CN1034953C - 脲润滑脂组合物 - Google Patents

脲润滑脂组合物 Download PDF

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CN1034953C
CN1034953C CN94106241A CN94106241A CN1034953C CN 1034953 C CN1034953 C CN 1034953C CN 94106241 A CN94106241 A CN 94106241A CN 94106241 A CN94106241 A CN 94106241A CN 1034953 C CN1034953 C CN 1034953C
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lubricating grease
weight
grease
urea grease
urea
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尾崎幸洋
川村靖
土谷哲夫
后藤文夫
露木英明
宫岛和浩
松田尚
冈野信彦
望月启史
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Showa Shell Sekiyu KK
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Abstract

本发明公开了一种脲润滑脂组合物，它包括脲润滑脂并混有作为添加剂的式(A)的硫化二烷基二硫代氨基甲酸钼，和式(B)的硫代磷酸三苯酯(其中R1和R2各自独立地代表具有1-24个碳原子的烷基，m+n＝4，m为0-3，n为4-1)。

Description

脲润滑脂组合物
本发明涉及一种适用于对某些部件用润滑脂予以润滑的脲润滑脂组合物，这种部件包括CV节(等速万向节)和汽车内的球窝节以及钢铁工业和其它各种工业内机器上的轴承和齿轮。
随着近年来机械技术的进步，人们日益期望着机器的尺寸减小，重量减轻，精确度增加和使用寿命增长等等。由于接头，轴承，齿轮和转动部件的其它构件也是小尺寸的并在高速和高负荷条件下操作的，施加到这些部件上的润滑油脂所处的环境越来越变得严峻。
下面将对上述情况以CVJ(即CV节)和轧钢机为例加以详细说明。
在汽车工业中，随着FF(前置发动机前轮驱动式)汽车数量的增加，使用CVJ的车辆数也增加。不仅FF车辆而且四轮驱动(4WD)的车辆数量最近以来也增加，因而用于汽车的CVJ数量增加很快。特别是，由于在FF车辆中趋向于动力和操作效能的增加，趋向于CVJ尺寸减小和重量减轻，以及由于CVJ的操作条件日趋严峻，对CVJ的耐用性的要求也越来越严峻。例如，由于使用了配有涡轮的或大尺寸的发动机，CVJ被放置在较大的角度上，并且以较高的速度在较大的负荷下操动，因此，有时在行驶时由于例如内热生成的增加，CVJ的温度急剧升高。目前有各种各样的CVJ存在，根据不同的用途正常地使用着。由于施加在CVJ上的润滑剂也要求应付扭矩和速度的增加，因此希望有一种润滑脂，它不但对高温具有优良的耐热性，而且在所谓的热抑制效应上，即减少滑动部件的摩擦以减少温度的增加的效应，也是卓越的。
从改进接头和密封套材料的耐久性和减慢润滑剂本身的劣化方面来看，通过减少摩擦来抑制温度的增长也是可取的。温度的过度增加加快了密封套材料的老化和润滑剂的变质，至使CVJ寿命的大大缩短。
另一方面，在钢铁工业中，因为需要节约能源，节约劳力，节约原材料，和防止环境污染，对诸如使用寿命长，耐热性能高的高品质润滑脂需求强烈。一座钢铁厂内有着各种各样的机器，其中所用的润滑脂根据环境条件在要求性能上有所不同。在轧钢阶段，那里消耗润滑脂最多，轴承，滑动面，螺杆及轧钢机的其它部件使用集中润滑法以润滑脂润滑，用在这里的润滑脂大部份都含有一种特压添加剂。由于炼钢设备中的这种机械部件受到负荷和热的影响很大，并在一个包含水和轧钢屑的环境中操作，亟需要一种耐磨性能，摩擦性质，和密封性能特别优良的润滑脂，以便延长这些机械部件的使用寿命。
为了迎合上述的要求，市场上主要使用特压锂基润滑脂。这些润滑脂中含有一种由硫化油、脂、或烯烃和二硫代磷酸锌、一种铝化合物添加剂，和二硫化钼结合组成的硫一磷特压添加剂。此外，具有比锂基润滑耐热性能更好的脲润滑脂最近的用量逐渐增加。
在这种情况下，有代表性的现有技术包括有美国专利4,840,740号和4,514,312号以及日本审定专利JP-B-4-34590号。美国专利4,840,140号中公开了一种含有一种有机钼化合物和二硫代磷酸锌组合物作为添加剂的脲润滑脂。美国专利4,514,312号公开了一种含有磷酸芳香胺的脲润滑脂。此外，日本审定专利JP-B-34590公开了一种脲润滑脂，它含有一种作为主要成份的硫一磷特压添加剂，这种添加剂由(A)一种硫化二烷基二硫代氨基甲酸钼和(B)选自包括硫化油或脂，硫化烯烃，磷酸三甲苯酯，硫代磷酸三烷基酯和二烷基二硫代磷酸锌中之至少一种组合而成。
然而，这些现有技术的润滑脂具有一个问题，即它们能使密封材料劣化。也就是，这些大部份是由氯丁二烯橡胶、硅橡胶，和聚酯树脂构成的密封套材料在高温时遇到通常的润滑脂会劣化。例如，含有这种添加剂如硫化油或脂和硫化烯烃的润滑脂可以使氯丁二烯橡胶劣化，造成在拉伸强度和伸长度上很大的变化。含有二烷基二硫代磷酸锌的润滑脂使硅橡胶劣化，而含有环烷酸铅的润滑脂则可以使硅橡胶和聚酯树脂加速劣化从而大大地影响其质量。
本发明的第一个目的是提供一种脲润滑脂，它能有效地减小摩擦从而具有极佳的热抑制性能和很好的耐磨性，它还具有好的耐热性。
本发明的第二个目的是提供一种从不劣化密封材料的脲润滑脂组合物。
本发明提供一种脲润滑脂组合物，它包括脲润滑脂并混有作为添加剂的式(A)的硫化二烷基二硫代氨基甲酸钼(Sulfurizedmoly-bdenum dialkyldithio carbamate)
(其中R1和R2各自独立代表具有1-24个碳原子的烷基，m+n＝4，m为0-3，n为4-1)，和式(B)的硫代磷酸三苯酯：
Figure C9410624100052
硫化二烷基二硫代氨基甲酸钼(A)的实例包括硫化二乙基二硫代氨基甲酸钼、硫化二丁基二硫代氨基甲酸钼、硫化二异丁基二硫代氨基甲酸钼、硫化二(2-乙基己基)二硫代氨基甲酸钼、硫化二戊基二硫代氨基甲酸钼、硫化二异戊基二硫代氨基甲酸钼、硫化二月桂基二硫代氨基甲酸钼、硫化二硬脂酰基二硫代氨基甲酸钼、硫化正丁基-2-乙基己基二硫代氨基甲酸钼和硫化2-乙基己基硬脂酰基二硫代氨基甲酸钼。化含物(A)的加入量基于脲润滑脂组合物的总量计算为0.5-10％(重量)，优选0.5-5％(重量)。如果其量低于0.5％(重量)，添加剂在增进耐磨性和摩擦性能方面没有效果。即使其量超过10％(重量)，也不能进一步增强效果。
硫代磷酸三苯酯(B)的用量为0.1-10％(重量)，优选0.1-5％(重量)，基于脲润滑脂组合物的总量计算。如果其量低于0.1％(重量)在增进磨损和摩擦性能方面没有改进。而如果其量超过10％(重量)，不能表现充分的润滑性能。
作为用作增稠剂的脲化合物，可使用任何已知的脲增稠剂，对其种类无任何特别限制。其实例包括双脲、三脲和四脲。
用矿物油和/或合成油作原油。脲化合物的用量基于原油和脲化合物总量计算为2-35％(重量)。
在本发明组合物中加入抗氧化剂、防锈剂、特压添加剂、聚合物添加剂和其它成分。
本发明将参照下列实施例和对比实施例更详细地解释，但本发明不限于此。
实施例和对比实施例
按表1至2所示配方向基本润滑脂中加入添加剂，将每个得到的混合物用三辊滚轧机处理，以得到实施例和对比实施例中的润滑脂。基本润滑脂组成具体表示如下。用粘度为15mm2/秒(100℃)的纯化矿物油作原油。
I、双脲润滑脂
在原油中，使1mol二苯甲烷-4，4′-二异氰酸酯与1mol对甲苯胺和1mol糠胺反应，得到的脲化合物均匀分散成为润滑脂。脲化合物的用量控制在15％(重量)。
II、四脲润滑脂
在原油中，使2mol二苯甲烷-4，4′-二异氰酸酯与2mol辛胺和1mol乙二胺反应，得到的脲化合物均匀分散成为润滑脂。脲化合物的用量控制在15％(重量)。
III、锂基润滑脂
将12-羟基硬脂酸锂溶于原油中并均匀分散得到润滑脂。将皂含量控制在9％(重量)范围内。
IV、铝配合物润滑脂
将苯甲酸和硬脂酸溶于原油中，然后向其中加入市售的异丙酸环铝氧化物(Cyclic alominum Oxide isopropylate)润滑剂(商品名Algomer，由日本Kawaken Fine Chemicals Co.，Ltd.，生产)并反应，得到的皂均匀分散得到润滑脂。将皂含量控制在11％(重量)苯甲酸(BA)与硬脂酸(FA)之比为BA/FA＝1.1(摩尔)，而苯甲酸和硬脂酸总量与铝(Al)之比(BA+FA)/Al＝1.9(摩尔)。
通过下列试验考察润滑脂的表中所列性能即摩擦系数、耐磨性、热抑制性、与密封材料配合使用的适应性和耐热性。
(i)摩擦系数
用Falex测试仪在下列条件下运转15分钟后测定摩擦系数(根据JP 241/69)。
转速：290转/分钟
负荷：200磅
温度：室温
时间：15分钟
润滑脂：用大约1g润滑脂作试样。
(2)耐磨性
通过4球磨损试验根据AS TM D2226测定耐磨性。
转速：1200转/分钟
负荷：40千克力
温度：75℃
时间：60分钟
(3)热抑制性能
温度测定
将CVJ摩擦部件用各样品润滑并密封。在下列条件下操作CVJ，然后测定外座圈表面温度。
CVJ型号：Tripod(万向)节
转速：2000转/分钟
连接角：10度
扭距：30千克力·米
时间：2小时
(4)与密封材料配合物使用的适应性
按照JISK6301提供的硫化橡胶的物理测试方法，用氯丁橡胶、硅橡胶和聚酯树脂作密封材料，在下列条件下将每个密封材料浸渍于每个润滑脂组合物中。测定各材料在浸渍试验前后的伸长度和拉伸强度，测定各性能的改变程度。
温度：140℃
浸渍时间：72小时
(5)耐热性
根据JIS K2220用滴点试验测定耐热性。
表1
    实施例     1     2     3     4     5     6     7     8     9
组成％(重量   基本润滑脂   双脲四脲   96.5 96.5   95.0 96.0 94.0   93.0 96.5   96.0   94.5
添加剂 A-1    *1A-2    *2B      *3   3.00.5   3.00.5   3.02.0   2.01.01.0   5.01.0   2.03.02.0 3.00.5   1.02.01.0 5.00.5
    总量   100.0   100.0   100.0   100.0   100.0   100.0   100.0   100.0   100.0
  测试结果     摩擦系数(μ)耐磨性  (mm)热抑制性能(℃)   0.0850.39151   0.0820.39145   0.0750.36142   0.0800.27145   0.0810.37146   0.0740.35144   0.0820.39150   0.0790.37148   0.0800.38147
  氯丁橡胶伸长率变化程度  ％氯丁橡胶拉伸强度变化程度％   -21.2+1.7   -22.0+1.1   -23.1-3.0   -20.8+1.2   -21.6+2.5   -23.2-4.0   -20.5-2.3   -21.7-1.1   -23.1+3.8
    硅橡胶伸长率变化程度    ％硅橡胶拉伸强度变化程度  ％   -8.1-6.6   -8.5-7.8   -10.0-10.1   -12.0-7.6   -10.5-7.9   -14.9-8.3   -8.5-7.9   -11.3-8.3   -10.1-9.1
    聚酯树脂伸长率变化程度  ％聚酯树脂拉伸强度变化程度％   +4.0-20.2   +3.9-19.6   +4.1-21.1   +3.8-18.3   +3.7-19.1   +4.9-20.1   +4.0-19.5   +4.0-18.7   +4.8-18.9
    耐热性(滴点℃)   ＞250   243   ＞250   245   243   ＞250   243   ＞258   ＞250
*1：A-1为硫化二烷基二硫代氨基甲酸钼，其中烷基是C4，n＝2.3。*2：A-2为硫化二烷基二硫代氨基甲酸钼，其中烷基为C4，n＝4。*3：B为硫代磷酸三苯酯。
       表2
    对比实施例     1     2     3     4     5     6     7     8       9     10
组成％(重量) 基本润滑脂 双脲四脲锂基润滑脂铝配合物润滑脂 97.0 98.0 98.0 95.0 95.0 95.0 95.0 96.5 95.0 95.0
添加剂 A-1  *1A-2  *2二烷基二硫代磷酸锌硫化烯烃硫化油或脂环烷酸铅磷酸三甲苯酯 3.0 2.0 2.0 3.02.0 3.02.0 3.02.0 3.02.0 3.00.5 3.02.0 3.02.0
    总量 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0
测试结果     摩擦系数(μ)耐磨性(mm)热抑制性能(℃) 0.1110.44164 0.1340.48173 0.1350.47179 0.1130.44167 0.1120.44165 0.1110.43165 0.0950.42157  --- 0.1100.44-  ---
    氯丁橡胶伸长率变化程度  ％氯丁橡胶拉伸强度变化程度％ -21.0+1.3 --  --  --  --  -- -- -76.4-64.4 -64.7-58.6  --
    硅橡胶伸长率变化程度    ％硅橡胶拉伸强度变化程度  ％ -8.0-6.8 -- --  --  --  -- -79.6-74.1  -- -- -70.9-66.6
    聚酯树脂伸长率变化程度  ％聚酯树脂拉伸强度变化程度％ +3.8-19.7 -- --  --  --  -- --  -- -- -35.1-41.7
    耐热性(滴点℃) ＞250 ＞250 244 195 ＞250 ＞250 ＞250  243 ＞250 ＞250
*1，*2，*3与表1相同评估
对比实施例1-6摩擦系数、耐磨性和热抑制制性能的数据均劣于实施例1-9的数据。对比实施例7的数据好于对比实施例1-6，但对比实施例7的润滑脂与硅橡胶配合使用的适应性极差。对比实施例8和9的润滑脂与氯丁橡胶配合使用的适应性差。对比实施例10的润滑脂与硅橡胶和聚酯树脂配合使用的适应性都很差。
相反，试验结果清楚地表明实施例1-9的润滑脂在摩擦系数、耐磨性和热抑制性能以及与任何密封材料配合使用的适应性方面均优秀。
本发明产生下列效果：(1)本发明润滑脂由于其减小摩擦作用，达到极佳耐磨性，它显示所谓热抑制性能，即抑制润滑的摩擦部件发热的性能。结果改进了接合点和轴承的耐久性，达到防止润滑剂劣化作用的目的。(2)本发明润滑脂与氯丁橡胶、硅橡胶和聚酯树脂配合使用时具有极佳的适应性从而延迟了密封装置中密封材料的劣化，即使高温下亦是如此。(3)本发明润滑脂滴点很高，具有极佳的耐热性。
已结合具体实施例方案描述了本发明，但进行不偏离本发明宗旨和范围的改变或改进对本领域技术人员来说应是显而易见的。

Claims (1)

1.一种脲润滑脂组合物，它包括脲润滑脂并混有作为添加剂的式(A)的硫化二烷基二硫代氨基甲酸钼：
Figure C9410624100021
其中R1和R2各自独立地代表具有1-24个碳原子的烷基，m+n＝4，m为0-3，n为4-1，和式(B)的硫代磷酸三苯酯：
Figure C9410624100022
其中化合物(A)的量为0.5-10％(重量)，(B)的量为0.1-10％(重量)，基于组合物总量计算；并且所述组合物包括2-35％(重量)脲化合物增稠剂，基于原油和脲化合物总量计算。
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