CN106883903B - 一种离子液体修饰的二硫化钨复合物极压抗磨剂的制备及含有该抗磨剂的发动机油 - Google Patents

一种离子液体修饰的二硫化钨复合物极压抗磨剂的制备及含有该抗磨剂的发动机油 Download PDF

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CN106883903B
CN106883903B CN201710137349.3A CN201710137349A CN106883903B CN 106883903 B CN106883903 B CN 106883903B CN 201710137349 A CN201710137349 A CN 201710137349A CN 106883903 B CN106883903 B CN 106883903B
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ionic liquid
tungsten disulfide
engine oil
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徐金玲
何茂伟
袁俊洲
乔良
纪祥娟
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SHANDONG YUANGEN PETROLEUM CHEMICAL CO Ltd
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Abstract

本发明属于四冲程发动机润滑剂领域，尤其涉及一种离子液体修饰的二硫化钨复合物极压抗磨剂的制备及含有该抗磨剂的发动机油。利用前驱体LixWS2与蒸馏水反应，调节PH再加入离子液，最后用四氟硼酸钾水溶液洗涤进行粒子交换，得到极压抗磨剂；发动机油则是将该极压抗磨剂与高温抗氧剂、清净剂、分散剂、粘度指数改进剂、降凝剂和消泡剂进行混合。使得本发明中合成的发动机油具有较低的摩擦系数、良好的极压抗磨性能。

Description

一种离子液体修饰的二硫化钨复合物极压抗磨剂的制备及含 有该抗磨剂的发动机油
技术领域
本发明属于四冲程发动机润滑剂领域，尤其涉及一种离子液体修饰的二硫化钨复合物极压抗磨剂的制备及含有该抗磨剂的发动机油。
背景技术
作为现代工业生产中不可或缺的润滑剂主要应用于交通运输行业的发动机中。具有减少摩擦、降低磨损、散热、清洁、密封和缓冲等功能，其目的是降低活塞磨耗、减少能量损失、提高燃油经济性。从2002年到2012年，我国年润滑剂的需求量从3625kt增加到6930kt，足以说明润滑剂在国民经济中的重要性。然而，随着国民经济的蓬勃发展，功率更大、结构更精密、效率更高的新型发动机逐渐步入我们的视野，这也对作为润滑剂的发动机油的性能指标提出了更高的要求。
美国摩擦学者与润滑工程师协会在2014年的调查报告中指出：未来对于润滑剂的要求是能够长时间在高温、高压、高速、高负荷的工作环境中为设备的相关部件提供稳定可靠的包括润滑、密封、散热和缓冲等在内的保护。此外，近些年随着公众环保意识的不断进步，润滑剂的环保性能越来越受到公众的关注，研究环境友好型的润滑剂已经势在必行。添加剂作为发动机油的重要组成部分，能够弥补和改善润滑剂基础油的不足，在一定程度上提高基础油的某些性能．所以研究开发新型添加剂来提高润滑剂的性能显得尤为关键。
二硫化钨作为一种新型润滑添加剂，最早是NASA(美国国家航空航天局)将其应用于宇宙飞船关键部位的润滑，并逐渐为大众所熟知。二硫化钨是一种类似石墨的灰黑色的六方晶格层状物质，每一层都是由两层硫原子夹一层钨原子按2：1的个数连接而成。其中硫原子和钨原子是由强共价键连接。层与层之间的硫原子则是由范德华力连接。特殊的晶体结构也使得二硫化钨相较于同类的二硫化钼润滑添加剂更为优秀，无论是在极压性能、抗磨减摩性能以及耐热耐氧化等方面，二硫化钨的表现都更加优秀。
虽然二硫化钨作为润滑油脂极压抗磨添加剂表现出广阔的应用前景和可观的经济效益，但是在这一领域的研究还处于起步阶段，还有很多问题没有研究，对其减摩、抗磨、极压机理的实际应用，还缺乏进一步的研究工作。
发明内容
本发明针对上述的问题，制备了离子液体修饰的二硫化钨复合物极压抗磨剂，并利用该极压抗磨剂制备了发动机油，即一种离子液体修饰的二硫化钨复合物极压抗磨剂的制备及含有该抗磨剂的发动机油。
为了达到上述目的，本发明采用的技术方案为，本发明提供一种离子液体修饰的二硫化钨复合物极压抗磨剂的制备方法，其特征在于，具体包括以下步骤：
a、在超声振荡的条件下，将0.4克前驱体LixWS2与1000ml的蒸馏水反应；
b、调节pH值，使其生产PH为7的二硫化钨单分子层悬浮液；
c、向该悬浮液中加入50ml离子液体，并在一定温度下65-75℃恒温搅拌24h；
d、用转速为2000rpm的离心机分离出固体产物；
e、用少量蒸馏水对产物进行多次洗涤，以确定除去LiOH和可溶性的物质；
f、最后用四氟硼酸钾水溶液洗涤数次进行粒子交换，干燥得样品，即得到离子液体修饰的二硫化钨复合物极压抗磨剂。
一种含有离子液体修饰的二硫化钨复合物极压抗磨剂的发动机油，其特征在于，按照重量百分比具体包括：
基础油 70%～90%；
离子液体修饰的二硫化钨复合物极压抗磨剂 0.5～1.5%；
高温抗氧剂 0.1～0.5%；
清净剂 2～5.7%；
分散剂 3～5%；
黏度指数改进剂 5～10%；
降凝剂 0.1～0.3%；
消泡剂 0.0001~0.0002%。
作为优选，所述基础油为50%～40%的聚内烯烃与50%～60%的Ⅱ类基础油复合。
作为优选，所述高温抗氧剂为硫磷双辛基碱性锌盐、二苯胺中的一种。
作为优选，所述清净剂为硫化烷基酚钙、烷基水杨酸镁、烷基水杨酸钙中的一种。
作为优选，所述分散剂为双烯基丁二酰亚胺、聚异丁烯基丁二酰亚胺中的一种。
作为优选，所述黏度指数改进剂为聚甲基丙烯酸酯、苯乙烯与双烯共聚物、氢化苯乙烯异戊二烯共聚物中的一种。
作为优选，所述降凝剂为聚丙烯酸甲酯、聚α烯烃和T803B降凝剂中的一种。
作为优选，所述消泡剂磷酸三丁酯、聚二甲基硅氧烷、聚氧乙烯聚氧丙烯季戊四醇醚、聚氧乙烯聚氧丙醇胺醚中的一种。
与现有技术相比，本发明的优点和积极效果在于，
本发明本专利合成了离子液体修饰的二硫化钨复合物并将其应用于发动机油中。负荷较低时，金属表面受机械能作用向外发射外逸电子，使摩擦副表面产生正电荷点，由于离子液体的双电性结构，能牢牢的吸附在金属表面形成物理吸附膜，有效地隔开摩擦面，从而起到减摩抗磨作用。当负荷较高、摩擦加剧时，二硫化钨与金属底材发生化学作用，进而生产熔点较低的FeS膜，有效的减少金属摩擦副之间的接触，从而降低金属表面的磨损。而在高温工况下，二硫化钨会缓慢生产氧化物，氧化物的形成能抑制二硫化钨的进一步氧化，而形成的氧化物也具有较低的摩擦系数和二硫化钨相似的润滑性能，从而也能降低金属表面间磨损作用。因而本发明调配的发动机油，机油具有较低的摩擦系数、良好的极压抗磨性能，产品投产后可以为国内润滑油的生产提供高品质的发动机润滑油。
具体实施方式
为了能够更清楚地理解本发明的上述目的、特征和优点，下面结合实施例对本发明做进一步说明。需要说明的是，在不冲突的情况下，本申请的实施例及实施例中的特征可以相互组合。
在下面的描述中阐述了很多具体细节以便于充分理解本发明，但是，本发明还可以采用不同于在此描述的其他方式来实施，因此，本发明并不限于下面公开说明书的具体实施例的限制。
本发明提供一种离子液体修饰的二硫化钨复合物极压抗磨剂的制备及含有该抗磨剂的发动机油，即利用制备出的离子液体修饰的二硫化钨复合物极压抗磨剂添加到发动机油中，得到性能良好的发动机油，发明人经过大量实验得出一种离子液体修饰的二硫化钨复合物极压抗磨剂的制备方法，具体步骤为：在超声振荡的条件下，将0.4克（1.61×10-3mol）前驱体LixWS2与1000ml的蒸馏水反应，并调节pH值（用1M的HCL调节）使其生产PH7的二硫化钨单分子层悬浮液；之后向该悬浮液中加入50ml离子液体，并在一定温度下65-75℃恒温搅拌24h；再用转速为2000rpm的离心机分离出固体产物，并用少量蒸馏水对产物进行多次洗涤，以确定除去LiOH和可溶性的物质；最后用四氟硼酸钾水溶液洗涤数次进行粒子交换，干燥得样品，就能得到离子液体修饰的二硫化钨复合物极压抗磨剂，然后再将其研细备用。
下面实施例中则具体说明利用上述离子液体修饰的二硫化钨复合物极压抗磨剂制备的发动机油，其中基础油、高温抗氧剂、清净剂、分散剂、黏度指数改进剂 、降凝剂和消泡剂都会选择发明内容中所给的最优选择。
实施例1（质量百分比，按%计量，以下同）
Figure DEST_PATH_IMAGE002
按照上述组分混合均匀，即得到发动机油A。
实施例2
Figure DEST_PATH_IMAGE004
按照上述组分混合均匀，即得到发动机油B。
实施例3
Figure DEST_PATH_IMAGE006
按照上述组分混合均匀，即得到发动机油C。
实施例4
Figure DEST_PATH_IMAGE008
按照上述组分混合均匀，即得到发动机油D。
实施例5
Figure DEST_PATH_IMAGE010
按照上述组分混合均匀，即得到发动机油E。
对上述实施例中发动机油进行检测，其检测项目主要为摩擦系数和PB值，具体如下表：
Figure DEST_PATH_IMAGE012
从上述表格中可以看出，利用本发明中所制备的离子液体修饰的二硫化钨复合物极压抗磨剂合成的发动机油，其性能要远远优于现在市面上所销售的发动机油。
以上所述，仅是本发明的较佳实施例而已，并非是对本发明作其它形式的限制，任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例应用于其它领域，但是凡是未脱离本发明技术方案内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。

Claims (8)

1.一种含有离子液体修饰的二硫化钨复合物极压抗磨剂的发动机油，所述离子液体修饰的二硫化钨复合物极压抗磨剂的制备方法，其特征在于，具体包括以下步骤：
a、在超声振荡的条件下，将0.4克前驱体LixWS2与1000ml的蒸馏水反应；
b、调节pH值，使其生产PH为7的二硫化钨单分子层悬浮液；
c、向该悬浮液中加入50ml离子液体，并在一定温度下65-75℃恒温搅拌24h；
d、用转速为2000rpm的离心机分离出固体产物；
e、用少量蒸馏水对产物进行多次洗涤，以确定除去LiOH和可溶性的物质；
f、最后用四氟硼酸钾水溶液洗涤数次进行粒子交换，干燥得样品，即得到离子液体修饰的二硫化钨复合物极压抗磨剂；含有所述离子液体修饰的二硫化钨复合物极压抗磨剂的发动机油，按照重量百分比具体包括：
基础油 70%～90%；
离子液体修饰的二硫化钨复合物极压抗磨剂 0.5～1.5%；
高温抗氧剂 0.1～0.5%；
清净剂 2～5.7%；
分散剂 3～5%；
黏度指数改进剂 5～10%；
降凝剂 0.1～0.3%；
消泡剂 0.0001～0.0002%。
2.根据权利要求1所述一种含有离子液体修饰的二硫化钨复合物极压抗磨剂的发动机油，其特征在于：所述基础油为50%～40%的聚内烯烃与50%～60%的 Ⅱ类基础油复合。
3.根据权利要求1所述一种含有离子液体修饰的二硫化钨复合物极压抗磨剂的发动机油，其特征在于：所述高温抗氧剂为硫磷双辛基碱性锌盐、二苯胺中 的一种。
4.根据权利要求1所述一种含有离子液体修饰的二硫化钨复合物极压抗磨剂的发动机油，其特征在于：所述清净剂为硫化烷基酚钙、烷基水杨酸镁、烷基 水杨酸钙中的一种。
5.根据权利要求1所述一种含有离子液体修饰的二硫化钨复合物极压抗磨剂的发动机油，其特征在于：所述分散剂为双烯基丁二酰亚胺、聚异丁烯基丁二 酰亚胺中的一种。
6.根据权利要求1所述一种含有离子液体修饰的二硫化钨复合物极压抗磨剂的发动机油，其特征在于：所述黏度指数改进剂为聚甲基丙烯酸酯、苯乙烯与 双烯共聚物、氢化苯乙烯异戊二烯共聚物中的一种。
7.根据权利要求1所述一种含有离子液体修饰的二硫化钨复合物极压抗磨剂的发动机油，其特征在于：所述降凝剂为聚丙烯酸甲酯、聚α烯烃和T803B降凝 剂中的一种。
8.根据权利要求1所述一种含有离子液体修饰的二硫化钨复合物极压抗磨剂的发动机油，其特征在于：所述消泡剂磷酸三丁酯、聚二甲基硅氧烷、聚氧乙 烯聚氧丙烯季戊四醇醚、聚氧乙烯聚氧丙醇胺醚中的一种。
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