烷醇酰胺类表面活性剂的合成及其性能研究

发布时间：2018-04-17 22:29

本文选题：烷醇酰胺 + 伴生物　；参考：《山东大学》2015年硕士论文

【摘要】：油／水界面张力能否降至超低(≤10-3mN/m)是在三次采油提高原油采收率过程中筛选驱油剂配方的一个重要指标,设计超低界面张力体系并研究超低界面张力产生机理对指导驱油剂的设计具有重要意义。本文采用“一锅法”合成了非离子表面活性剂烷醇酰胺,研究了合成条件、无机盐浓度以及增溶油相对该类表面活性剂界面活性的影响,结合FT-IR光谱、界面扩张流变、分子模拟等手段研究了非离子表面活性剂烷醇酰胺的分子行为以及在不同条件下产生超低界面张力及具有油相适应性的机理。本论文取得的认识为建立表面活性剂的构效关系提供理论基础,并为设计三次采油中超低界面张力体系提供指导。本文主要分为以下三个部分：第一部分采用月桂酸甲酯和二乙醇酰胺为原料在碱性催化剂甲醇钠条件下利用“一锅法”合成了非离子表面活性剂月桂酸二乙醇酰胺,分别采用石油醚和水进行纯化,得到了高纯度的月桂酸二乙醇酰胺,借助核磁、红外等手段进行了表征。结果表明,由合成引入的月桂酸甲酯、二乙醇酰胺、胺单脂、胺双脂等伴生物分子与主剂月桂酸二乙醇酰胺协同吸附在油／水界面且分布在不同的位置,导致该体系具有高的界面活性和油相适应性。通过单一变量法研究了合成条件对月桂酸二乙醇酰胺体系界面性能的影响。第二部分实验结果表明,非离子表面活性剂烷醇酰胺在ca2+/Mg3+存在下,可以将十二烷／水的界面张力降低至10-3nN/m数量级,且在一定范围内随着盐度的增加界面张力逐渐减小,为我们提供一个很好的研究超低界面张力机理的模型。通过测定FT-IR光谱我们发现,Ca2+/Mg2+存在时,界面层内与烷醇酰胺亲水头基相互作用的水分子数目减小,相互作用减弱。红外光谱的分析数据表明Mg2+结合自由水的能力要强于Ca2+,在相同浓度条件下,Mg2+在界面层内结合水分子数目要远多于Ca2+。表面活性剂疏水性增强,界面张力降低。Mg2+存在条件下烷醇酰胺疏水性增强的幅度要大于ca2+,Mg2+降低油/水界面张力的能力要强于Ca2+。第三部分研究了烷醇酰胺及增溶癸烷的溶胀胶束体系与不同油相间的界面扩张流变性质。结果表明,当烷醇酰胺胶束增溶一定量癸烷分子后,与不同油相的界面扩张模量的变化趋势较单一烷醇酰胺时要小。通过计算界面生成能发现,当适量癸烷增溶于烷醇酰胺疏水尾链间时形成的界面层界面能低,因此当增溶了癸烷的溶胀胶束与油相接触时,烷醇酰胺和增溶的癸烷分子在油水界面由热力学驱动组装形成界面层,油相分子对界面层的组成和性质的影响程度降低,因此在采用不同油相时界面流变性的差异减小。因此只要确定表面活性剂与癸烷的最佳比例,取得最低的界面生成能,便可以通过预组装的溶胀胶束在油水界面吸附形成界面层,避免油相分子进入界面层,从而保障体系对不同油相的适应性。综上所述,本论文研究了月桂酸二乙醇酰胺合成过程中产生的副产物及伴生物分子对主剂界面活性的影响；仅通过改变盐度使得烷醇酰胺将十二烷／水界面张力降至超低,利用FT-IR (ATR)光谱研究了钙、镁变化对界面层内分子行为的影响；研究了增溶油相的烷醇酰胺溶胀胶束的界面扩张流变性质,探索了取得油相适应性的理论机制。本文取得的结果和认识可为揭示表面活性剂构效关系和揭示超低界面张力机理提供一定的理论依据。本论文的主要创新点：(1)本文深入探讨了表面活性剂合成过程中的副产物及伴生物对产物界面活性的影响,揭示了烷醇酰胺取得高界面活性的关键机制,为表面活性剂的合成与应用相结合提供了新的思路,避免了合成过程中资源的浪费以及相关性能的降低。(2)结合分子模拟理论研究方法和FT-IR (ATR)光谱等实验方法,研究了表面活性剂分子行为对界面性能的影响,为揭示超低界面张力机理提供了重要依据。(3)结合界面流变实验研究方法,将界面扩张模量与表面活性剂油相适应性相关联,揭示了取得油相适应性的关键理论机制,为设计具有油相适应性的驱油剂体系提供新的技术路线。
[Abstract]:The oil / water interfacial tension can be reduced to very low (less than 10-3mN/m) is to improve the oil recovery process in three oil recovery were an important indicator of oil displacement agent, the design of ultra low interfacial tension system and study of ultra low interfacial tension mechanism to guide the design of oil displacement agent has important significance. In this paper, non ion surfactant alkanolamide was synthesized by one pot method, studied the influence of synthesis conditions, inorganic salt concentration and the solubilization of oil relative to the surfactant interface activity, combined with FT-IR spectroscopy, interfacial dilational rheology, molecular simulation research the molecular behavior of nonionic surfactant alkanolamide and the mechanism of ultra low interfacial tension and oil adaptability under different conditions. To provide a theoretical basis for understanding the structure-activity relationship of surfactant, and for the design of the three oil recovery in low The interfacial tension of system to provide guidance. This paper is mainly divided into the following three parts: the first part of the lauric acid methyl ester and two ethanol amide synthesis of non-ionic surfactant lauric acid two ethanol amide was synthesized by one pot method in alkaline sodium methoxide catalyst under the condition of using petroleum ether and water purification, the laurel two ethanol acid amide, high purity by NMR, IR were characterized. The results show that by introducing the synthesis of methyl laurate, two ethanol amide, amine monoester, diester amine etc. with biological molecules and the main agent of lauric acid two ethanol amide CO adsorption in the oil / water interface and distribution in different the position, the system has led to high interfacial activity and oil adaptability. Through the single variable method is used to study the effects of synthesis conditions on lauric acid two ethanol amide system interface performance. In the second part, the experiment result The nonionic surfactant alkyl alcohol amide in the presence of ca2+/Mg3+ can be twelve alkane / water interfacial tension decreased to 10-3nN/ m magnitude, and in a certain range, with the increase of salinity decreases the interfacial tension, provides a good study of ultra low interfacial tension mechanism model through the determination for us. We found that the FT-IR spectra, the presence of Ca2+/Mg2+, the number of water molecules in the interface layer and alkylolamide hydrophilic headgroup interaction decreases, interaction is weakened. Analysis of data of infrared spectra showed that Mg2+ combined with free water is stronger than Ca2+, in the same concentration, the Mg2+ in the interface layer with the water molecule number far more than Ca2+. of surfactant hydrophobicity enhanced, interfacial tension decreased.Mg2+ amplitude alkylolamide hydrophobic enhanced conditions than ca2+, Mg2+ reduce the oil / water interfacial tension is stronger than Ca2+ third. Interfacial rheological properties and part of alkanolamide and solubilization of decane swelling micellar system with different oil. The results show that when a certain amount of micellar solubilization of alkanolamide decane molecules, small to change trend with different oil phase interfacial dilational modulus than single alkylolamide. Through the calculation of interface can be found when the interface layer interface, the amount of decane alkanolamide solubilized in the hydrophobic chain between the formation of energy is low, so when the oil swollen micelles and solubilization of decane contact, decane molecular alkanolamide and solubilization in the oil-water interface driven by thermodynamics assemble into interface layer, the influence degree of oil phase composition and molecular properties of the interface layer is reduced, so in different oil phase difference of the interfacial rheological property decreases. So long as to determine the optimal proportions of surfactants and decane, has the lowest interface can be. The adsorption interface layer formed by pre assembled micelles swelling at the oil-water interface, avoid oil molecules into the interface layer, so as to guarantee the system of different oil phase adaptability. In summary, this thesis the by-product of lauric acid two ethanol amide synthesis process and the influence of the main agent of biological molecules with interfacial activity; twelve alkane / water interfacial tension to ultra low only by changing the salinity makes alkanolamide, using FT-IR (ATR) spectroscopy to investigate the effect of magnesium on calcium, changes of molecular behavior in the interface layer; on the interfacial rheological properties of alkanolamide swelling micellar phase solubilization of oil exploration, the theoretical mechanism of oil adaptability the main results and understanding. To reveal the surfactant structure-activity relationship and reveal to provide a theoretical basis for ultra low interfacial tension mechanism. The main innovation of this thesis: (1) this paper To investigate the byproduct synthesis process of the surfactant and the influence on the product interface with biological activity, reveals the alkylolamide key mechanism of high interfacial activity, provides a new way for the synthesis and application of surfactant combination, to avoid and reduce the resource waste in the process of synthesis and related properties. (2) simulation theory research method and FT-IR (ATR) combined with molecular spectroscopy experiments, the effects of surfactant molecular behavior influence on interfacial properties, provides an important basis for revealing the mechanism of ultra low interfacial tension. (3) combined with the interfacial rheological experiment, the dilational modulus and surfactant in oil phase adaptability is associated, reveals the key mechanism of the theory of oil adaptability, provide a new technical route for the design with oil adaptability of oil displacement agent system.

【学位授予单位】：山东大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ423;TE357.46

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