ISSN   1004-0595

CN  62-1224/O4

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复合锂基润滑脂的高纯净制备及其预制皂的结构探讨与复合过程研究

Preparation of High Purity of Complex Lithium and Discussion on the Structure of its Prefabricated Thickener and Recombination Process

  • 摘要: 复合过程的优良是决定复合锂基润滑脂性能高低的主要因素之一,因此一直以来是人们研究的难点和重点. 为研究复合锂基润滑脂的复合过程,区别于传统的油-皂混合体系,采用乙醇为反应介质基于两步法复合锂润滑脂制备过程间接地制备得到高纯净的12-羟基硬脂酸锂、癸二酸锂以及不同二元酸种类的复合锂预制稠化剂粉末. 通过红外光谱和扫描电子显微镜确定其结构和形貌,并利用X射线粉末衍射仪、在线红外光谱以及固/液核磁等手段辅以形貌演变过程揭示了复合锂基润滑脂复合过程的实质. 结果表明:间接法制备其复合过程涉及到2种酸和2种盐之间的相互转化和作用,获得的预制皂粉末具有良好的双螺旋纤维结构,以此为稠化剂制备的复合锂基润滑脂基本理化性能相比直接油-皂法制备的脂表现出较好的外观及胶体安定性. 该工作为后续深入探究复合锂基润滑脂复合过程以及研制高性能润滑脂提供了理论支撑和数据积累.

     

    Abstract: Complex lithium grease can be used under high temperature conditions that traditional lithium grease cannot be applied to, it has been widely used in countries around the world since its development in the 1960s. Although there are many kinds of complex lithium base greases, the most advanced one is the compound lithium grease prepared by fatty dibasic acid and 12-hydroxy-stearic acid or stearic acid. The drop point and various physicochemical indexes are mainly affected by the content of thickening agent, additives and compound agent. The excellent recombination process is one of the main factors to determine the performance of complex lithium grease, so it has always been the difficulty and focus of people's research. Domestic and foreign scholars have carried out a lot of research work on the essence and mechanism of compound lithium grease recombination process. Researchers believe that the key factor for the formation of high drop point of complex lithium grease lies in the formation of appropriate hydrogen bond or lithium bond association similar to hydrogen bond between the two thickeners, dicarboxylate and 12-hydroxy-stearate. However, most of the reported research work is based on the direct oil-soap preparation method and process of traditional composite lithium grease, which is usually affected by the large viscosity of the base oil used and the complex parameter variables of the preparation process, so it is difficult to explore the compounding process and mechanism. Therefore, in order to study the composite process of lithium complex grease, and different from the traditional oil-soap mixing system, ethanol was used as the reaction medium to prepare high-purity lithium 12-hydroxy-stearate, lithium sebacate and prefabricated lithium complex thickener powders of different dibasic acids indirectly by the two-step preparation process of lithium complex grease. The structure and morphology of the compound lithium grease were determined by infrared and scanning electron microscopy, and the substance of the compound process was revealed by means of X-ray powder diffractometer, in-line infrared and solid/liquid nuclear magnetic field. The results showed that the prepared soap powder had a good double helix fiber structure, and there was a process of strong acid replacement of weak acid in the compound process of lithium complex grease, which essentially involved the mutual conversion and chemical interaction between 12-hydroxy-stearic acid, 12-hydroxy-stearate lithium and sebacic acid, and lithium sebacate. By monitoring the change of microstructure during the preparation of prefabricated thickener, it was further verified that there was an interaction between strong acidic dibasic acid and formed 12-hydroxy-stearate lithium salt in the compound lithium base grease. The performance of indirect lithium compound grease was better in appearance and colloid stability than that of traditional lithium compound grease prepared by direct method, and other properties are comparable. This work provided theoretical support and data accumulation for further research on the compounding process of complex lithium grease and development of high-performance grease.

     

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