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Preparation Of Novel Porous ?-cyclodextrin Polymer Sorbents For Adsorption And Separation Of Organic Pollutants

Posted on:2019-05-02Degree:MasterType:Thesis
Country:ChinaCandidate:Y R LiFull Text:PDF
GTID:2371330566459701Subject:Organic Chemistry
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In this dissertation,two types of porous?-cyclodextrin polymer were prepared and subsequently characterized by several different approaches.Using three bisphenols as analytes,the solid-phase extraction ability of the first sorbent was investigated.Coupled with HPLC,the first sorbent was applied to the extraction and determination of these three analytes in environmental water samples and juice.In addition,using four different environmental pollutants as target compounds,the adsorption and removal ability of the second sorbent was studied.The main research contents are listed as follows:In the first part,a new microporous?-cyclodextrin polymer?MP-CDP?was prepared for the simultaneous solid-phase extraction?SPE?of bisphenol F?BPF?,bisphenol A?BPA?and bisphenol AF?BPAF?.The MP-CDP was characterized by Fourier transform infrared spectroscopy?FT-IR?,solid-phase 13C nuclear magnetic resonance(13C-NMR),thermo-gravimetric analysis?TGA?,scanning electron microscopy?SEM?,and nitrogen adsorption-desorption analysis.Results indicated that the MP-CDP had micron-level particle size,microporous structure,a high BET surface area,and a high product yield.Adsorption tests showed that the MP-CDP sorbent had high adsorption ability and fast binding kinetics for bisphenols.Moreover,the MP-CDP presented high extraction efficiencies,high enrichment factor,good reusability and good batch-to-batch reproducibility for SPE of bisphenols.Based on the MP-CDP sorbent,a SPE-HPLC-UV method was developed and successfully applied to simultaneously detect three bisphenols in water samples and orange juice with the recoveries of 95.7-106.3%?RSD=2.0-5.2%?for BPF,92.9-107.0%?RSD=1.5-5.1%?for BPA,and 96.0-103.5%?RSD=1.7-5.0%?for BPAF,respectively.The limit of detection?S/N=3?and the limit of quantification?S/N=10?for all bisphenols in these samples were 0.15 ng/mL and 0.5ng/mL,respectively.The new MP-CDP can be potentially utilized as a good sorbent for simultaneous SPE of trace bisphenols in environmental water samples and beverages.In the second part,a new microporous?-cyclodextrin-pillar[5]arene polymer?P-CD-P5A-P?sorbent was prepared,using?-cyclodextrin??-CD?and pillar[5]arene?P5A?as monomers and decafluorobiphenyl?DFB?as a cross-linking,for the simultaneous rapid removal of four different organic micropollutants,including bisphenol A?BPA,an environmental estrogen?,propranolol?a?-inhibitor?,1-naphthylamine?1-NA,a cancerogen?and methylence blue?MB,a organic dye?,from water.The P-CD-P5A-P was characterized by FT-IR,13C NMR,TGA,SEM,and nitrogen adsorption-desorption analysis.Results indicated that P-CD-P5A-P had a high BET surface area?463m2/g?and a porous structure with meso-and micro-pores.Adsorption tests showed that the P-CD-P5A-P had excellent adsorption ability including high adsorption capacity,rapid binding kinetics?with an equilibrium time of less than 30 s?and good reusability for four organic pollutants.The new sorbent can rapidly remove four pollutants at environmental concentrations with removal efficiency of 75-95%.Moreover,the sorbent also showed good reproducibility.The new sorbent could address the problems that the?-CD polymer had a low surface area and a low adsorption capacity and the P5A polymer was inconvenent for binding pollutants in aqueous solution due to its strong hydrophobicity.It can be used as an excellent sorbent for rapid removal of different organic pollutants.Furthermore,the study in this part would open up a new way for preparing broad-spectrum sorbents.
Keywords/Search Tags:?-Cyclodextrin, Solid-phase extraction, Pillar[5]arene, Bisphenols, Propranolol, 1-Naphthylamine, Methylence blue
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