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以羟甲基-12-冠-4和1,6-二溴己烷、1,10-二溴癸烷为原料,在KH催化下,分别合成一溴己氧基12-冠-4和一溴癸氧基12-冠-4;将一溴癸氧基12-冠-4与硫脲加到无水乙醇中,反应过夜合成至今还未见报道的巯基癸氧基12-冠-4,并对其进行表征确认。在不同的pH条件下,分别比较了3种化合物对Li+和Na+的选择配合情况。结果表明,一溴己氧基12-冠-4和一溴癸氧基12-冠-4对Li的配合比都是1∶1,在氯仿中的萃取率不随冠醚环上支链的长短变化而变化,但随pH的增大而增大,达峰值97.69%后趋于稳定;巯基癸氧基12-冠-4由于巯基水解的效应对Li配合物的萃取能力稍差,且随pH的增大而减小,在75.76%后趋于稳定。同时它们对钠的萃取能力则较差。由此可见,12-冠-4对Li具有很好的选择配合能力,该研究为冠醚更广应用提供了一定的基础。
With hydroxymethyl-12-crown-4 and 1,6-dibromohexane, 1,10-dibromodecane as raw materials, under KH catalysis, monobutyroxy 12-crown-4 and Bromodecyloxy 12-crown-4; adding bromo-decyloxy-12-crown-4 and thiourea into anhydrous ethanol and reacting overnight to synthesize mercaptodecyloxy 12-crown-4, And its characterization confirmation. Under different pH conditions, the three compounds were compared for Li + and Na + selection and cooperation. The results showed that the molar ratio of mono-bromo-hexoxy-12-crown-4 and mono-bromo-decyloxy-12-crown-4 to Li was 1: 1 and the extraction rate in chloroform did not vary with the length of branches But increased with the increase of pH, reaching a peak value of 97.69% and then stabilized. The mercapto-decyloxy-12-crown-4 had slightly poorer ability to extract Li complex due to the effect of sulfhydryl hydrolysis, Of the increase and decrease, after 75.76% tends to be stable. At the same time, their ability to extract sodium is poor. Thus, 12-crown-4 has a good choice of Li with the ability to adapt to the wider use of crown ether to provide a certain basis.