仿生催化环己烷空气氧化联产环己醇、环己酮和己二酸工艺的产物分离与分析

Separation and Analysis of Mixtures from Biomimetic Catalytic Oxidation of Cyclohexane with Air

针对仿生催化环己烷空气氧化联产环己醇(ROH)、环己酮(RO)和己二酸(AA)工艺的复杂混合物体系,建立了产物分离和分析方法。通过过滤和分液过程将反应产物体系分成油相、水相和固相混合物,然后分别建立定量分析方法。油相采用GC分析环己醇和环己酮含量;水相联合采用GC分析环己醇、环己酮和己二酸环己酯(CHA),HPLC分析丁二酸(SA)、戊二酸(GA)、己二酸、戊酸(VA)和6-醛基己酸(OCA)含量,水相总有机碳含量由总有机碳分析仪(TOC)测定;固体采用HPLC分析丁二酸、戊二酸、己二酸和6-醛基己酸含量,固相总有机碳含量由元素分析仪测定。该方法可准确给出环己烷的转化率以及环己醇、环己酮和己二酸的选择性。对混合样品的判别分析表明,产物的回收率为99.83%～100.30%,相对标准偏差(RSD)为0.115%～0.631%。

The oxydates of the catalytic oxidation of cyclohexane by air under certain conditions were analyzed by three methods,including GC, HPLC and element analysis. Cyclohexane oxydates could be separated into organic liquid phase, aqueous phase and solid phase. GC was used for the analysis of cyclohexanol and cyclohexanone in the oorganic phase,and cyclohexanol, cyclohexanone and cyclohexyl adipate in the aqueous phase. HPLC was applied for the determination of succinic acid （SA）, glutaric acid （GA）, adipic acid （AA）, valeric acid and 6-oxohexanoic acid（OCA） in the aqueous phase. The total organic carbon （TOC） was quantified by using element analysis. SA, GA, AA and OCA in the solid phase were analysized with HPLC. The recovery of products was 99.83%-100.30% with the RSD of 0.115%-0.631%.