CN106520255B - 锂类增稠剂和包含该锂类增稠剂的润滑油组合物 - Google Patents

锂类增稠剂和包含该锂类增稠剂的润滑油组合物 Download PDF

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CN106520255B
CN106520255B CN201610048230.4A CN201610048230A CN106520255B CN 106520255 B CN106520255 B CN 106520255B CN 201610048230 A CN201610048230 A CN 201610048230A CN 106520255 B CN106520255 B CN 106520255B
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lubricating oil
oil composition
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金宰显
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Hyundai Motor Co
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Abstract

本发明提供一种锂盐增稠剂，其增强高温下的热稳定性和低温下的可操作性。本发明还提供一种包含该锂盐增稠剂的润滑油组合物。

Description

锂类增稠剂和包含该锂类增稠剂的润滑油组合物
技术领域
本公开涉及一种锂盐增稠剂，以及包含该锂盐增稠剂的润滑油组合物。更具体而言，本公开涉及一种锂盐增稠剂，其增强高温下的热稳定性和低温下的可操作性。
背景技术
在当前部分中的陈述仅提供与本公开相关的背景信息，可能不构成现有技术。
润滑油是用于润滑机械系统例如轴承和传动装置的半固态型润滑剂，其中机械系统用作车辆和工业机械中的部件。通常而言，润滑油由基础油、增稠剂和添加剂构成。
基础油是为使润滑油根据温度的粘度变化降至最低而包含其中的成分。作为基础油的实例，存在酯类油、硅类油、和氟类油，然而，由于例如高成本等的问题，其应用受到限制，因此，主要使用成本较低的合成性聚α-烯烃(PAO)基础油。
增稠剂是决定润滑油的主要特性例如耐热性或耐水性的成分。作为常用的增稠剂，存在金属皂类增稠剂例如钡、锂、钙、钠和铝皂，以及非金属皂类增稠剂，例如硅胶、膨润土和尿素。金属皂类增稠剂的实例包括脂肪酸的金属盐材料，作为其代表性的实例，存在12-羟基硬脂酸锂。然而，包含在金属皂类增稠剂中的金属成分会作用为引起氧化和腐蚀的催化剂。此外，其在高负荷下对润滑条件的应用受到限制，因此特性例如耐磨性降低。
由于润滑油的特性会随着所选的添加剂类型而做出极大的改变，对于合适添加剂的选择连同对于增稠剂的选择较为重要。包含有锂类增稠剂的润滑油组合物还包含聚合物材料作为粘度调节剂。这类粘度调节剂的实例包括烯烃类粘度改良剂，例如聚丙烯、聚异丁烯、聚乙烯-丙烯、和聚乙烯-丁烯；烯烃亚芳基类粘度改良剂，例如苯乙烯-乙烯和苯乙烯-异戊二烯；聚亚芳基类粘度改良剂，例如聚苯乙烯；以及聚甲基丙烯酸酯类粘度改良剂。此外，为改善高温耐久时间，将抗氧化剂、极压添加剂和缓蚀剂用作添加剂。
韩国专利第10-0513625、10-0135414和10-1438916号，以及韩国专利特开第10-2014-0054557号描述了润滑油组合物，其包含添加剂例如PAO基础油、锂类增稠剂和粘度调节剂，如上所述。然而，大多数润滑油组合物在不同温度环境下的增强耐久性和保持车辆部件可操作性方面受到限制。
发明内容
本公开提供一种锂类增稠剂其增强高温下的稳定性和低温下的可操作性。本公开还提供一种由该锂类增稠剂制备的润滑油组合物。
在一方面，本公开提供一种由以下式1表示的锂类增稠剂：
Figure GDA0002755230240000021
其中，m和n相同或不同，且为5～20的整数。
在另一方面，本公开提供一种润滑油组合物，其包含a)合成性聚α-烯烃(PAO)基础油、b)由式1表示的锂类增稠剂、以及任选的c)常规的润滑油添加剂。
基于本文提供的说明书，其他的适用范围将变得明晰。应当理解的是，说明书和具体实施例仅出于示例说明的目的而并非旨在限制本公开的范围。
具体实施方式
以下说明在本质上仅是示例说明性的，并非旨在限制本公开、应用或用途。在下文中，将对本发明的多种形式做出详细参考，而多种形式的示例在以下示出并说明。尽管将结合多种形式来描述本公开，将理解的是，本说明书并非旨在将本公开限制于那些形式。相反，本公开旨在不仅涵盖所记载的多种形式，而且还涵盖多种替换形式、修改形式、等价形式和其他形式，其可以包括在由所附权利要求定义的本公开的主旨和范围之内。
本公开提供一种锂盐增稠剂，其能够同时增强高温下的热稳定性和低温下的可操作性。本公开还提供一种包含该锂盐增稠剂的润滑油组合物。根据本公开的锂盐增稠剂可以不限于由以下式1表示的9,10,12-三取代硬脂酸锂盐：
Figure GDA0002755230240000031
其中，m和n相同或不同，且为5～20的整数。在式1表示的锂盐增稠剂中，m和n可以二者择一地相同或不同，且为7或8的整数。或者，锂盐增稠剂为9,10,12-三取代的硬脂酸锂盐。
根据本公开的锂盐增稠剂可以通过常规有机合成而制备。例如，如以下反应(Rxn)1中所示，由式1表示的9,10,12-三取代硬脂酸锂盐可以通过使由式2表示的9,10,12-三羟基硬脂酸酯与由式3表示的脂肪族二羧酸进行酯化并然后使其与氢氧化锂反应而制备：
Figure GDA0002755230240000032
在Rxn 1所示的式1和式3中，m和n相同或不同，且为5～20的整数。
根据本公开的增稠剂具有的化学结构为，羧烷基额外加至常规12-羟基硬脂酸锂盐增稠剂的硬脂酸的C9和C10位点。尽管不希望受到理论的束缚，这一化学结构可以影响润滑油的低温可操作性和高温下油分离特性的同时增强的发生。
包含根据本公开的由式1表示的增稠剂的润滑油组合物具有以下特性。根据本发明的润滑油组合物包含：a)合成性聚α-烯烃(PAO)基础油；b)由式1表示的锂类增稠剂；以及任选的c)常规的润滑油添加剂。在下文中，更具体地描述构成本公开润滑油组合物的各个成分。
根据本公开的润滑油组合物包含合成性聚α-烯烃(PAO)基础油作为基础油。PAO合成性基础油具有40℃下30～100厘沲(cSt)的运动粘度和低温下30℃或更低温度的流动点。当运动粘度小于30cSt时，容易发生蒸发且耐热性可能不足。当运动粘度大于100cSt时，扭矩较高且热值增加。
在根据本公开的润滑油组合物中，可以以70wt％～85wt％的量包含PAO合成性基础油。在此，当基础油的含量小于70wt％时，发生过度的固结，因此生成的润滑油不实用。当基础油的含量大于85wt％时，可能引起过高的油分离程度和高温下液化。
根据本公开的润滑油组合物包含由式1表示的9,10,12-三取代硬脂酸锂盐作为增稠剂。该增稠剂具有的结构是，向12-羟基硬脂酸锂盐的结构额外添加羧烷基。润滑油的高温稳定性和低温可操作性可以同时得到增强。
在根据本公开的润滑油组合物中，可以以10wt％～20wt％的量包含由式1表示的增稠剂。当增稠剂的含量低于10wt％时，预期的高温稳定性和低温可操作性可能无法同时得到增强。当增稠剂以高于20wt％大量使用时，润滑剂的稠度(NLGI)降低，由此低温可操作性会变差。
润滑油可以在无添加剂的情况下实现润滑功能，但是，为进一步提高润滑油的性能并满足用户需求，可以在其中包含多种添加剂。
在本公开中，可以包含粘度调节剂来作为添加剂。粘度调节剂是通常用来控制粘度指数并增强对基础油的附着力的添加剂。常用的粘度调节剂具有室温下大于10,000cSt的粘度，由此其在对使用低粘度材料的部件的应用中受到限制。因此，在本公开中，基于润滑油组合物的总重量，以1wt％至7wt％的量使用室温下粘度为500～1000cSt的酯类粘度调节剂。当酯类粘度调节剂包含在该范围内时，除粘度调节剂的固有效果例如粘度指数控制和增强对基础油的粘着性之外，还实现低温可操作性的增强效果。粘度调节剂的实例包括，但不限于，市售可得的VL 1200H，其是Lubrizol公司制备的复合烯烃酯共聚物产品。
此外，在本公开中，可以包含油分离调节剂作为添加剂。润滑油呈现出油分离现象，其中基础油和增稠剂会在存贮期间变得分离，由此油成分被分离。这样的油分离现象在高温下更容易发生。因此，在本公开中，可以在润滑油组合物中包含苯乙烯类共聚物作为油分离调节剂，即使在高温下也可以减少油分离。具体而言，可以包含选自苯乙烯-乙烯/丙烯嵌段共聚物和苯乙烯-异戊二烯共聚物中的一种或多种作为油分离调节剂。基于润滑油组合物的总重量，油分离调节剂可以以0.5wt％～3wt％的量使用。当油分离调节剂的含量大于3wt％时，润滑油的粘度增加，由此在低温甚至在室温下的操作感会降低。
此外，根据本公开的润滑油组合物可以包含极压添加剂、抗氧化剂、缓蚀剂等作为常规添加剂。如果需要，另外可以包含防锈剂、金属钝化剂等。
加入极压添加剂来增强负荷携带容量和极压特性。当向金属的接触面施加高负荷且因此摩擦热增加时，仅以油膜难以维持润滑功能。因此，在润滑油组合物中包含极压添加剂，由此防止接触面的磨损或灼热。在本公开中，极压添加剂不受具体限制，且其用量可以适当地控制在对这些添加剂来说通常使用的含量范围内。
极压添加剂可以不受限制地包括有机金属类添加剂、硫类添加剂、磷酸盐(酯)类添加剂或卤素类添加剂。有机金属类极压添加剂的一些具体实例包括，但不限于，有机钼化合物，例如二硫代氨基甲酸钼或二硫代磷酸钼；有机锌化合物，例如二硫代氨基甲酸锌、二硫代磷酸锌或锌片(zinc pennate)；有机锑化合物，例如二硫代氨基甲酸锑或二硫代磷酸锑；有机硒化合物，例如二硫代氨基甲酸硒；有机铋化合物，例如环烷酸铋或二硫代氨基甲酸铋；有机铁化合物，例如二硫代氨基甲酸铁和辛酸铁；有机铜化合物，例如二硫代氨基甲酸铜或环烷酸铜；有机锡化合物，例如马来酸锡或二丁基硫化锡；有机磺酸盐，例如磺酸碱金属盐或磺酸碱土金属盐；有机磷酸盐，例如磷酸碱金属盐或磷酸碱土金属盐；或有机金属化合物，例如金、银、钛和镉。作为硫类极压添加剂，可以使用硫化物，例如二苄基二硫醚或多硫化物、硫化油、不含矿物的氨基甲酸盐、硫脲类化合物、或硫代碳酸盐。作为磷酸酯(盐)类极压添加剂，可以使用磷酸酯，例如磷酸三辛酯或磷酸三甲苯酯；或者磷酸酯类化合物，例如酸性磷酸酯、亚磷酸酯、或酸性亚磷酸酯。此外，可以使用卤素类极压添加剂，例如氯化烯烃。
作为抗氧化剂，可以使用通常添加至橡胶、塑料或润滑剂配方中的耐老化剂、臭氧降解抑制剂或抗氧化剂。在本公开中，抗氧化剂不受具体限制，且其用量可以适当地控制在常用添加剂的含量范围内。抗氧化剂的具体实例包括胺类化合物，例如苯基-1-萘胺、苯基-2-萘胺、二苯基-对苯二胺、二吡啶胺、吩噻嗪、N-甲基吩噻嗪、N-乙基吩噻嗪、3,7-二辛基吩噻嗪、p,p’-二辛基二苯胺、N,N’-二异丙基-对苯二胺、N,N’-二-仲丁基-对苯二胺；酚类化合物，例如2,6-二(叔丁基)苯酚；其有机金属化合物等等。
缓蚀剂也是常用的成分且其选择在本公开中不受具体限制。其用量也可以适当地控制在常用添加剂的含量范围之内。这种缓蚀剂的具体实例包括有机磺酸的铵盐；碱土金属的有机磺酸盐或有机碳酸盐；羟基脂肪酸，例如油酰基肌氨酸；巯基脂肪酸，例如1-巯基硬脂酸酯；噻唑；咪唑，例如2-(癸基二硫代)-苯并咪唑和苯并咪唑；磷酸酯，例如三(壬苯基)亚磷酸酯；以及硫代羧酸酯，例如二月桂基硫代丙酸酯。此外，可以使用亚硝酸盐等。
基于润滑油组合物的总重量，上述添加剂的总量可以为0.1wt％～10wt％。
以下实施例示例说明本公开的教导，而不旨在对其进行限制。
制备例：增稠剂的合成
将总共1摩尔的9,10,12-三羟基硬脂酸酯溶解在90℃温水中，然后，向其中加入壬二酸(1.2摩尔)和癸二酸(1.2摩尔)，接着在80℃反应。随后，向其中加入氢氧化锂(1.2mol)并在60℃反应，由此制备出由以下式1a表示的9,10,12-三取代硬脂酸锂盐：
Figure GDA0002755230240000071
实施例1～7和比较例1～2：润滑油的制备
使用在以下列表和表1中总结的成分和组成比来制备润滑油组合物。此外，根据在以下表2中总结的方法来测定各个所制备的润滑油组合物的特性。结果总结在以下表3中。用于制备润滑油的成分包括以下(i～v)：
[所用的成分]
(1)基础油：40℃下运动粘度为65cSt的PAO合成基础油。
(2)增稠剂：(a)12-羟基硬脂酸锂盐，作为常规的锂类增稠剂；或(b)根据制备例合成的增稠剂。
(3)粘度调节剂：可得自Lubrizol的VL 1200H，作为室温下粘度为800cSt的复合烯烃酯共聚物。
(4)油分离调节剂：可得自Lubrizol的7460，作为苯乙烯-乙烯/丙烯嵌段共聚物；或可得自Lubrizol的7306，作为苯乙烯-异戊二烯共聚物。
(5)常用添加剂：常用添加剂例如可得自ADEKA的磷酸胺抗氧化剂和可得自Vanderbilt Minerals,LLC的磺酸钙缓蚀剂。
表1-润滑油组合物
Figure GDA0002755230240000072
Figure GDA0002755230240000081
表2-特性测定方法
Figure GDA0002755230240000082
表3-特性测定
Figure GDA0002755230240000083
如表3所示，可以确定，连同作为增稠剂的9,10,12-三取代硬脂酸锂盐，根据实施例1～5的润滑油组合物包含酯类粘度调节剂和苯乙烯类油分离调节剂(具有室温下800cSt的粘度)。因此，表明部件在低温下可操作性的低温扭矩和剪切粘度以及油分离程度均较低。另一方面，比较例1～3的润滑油组合物包含12-羟基硬脂酸锂盐作为增稠剂，由此，在100℃油分离程度评估中，与根据实施例1～5的润滑油组合物中的0.2wt％～0.4wt％的值相比，显示出1.8wt％～2.8wt％的较高值。此外，能够确认的是，根据比较例4～6的润滑油组合物包含9,10,12-三取代硬脂酸锂盐作为增稠剂，但是不包含粘度调节剂和/或油分离调节剂，因此，与实施例相比，其低温扭矩、剪切粘度和油分离程度未得到满足。
根据实施例的实验结果可知，由根据本公开式1表示的9,10,12-三取代硬脂酸锂盐在作为包含PAO合成基础油的润滑油组合物中的增稠剂时是有效的。此外，由式1表示的9,10,12-三取代硬脂酸锂盐连同具有特定粘度范围的酯类粘度调节剂和苯乙烯类油分离调节剂均包含在润滑油组合物中，因此，高温下的热稳定性和低温下的可操作性可以同时得到改善。
根据本发明的增稠剂连同合成性聚α-烯烃(PAO)基础油均包含在润滑油组合物中，由此同时增强高温下的稳定性和低温下的可操作性。
作为油分离调节剂的苯乙烯类共聚物还另外包含在根据本发明的润滑油组合物中，因此，高温下的油分离特性和低温下的可操作性得到进一步增强。
具有特定粘度的酯类粘度调节剂还另外包含在根据本发明的润滑油组合物中，因此，低温可操作性可以得到进一步增强。
本公开已参考其多种形式进行了详细描述。然而，本领域技术人员将领会到，在不偏离本公开的原则和精神的前提下，可以在多种形式中做出改变，本公开的范围在所附权利要求及其等同方式中限定。

Claims (8)

1.一种锂类增稠剂，其由以下通式1表示：
Figure FDA0002755230230000011
在该通式中，m和n相同或不同，且为5～20的整数。
2.根据权利要求1所述的锂类增稠剂，其中，m和n相同或不同，且为7或8的整数。
3.一种润滑油组合物，其包含合成性聚α-烯烃基础油、锂类增稠剂和常规润滑油添加剂，所述锂类增稠剂是由以下通式1表示的9,10,12-三取代硬脂酸锂盐：
Figure FDA0002755230230000012
在该通式中，m和n相同或不同，且为5～20的整数。
4.根据权利要求3所述的润滑油组合物，其中，所述润滑油组合物包含：
70～85重量％的所述合成性聚α-烯烃基础油；
10～20重量％的所述锂类增稠剂；以及
0.1～10重量％的所述添加剂。
5.根据权利要求3所述的润滑油组合物，其中，包含室温下粘度为500～1000cSt的酯类粘度调节剂作为所述添加剂。
6.根据权利要求5所述的润滑油组合物，其中，基于所述润滑油组合物的总重量，以1～7重量％的含量范围包含所述酯类粘度调节剂。
7.根据权利要求3所述的润滑油组合物，其中，包含一种或多种选自苯乙烯-乙烯/丙烯嵌段共聚物和苯乙烯-异戊二烯共聚物中的苯乙烯类油分离调节剂作为所述添加剂。
8.根据权利要求7所述的润滑油组合物，其中，基于所述润滑油组合物的总重量，以0.5～3重量％的含量范围包含所述苯乙烯类油分离调节剂。
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