Preparation Of Triphenylphosphine Complex Catalyst And Research Its Catalytic In Aldol Condensation Reaction

In order to solve triphenylphosphine (TPP) catalyst in organic synthesishindering product separation, and difficultly recycling, the immobilization of TPP wasstudied in this paper, Triphenylphosphine complex catalyst was prepared byimpregnation method, Coprecipitation method and sol-gel method, and the synthesisconditions of catalyst were optimized. its catalytic activity for synthesis of chalconealso has been investigated.First, the triphenylphosphine were purified by recrystallization, and the purityand stability of triphenylphosphine were detected. the results of ultravioletspectrophotometry (UV) and thermogravimetric analysis (TGA) showed that insynthesis conditions of chalcone, the chemical and thermal stability of TPP weresufficient, and structure of TPP had not changed.TPP/AC catalyst was prepared by using AC pretreated in10%NaOH solution for2hr, to been impregnated in TPP alcohol-water solution for1.5hr, at30℃;TPP/γ-A12O3catalyst was prepared by using the ultrasonic cleaning instrument whichits ultrasonic irradiation frequency is28kHz and the power is200W, to beenimpregnated in TPP alcohol-water solution for2h. Scanning electron microscopy(SEM) results revealed that the multilayer and porous structure of AC and Al2O3wereconvenient for supporting TPP and distributing evenly active centers.The TPP/Al(OH)3catalyst was prepared by using the coagulation effect ofAl(OH)3colloidal solution, SEM results revealed that Al(OH)3absorbed the TPP toform the TPP/Al(OH)3catalyst.The supported catalyst of TPP was prepared by using the Aluminumisopropoxide as Sol and the HNO3as Solvent adhesive, when the temperature is80℃,the pH is2.4and the molar ratio of water and aluminium isopropoxide is100:1, thesurface morphology of gel is best.Infrared spectroscopy (IR) and nuclear magnetic resonance hydrogenspectroscopy (1HNMR) analysis showed that, TPP/Al(OH)3catalyst enhanced theactivity and selectivities of condensation reaction of chalcone with benzaldehyde andacetophenone, and gas chromatography (GC) analysis confirmed that the purity of theproduct was99.3%, the yield reached83%.