Key Techniques On Synthesis Of Cyclohexene Oxide With Hydrogen Peroxide As Oxidant

This dissertation was financial supported by the Natural Science Funds of Henan Province (511020800).Cyclohexene oxide (CHO) is an important fine organic intermediate materal. Its application is wide range, for example, agricultural, medication, coating, resin and other fields. And CHO can also be used to produce other chemicals, such as cyclohexenediol, adipic acid and so on.In this work, We used hydrogen peroxide (HP) and cyclohexene (CH) which were rich in Henan Province as the main raw materials to carry out the key techniques on synthesis of CHO with HP as oxidant. The main works and results as follows:A new kind of production scheme of reaction controlled phase transfer catalyst has been developed. The yield of catalyst (based on the amount of quaternary ammonium salt) was 94%. The production process of this catalyst is convenient, and materials and energy exhaustion is lower than the process of Xi Zuwei. The catalyst was characterized by FT-IR and elementary analysis. The catalyst has high activity, selectivity and the characteristic of reaction controlled phase transfer catalyst.We study the technology of synthesis of CHO by fine cyclohexene (w(C₆H₁₀)≈94%) and reagent HP (w(H₂O₂)≈30%)with the reaction-controlled phase transfer catalyst. The effects of many factors, such as reaction time, reaction temperature, amount of catalysts, the volum of solvent chloroforme, mole ratio of CH to HP on epoxidation process were studied preliminary. Using orthogonal experiment technology twice, and the proper technological conditionis detailed as follows: based on 0.016 mol of H₂O₂, n(C₆H₁₀): n(H₂O₂) = 1.75 : 1, reaction temperature 40℃, reaction time 180 min, the amount of catalyst 0.2 g, the volum of solvent chloroform 24 mL. Under the condition, the conversion of HP is nearly 100%, selectivity of CHO is 93.40%, the recovery efficiency of fresh catalyst is about 60%; FT-IR spectra proved that the structure of the used catalyst has been changed.The technology research of CHO production has been carried out with raw CH (w(C₆H₁₀) ≈77%) and industry HP (w(H₂O₂)≈30%). The main factors influencing the epoxidation were also studied, such as amount of catalysts, reaction temperature, reaction time, mole ratio of CH to HP, the volum of solvent 1,2-dichloroethane and so on. The proper synthesis condition has been obtained with the methods of single factor and orthogonal experiment. The...