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Study On Green Catalytic Oxidation Of 1,2-benzen Dimethanol

Posted on:2018-07-04Degree:MasterType:Thesis
Country:ChinaCandidate:L ZhangFull Text:PDF
GTID:2321330515488765Subject:Chemical engineering
Abstract/Summary:PDF Full Text Request
O-phthalaldehyde(OPA)is a new type of medical disinfectant developed in recent years.Compared with traditional glutaraldehyde disinfectant,it has the advantages of short service time and excellent sterilization performance,and can be widely used in the disinfection of medicine and medical instruments.The traditional synthesis process of OPA has some disadvantages,such as higher cost,difficult recovery of catalyst and environmental pollution,however.In this paper,the supported catalyst was prepared for the synthesis of OPA,using 1,2-benzenedimethanol as raw material and hydrogen peroxide as oxidant.Firstly,the catalyst carrier and active component were screened.The catalysts were prepared by impregnation method,and the effects of different impregnation methods on the structure and catalytic activity of the catalysts were investigated.The single factor experiments were designed to screen the conditions for the preparation of the catalyst.The effects of loading,impregnation time and calcination temperature on the catalytic performance were investigated.Orthogonal experiment was designed to determine the optimized preparation process.Then OPA was prepared using hydrogen peroxide as oxidizing agent in catalytic oxidation of 1,2-benzenedimethanol.The effects of hydrogen peroxide weight,reaction time and reaction temperature on the yield of OPA were investigated,and the experimental parameters of single factor were obtained.On the basis of single factor experiments,the response surface methodology was used to optimize the process parameters,and the optimum synthetic process conditions of catalytic oxidation were determined.Finally,the strengthening effect of ultrasound on the reaction was also investigated.The main conclusions are as follows:(1)The optimum preparation condition of catalyst: A two-step impregnation process was adopted to impregnate cobalt and then to impregnate molybdenumthe;the mass fraction of cobalt and molybdenum was 5% and 13% respectively,the immersion time was 12 h,then the catalyst was calcined at 500 ? for 3 h.The catalyst prepared under this condition can greatly increase the yield of OPA.It has good catalytic activity for the synthesis of OPA by oxidation of 1,2-benzenedimethanol with hydrogen peroxide.(2)Optimum synthesis process of OPA: the reaction time was 3 h,the reaction temperature was 81?,the mass of 1,2-benzenedimethanol and hydrogen peroxide were 5 g and 15 g,respectively,and the catalyst was Co/Mo/?-Al2O3.Under these conditions,the yield of OPA was 51.4%.Finally,The effect of ultrasonic treatment on the synthesis process of OPA was investigated.The catalytic synthesis reaction was enhanced by ultrasonic,the yield of the OPA was up to 55.6%,and the yield was increased by 4.2%.Using hydrogen peroxide as the oxidant,the synthesis process has the advantages of environmental friendly,pollution-free,easy recovery of catalyst.It is the optimum synthesis process of OPA.(3)The structure and properties of the catalysts were characterized by different characterization methods,such as TG-DTA,XRD,BET,SEM,XPS,NH3-TPD et al.It is proved that the catalyst has the characteristics of high dispersion and stable structure.The catalyst has good catalytic activity for the synthesis process.(4)The structure and yield of OPA were characterized by IR,1H NMR and gas chromatography respectively.The results show that the synthesized product has an expected structure with a yield of 55.6%.
Keywords/Search Tags:disinfectant, o-phaladehyde, catalyst, hydrogen peroxide, oxidation
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