、氧化蜡的高碱性钙盐、石油磺酸的高碱性钙盐、烷基芳基磺酸的高碱性钙盐、水扬酸的高碱性钙盐和酚的高碱性钙盐；
(e)0.1-3％的不含金属的硫-磷极压剂；和
(f)0.1-5％的二硫代氨基甲酸钼。
2.权利要求1的用于等速万向节的润滑脂组合物，其中，不含金属的硫-磷极压剂(e)中硫的含量为15-35％(重)，磷的含量为0.5-3％(重)。
3.权利要求1或2的用于等速万向节的润滑脂组合物，其中，所说的等速万向节是等速滑叉式球形万向节。
4.权利要求1或2的用于等速万向节的润滑脂组合物，其中，所说的等速万向节是等速固定球形万向节。
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US5160645A (en) * 1991-04-30 1992-11-03 Ntn Corporation Grease composition for constant velocity joint
US5449471A (en) * 1993-05-25 1995-09-12 Showa Shell Seikyu K.K. Urea grease compostition
US5516439A (en) * 1994-07-15 1996-05-14 Kyodo Yushi Co., Ltd. Grease composition for constant velocity joints

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102575719A (zh) * 2009-10-22 2012-07-11 Ntn株式会社 固定型等速万向接头
CN102575719B (zh) * 2009-10-22 2016-01-20 Ntn株式会社 固定型等速万向接头

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JP3320611B2 (ja) 2002-09-03
JPH09324189A (ja) 1997-12-16
EP0811675B1 (en) 2001-12-12
EP0811675A1 (en) 1997-12-10
KR100410724B1 (ko) 2004-03-30
ES2164991T3 (es) 2002-03-01
KR980002219A (ko) 1998-03-30
TW349118B (en) 1999-01-01
DE69708974T2 (de) 2002-08-08
DE69708974D1 (de) 2002-01-24
CN1168916A (zh) 1997-12-31

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