Synthesis and Modification of Core-Shell Magnetic Microspheres and Their Adsorption of Salicylic Acid
With γ-Fe2O3 as raw material and tetraethyl orthosilicate(TEOS)as silicon source,γ-Fe2O3@SiO2 nanocomposites were prepared by sol-gel method,and then magnetic microspheres(γ-Fe2O3@SiO2-NH2-COOH)were prepared by covalent modification of 3-aminopropyltrimethoxysilane(APT-MS)and glutaric anhydride(GTA).The magnetic microspheres(γ-Fe2O3@SiO2-NH2-COOH),terephthalic acid(H2BDC)and ZrCl4 were used for the preparation of core-shell magnetic microspheres(γ-Fe2O3@SiO2-NH2-COOH/UiO-66).Furthermore,γ-Fe2O3@SiO2-NH2-COOH/UiO-66-NH2 core-shell magnetic mi-crospheres were prepared by 2-amino terephthalic acid(H2N-BDC)and ZrCl4,and γ-Fe2O3@SiO2-NH2-COOH/UiO-66-2,3-NH2 core-shell magnetic microspheres were modified by diethylenetriamine(2,3-NH2).And diethylenetriamine(2,3-NH2)could be replaced by triethylenetetramine(3,4-NH2),and γ-Fe2O3@SiO2-NH2-COOH/UiO-66-3,4-NH2 core-shell magnetic microspheres could be obtained.The structure information of core-shell magnetic microspheres was obtained by Infrared spectrum(IR)and X-ray diffraction(XRD),and the results showed that the product was successfully modified.The samples of magnetic solid phase extraction(MSPE)of salicylic acid(SA)were measured by fluorescence spectrophotom-eter.The different gradient pH and different eluents were set to observe the elution effect and influence of pH and eluant on modified magnetic microspheres.The results showed that the modified magnetic micro-spheres had good adsorption effect in alkaline(pH=8)environment.The elution effect of γ-Fe2O3@SiO2-NH2-COOH/UiO-66-2,3-NH2 particles in 0.1 mol/L NaOH eluent is the best,the elution effect of γ-Fe2O3@SiO2-NH2-COOH/UiO-66-3,4-NH2 magnetic microspheres in MeOH eluent is the best,the elu-tion effect of γ-Fe2O3@SiO2-NH2-COOH/UiO-66-NH2 magnetic microspheres in 1％SDS eluent is the best.However,the skeleton structure of γ-Fe2O3@SiO2-NH2-COOH/UiO-66-3,4-NH2 magnetic micro-spheres eluted by MeOH eluent collapsed.
γ-Fe2O3core-shell magnetic microspheresmagnetic solid phase extractionadsorption
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