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Study on green catalytic oxidation of o-phthalaldehyde

Release time:

2022-08-15

o-phthalaldehyde ( OPA ) is a new medical disinfectant developed in recent years. Compared with the traditional glutaraldehyde disinfectant, It has the characteristics of short time and excellent sterilization performance, and is widely used in the disinfection of medicine and medical equipment. o-phthalaldehyde The traditional synthesis process has the disadvantages of high cost, difficult catalyst recovery and large environmental pollution. In this paper, phthalic two methyl Alcohol as raw material, hydrogen peroxide as oxidant, in the preparation of the supported catalyst under the action of the synthesis of o-phthalaldehyde. Art was explored. First of all, the catalyst carrier and active components were screened to prepare the catalyst by impregnation method, to explore The effects of different impregnation methods on the structure and performance of the catalyst were investigated. Design of single-factor experiments, the preparation conditions of the catalyst were carried out. Preliminary screening, using orthogonal design experiments on the basis of single-factor experiments, the load, impregnation time, roasting temperature were investigated. The effect of the degree on the performance of the catalyst is determined to optimize the catalyst preparation process. Catalytic action in the preparation of supported catalysts catalytic oxidation of hydrogen peroxide synthesis process of o-phthalaldehyde were studied, the hydrogen peroxide dosage, reaction time, The effect of reaction temperature on the synthesis yield of o-phthalaldehyde was obtained, and the single-factor experimental parameters were obtained, The process parameters were optimized by the response surface method to determine the optimal synthesis process conditions for catalytic oxidation; intensifying effect on the reaction. The following conclusions are obtained:

（ 1 ) The best preparation conditions of the catalyst: the use of step-by-step impregnation process, the first impregnation of cobalt, after the impregnation of molybdenum, cobalt, molybdenum. The mass fraction content is respectively 5% , 13% Impregnation time is 12 h , 500 roasting at ℃ 3 h . prepared under this condition The catalyst can greatly improve the yield of o-phthalaldehyde, and the pollution is small, easy to recover, the hydrogen peroxide oxidation of two benzene methanol The synthesis of o-phthalaldehyde has good catalytic activity.

（ 2 ) The optimal synthesis process parameters for the synthesis of o-phthalaldehyde by hydrogen peroxide catalytic oxidation: the reaction time is 3 h , reaction The temperature is 81 ℃ 2. Hydrogen peroxide dosage 15 g Selection of catalyst 0.3 g Co/Mo/γ-Al 2 O 3 . The ortho-benzene diphenyl obtained under these conditions Formaldehyde yield is 51.4% . The strengthening effect of ultrasonic on the synthesis process of o-phthalaldehyde The yield can reach 55.6% The yield is improved. 4.2% It shows that the ultrasonic field has a promoting effect on the synthesis of o-phthalaldehyde. The The synthesis process has the advantages of green environmental protection, no pollution, easy recovery of catalyst and small pollution, and is the preferred combination of o-phthalaldehyde. into the process.

（ 3 ) using different characterization means such TG-DTA , XRD , BET , SEM , XPS , NH 3 -TPD Wait, yes. The structure and properties of the catalyst are characterized, which proves that the catalyst has the properties of high dispersion and stable structure. into process needs.

（ 4 ) The structure and yield of o-phthalaldehyde were analyzed by infrared spectroscopy, nuclear magnetic hydrogen spectroscopy and gas chromatography. The results show that the synthesis product has the expected structure and the yield can reach. 55.6%.