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应用硅胶薄层层析分离和鉴定了羟肟类萃取剂中顺、反式异构体和杂质组分;通过铜络合物重结晶法分离纯化反式异构体;用硅胶柱层析法分离顺、反式异构体。所得羟肟类萃取剂2-羟基-5-仲辛基二苯甲酮肟(N-510)和2-羟基-4-仲辛氧基二苯甲酮肟(N-530)的顺式和反式异构体,薄层层析和元素分析鉴定证明为纯化合物。用非水电位滴定法测得羟肟含量在98.5％以上. 应用紫外光谱,红外光谱,核磁共振谱和表观分子量的测定等方法对羟肟的顺、反式异构体的分子结构和在有机溶剂中的状态进行了研究.羟肟的顺式异构体以酚羟基及肟基形成分子间氢键,且两种质子进行快速交换.反式异构体的酚羟基质子除与肟基氮原子形成分子内氢键外,还可通过肟羟基形成分子间氢键.在聚集态或浓溶液中形成多聚体.
Silicone thin layer chromatography was used to separate and identify the cis, trans isomers and impurities in the hydroxyoxime extractant. The trans isomer was isolated by recrystallization of copper complex and purified by silica gel column chromatography Separation of cis, trans isomers. The resulting cis-and (2-hydroxy-4-sec-octyloxybenzophenone oxime (N-530) Trans-isomers, thin-layer chromatography and elemental analysis proved to be pure compounds. The content of hydroxyoxime was above 98.5% by non-aqueous potentiometric titration.The molecular structures of cis and trans isomers of hydroxyoxime were studied by UV, IR, NMR and apparent molecular weight methods Organic solvent. The cis isomers of hydroxyoxime form intermolecular hydrogen bonds with phenolic hydroxyl groups and oxime groups, and the two protons undergo rapid exchange.The phenolic hydroxyl proton of the trans isomer except the hydroxyl group Nitrogen atoms form intramolecular hydrogen bonds, but also form intermolecular hydrogen bonds through the oxime hydroxyl groups, forming multimers in aggregated or concentrated solutions.