CN106957705B - 一种二硫化钨修饰的石墨烯复合物极压抗磨剂的制备及含有该抗磨剂的润滑脂 - Google Patents

一种二硫化钨修饰的石墨烯复合物极压抗磨剂的制备及含有该抗磨剂的润滑脂 Download PDF

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CN106957705B
CN106957705B CN201710137738.6A CN201710137738A CN106957705B CN 106957705 B CN106957705 B CN 106957705B CN 201710137738 A CN201710137738 A CN 201710137738A CN 106957705 B CN106957705 B CN 106957705B
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extreme pressure
tungsten disulfide
lubricating grease
modified graphene
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徐金玲
袁俊洲
何茂伟
纪祥娟
乔良
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Shandong Source Root Petrochemical Co Ltd
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Abstract

本发明属于工程机械专用润滑脂领域，尤其涉及一种二硫化钨修饰的石墨烯复合物极压抗磨剂的制备及含有该抗磨剂的润滑脂。利用前驱体LixWS2与蒸馏水反应，调节PH再加入石墨烯，洗涤干燥后得到极压抗磨剂；润滑脂则是将该极压抗磨剂与十二羟基硬脂酸、葵二酸、氢氧化锂、增粘剂、抗氧化添加剂、金属钝化剂、多功能剂、基础油、稠化剂磺酸钙进行混合，使得本发明中合成的润滑脂具有较低的摩擦系数、良好的极压抗磨性能。

Description

一种二硫化钨修饰的石墨烯复合物极压抗磨剂的制备及含有 该抗磨剂的润滑脂
技术领域
本发明属于工程机械专用润滑脂领域，尤其涉及一种二硫化钨修饰的石墨烯复合物极压抗磨剂的制备及含有该抗磨剂的润滑脂。
背景技术
随工程机械在公路建设和养护中发挥的作用是人力无法替代的，如何提高机械效率，延长机械的经济寿命，是设备管理者和操作者的共同课题。然而工程机械的工作环境大多比较恶劣，使用频率较高，各零件间摩擦频繁、磨损严重。工程机械润滑脂无论在工作环境，还是工作负荷变化，都与一般设备润滑脂存在着较大的差异。目前市场上普遍采用的润滑脂很难满足工程机械在以上多方面的要求。为了适应工程机械发展的要求，必须研发性能更加优秀的工程机械润滑脂，应具有更好的润滑性、极压抗磨性。
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，制备了二硫化钨修饰的石墨烯复合物极压抗磨剂，并利用该极压抗磨剂制备成润滑脂，即一种二硫化钨修饰的石墨烯复合物极压抗磨剂的制备及含有该抗磨剂的润滑脂。
为了达到上述目的，本发明采用的技术方案为，本发明提供一种二硫化钨修饰的石墨烯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石墨烯，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、干燥得样品，即得到二硫化钨修饰的石墨烯复合物极压抗磨剂。
一种含有二硫化钨修饰的石墨烯复合物极压抗磨剂的润滑脂，其特征在于，按重量份数具体包括：
十二羟基硬脂酸 9-13.5份；
葵二酸 3-4.5份；
氢氧化锂 2.6-3.9份；
增粘剂 0.5-1份；
抗氧化添加剂 0.5-1份；
二硫化钨修饰的石墨烯复合物极压抗磨剂 1-3份；
金属钝化剂 1-3份；
多功能剂 0.1-0.3 份；
基础油 50-68份；
稠化剂磺酸钙 15-25份。
作为优选，所述增粘剂为聚异丁烯、乙烯丙烯共聚合物、聚甲基丙烯酸酯中的一种。
作为优选，所述抗氧化剂为二苯胺、吩噻嗪、2- 萘酚或萘胺类化合物、二烷基苯基胺中的一种。
作为优选，所述金属钝化剂为苯三唑衍生物、噻二唑衍生物中的一种。
作为优选，所述二烷基二硫代氨基甲酸锌和亚甲基- 双（二丁基二硫代氨基甲酸酯）的混合物，所述二烷基二硫代氨基甲酸锌与亚甲基- 双（二丁基二硫代氨基甲酸酯）的重量比例为1：3。
作为优选，所述基础油为100℃粘度为2-12厘斯的聚α- 烯烃油合成油。
与现有技术相比，本发明的优点和积极效果在于，
本发明合成了二硫化钨修饰的石墨烯复合物并将其应用于润滑脂中。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。因而本发明生产的工程机械专用润滑脂，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工程机械专用润滑脂的生产提供高品质的润滑脂。
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。
本发明提供一种二硫化钨修饰的石墨烯复合物极压抗磨剂的制备及含有该抗磨剂的润滑脂，即利用制备出的二硫化钨修饰的石墨烯复合物极压抗磨剂添加到润滑脂中，得到性能良好的润滑脂，发明人经过大量实验得出一种二硫化钨修饰的石墨烯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PH=7的二硫化钨单分子层悬浮液，之后向该悬浮液中加入50ml石墨烯，并在一定温度下65-75℃恒温搅拌24h。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。 干燥得样品，得到二硫化钨修饰的石墨烯复合物极压抗磨剂，再将其研细备用。
下面则具体说明利用上述二硫化钨修饰的石墨烯复合物极压抗磨剂制备润滑脂各成分配比。
实施例1（重量份数，按份计量，以下同）
按照上述组分混合均匀，即得到润滑脂A。
实施例2
Figure DEST_PATH_IMAGE004
按照上述组分混合均匀，即得到润滑脂B。
实施例3
Figure DEST_PATH_IMAGE006
按照上述组分混合均匀，即得到润滑脂C。
实施例4
Figure DEST_PATH_IMAGE008
按照上述组分混合均匀，即得到润滑脂D。
实施例5
按照上述组分混合均匀，即得到润滑脂E。
对上述实施例中润滑脂进行检测，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二硫化钨修饰的石墨烯复合物极压抗磨剂合成的润滑脂，其性能要远远优于现在市面上所销售的润滑脂。
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 (6)

1.一种含有二硫化钨修饰的石墨烯复合物极压抗磨剂的润滑脂，按重量份数具体包括：
十二羟基硬脂酸9-13.5份；
癸二酸3-4.5份；
氢氧化锂2.6-3.9份；
增粘剂0.5-1份；
抗氧化添加剂0.5-1份；
二硫化钨修饰的石墨烯复合物极压抗磨剂1-3份；
金属钝化剂1-3份；
多功能剂0.1-0.3份；
基础油50-68份；
稠化剂磺酸钙15-25份；
该二硫化钨修饰的石墨烯复合物极压抗磨剂的制备方法，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石墨烯，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、干燥得样品，即得到二硫化钨修饰的石墨烯复合物极压抗磨剂。
2.根据权利要求1所述的含有二硫化钨修饰的石墨烯复合物极压抗磨剂的润滑脂，其特征在于：所述增粘剂为聚异丁烯、乙烯丙烯共聚合物、聚甲基丙烯酸酯中的一种。
3.根据权利要求1所述的含有二硫化钨修饰的石墨烯复合物极压抗磨剂的润滑脂，其特征在于：所述抗氧化剂为二苯胺、吩噻嗪、2-萘酚或萘胺类化合物、二烷基苯基胺中的一种。
4.根据权利要求1所述的含有二硫化钨修饰的石墨烯复合物极压抗磨剂的润滑脂，其特征在于：所述金属钝化剂为苯三唑衍生物、噻二唑衍生物中的一种。
5.根据权利要求1所述的含有二硫化钨修饰的石墨烯复合物极压抗磨剂的润滑脂，其特征在于：所述多功能剂为二烷基二硫代氨基甲酸锌和亚甲基-双（二丁基二硫代氨基甲酸酯）的混合物，所述二烷基二硫代氨基甲酸锌与亚甲基-双（二丁基二硫代氨基甲酸酯）的重量比例为1：3。
6.根据权利要求1所述的含有二硫化钨修饰的石墨烯复合物极压抗磨剂的润滑脂，其特征在于：所述基础油为100℃粘度为2-12厘斯的聚α-烯烃油合成油。
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