用于乙腈精制的高效氧化剂的筛选

基于正交实验,筛选出用于乙腈精制的过氧化钠系列(过氧化钠、过氧化钠-高锰酸钾和过氧化钠-浓硫酸)高效氧化剂,解决了传统乙腈精制工艺中氧化剂的低效性及釜残渣难于去除等问题。采用紫外分光光度法及红外光谱对精制后的乙腈进行分析,并与传统的最优氧化剂浓硫酸、氢氧化钠-高锰酸钾精制后的乙腈进行对比。实验结果表明,经过氧化钠系列氧化剂精制所得的高纯乙腈较传统氧化剂精制所得的乙腈在相应波长范围内具有更低的紫外吸光度,且与市售色谱纯乙腈的红外谱图无明显差异,其中以过氧化钠-浓硫酸为氧化剂所得的精制乙腈在波长190～205nm内的紫外吸光度明显低于市售色谱纯乙腈。

Selection of High-Performance Oxidant Used in Acetonitrile Purification

In order to heighten the oxidant efficiency in acetonitrile purification and more easily remove the residue from the purification process,several high-performance sodium peroxide oxidant systems,namely sodium peroxide,sodium peroxide-potassium permanganate and sodium peroxide-concentrated sulfuric acid,were selected through orthogonal experimental design.Purified acetonitrile was analyzed by means of UV absorption spectrometry and IR.The high-performance sodium peroxide oxidant systems were compared with traditional oxidant systems,such as concentrated sulfuric acid and sodium hydroxide-potassium permanganate,to determine effect of the acetonitrile purification.Results showed that acetonitrile obtained by treatment with the sodium peroxide oxidant systems exhibited lower UV absorption than that with traditional oxidant system.Furthermore,IR results showed no evident difference between acetonitrile obtained by treatment with sodium peroxide oxidant systems and commercially chromatographically pure acetonitrile.UV absorption of acetonitrile obtained by treatment with sodium peroxide-concentrated sulfuric acid was significantly lower than that of the chromatographically pure acetonitrile in 190-205 nm wavelength.