CN1269818A - 润滑组合物 - Google Patents

润滑组合物 Download PDF

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CN1269818A
CN1269818A CN98809022A CN98809022A CN1269818A CN 1269818 A CN1269818 A CN 1269818A CN 98809022 A CN98809022 A CN 98809022A CN 98809022 A CN98809022 A CN 98809022A CN 1269818 A CN1269818 A CN 1269818A
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lubricating grease
zinc
molybdenumdisulphide
weight ratio
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R·A·福莱彻
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Shell Internationale Research Maatschappij BV
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Abstract

一种润滑组合物,它包含矿物和/或合成来源的基础油,以及作为减摩添加剂的二硫化钼、一或多种二硫代氨基甲酸锌与一或多种金属二硫代磷酸盐的混合物,该组合物不含显著数量的环烷酸锌。

Description

润滑组合物
本发明涉及润滑组合物，具体地涉及含有这种组合物的润滑脂，更具体地涉及用于所有类型等速万向节，例如等速刚性球节和柱塞型等速万向节的润滑脂。
润滑的主要目的是使相对运动的固体表面分离，以使摩擦和摩损减至最小。最常用于这一目的的物质是油和油脂。润滑剂的选择大多由具体应用来确定。
在存在高压的情况下采用润滑脂，其中不希望油从轴承中滴落或接触表面不连续地运动，使得难以在轴承中保持独立的膜。由于设计简化、密封要求降低和减少维护需求，对电动机、家用器具、车轮轴承、机床或飞行器附件中滚珠和滚柱轴承的润滑来说，几乎普遍地首先考虑润滑脂。润滑脂还用于润滑小型的齿轮传动装置及许多低速滑动应用。
润滑脂主要由如油的液体润滑剂和增稠剂组成。必要的是，配制润滑脂所采用的油的类型与一般选择用于油润滑的油相同。最常用作增稠剂的是锂、钙、钠、铝和钡的脂肪酸皂。然而，增稠剂可以是一系列固体物质中的一种，包括粘土、肥皂和如锂的配合物及尿素类化合物。
基础油可以是矿物或合成来源的。矿物来源的基础油可以是矿物油，如通过溶剂精炼或加氢加工所制备的那些。合成来源的基础油通常是C10-50烃聚合物的混合物，例如α-烯烃的液体聚合物。它们还可以是常规的酯，如多元醇酯。所述基础油还可以是这些油的混合物。优选基础油是由Royal Dutch/Shell Group of Companies以名称“HVI”或“MVIN”出售的矿物来源基础油，聚α-烯烃、或是这两者的混合物。也可使用合成烃基础油如由Royal Dutch/Shell Group of Companies以名称“XHVI”(商标)出售的那些。
润滑脂优选含有5至20wt％增稠剂。
锂皂增稠的润滑脂多年来便已属于公知内容了。通常，锂皂由C10-24、优选C15-18、饱和或不饱和脂肪酸或其衍生物来制备。一种具体的衍生物是是加氢蓖麻油，它是12-羟基硬脂酸的甘油酯。12-羟基硬脂酸是特别优选的脂肪酸。
用复合增稠剂增稠的润滑脂也已属于公知内容。除脂肪酸盐外，向增稠剂中引入配位剂，通常是低至中等分子量的酸或二元酸或其一种盐，如苯甲酸或硼酸或硼酸锂。
在润滑脂中用作增稠剂的尿素化合物在其分子结构中包括脲基团(-NHCONH-)。这些化合物根据脲链数包括单、二、或多脲化合物。
各种常规润滑脂添加剂均可以这一应用领域常用数量加入到润滑脂中，以赋予所述润滑脂以一些所需的特性，如氧化稳定性、胶粘性、极压性能和腐蚀抑制性。适用的添加剂包括一或多种极压/抗磨剂，例如锌盐如锌的二烷基或二芳基二硫代磷酸盐、硼酸盐、被取代的噻二唑、通过例如二烷氧胺与被取代的有机磷酸盐反应制备的氮/磷聚合化合物、磷酸胺、天然或合成来源的硫化鲸蜡油、硫化猪脂、硫化酯、硫化脂肪酸酯、和相似的硫化物质、例如通式(OR)3P＝O(其中R为烷基、芳基或芳烷基)的有机磷酸盐、和三苯基硫逐磷酸酯；一或多种高碱性含金属洗涤剂，如钙或镁的烷基水杨酸盐或烷基芳基磺酸盐；一或多种无灰分散剂添加剂，如聚异丁烯基琥珀酸酐与胺或酯的反应产物；一或多种抗氧剂，如受阻酚或胺，例如苯基α-萘胺；一或多种防锈添加剂；一或多种摩擦改进添加剂；一或多种粘度指数改进剂；一或多种倾点下降剂；和一或多种胶粘剂。还可添加固体物质如石墨、微细分散的二硫化钼、滑石粉、金属粉末和各种聚合物如聚乙烯蜡来赋予特殊性能。
在一些润滑剂如柴油和汽油机油和工业油中有时将二硫代氨基甲酸锌用作抗氧剂并同时用作防腐剂。
在润滑剂中，一般非常希望在减少摩擦(即增加滑动性)的同时减少磨损(即减少由机械和/或腐蚀作用造成的表面破坏)。
已有一些方案建议使用各种添加剂来减少摩擦程度，通常是引入基于有机钼的配剂。减摩作用时常取决于增稠剂，即，与某种增稠剂配伍良好的添加剂与另一种增稠剂结合时并非如此。
二硫化钼(一种非有机钼化合物)是公知的高度耐磨的固体润滑剂，并被用于多种润滑剂中。同样被公知的是在润滑剂中使用金属(二烷基或二芳基)二硫代磷酸盐作为极压或抗磨剂。
Tribology Transactions，vol 33，no.3，(1990)345至354页综述了有机钼化合物(如二烷基二硫代氨基甲酸钼(MoDTC)和二硫代磷酸钼(MoDTP)与含二烷基二硫代磷酸锌(ZnDTP)的润滑剂混合物对磨损和摩擦的作用。在该综述的前半部分，对润滑油中各种组分的测试尤其证实，包括二硫代氨基甲酸锌的锌化合物表现出与二硫代氨基甲酸钼相似的高负荷抗磨性。在该综述的后半部分，普遍被视为MoDTC或MoDTP和ZnDTP添加剂的分解产物的物质悬浮到用来独立评价的参考润滑脂中以确定这些产物的任一种是否确实具有良好的摩擦和抗磨性能。被一些人认为是这类分解产物的二硫化钼在一种参考润滑脂中进行测试，该参考润滑脂用12-羟基硬脂酸锂皂增稠，并含有0.5％(质量)作为防氧化剂的二丁基二硫代氨基甲酸锌。所获得的润滑脂表现出高(即不希望的)摩擦性，并仅具有中等的抗磨性；在相同的参考润滑脂中独立测试的锌化合物也未表现出降低的摩擦性。
在WO97/03152中，叙述了一种减摩添加剂组合物，其中包含二硫化钼、环烷酸锌和金属二硫代磷酸盐，视具体情况存在的组合成分金属二硫代氨基甲酸盐。在实施例22中，表明环烷酸锌的存在是必要的。
现在意外地发现，二硫化钼、二硫代氨基甲酸锌和金属二硫代磷酸盐相组合在润滑组合物、特别是润滑脂中能协同地作为减摩剂发挥作用，同时保持良好的、低抗磨性。已发现在这种组合物中不必须存在环烷酸锌。再有，这种组合物是不依赖增稠剂的。针对二硫化钼单独或与另外两种组分中的一种组合使用进行的测试表明，减摩作用产生明显的出人预料的效果。
WO94/11470和GB-A-2255103叙述了含有二硫化钼、二硫代氨基甲酸钼和金属二硫代磷酸盐的润滑油组合物的用途。WO94/11470或GB-A-2255103未指出或暗示二硫代氨基甲酸钼可被另一种金属二硫代氨基甲酸盐替代。
因此，本发明提供一种润滑组合物，它包含矿物和/或合成来源的基础油和二硫化钼、一或多种二硫代氨基甲酸锌和一或多种金属二硫代磷酸盐的组合物，所述组合物不含显著数量的环烷酸锌。
本发明的组合物不含显著数量的环烷酸锌。这意味着所述组合物以润滑组合物的总重量为基准计含有少于0.3wt％环烷酸锌。环烷酸锌的数量是不包括市售产物如矿物油中存在的其它化合物在内的化合物本身的数量。所述组合物优选含有少于0.05wt％环烷酸锌，更优选少于0.01wt％。最优选，所述组合物不含环烷酸锌。
优选在润滑脂中使用减摩添加剂组合物，所述润滑脂包含矿物和/或合成来源的基础油和增稠剂，所述增稠剂优选是简单的或配合的锂皂，或尿素化合物。
这类润滑脂优选含0.5至10wt％，更优选为1至4wt％二硫化钼。独立地，对于尿素增稠的润滑脂和配合锂皂增稠的润滑脂来说，润滑脂优选含有二硫代氨基甲酸锌0.01至5wt％，更优选为0.3至2.4wt％，对于简单锂皂增稠的润滑脂来说，该数量为0.5至10wt％，更优选为1至4wt％。本发明的润滑脂还优选含有总量为0.15至10wt％，更优选为1至3wt％所述一或多种金属二硫代磷酸盐。所有数量均以润滑脂组合物的总重量为基准计。
如所述三种组分以相互关联的或三元比例存在是特别有用的，这样，对于尿素增稠的润滑脂和配合锂皂增稠的润滑脂来说，二硫化钼与金属二硫代磷酸盐的重量比值范围为1∶0.15至1∶1，金属二硫代磷酸盐与二硫代氨基甲酸锌的重量比值为1∶0.25至1∶1.5，二硫化钼与二硫代氨基甲酸锌的重量比值范围为1∶0.4至1∶1.5。对于简单的锂皂增稠的润滑脂来说，二硫化钼与金属二硫代磷酸盐的重量比值范围优选为1∶0.15至1∶1，金属二硫代磷酸盐与二硫代氨基甲酸锌的重量比值为1∶1至1∶4.5，二硫化钼与二硫代氨基甲酸锌的重量比值范围为1∶0.4至1∶1.5。
优选，所述一或多种金属二硫代磷酸盐选自二烷基-、二芳基-或烷基芳基-二硫代磷酸锌，所述一或多种二硫代氨基甲酸锌选自二烷基-、二芳基-或烷基芳基-二硫代氨基甲酸锌，其中在二硫代磷酸盐和/或二硫代氨基甲酸盐中适用的任何烷基部分是直链或支链的，且优选含1至12个碳原子。
润滑脂中的增稠剂，如上所述，优选包括尿素化合物、简单的锂皂或配合锂皂。优选的尿素化合物是聚脲化合物。这类增稠剂在润滑脂技术中是公知的。本发明的意外有效的组合物使用简单的锂皂作为增稠剂。
本发明的润滑组合物可通过将所述添加剂组合物以常规方式添加到基础油中来制备。对于润滑脂来说，这可通过热或冷混合并随后匀化来实现以确保添加剂组分的均匀分散。如必要或需要，可添加其它的添加剂如抗氧化剂。
本发明还提供一种润滑等速万向节的方法，包括用本发明的润滑脂来填充所述万向节。
本发明还提供用本发明润滑脂填充的等速万向节。
现在参照如下实施例说明本发明，其中所有百分比均以重量为基准计。
实施例1
通过向在冷基础油(MVIN与HVI油的混合物)中的9.15wt％氢化蓖麻油脂肪酸中添加比例为1份LiOH·H2O比5份水的1.12wt％LiOH·H2O与水的浆状物、并将该混合物在密封的高压釜中加热至150℃，来制备锂皂润滑脂。排空蒸汽并持续加热至220℃，之后将反应物快速冷却(速率为6至7℃每分钟)并将产物均化。向所述润滑脂中添加添加剂。在所有情况下，使用0.5wt％芳族胺作为抗氧化剂。
制备本发明的润滑脂和一些对比润滑脂并进行测试。对于各种润滑脂，按表1所示改变二硫化钼、ZnDTC(二戊基二硫代氨基甲酸锌)和ZnDTP(4-甲基-2-戊基二硫代磷酸锌)的数量。
对于各种润滑脂评价摩擦系数和磨痕直径；结果也示于表1中。
使用摆动SRV摩擦试验机测量摩擦和磨损。对于摩擦测量，摆动SRV摩擦试验机(来自Optimol Instruments)使用在平面重叠表面上的10mm球作为试样几何形状。在全过程中使用50赫兹的摆动频率和1.5mm的冲程。在300牛顿负荷、温度100℃的测试条件下操作2小时后记录摩擦系数。通过在使用光学计数线(optical graticule)在两小时测试结束时测量在球上的磨痕的直径来评价磨损。
在均具有相同的基础润滑脂加增稠剂加抗氧化剂的条件下，将本发明润滑脂与仅具有二硫化钼或二硫化钼加二硫代氨基甲酸锌或二硫化钼加二硫代磷酸锌的锂润滑脂相对比。结果中清楚可见，本发明的润滑脂的摩擦系数和磨痕直径显著低于任一种对比润滑脂。
实施例2
通过将在基础油(75wt％HVI 160B与25wt％HVI 650的混合物)中的5wt％4，4-二苯基甲烷二异氰酸酯加热到70℃然后添加10.8wt％十八烷胺来制备尿素润滑脂C。然后在冷却到80℃之前将该混合物再加热到150℃。随后添加要在配剂中包含的其它添加剂。然后在室温下将配制的润滑脂均化。
制备并测试本发明的润滑脂和一些对比润滑脂。
在所有情况下，均添加0.5wt％作为抗氧化剂的芳族胺，并改变各种润滑脂的二硫化钼、ZnDTC(二戊基二硫代氨基甲酸锌)和ZnDTP(4-甲基-2-戊基二硫代磷酸锌)的数量。按照实施例1评价各润滑脂的摩擦系数和磨损。结果示于表2中。
可见，对于尿素增稠的润滑脂也表现出显著低的摩擦系数并伴之以低的磨损，但其ZnDTC的比例低于实施例1的锂皂增稠的润滑脂。
表1润滑脂实施例No.  二硫化钼wt％  ZnDTCwt％  ZnDTPwt％  摩擦系数  磨痕直径(nm)1                3             2          1          0.055     0.50对比A            -             -          -          0.143     0.85对比B            3             -          -          0.138     0.84对比C            3             2          -          0.075     0.58对比D            3             -          1          0.075     0.65
表2润滑脂实施例No.  二硫化钼wt％  ZnDTCwt％  ZnDTPwt％  摩擦系数  磨痕直径(nm)2                3             0.5        1          0.055     0.57对比E            -             -          -          0.100     0.46对比F            3             -          -          0.153     0.78对比G            3             -          1          0.080     0.67对比H            3             2          1          0.093     0.53
实施例3
通过向载于基础油(HVI油的混合物)中的常规比例的氢化蓖麻油脂肪酸、烷基水杨酸钙、辛酸钙中添加50wt％LiOH·H2O和硼酸在水中的浆状物以及常规抗氧化剂、然后在搅拌条件下将该混合料加热到210℃来制备锂配合物润滑脂。在将该混合物缓慢冷却到160℃后，添加喹啉和羟基苯基作为附加抗氧化剂。将全体混合物缓慢冷却到室温，添加二硫化钼、ZnDTC(二戊基二硫代氨基甲酸锌)和ZnDTP(4-甲基-2-戊基二硫代磷酸锌)；然后将得到的润滑脂均化。
所获得的润滑脂含有3wt％二硫化钼、1.5wt％ZnDTC和1.5wt％ZnDTP作为减摩添加剂。
使用与以上实施例1相同的试验方法，在300N和100℃下测量的摩擦系数和磨损分别为0.058和0.48nm。从而，当使用锂配合物增稠的润滑脂时也给出了出人意料低的摩擦系数并伴之以低的磨损性能。

Claims (9)

1.一种润滑组合物，其中包括矿物和/或合成来源的基础油和二硫化钼、一或多种二硫代氨基甲酸锌与一或多种金属二硫代磷酸盐的混合物，该组合物不含显著数量的环烷酸锌。
2.权利要求1的组合物，其中所述一或多种二硫代氨基甲酸锌选自二烷基-、二芳基-和烷基芳基二硫代氨基甲酸锌。
3.权利要求1或2的组合物，其中所述一或多种金属二硫代磷酸盐选自二烷基-、二芳基-和烷基芳基二硫代磷酸锌。
4.权利要求1至3中任一项的组合物，它是一种润滑脂并进一步含有增稠剂。
5.权利要求4的组合物，其中所述增稠剂是简单的锂皂。
6.权利要求5的组合物，其中二硫化钼与金属二硫代磷酸盐的重量比范围为1∶0.15至1∶1，金属二硫代磷酸盐与二硫代氨基甲酸锌的重量比范围为1∶1至1∶4.5，二硫化钼与二硫代氨基甲酸锌的重量比范围为1∶0.4至1∶1.5。
7.权利要求4的组合物，其中所述增稠剂是尿素组合物或配合物锂皂，且其中二硫化钼与金属二硫代磷酸盐的重量比范围为1∶0.15至1∶1，金属二硫代磷酸盐与二硫代氨基甲酸锌的重量比范围为1∶0.25至1∶1.5，二硫化钼与二硫代氨基甲酸锌的重量比范围为1∶0.4至1∶1.5。
8.一种润滑等速万向节的方法，包括用权利要求4至7中任一项的润滑脂来对其填充。
9.采用权利要求4至7中任一项的润滑脂填充的等速万向节。
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CN106635302A (zh) * 2016-09-21 2017-05-10 广西大学 一种625合金冷冲压润滑剂组合物

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EP1036142A1 (en) 2000-09-20
WO1999014292A1 (en) 1999-03-25
BR9812074A (pt) 2000-09-26
AR017087A1 (es) 2001-08-22
PL339174A1 (en) 2000-12-04
KR20010023924A (ko) 2001-03-26
CA2303345A1 (en) 1999-03-25
AU9744098A (en) 1999-04-05

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