化学氧化法精制11-氰基十一酸

Study on chemical oxidation method for refining 11-cyanoundecanoic acid

以11-氰基十一酸(11-CUA)的纯度和收率为目标函数,采用三种不同的氧化剂精制粗品11-氰基十一酸,通过对比实验及对氧化产物的红外光谱解析与熔点测定,确定了双氧水是合适的氧化剂.再利用正交试验对双氧水精制11-氰基十一酸的工艺条件进行研究,得到优化实验条件:在双氧水质量分数为15%、温度为20℃、pH值为2.0、反应时间30min的条件下精制粗品11-CUA,产品纯度达99.86%,收率93.62%.

The purity and recovery of ll-cyanoundercanoic acid（11-CUA, as intermediate of nylon-12） were taken as target functions to investigate the crude ll-CUA （from the 1, l＇-peroxydicyclohexylamine pyrolysis） refining by three self-chosing oxidants. On the basis of comparing the experiment efffects of refining crude 11-CUA by these different oxidants, analyzing IR spectra and measuring melting points of the refined compounds, Hydrogen peroxide was thereby selected as reasonable oxidant. Then technological parameters of this process were optimized by orthogonal test. The optimized process parameters are： pH value and temperature when oxidating crude 11-CUA are 2.0 and 20℃Crespectively, mass percent of hydrogen peroxide in its aqueous is 15%, time of oxygenating crude ll-CUA is 30 minutes. Using above-mentioned optimized process parameters to refine crude l l-CUA, product purity and recovery rate can reach 99.86% and 93.62%, respectively.