CN111621355A - 用于齿轮油的润滑剂组合物 - Google Patents

用于齿轮油的润滑剂组合物 Download PDF

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CN111621355A
CN111621355A CN201911106434.9A CN201911106434A CN111621355A CN 111621355 A CN111621355 A CN 111621355A CN 201911106434 A CN201911106434 A CN 201911106434A CN 111621355 A CN111621355 A CN 111621355A
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lubricant composition
olefin copolymer
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oil
lubricant
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CN111621355B (zh
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李炯镇
罗景柱
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DL Chemical Co Ltd
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Daelim Industrial Co Ltd
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Abstract

本发明涉及润滑剂组合物，并且更具体地涉及这样的润滑剂组合物：其包含乙烯‑α烯烃低聚物和烷基化鏻化合物，从而实现能量减少和增加的耐久寿命，并因此其适用于齿轮油。本发明的润滑剂组合物包含基础油、液态烯烃共聚物和烷基化鏻化合物。

Description

用于齿轮油的润滑剂组合物
技术领域
本发明涉及润滑剂组合物，并且更具体地涉及这样的润滑剂组合物：其包含乙烯-α烯烃低聚物和烷基化鏻化合物，从而实现能量减少和增加的耐久寿命，并因此其适用于齿轮油。
背景技术
近来，随着诸如全球变暖、臭氧层破坏等的环境问题涌现出来，环境法规变得严格。因此，减少二氧化碳排放正受到大量的关注。为了减少二氧化碳排放，迫切需要减少车辆、建筑机械、农业机械等中的能量消耗，即提高燃料经济性，因此强烈需要能够有助于发动机、变速器、主减速器、压缩机、液压装置等中的能量减少的措施。因此，与常规情况相比，要求用于这样的装置的润滑剂具有降低搅拌阻力或摩擦阻力的能力。
润滑剂是用于减少机器的摩擦表面上的摩擦力的产生或者使从摩擦表面产生的摩擦热消散的油性材料。润滑剂是通过向基础油中添加添加剂而制造的，并且根据基础油的类型，大致分为基于矿物油的润滑剂(基于石油的润滑剂)和合成润滑剂，合成润滑剂分为基于聚α烯烃的润滑剂和基于酯的润滑剂。
作为用于提高变速器和减速器齿轮的燃料经济性的手段，通常使用降低润滑剂的粘度。例如，在变速器中，用于车辆的自动变速器或无级变速器具有变矩器、湿式离合器、齿轮轴承机构、油泵、液压控制机构等，而手动变速器或减速器具有齿轮轴承机构，因此当进一步降低其所用润滑剂的粘度时，变矩器、湿式离合器、齿轮轴承机构和油泵的搅拌阻力和摩擦阻力降低，从而提高了动力传递效率，最终使得可以提高车辆的燃料经济性。
然而，当降低常规润滑剂的粘度时，由于摩擦性能的劣化，因此装配性能大大降低，并且发生粘着等，从而导致变速器等的缺陷。特别是，在低粘度的情况下，粘度改进剂在其使用期间被剪切，因此粘度降低，使得齿轮的耐磨性受损并且装配性能容易劣化。此外，即使当添加硫/磷极压剂以提高低粘度油的极压性能时，装配性能和耐久寿命也显著降低，使得难以实现其长期使用。
因此，本发明人已经开发了用于齿轮油的润滑剂组合物，其能够减少齿轮部件的机械磨损和能量消耗，并且还能够表现出优异的热稳定性和氧化稳定性，因此可以在工业上长时间使用。
[引用列表]
[专利文献]
(专利文献0001)韩国专利第10-1420890号
(专利文献0002)韩国专利第10-1347964号
发明内容
技术问题
因此，牢记相关技术中遇到的问题而做出了本发明，并且本发明的一个目的是提供这样的润滑剂组合物：其中将用于减小摩擦的功能添加剂和乙烯-α烯烃液态无规共聚物混合，从而表现出优异的摩擦特性、热稳定性和氧化稳定性。
本发明的另一个目的是提供用于齿轮油的润滑剂组合物，当应用于变速器和减速器的齿轮时，该润滑剂组合物能够减少齿轮部件的机械磨损和能量消耗，并且由于齿轮油的物理特性的低变化而可以长时间使用。
技术方案
为了实现上述目的，本发明提供了一种润滑剂组合物，其包含基础油、液态烯烃共聚物和烷基化鏻化合物。
基础油可以是选自矿物油、聚α烯烃(PAO)和酯中的至少一者。
液态烯烃共聚物可以通过使乙烯和α烯烃在单位点催化剂体系的存在下共聚合来制备，并且单位点催化剂体系优选包含茂金属催化剂、有机金属化合物和离子化合物。
液态烯烃共聚物的热膨胀系数可以为3.0至4.0。
在本发明的润滑剂组合物中，液态烯烃共聚物可以以0.1重量％至30重量％，并且优选0.5重量％至25重量％的量包含在内。烷基化鏻化合物可以以0.1重量％至5.0重量％，并且优选0.3重量％至4.0重量％的量包含在内。
润滑剂组合物可以具有0.2至0.3的SRV摩擦系数和0.15至0.3的牵引系数。此外，在FZG齿轮效率试验中，润滑剂组合物的由于摩擦导致的小齿轮扭矩损失率可以小于1％。
发明效果
根据本发明，除了现有的硫/磷极压剂之外，润滑剂组合物还包含烷基化鏻化合物作为减摩剂，从而使摩擦性能最大化以因此当应用于变速器和减速器的齿轮时减小齿轮部件的机械磨损和能量消耗，最终使节能效果最大化。
另外，根据本发明，润滑剂组合物包含在茂金属化合物催化剂的存在下制备的烯烃共聚物作为粘度改进剂，并因此可以表现出高粘度指数和优异的低温稳定性。
因此，本发明可以提供用于齿轮油的润滑剂组合物，其由于齿轮油的物理特性的低变化而使得能够长期使用。
具体实施方式
在下文中，将给出本发明的详细描述。
本发明涉及润滑剂组合物，其具有优异的氧化稳定性和摩擦特性并因此适用于齿轮油。因此，本发明的润滑剂组合物包含基础油、液态烯烃共聚物和烷基化鏻化合物。
在此，基础油根据制造方法或精炼方法而在粘度、耐热性、氧化稳定性等方面有所不同，但是通常分为矿物油和合成油。API(American Petroleum Institute，美国石油学会)将基础油分为五种类型，即第I类、第II类、第III类、第IV类和第V类。基于API范围，这些类型在2002年4月的API出版物1509，第15版，附录E中定义，并示于下表1中。
[表1]
Figure BDA0002271451800000031
Figure BDA0002271451800000041
在本发明的润滑剂组合物中，基础油可以是选自矿物油、聚α烯烃(PAO)和酯中的至少一者，并且可以是基于API范围的第I至V类中的任何类型。
更具体地，基于API范围，矿物油属于第I至III类，并且矿物油可以包括：由使通过原油的常压蒸馏和/或真空蒸馏获得的润滑剂馏出物馏分经历溶剂脱沥青、溶剂萃取、氢解、溶剂脱蜡、催化脱蜡、加氢精制、硫酸清洗和白粘土处理中的至少一种精炼过程而得到的油；蜡异构化矿物油；或经由费-托法(Fischer-Tropsch process)获得的天然气制油(gas-to-liquid，GLT)。
基于API范围，合成油属于第IV类或第V类，属于第IV类的聚α烯烃可以通过使用酸催化剂的高级α烯烃的低聚反应来获得，如美国专利第3,780,128号、美国专利第4,032,591号、日本专利申请公开号平1-163136等中所公开的，但是本发明不限于此。
属于第V类的合成油的实例包括烷基苯、烷基萘、异丁烯低聚物或其氢化物、石蜡、聚氧化亚烷基二醇、二烷基二苯醚、聚苯醚、酯等。
在此，烷基苯和烷基萘通常是烷基链长度为6至14个碳原子的二烷基苯或二烷基萘，并且烷基苯或烷基萘通过苯或萘与烯烃的弗瑞德-克来福特(Friedel-Crafts)烷基化来制备。用于制备烷基苯或烷基萘的烷基化烯烃可以是线性或支化的烯烃或其组合。
另外，酯的实例包括但不限于：戊二酸双十三烷基酯、己二酸二-2-乙基己酯、己二酸二异癸酯、己二酸双十三烷基酯、癸二酸二-2-乙基己酯、壬酸十三烷基酯、己二酸二-2-乙基己酯、壬二酸二-2-乙基己酯、三羟甲基丙烷辛酸酯、三羟甲基丙烷壬酸酯、三羟甲基丙烷三庚酸酯、季戊四醇2-乙基己酸酯、季戊四醇壬酸酯、季戊四醇四庚酸酯等。
在本发明的润滑剂组合物中，液态烯烃共聚物通过使乙烯和α烯烃单体在单位点催化剂体系的存在下共聚合以使α烯烃单元均匀地分布在共聚物链中来制备。优选地，液态烯烃共聚物通过使乙烯和α烯烃单体在单位点催化剂体系的存在下反应来制备，所述单位点催化剂体系包含交联的茂金属化合物、有机金属化合物和用于通过与交联的茂金属化合物反应形成离子对的离子化合物。
在此，单位点催化剂体系中包含的茂金属化合物可以是选自以下化学式1至6中的至少一者。
[化学式1]
Figure BDA0002271451800000051
[化学式2]
Figure BDA0002271451800000052
[化学式3]
Figure BDA0002271451800000053
[化学式4]
Figure BDA0002271451800000061
在化学式1至4中，
M是选自钛、锆和铪的过渡金属，
B不存在或者为包括以下的连接基团：C1-C20亚烷基、C6-C20亚芳基、C1-C20二烷基硅、C1-C20二烷基锗、C1-C20烷基膦基或C1-C20烷基胺基，
X1和X2彼此相同或不同，各自独立地为卤素原子、C1-C20烷基、C2-C20烯基、C2-C20炔基、C6-C20芳基、C7-C40烷基芳基、C7-C40芳基烷基、C1-C20烷基酰胺基、C6-C20芳基酰胺基、C1-C20烷叉基或C1-C20烷氧基，以及
R1至R10彼此相同或不同，各自独立地为氢、C1-C20烷基、C2-C20烯基、C6-C20芳基、C7-C20烷基芳基、C7-C20芳基烷基、C5-C60环烷基、C4-C20杂环基、C1-C20炔基、含C6-C20芳基的杂基或甲硅烷基。
[化学式5]
Figure BDA0002271451800000062
[化学式6]
Figure BDA0002271451800000071
在化学式5和6中，
M是选自钛、锆和铪的过渡金属，
B不存在或者为包括以下的连接基团：C1-C20亚烷基、C6-C20亚芳基、C1-C20二烷基硅、C1-C20二烷基锗、C1-C20烷基膦基或C1-C20烷基胺基，
X1和X2彼此相同或不同，各自独立地为卤素原子、C1-C20烷基、C2-C20烯基、C2-C20炔基、C6-C20芳基、C7-C40烷基芳基、C7-C40芳基烷基、C1-C20烷基酰胺基、C6-C20芳基酰胺基、C1-C20烷叉基或C1-C20烷氧基，以及
R1至R10彼此相同或不同，各自独立地为氢、C1-C20烷基、C2-C20烯基、C6-C20芳基、C7-C20烷基芳基、C7-C20芳基烷基、C5-C60环烷基、C4-C20杂环基、C1-C20炔基、含C6-C20芳基的杂基或甲硅烷基。
此外，R11、R13和R14全部为氢，每个R12基团彼此相同或不同，可以独立地为氢、C1-C20烷基、C2-C20烯基、C6-C20芳基、C7-C20烷基芳基、C7-C20芳基烷基、C5-C60环烷基、C4-C20杂环基、C1-C20炔基、含C6-C20芳基的杂基或甲硅烷基。
另外，化学式2至6的茂金属化合物可以包括通过加氢反应取代的化合物，并且其优选实例包括二甲基甲硅烷基双(四氢茚基)二氯化锆。
单位点催化剂体系中包含的有机金属化合物可以是选自有机铝化合物、有机镁化合物、有机锌化合物和有机锂化合物中的至少一者，并且优选为有机铝化合物。有机铝化合物可以是选自以下中的至少一者：例如，三甲基铝、三乙基铝、三异丁基铝、三丙基铝、三丁基铝、二甲基氯铝、二甲基异丁基铝、二甲基乙基铝、二乙基氯铝、三异丙基铝、三异丁基铝、三环戊基铝、三戊基铝、三异戊基铝、乙基二甲基铝、甲基二乙基铝、三苯基铝、甲基铝氧烷、乙基铝氧烷、异丁基铝氧烷和丁基铝氧烷，并且优选为三异丁基铝。
单位点催化剂体系中包含的离子化合物可以是选自有机硼化合物例如二甲基苯胺四(全氟苯基)硼酸盐/酯、三苯基碳鎓四(全氟苯基)硼酸盐/酯等中的至少一者。
可以考虑到催化活性来确定单位点催化剂体系的组分比，并且茂金属催化剂:离子化合物:有机金属化合物的摩尔比优选在1:1:5至1:10:1000的范围内调整以确保期望的催化活性。
此外，单位点催化剂体系的组分可以同时或以任何顺序添加到合适的溶剂中并且因此可以起活性催化剂体系的作用。在此，溶剂可以包括但不限于烃溶剂例如戊烷、己烷、庚烷等，或芳族溶剂例如苯、甲苯、二甲苯等，并且可以使用可用于制备的任何溶剂。
另外，用于制备液态烯烃共聚物的α烯烃单体包括C2-C20脂族烯烃，并且具体地可以是选自以下中的至少一者：乙烯、丙烯、1-丁烯、1-戊烯、3-甲基-1-丁烯、1-己烯、4-甲基-1-戊烯、3-甲基-1-戊烯、1-庚烯、1-辛烯、1-癸烯、1-十二碳烯和1-十四碳烯，并且可以包括异构形式，但是本发明不限于此。在共聚合中，单体含量为1mol％至95mol％，优选5mol％至90mol％。
本发明中需要的液态烯烃共聚物具有3.0至4.0的热膨胀系数和0.1或更小的溴值。
基于100重量％的润滑剂组合物，液态烯烃共聚物可以以0.1重量％至30重量％，并且优选0.5重量％至25重量％的量包含在内。如果基于100重量％的润滑剂组合物，液态烯烃共聚物的量小于0.1重量％，则低温稳定性可能劣化。另一方面，如果其量超过30重量％，则无法实现足够的粘度，并因此将所得组合物应用于齿轮油变得困难，这是不期望的。
用作减摩剂的烷基化鏻化合物可以是选自四辛基化双乙基己基磷酸鏻、双(2-乙基己基)磷酸三丁基十四烷基鏻、双(2-乙基己基)磷酸四乙基鏻和双(2-乙基己基)磷酸三丁基鏻中的至少一者。当润滑剂组合物中包含烷基化鏻化合物时，其可以表现出与现有的耐磨剂的协同效应和减小摩擦的效果，此外，可以通过减小摩擦来实现节能效果。
基于100重量％的润滑剂组合物，烷基化鏻化合物可以以0.1重量％至5.0重量％，并且优选0.3重量％至4.0重量％的量包含在内。如果基于100重量％的润滑剂组合物，烷基化鏻化合物的量小于0.1重量％，则减小摩擦的效果不明显。另一方面，如果其量超过5.0重量％，则尽管其过量添加，但是附加的减小效果不明显，这是不期望的。
本发明的润滑剂组合物还可以包含选自抗氧化剂、金属清洗剂、防腐剂、泡沫抑制剂、倾点下降剂、粘度改进剂、耐磨剂、及其组合的添加剂。
基于100重量％的润滑剂组合物，抗氧化剂可以以0.01重量％至5.0重量％的量包含在内，并且优选以酚类抗氧化剂和胺类抗氧化剂的混合物，更优选0.01重量％至3.0重量％的酚类抗氧化剂和0.01重量％至3.0重量％的胺类抗氧化剂的混合物的形式使用。
酚类抗氧化剂可以是选自2,6-二丁基苯酚、受阻双酚、高分子量受阻酚和受阻酚与硫醚中的任一者。
胺类抗氧化剂可以是选自二苯胺、烷基化二苯胺和萘胺中的任一者，并且优选地，烷基化二苯胺是二辛基二苯胺、辛基化二苯胺或丁基化二苯胺。
金属清洗剂可以是选自金属酚盐、金属磺酸盐和金属水杨酸盐中的至少一者，并且优选地，基于100重量％的润滑剂组合物，金属清洗剂以0.1重量％至10.0重量％的量包含在内。
防腐剂可以是苯并三唑衍生物，并且优选是选自苯并三唑、2-甲基苯并三唑、2-苯基苯并三唑、2-乙基苯并三唑和2-丙基苯并三唑中的任一者。基于100重量％的润滑剂组合物，防腐剂可以以0重量％至4.0重量％的量包含在内。
泡沫抑制剂可以是聚氧化烯多元醇，并且优选地，基于100重量％的润滑剂组合物，泡沫抑制剂以0重量％至4.0重量％的量包含在内。
倾点下降剂可以是聚(甲基丙烯酸甲酯)，并且优选地，基于100重量％的润滑剂组合物，倾点下降剂以0.01重量％至5.0重量％的量包含在内。
粘度改进剂可以是聚异丁烯或聚甲基丙烯酸酯，并且优选地，基于100重量％的润滑剂组合物，粘度改进剂以0重量％至15重量％的量包含在内。
耐磨剂可以是选自有机硼酸盐/酯、有机亚磷酸盐/酯、有机含硫化合物、二烷基二硫代磷酸锌、二芳基二硫代磷酸锌和磷硫化烃中的至少一者，并且优选地，耐磨剂以0.01重量％至3.0重量％的量包含在内。
本发明的润滑剂组合物具有0.2至0.3的SRV摩擦系数和0.15至0.3的牵引系数。另外，如通过作为齿轮油台架(rig)试验的FZG齿轮效率试验所测量的，本发明的润滑剂组合物的由于摩擦导致的小齿轮扭矩损失率小于1％。
发明实施方式
通过以下实施例更好地理解本发明。然而，本发明不限于这些实施例，而是可以以其他形式来实施。提供这些实施例以彻底解释本发明并将本发明的精神充分地传达给本领域技术人员。
1.添加剂组合物的制备
如下表2所示制备用于本发明的润滑剂组合物的添加剂组合物。
[表2]
Figure BDA0002271451800000101
2.液态烯烃共聚物
使用低聚方法通过催化反应过程制备液态烯烃共聚物。根据随后的反应时间和条件，制备具有不同分子量的液态烯烃共聚物，并且其特性示于下表3中。
反应时间和条件从20小时开始各自增加4小时。在此，向其中添加的氢和共聚单体C3的量各自增加10％，并在单独的条件下进行聚合，并且根据其分子量对所得聚合物进行分类。
[表3]
Figure BDA0002271451800000102
Figure BDA0002271451800000111
3.用于齿轮油的润滑剂组合物的制备
如下表4和5所示，通过将基础油、液态烯烃共聚物、烷基化鏻化合物和以上制备的添加剂混合来制备润滑剂组合物。在此，基础油是在100℃下运动粘度为4cSt的聚α烯烃(PAO 4cSt，可获自Chevron Philips)，烷基化鏻化合物是四辛基化双乙基己基磷酸鏻。
制备例1至72和比较例1至9.包含添加剂A的用于齿轮油的润滑剂组合物
[表4]
Figure BDA0002271451800000112
Figure BDA0002271451800000121
Figure BDA0002271451800000131
制备例73至148和比较例10至16.包含添加剂B的用于齿轮油的润滑剂组合物
[表5]
Figure BDA0002271451800000132
Figure BDA0002271451800000141
Figure BDA0002271451800000151
Figure BDA0002271451800000161
4.特性评估
如下测量制备例和比较例中制备的润滑剂组合物的特性。结果示于下表6和7中。
摩擦系数
在盘上球(ball-on-disc)模式下，通过在50Hz下依次将温度以10℃的增量从40℃升高至120℃并比较在各个温度下的平均摩擦系数来评估摩擦性能。在此，摩擦系数值随着有效性的增加而减小。
牵引系数
使用PCS Instruments制造的MTM仪器测量牵引系数。在此，将测量条件固定为50N和SRR 50％，并且根据温度变化观察摩擦力和牵引力。温度从40℃变化至120℃，并比较平均值。
耐磨性
在20kg负载、1200rpm和54℃的条件下，使四个钢球在有润滑剂组合物的情况下经历摩擦60分钟，比较磨痕的尺寸，并根据ASTM D4172进行评估。在此，磨痕(平均磨痕直径，μm)值随着有效性的增加而减小。
氧化稳定性
根据ASTM D2271，使用RBOT(Rotational Bomb Oxidation Test，旋转氧弹试验)仪测量氧化稳定性。
摩擦损失
作为齿轮油台架试验，进行FZG齿轮效率试验。在FZG效率试验中，在其中油温固定为100℃且不施加负载的条件下，通过用根据油的类型指定的电机驱动器旋转来测量小齿轮扭矩，并由此计算现有的油和使用α烯烃共聚物和烷基化鏻化合物的油的小齿轮扭矩损失率，并比较其相对值。
[表6]
Figure BDA0002271451800000171
Figure BDA0002271451800000181
Figure BDA0002271451800000191
[表7]
Figure BDA0002271451800000192
Figure BDA0002271451800000201
Figure BDA0002271451800000211
从表6和7可以明显看出，与比较例的润滑剂组合物相比，包含本发明的量范围内的液态烯烃共聚物和烷基化鏻化合物的润滑剂组合物在磨痕和摩擦系数方面显著降低，并且还表现出优异的氧化稳定性。
此外，所得的FZG齿轮效率试验中的至少5％至12％的效率提高表明，即使在实际使用中，本发明的润滑剂组合物也能够减少齿轮损失，从而显著改善燃料经济性或节能效果。
因此，结论是，本发明的润滑剂组合物在摩擦特性和稳定性方面得到改善，并因此适用于齿轮油。
尽管已经出于说明目的公开了本发明的实施方案，但是本领域技术人员将理解，在不脱离如所附权利要求中公开的本发明的范围和精神的情况下，可以进行各种修改、添加和替换。

Claims (13)

1.一种润滑剂组合物，包含
基础油、液态烯烃共聚物和烷基化鏻化合物。
2.根据权利要求1所述的润滑剂组合物，其中所述液态烯烃共聚物通过使用单位点催化剂体系使乙烯和α烯烃共聚合来制备。
3.根据权利要求2所述的润滑剂组合物，其中所述单位点催化剂体系包含茂金属催化剂、有机金属化合物和离子化合物。
4.根据权利要求1所述的润滑剂组合物，其中所述液态烯烃共聚物的热膨胀系数为3.0至4.0。
5.根据权利要求1所述的润滑剂组合物，其中所述液态烯烃共聚物的溴值为0.1或更小。
6.根据权利要求1所述的润滑剂组合物，其中所述烷基化鏻化合物以0.1重量％至5.0重量％的量包含在所述润滑剂组合物中。
7.根据权利要求1所述的润滑剂组合物，其中所述液态烯烃共聚物以0.1重量％至30重量％的量包含在所述润滑剂组合物中。
8.根据权利要求1所述的润滑剂组合物，其中所述基础油是选自矿物油、聚α烯烃(PAO)和酯中的至少一者。
9.根据权利要求1所述的润滑剂组合物，还包含选自以下的添加剂：抗氧化剂、金属清洗剂、防腐剂、泡沫抑制剂、倾点下降剂、粘度改进剂、耐磨剂、及其组合。
10.根据权利要求1所述的润滑剂组合物，其中所述润滑剂组合物的SRV摩擦系数为0.2至0.3。
11.根据权利要求1所述的润滑剂组合物，其中所述润滑剂组合物的牵引系数为0.15至0.3。
12.根据权利要求1所述的润滑剂组合物，其中在FZG齿轮效率试验中，所述润滑剂组合物的由于摩擦导致的小齿轮扭矩损失率小于1％。
13.根据权利要求1所述的润滑剂组合物，其中所述润滑剂组合物用作齿轮油。
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