▎ 摘 要
NOVELTY - Preparation of selective separation palladium ion adsorption material involves dispersing graphene oxide in N,N-dimethylformamide and ultrasonically processing to obtain mixture (m1), heating, suction filtering and drying, dispersing obtained graphene oxide-loaded silica gel composite in toluene to obtain a mixture (m2), adding N-aminoethyl- gamma -aminopropyltriethoxysilane to mixture (m2), heating, suction filtering and drying, dispersing obtained silica gel/graphene oxide composite material in an acetic acid solution to obtain a mixture (m3), stirring, suction filtering and drying to obtain silica graphene material, adding silica graphene material in a palladium-containing solution to obtain a mixture (m4), suction filtering, drying to obtain a material having adsorbed palladium ions, dispersing the material in acetonitrile solvent to obtain a mixture (m5), reacting, suction filtering, washing, drying and eluting all the palladium ions adsorbed in the material. USE - Preparation of adsorption material (claimed) used for selectively separating palladium ion. ADVANTAGE - The method enables preparation of adsorption material with improved significant recognition characteristics and affinity for palladium ions. DETAILED DESCRIPTION - Preparation of selective separation palladium ion adsorption material involves (i) dispersing activated silica gel in toluene, adding gamma -aminopropyltriethoxysilane and aniline while stirring, maintaining the temperature to 100-120 degrees C, refluxing the obtained reaction mixture for 3-24 hours and suction filtering to obtain a silica gel composite material comprising an amino group, (ii) dispersing graphene oxide in N,N-dimethylformamide and ultrasonically processing for 30 minutes to obtain mixture (m1), adding silica gel composite material to the mixture (m1) and adding N,N-dicyclohexylcarbodiimide as a catalyst, heating the obtained mixture to 40-80 degrees C for 20-35 hours, suction filtering to obtain a solid and drying the solid under vacuum at 30-60 degrees C for 8-12 hours to obtain a graphene oxide-loaded silica gel composite, (iii) dispersing graphene oxide-loaded silica gel composite in toluene to obtain a mixture (m2), adding N-aminoethyl- gamma -aminopropyltriethoxysilane and gamma -mercaptopropyltrimethoxysilane to mixture (m2), heating to 80-120 degrees C and refluxing for 15-17 hours, suction filtering to obtain a solid and drying the obtained solid at 110 degrees C for 12 hours to obtain a silica gel/graphene oxide composite material comprising both amino and mercapto groups, (iv) dispersing silica gel/graphene oxide composite material in an acetic acid solution to obtain a mixture (m3), further adding maleic anhydride to mixture (m3), and stirring the obtained reaction mixture at room temperature for 8-24 hours, suction filtering to obtain a solid, washing the obtained mixture with a washing solution several times and drying at a temperature of 60-90 degrees C for 8-12 hours to obtain silica graphene material comprising both a double bond and a mercapto group, (v) adding silica graphene material in a palladium-containing solution to obtain a mixture (m4), leaving still for adsorption saturation, suction filtering to obtain a solid, drying the obtained solid at a temperature of 80-110 degrees C for 8-12 hours to obtain a material having adsorbed palladium ions, and (vi) dispersing the material having adsorbed palladium ions in acetonitrile solvent to obtain a mixture (m5), adding azobisisobutyronitrile and ethylene glycol dimethacrylate to mixture (m5) in sequence, reacting under nitrogen atmosphere, stirring the reaction mixture at 60 degrees C for 10-24 hours, suction filtering to obtain a solid, washing the obtained solid with a washing solution several times, and drying in a vacuum drying box at 40-60 degrees C for 8-12 hours and using an eluent to elute all the palladium ions adsorbed in the material to obtain a printed polymer material with selective adsorption of palladium ions. The eluent comprises one or more of hydrochloric acid, sulfuric acid, nitric acid and thiourea. The concentration of hydrochloric acid, sulfuric acid, nitric acid is 0.05-2 mol/L. The usage amount of thiourea is 25-50 %mass.