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CN1446251A - 具有改进的防锈和耐磨损性能的润滑脂组合物 - Google Patents

具有改进的防锈和耐磨损性能的润滑脂组合物 Download PDF

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Publication number
CN1446251A
CN1446251A CN01813908A CN01813908A CN1446251A CN 1446251 A CN1446251 A CN 1446251A CN 01813908 A CN01813908 A CN 01813908A CN 01813908 A CN01813908 A CN 01813908A CN 1446251 A CN1446251 A CN 1446251A
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Prior art keywords
grease composition
benzotriazole
grease
additives
composition according
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CN01813908A
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CN1191341C (zh
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尾崎幸洋
筱田宪明
中沢贡一
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Shell Internationale Research Maatschappij BV
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Shell Internationale Research Maatschappij BV
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Abstract

一种含有基础油和增稠剂的润滑脂组合物，以整个润滑脂组合物为基准，该润滑脂中附加含有0.05wt％－30wt％的硫代硫酸钠和至少0.1wt％的一种或多种选自水杨酸钙、水杨酸镁、苯酚钙和/或磺酸钙的添加剂(A)；使用所述润滑脂组合物以改进防锈和抗磨损性，以及制备所述润滑脂组合物的方法。

Description

具有改进的防锈和耐磨损性能的润滑脂组合物
本发明涉及具有改进的防锈和耐磨损性能的润滑脂组合物。
极限压力润滑脂具有许多用途，因为其具有良好的耐磨损性以及抗负荷能力，例如用于汽车的轴承和齿轮、钢铁、轨道和各种其它工业机械设备上。
一般来说，典型的极限压力润滑脂组合物包括各种类型的润滑脂、添加剂例如硫化烯烃、硫化油脂、硫-磷基极限压力剂、油制品、二硫化钼、有机钼化合物、铅化合物和二硫代磷酸锌。
近来的技术已经公开了含有硫代硫酸钠的润滑脂组合物，其具有良好的极限压力性能：在日本公开专利3-131690、日本公开专利11-35965和美国专利4,923,625中已经公开。
但是，在这些现有技术文献中，耐磨损性不能令人满意，并且更进一步存在生锈的可能，这是因为硫代硫酸钠具有吸湿性能。具体来说，由于在含有大量水的条件下，使钢设备和粮食机器的轴承和齿轮润滑，这样会促进产品生锈而且容易产生与润滑相关的问题。
所以，非常需要提供一种润滑脂组合物，其中含有硫代硫酸钠的润滑脂组合物的极限压力性能保持良好，同时能抑制铁锈的产生并且也改进抗磨损性。
本发明提供一种含有基础油和增稠剂的润滑脂组合物，以整个润滑脂组合物为基准，该润滑脂中附加含有0.05wt％-30wt％的硫代硫酸钠和至少0.1wt％的一种或多种选自水杨酸钙、水杨酸镁、苯酚钙和/或磺酸钙的添加剂(A)。
在优选的具体实施方式中，以整个润滑脂组合物为基准，本发明的润滑脂组合物更进一步含有至少0.1wt％的苯并三唑化合物(B)。
在根据本发明的润滑脂组合物中，增稠剂可以是如尿素化合物、锂皂、锂复合皂和铝复合皂的试剂，其可以单独或混合使用。除了具有尿素键的化合物之外，尿素化合物本质上可以是含有尿素键和尿烷键的化合物。可以便利地使用双脲、三脲和/或四脲增稠剂。也可以便利地使用脲亚氨化合物作为增稠剂。
在本发明的优选具体实施方案中，以整个润滑脂组合物为基准，使用2-35wt％的增稠剂。
根据本发明使用的基础油可以是植物油、矿物油和合成油例如酯油、醚油和烃油。
根据本发明使用的硫代硫酸钠可以是Na2S2O3(无水的)或者Na2S2O3·5H2O(五水合物)，或其混合物。也可以使用含有硫代硫酸钠的商业添加剂(例如Desilube 88，Desilube Technology Incorporated，USA)。
以整个润滑脂组合物为基准，优选添加硫代硫酸钠用量的范围是0.2wt％-20wt％，更优选的范围是0.2wt％-10wt％，更优选的范围是0.2wt％-8wt％和最优选的范围是0.5wt％-6wt％。
以整个润滑脂组合物为基准，优选地，选自水杨酸钙、水杨酸镁、苯酚钙和/或磺酸钙的一种或多种添加剂(A)，每种用量的范围是0.1wt％-5wt％，更优选范围是0.2wt％-3wt％。
以整个润滑脂组合物为基准，优选苯并三唑(B)用量的范围是0.1wt％-5wt％，更优选的范围是0.2wt％-3wt％。
当上述添加剂(A)的量少于0.1wt％时，防锈作用不够，当上述添加剂(B)的量少于0.1wt％时，抗磨损性促进作用不够。
当任何一种添加剂的量多于5％时，在其效果方面具有局限性或没有更进一步的增加。
上述苯并三唑(B)的实施例包括1，2，3-苯并三唑，2-(2’-羟基-5’-甲基苯基)苯并三唑，2-[2’-羟基-3’-(3″，4″，5″，6″-四氢邻苯二甲酰亚氨基甲基)-5’-甲基苯基]苯并三唑，2-(2’-羟基-3’，5’-二叔丁基苯基)苯并三唑，2-(2’-羟基-5’-叔辛基苯基)苯并三唑，2-(2’-羟基-3’，5’-二叔戊基苯基)苯并三唑，2-[2-羟基-3，5-双(α，α-二甲基苄基)苯基]-2H-苯并三唑和2-(2’-羟基-3’-十一烷基-5’-甲基苯基)苯并三唑。
本发明的润滑脂组合物可以更进一步含有附加添加剂，例如抗氧化剂如胺和苯酚；极限压力添加剂如硫化烯烃和硫化油脂；抗极限压力/磨损剂如亚磷酸盐和磷酸盐；增稠剂如聚丁烯和聚甲基丙烯酸酯；固体润滑剂如氮化硼和二硫化钼；和各种其它添加剂。
根据本发明的润滑脂组合物可以通过预先混合硫代硫酸钠，选自水杨酸钙、水杨酸镁、苯酚钙和/或磺酸钙的一种或多种添加剂(A)，和任何其它要加入到基础油中的添加剂，然后将混合物加入到含有基础油和增稠剂的基础润滑脂中来制备；或者通过将每种添加剂都单独加入到基础润滑脂中来制备。这些可以通过热混合或冷混合得到，随后通过均质化以确保添加剂组分的均匀分散。
根据本发明的润滑脂组合物可以方便地应用在轴承、齿轮和接头处如等速接头。
用下面的相关实施例描述本发明，但是无论如何，这些实施例不限制本发明的保护范围。
实施例 润滑脂组合物的制备
实施例和对比实施例的润滑脂是根据表1-9所给的配方得到的，将相应于上述(A)和(B)的添加剂或其他添加剂加入到基础润滑脂中，用三辊磨(three-roll mil1)处理这些物质。基础润滑脂组合物如下所示。I.尿素基础润滑脂
在纯化的矿物油(在100℃下，运动粘度大约为15毫米2/秒；5400克)中，二苯基甲烷-4，4’-二异氰酸酯(295.2克)和辛胺(304.8克)反应；将得到的尿素化合物均匀分散，由此得到稠度为289(在25℃下，60W)和滴点为263℃的尿素基础润滑脂。尿素化合物的含量为10wt％。II.锂皂基础润滑脂
将12-羟基硬脂酸锂(600克)溶解和均匀分散在纯化的矿物油中(在100℃下，运动粘度大约为15毫米2/秒；5400克)，得到稠度为268(在25℃下，60W)和滴点为199℃的锂皂基础润滑脂。锂皂的含量为10wt％。III.锂复合皂基础润滑脂
在纯化的矿物油(在100℃下，运动粘度大约为11毫米2/秒；4165克)中，12-羟基硬脂酸(350克)和氢氧化锂(50.5克)反应，然后，通过壬二酸(120.65克)和氢氧化锂(59.0克)的反应和均匀分散处理，得到稠度为281(在25℃下，60W)和滴点为259℃的复合锂皂基础润滑脂。锂复合皂的含量为10.4wt％。IV.铝复合皂基础润滑脂
将苯甲酸(158.22克)和硬脂酸(334.8克)溶解在纯化的矿物油(在100℃下，运动粘度大约为11毫米2/秒；4272克)中，然后，通过添加商业上的环状氧化铝丙醇盐(cyclic aluminium oxide propylate)润滑液[商品名：Arugoma(Algomer)，Sengen Fain Kemikaru(Sengen Fine Chemicals)K.K.生产]进行反应，得到稠度为279(在25℃下，60W)和滴点为258℃的复合铝皂基础润滑脂；处理所生产的皂以使其均匀分散。锂复合皂的含量为11wt％。苯甲酸(BA)和硬脂酸(FA)的摩尔比表示为BA/FA＝1.1∶1，苯甲酸加上硬脂酸与铝的摩尔比表示为(BA+FA)/Al＝1.9∶1。
通过进行防锈测试(湿度测试)和四球(four-ball)测试(EP测试和抗磨损测试)可以确定防锈性能、极限压力和磨损性能。湿度测试
根据JIS(日本工业标准)K2220 5.17湿度测试，将润滑脂样品均匀涂布在测试片的整个表面上，用这样的方法，涂布到测试片表面上的润滑脂的量为0.30克±0.05克。将涂布有润滑脂的钢板悬挂在49℃温度下和相对湿度至少为95％的潮湿橱柜中，2个星期之后，用生锈程度表示JIS K2246等级。
    等级     ％产生的锈
    等级A     0
    等级B     1-10
    等级C     11-25
    等级D     26-50
    等级E     51-100
EP测试
根据ASTM(美国材料测试学会)D2596，通过四球试验测定膨胀负载(N)。
测试条件：  旋转速率：1770±60转数/分
                温度：27±8℃
                时间：10±0.2秒抗磨损性测试
根据ASTM D2266测定在四球试验中所使用球上面的磨损标记的直径。
测试条件：  旋转速率：    1200±50转数/分
                温度：    75±1.7℃
                负载：    40±2千克力(392±2牛顿)
                时间：    60±1分钟添加剂
在下表中，如*1-*10所示：
Desilube 88，*1是Desilube Technology Incorporated的含硫代硫酸钠的无机S-P添加剂的商品名。
下面是根据本发明相应于上述添加剂(A)的产品。
SAP001，*2，是Infineum Limited的水杨酸钙的商品名。
SAP007，*3，是Infineum Limited的水杨酸镁的商品名。
OLOA219，*4，是Oronaito Japan(K.K)的苯酚钙的商品名。
NA-SUL 729，*5，是King Industries Incorporated的磺酸钙的商品名。
下面是根据本发明相应于上述添加剂(B)的产品。
BT-120，*6，是Shirokita Kagaku(Shirokita Chemicals)(K.K.)的1，2，3-苯并三唑的商品名。
下面是除了(A)和(B)之外的添加剂。
NA-SUL ZS，*7，是King Industries Incorporated的磺酸锌的商品名。
Dailube Z-500，*8，是Dainippon Inki Kagaku Kogyo(Dainippon Inkand Chemicals)(K.K)的稀释在矿物油(5％锌金属)中的环烷酸锌的商品名。
NA-SUL SS，*9，是King Industries Incorporated的磺酸钠的商品名。
NA-SUL 707，*10，是King Industries Incorporated的磺酸锂的商品名。
                                                           表1
实施例 1  2  3  4  5  6  7  8  9  10
组合物wt％  基础润滑脂  尿素润滑脂  95.0  95.0  95.0  95.0  95.0  95.0  95.0  95.0  95.0  95.0
添加剂  Na2S2O3  3.0  3.0  3.0  3.0
 Na2S2O3·5H2O  3.0  3.0  3.0  3.0
 Desilube 88  *1  3.0  3.0
 SAP001       *2  2.0  2.0  2.0
 SAP007       *3  2.0  2.0  2.0
 OLOA219      *4  2.0  2.0
 NA-SUL 729   *5  2.0  2.0
 BT-120       *6
  总计  100  100  100  100  100  100  100  100  100  100
测试结果   防锈测试  湿度测试  A  A  A  A  A  A  A  A  A  A
  四球测试  膨胀负载，牛顿磨损标记直径，毫米  78450.71  78450.71  78450.63  78450.71  60800.71  60800.71  60800.58  60800.68  78450.70  78450.69
                                                       表2
实施例 11  12  13  14  15  16  17  18  19  20
组合物wt％ 基础润滑脂  尿素润滑脂 95.0  95.0  93.0  93.0  94.5  94.5  94.5  92.5  93.0  93.0
添加剂  Na2S2O3  3.0  3.0  3.0  2.0
 Na2S2O3·5H2O  1.0  3.0  1.0  2.0
 Desilube 88    *1  3.0  3.0  2.0  3.0  1.0
 SAP001    *2  2.0  2.0  2.0  2.0  1.0
 SAP007    *3  2.0  1.0  1.0  1.0
 OLOA219   *4  2.0  1.0  0.5  1.0
 NA-SUL 729    *5  2.0  2.0  2.0
 BT-120        *6  0.5  0.5  2.0  0.5  2.0  2.0
总计  100  100  100  100  100  100  100  100  100  100
测试结果 防锈测试  湿度测试  A  A  A  A  A  A  A  A  A  A
四球测试  膨胀负载，牛顿磨损标记直径，毫米  78450.55  78450.68  78450.69  78450.67  78450.46  60800.43  78450.45  78450.39  78450.39  78450.45
                                                       表3
实施例  21  22  23  24  25  26  27  28  29  30
组合物wt％ 基础润滑脂 锂皂润滑脂  95.0  95.0  93.0  93.0  94.5  93.0  93.0  93.0  93.0  93.0
添加剂  Na2S2O3  2.0  2.0  3.0  2.0  2.0
 Na2S2O3·5H2O  1.0  2.0  1.0  1.0  2.0
 Desilube 88    *1  3.0  1.0  1.0  3.0  3.0  1.0
 SAP001    *2  1.0  1.0
 SAP007    *3  2.0  2.0  2.0  1.0
 0LOA219   *4  2.0  2.0  2.0  0.5  1.0  1.0  1.0  2.0
 NA-SUL 729    *5  2.0  2.0
 BT-120        *6  2.0  2.0  2.0  2.0  2.0
总计 100  100  100  100  100  100  100  100  100  100
测试结果 防锈测试  湿度测试  A  A  A  A  A  A  A  A  A  A
四球测试  膨胀负载，牛顿磨损标记直径，毫米  60800.72  60800.72  60800.71  60800.68  60800.72  60800.47  60800.49  60800.39  60800.49  60800.50
                                                       表4
实施例 31  32  33  34  35  36  37  38  39  40
组合物wt％ 基础润滑脂  锂复合皂润滑脂 95.0  95.0  95.0  94.0  95.0  93.0  93.0  93.0  94.0  94.0
添加剂  Na2S2O3  3.0  3.0
 Na2S2O3·5H2O  3.0  3.0  1.0  3.0  3.0  1.0
 Desilube 88    *1  3.0  2.0  3.0  2.0
 SAP001    *2  2.0  2.0  1.0
 SAP007    *3  2.0  2.0
 OLOA219   *4 2.0  1.0  1.0  2.0  1.0  1.0
 NA-SUL 729    *5  2.0  1.0
 BT-120    *6  2.0  2.0  2.0  2.0  1.0
总计  100  100  100  100  100  100  100  100  100  100
测试结果 防锈测试  湿度测试  A  A  A  A  A  A  A  A  A  A
四球测试  膨胀负载，牛顿磨损标记直径，毫米  60800.60  49030.79  60800.78  49030.78  60800.77  60800.47  49030.48  60800.54  49030.56  60800.51
                                                            表5
实施例 41  42  43  44  45  46  47  48  49  50
组合物wt％ 基础润滑脂  铝复合皂润滑脂  93.0  93.0  93.0  93.0  93.0  93.0  93.0  93.0  93.0  93.0
添加剂  Na2S2O3  3.0  3.0  1.0  2.0
 Na2S2O3·5H2O  3.0  3.0  3.0  2.0
 Desilube 88  *1  3.0  3.0  2.0  1.0  1.0
 SAP001       *2  2.0  2.0  1.0
 SAP007       *3  2.0  1.0  2.0  1.0
 OLOA219      *4  2.0  1.0  1.0  1.0
 NA-SUL 729   *5  2.0  1.0  1.0
 BT-120       *6  2.0  2.0  2.0  2.0  2.0  2.0  2.0  2.0  2.0  2.0
总计  100  100  100  100  100  100  100  100  100  100
测试 防锈测试  湿度测试  A  A  A  A  A  A  A  A  A  A
四球测试  膨胀负载，牛顿磨损标记直径，毫米  39220.73  39220.71  30890.72  30890.68  39220.70  39220.73  30890.70  39220.67  39220.72  39220.71
                                                        表6
对比实施例     1     2     3     4     5     6     7     8     9     10
组合物wt％ 基础润滑脂  尿素润滑脂    100.0     97.0     97.0     94.0     93.0     93.0     93.0     93.0     93.0     93.0
添加剂  Na2S2O3     3.0     3.0     2.0     3.0
 Na2S2O3·5H2O     3.0     1.0     3.0     2.0
 Desilube 88    *1     3.0     3.0     1.0
 SAP001    *7     4.0
 Dailube Z-500  *8   4.0   2.0
 NA-SUL SS    *9   4.0   2.0     2.0
 NA-SUL 707    *10     4.0     2.0
 总计     100     100     100     100     100     100     100     100     100     100
测试结果 防锈测试  湿度测试     A     E     E     E     E     E     E     E     E     E
四球测试  膨胀负载，牛顿磨损标记直径，毫米     15700.88     78450.68     60800.72     78450.68     78450.72     78450.78     78450.89     60800.84     78450.81     78450.87
                                                             表7
对比实施例 11  12  13  14  15  16  17  18  19  20
组合物wt％ 基础润滑脂  锂皂润滑脂 100.0  97.0  97.0  97.0  93.0  93.0  93.0  93.0  93.0  93.0
添加剂  Na2S2O3  3.0  3.0  2.0  3.0
 Na2S2O3·5H2O  3.0  1.0  3.0  2.0
 Desilube 88    *1  3.0  3.0  1.0
 SAP001    *7  4.0
 Dailube  Z-500    *8  4.0  2.0
 NA-SUL SS    *9  4.0  2.0  2.0
 NA-SUL 707    *10  4.0  2.0
 Na2S2O3  100  100  100  100  100  100  100  100  100  100
测试结果 防锈测试  湿度测试  A  E  E  E  E  E  E  E  E  E
四球测试  膨胀负载，牛顿磨损标记直径，毫米  12360.93  60800.74  49030.72  60800.69  60800.71  60800.70  60800.69  49030.68  60800.74  60800.66
                                                               表8
对比实施例 21  22  23  24  25  26  27  28  29  30
组合物wt％ 基础润滑脂  锂皂润滑脂  100.0  97.0  97.0  97.0  93.0  93.0  93.0  93.0  93.0  93.0
添加剂  Na2S2O3  3.0  3.0  2.0  3.0
 Na2S2O3·5H2O  3.0  1.0  3.0  2.0
 Desilube 88    *1  3.0  3.0  1.0
 SAP001    *7  4.0
 Dailube Z-500    *8  4.0  2.0
 NA-SUL SS    *9  4.0  2.0  2.0
 NA-SUL 707    *10  4.0  2.0
 Na2S2O3  100  100  100  100  100  100  100  100  100  100
测试结果 防锈测试  湿度测试  A  E  E  E  E  E  E  E  E  E
四球测试  膨胀负载，牛顿磨损标记直径，毫米  15700.79  60800.78  60800.77  60800.76  60800.78  60800.76  60800.65  60800.79  60800.71  60800.69
                                                           表9
对比实施例 31  32  33  34  35  36  37  38  39  40
组合物wt％ 基础润滑脂  铝复合皂润滑脂  100.0  97.0  97.0  97.0  93.0  93.0  93.0  93.0  93.0  93.0
添加剂  Na2S2O3  3.0  3.0  2.0  3.0
 Na2S2O3·5H2O  3.0  1.0  3.0  2.0
 Desilube 88    *1  3.0  3.0  1.0
 SAP001    *7  4.0
 Dailube Z-500    *8  4.0  2.0
 NA-SUL SS    *9  4.0  2.0  2.0
 NA-SUL 707  *10  4.0  2.0
 Na2S2O3  100  100  100  100  100  100  100  100  100  100
测试结果 防锈测试  湿度测试  A  E  E  E  E  E  E  E  E  E
四球测试  膨胀负载，牛顿磨损标记直径，毫米  15700.98  30890.71  30890.70  39220.69  39220.72  39220.72  39220.76  30890.81  39220.70  39220.84
发明效果
从表1-5的实施例和表6-9的对比实施例可以清楚地看出，根据本发明的润滑脂组合物，其中将上述添加剂(A)加入到润滑脂组合物中并且将硫代硫酸钠复合在其中，具有良好的极限压力性能并且显著增加其防锈性能。润滑脂组合物，其中将上述添加剂(A)和上述苯并三唑化合物(B)加入到润滑脂中并且将硫代硫酸钠复合在其中，也具有良好的极限压力和防锈性能并且附加地具有抗磨损性。在尿素润滑脂、锂皂润滑脂和锂复合皂润滑脂中，抗磨损性明显增加。很长时间，硫代硫酸钠被认作食品添加剂，也被称作解毒剂，它是一种不仅对人体而且对全球环境温和的添加剂。所以，根据本发明的组合物是与环境不矛盾的良好润滑脂。

Claims (10)

1.一种含有基础油和增稠剂的润滑脂组合物，以整个润滑脂组合物为基准，该润滑脂中附加含有0.05wt％-30wt％的硫代硫酸钠和至少0.1wt％的一种或多种选自水杨酸钙、水杨酸镁、苯酚钙和/或磺酸钙的添加剂(A)。
2.根据权利要求1的润滑脂组合物，以整个润滑脂组合物为基准，其中所述一种或多种添加剂(A)中的每种用量的范围是0.1wt％-5wt％。
3.根据权利要求1或2的润滑脂组合物，以整个润滑脂组合物为基准，其中所述一种或多种添加剂(A)中的每种用量的范围是0.2wt％-3wt％。
4.根据权利要求1-3之任一项的润滑脂组合物，以整个润滑脂组合物为基准，其中所述组合物更进一步含有至少0.1wt％的苯并三唑化合物(B)。
5.根据权利要求4的润滑脂组合物，以整个润滑脂组合物为基准，其中所述苯并三唑化合物(B)的用量范围是0.1wt％-5wt％。
6.根据权利要求4或5的润滑脂组合物，以整个润滑脂组合物为基准，其中所述苯并三唑化合物(B)的用量范围是0.2wt％-3wt％。
7.根据权利要求4-6之任一项的润滑脂组合物，其中所述苯并三唑化合物(B)选自1，2，3-苯并三唑，2-(2’-羟基-5’-甲基苯基)苯并三唑，2-[2’-羟基-3’-(3″，4″，5″，6″-四氢邻苯二甲酰亚氨基甲基)-5’-甲基苯基]苯并三唑，2-(2’-羟基-3’，5’-二叔丁基苯基)苯并三唑，2-(2’-羟基-5’-叔辛基苯基)苯并三唑，2-(2’-羟基-3’，5’-二叔戊基苯基)苯并三唑，2-[2-羟基-3，5-双(α，α-二甲基苄基)苯基]-2H-苯并三唑和2(2’-羟基-3’-十一烷基-5’-甲基苯基)苯并三唑。
8.根据权利要求1-7之任一项的润滑脂组合物，其中增稠剂是一种或多种尿素化合物，一种或多种锂皂和/或锂复合皂，或一种或多种铝复合皂。
9.根据权利要求1-8之任一项的润滑脂组合物的应用，可以改进防锈和抗磨损性。
10.根据权利要求1-8之任一项的润滑脂组合物的制备方法，其中预先混合硫代硫酸钠和选自水杨酸钙、水杨酸镁、苯酚钙和/或磺酸钙的一种或多种添加剂(A)，将混合物加入到含有基础油和增稠剂的基础润滑脂中，或者其中将硫代硫酸钠和所述一种或多种添加剂(A)单独加入到基础润滑脂中。
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CN101061205B (zh) * 2004-11-08 2010-11-10 Thk株式会社 适于振动的润滑脂组合物及采用该组合物的导向装置

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BR0113118B1 (pt) 2011-07-12
HUP0302687A3 (en) 2005-11-28
CN1191341C (zh) 2005-03-02
WO2002012418A3 (en) 2002-04-25
DE60121341T2 (de) 2007-07-26
WO2002012418A2 (en) 2002-02-14
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AU7981501A (en) 2002-02-18
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US20030176295A1 (en) 2003-09-18
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US6800595B2 (en) 2004-10-05
KR100787403B1 (ko) 2007-12-21
CZ295732B6 (cs) 2005-10-12
CA2418850A1 (en) 2002-02-14
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