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出 处:《分析化学》2005年第5期643-646,共4页Chinese Journal of Analytical Chemistry
基 金:天津石化公司基金资助项目(No.2002205)
摘 要:通过对常压硅胶柱色谱分离条件的研究,实现了对工业合成烷基磷酸酯盐的分离。对两种分离产物进行IR、1HNMR、31PNMR和原子发射光谱分析,确定出其结构,验证了用常压硅胶柱色谱分离烷基磷酸单酯和双酯盐的可行性,并对硅胶柱色谱分离烷基磷酸酯盐进行了初步探讨。Under optimum separation conditions, the monoalkyl and dialkyl phosphate salts, in the alkyl phosphate salts of industrial products were separated by silica get column chromatography successfully. In this study, the strong acid type styrene cation exchange resin was used to separate inorganic salts from the industrial products. After pretreatment, the sample of 500 mg changed into a kind of milky white solid, and then it was dissolved with a little hot chloroform, and added to the silica gel column which activated at 110 degrees C for 2.0 h and in the chromatographic column was about 40 cm high while the solution was still hot. Finally, the mixtures of chloroform and methanol with: different propotions of 9:1, 8:1, 7:1, 6:1, 5:1 and 3:1. were used to elute the silica gel column in turn. Two kinds of components, were collected and. purified once aganin by silica gel column chromatography. In order to evaluate, the separation effect of silica. gel column. chromatography, the two kinds of alkyl phosphate salts. separated were analyzed by Fourier transform infrared (FTIR), H-1-nuclear magnetic resonance (NMR), P-31-NMR and atomic emission spectrometry, and their structures were determined. The separation process, of the alkyl phosphate salts by silica gel column chromatography was discussed preliminarily.
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