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Prepa Ration And Studying On A Dual-core (Ⅱ) Catalyzer

Posted on:2011-07-15Degree:MasterType:Thesis
Country:ChinaCandidate:C H ZhouFull Text:PDF
GTID:2121330332958895Subject:Chemical processes
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In the work, the cyclohexene was used as a crude material, and the cheap and facile molecular oxygen was used as an oxidant. The process of synthesizing cyclohexenone by a catalyst under the atmospheric pressure was studied,which included two important sections:Synthesizing,and Characterization of a new catalyst and the optimization ofthe synthetic process.In the "one-pot" approach, an N-N bridge group was used to generate a macrocyclic metal complexes, ([Cu(II)aneN5]2(DDS))(ClO4)4, containing two Cu in the core. The IR and elemental analysis were used to characterize the structuration of the complex. The results showed that the complex had two Cu metal ions in the center connected to the 4-Coordinated ligand.We also synthesized a mononuclear complex, Cu(Pn)2(ClO4)2,and an inorganic salts, Cu(C104)2·6H20.Under the atmospheric pressure, these complexes were used as a homogeneous catalyst respectively to catalytically oxidize the cyclohexene to the cyclohexenone, compared with the blank experiment. Comparisons demonstrated that the dual-core metal complexes as a homogeneous catalyst in the oxidation system, showed a higher conversion rate and selectivity than the other situations.Under atmospheric pressure of molecular oxygen, process of cyclohexene oxidation reaction by O2 using{[Cu(Ⅱ)aneN5]2(DDS)}(C104)4 as a catalyst to synthesize 2-cyclohexene-l-one was investigated.Effects of many factors on the oxidation reaction were discussed.And the optimum reaction conditions had been obtained:the amount of catalyst was 2mg, reaction time was about 12h, reaction temperature was about 338k, and volume of solvent was about 12mL,basing the conditions:volume of O2 was about 5mL/min, volume of substrate was 4mL. On the optimum reaction conditions, the conversion of cyclohexene was about 65.9%, and the selectivity to 2-cyclohexene-l-one was about 78.3%.Several repeated experiments had been carried,which demonstrated a more stable catalytic performance using the dual-core metal complex as a catalyst. For the product analysis of the oxidation of cyclohexene by molecular oxygen, the gas chromatography method was established.And the accuracy of the method was verifired,which showed that this method is accurate and effective enough to analyze the production.■...
Keywords/Search Tags:Copper(Ⅱ), Bis(macrocycle), Cyclohexene, 2-cyclohexene-1-one, Dioxygen, Catalytic oxidation
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