The Establishment And Application Of Cyclohexane Biomimetic Catalytic Oxidation Products Complete Analysis Method

Air oxidation of cyclohexane as an important industrial chemical reactions, the products of KA oil and adipic acid are important organic chemical raw materials. Currently the air oxidation of cyclohexane have catalyzed oxidation of cobalt salt, no catalyzed oxidation and biomimetic catalytic oxidation, the main products of the three method are the same in basic, but the proportion of main products and by-products are quite different.In this paper, the products were qualitatively analyzed by using GC-MS, HPLC and GC. We also established a new set analysis method of full products. Using this analysis method, We researched the trends of products in the intermittent air oxidation of cyclohexane biomimetic catalytic reaction system. And the ratio of organic carbon in the water phase and solid material was quantitative analyzed . The main works of this thesis are presented as follows:1. Cyclohexyl formate and dicyclohexyl adipate were synthesized and also characterized by GC-MS.2. The products were qualitatively analyzed by using GC-MS and comparing the retention time of the standard samples with the products. And cyclohexyl hydroperoxide,ε-caprolactone, cyclohexyl formate were qualitatively analyzed at first.3. Established cyclohexane biomimetic catalytic oxidation products complete analysis method: The GC internal standard quantitative analysis method of cyclohexyl hydroperoxide was established, which was more simple and accurate comparing with chemic titration method; The quantitative analysis conditions of cyclohexanol and cyclohexanone was optimized and added excessive PPh3 before the injection, which can get rid of cyclohexyl decomposition of hydrogen peroxide and cyclohexanol, cyclohexanone,ε-caprolactone can be quantified accurately; We also established the quantitative analysis method of cyclohexyl formate, cyclohexyl pentanoate, 6-(cyclohexyloxy)-6-oxohexanoic acid and dicyclohexyl adipate. The HPLC analysis condition was optimized, and monacids , dicarboxylic acids, etal can be quantified. We also established organic carbon analysis methoda by TOC and elemental analysis and analyzed the water content in the samples by automatic moisture teller.4. Using this analysis method, we researched the trends of products in the intermittent air oxidation of cyclohexane biomimetic catalytic reaction system and improved the experimental apparatus. The ratio of organic carbon in the water phase and solid material was also quantitative analyzed .