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润滑油硫化烷基酚钙清净分散剂组成研究

Structure and Composition Analysis of Sulfurized Calcium Alkyl Phenolate

【作者】 黄莉云

【导师】 李少萍;

【作者基本信息】 华东理工大学 , 油气储运工程, 2011, 硕士

【摘要】 清净剂在润滑油添加剂中所占比例将近一半,应用极为广泛。其组成对润滑油性能有很大的影响,不同厂家甚至不同批次的产品在分水和抗水洗性能上都会存在差异,因而对此类添加剂的结构和组成进行研究是十分必要的,这对其生产、合成和使用有着指导作用。本文以国外清净剂S206Ⅰ及国内生产的两个批次润滑油清净剂(S206Ⅱ和S206Ⅲ)为样本,着重剖析了这几个典型硫化烷基酚钙的组成、结构,并研究了不同组分对分水性和抗水洗性能的影响。本文采用动态薄膜渗析法,提取了有效成分。利用色谱、核磁共振质谱等手段比较了三者在结构组成上的差别,并考察了分水性能影响因素。研究表明国外型号S206Ⅰ的产品无论是从有效含量和分子量上看,都比国内两个产品高,并且具有分散度较小的优点。从组成上研究,国外样品S206Ⅰ在产品合成中残余的游离烷基酚含量最小,性能最差的样品S206Ⅱ则游离烷基酚残余含量最高;国内产品中含有脂肪酸等物质,特别是其中性能较次的样品S206Ⅲ中,还含有胺类物质等杂质。从结构上研究,国内外钙盐样品都为对位取代,但国外样品烷基链的支化度较大,而国内S206Ⅲ支化度最小。研究还发现,样品合成中作为助剂而少量残余的脂肪酸,会使分水性能变差,乳化层增加;样品中存在少量脂肪胺,虽可提高碱值,但会造成添加剂有效组成(碱性部分)在水中稳定性变差。两者对润滑油分水和抗水洗性能都不利。

【Abstract】 High-alkaline detergent is applied widely in lubricant additives. It is quiet different in water separation and washing resistance among productions from different companies or batches even in the same company, which has a great impact on lubricant performance.For guiding the production, synthesis and use of the product, this paper analyses the differences in compositions and structures of three typical sulfurized calcium alkyl phenolates which are used as detergents in lubricate base oil. In addition, the effect factors of water separation and washing resistance from different compositions is also studied. The effective components are extracted by rubber membrane dialysis. The differences in the structures and compositions of three detergents have been compared on the basis of elemental analyses, infrared spectroscopy (IR), and nuclear magnetic resonance (NMR), etc.The results show that the detergent with excellent performance, S206Ⅰhas the greatest advantage of effective content among these three detergents. Besides, its average molecular weight is the largest and its dispersion degree is the smallest. From the composition, S206Ⅰcontains the least free alkylphenol remained in the synthesis, S206Ⅱa little more, S206Ⅲthe most. In addition, several compositions such as stearic acid can be found in S206. And S206Ⅱ, performance inferior sample in S206, contains most impurities such as amine compounds. From the structure, all the samples are para-sulfurized alkyl phenolate. But the long alkyl branching degree in S206Ⅰis the greatest, then S206Ⅱ, the smallest is in S206Ⅲ. The study also finds that stearic acid remained in samples can lead to poor water-dividing performance and increasing the emulsification layer. Meanwhile, amine compound will decrease additive’s stability in water although it can enhance additive’s total based number.

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