无溶剂法AKD合成过程TEA-HCl晶体结构及形貌特征研究

卢素敏, 朱峰, 王玺督, 田一哲

现代化工 ›› 2018, Vol. 38 ›› Issue (12) : 175 -180.

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现代化工 ›› 2018, Vol. 38 ›› Issue (12) : 175-180. DOI: 10.16606/j.cnki.issn0253-4320.2018.12.039
科研与开发

无溶剂法AKD合成过程TEA-HCl晶体结构及形貌特征研究

    卢素敏, 朱峰, 王玺督, 田一哲
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Studies on crystal structure and morphology of TEA-HCl in solvent-free preparation of AKD

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摘要

以三乙胺和硬脂酰氯为原料,采用无溶剂法合成烷基烯酮二聚体,为了研究反应过程中高黏度产生的机理,利用单晶X射线衍射、SEM、FR-IR及HNMR对副产物三乙胺盐酸盐(TEA-HCl)的晶体结构和形貌特征进行了分析。结果表明,三乙胺盐酸盐晶体易于沿着c轴方向生长并枝状延伸,在(001)晶面方向叔胺阳离子链间相互作用力较弱。实验条件下,三乙胺盐酸盐晶粒基本呈球形、纳米级,当三乙胺盐酸盐浓度增加时,颗粒间相互碰撞极易形成交联结构。三乙胺盐酸盐的枝状形貌特征、与AKD分子间很强的作用力、巨大的颗粒比表面积是产生高黏度的主要原因。

Abstract

Alkyl ketene dimer is prepared by reacting triethylamine with stearyl chloride in the absence of organic solvents.To investigate the mechanism of the high viscosity generated in the reaction,the crystal structure and morphology of byproduct triethylamine hydrochloride (TEA-HCl) is analyzed by single crystal X-ray diffraction,SEM,FR-IR and HNMR.The structural analysis shows that TEA-HCl crystal prefers to grow along c axis and extends branching,and the interaction of tertiary ammonium cation chains is weak in the (001) crystal plane.Under the experimental conditions,TEA-HCl grains are basically in spherical shape and have nano-scale sizes.When the concentration of TEA-HCl increases,the grains collide each other and are easy to form cross-linking structure.The branching cross-linking structure of TEA-HCl,strong interaction force between TEA-HCl and AKD molecular,and large specific surface area of the grains are the main cause of the high viscosity.Any favorable changes on the crystal morphology and particle size will be effective measures to reduce the viscosity of the reaction mixture.

关键词

黏度 / 无溶剂法 / 长链烷基烯酮二聚体 / TEA-HCl形貌特征 / TEA-HCl晶体结构

Key words

viscosity / solvent-free / AKD / morphology of TEA-HCl / crystal structure of TEA-HCl

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无溶剂法AKD合成过程TEA-HCl晶体结构及形貌特征研究[J]. 现代化工, 2018, 38(12): 175-180 DOI:10.16606/j.cnki.issn0253-4320.2018.12.039

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