Newly synthesised diglycolamide functionalised silica gel with terminal 2-ethylhexyl alkyl chain, Silica-DGA (2EH) having high ligand density for adsorption of trivalent actinide and lanthanide from acidic medium
{"title":"Newly synthesised diglycolamide functionalised silica gel with terminal 2-ethylhexyl alkyl chain, Silica-DGA (2EH) having high ligand density for adsorption of trivalent actinide and lanthanide from acidic medium","authors":"","doi":"10.1016/j.cherd.2024.08.004","DOIUrl":null,"url":null,"abstract":"<div><p>A novel diglycolamide resin with 2-ethylhexyl terminal alkyl chain functionalised to silica gel was synthesised and characterised by ATR-FTIR, SEM, TG/DSC, & <sup>13</sup>C (CP/MAS) solid state NMR techniques. Effective functionalization of the organic ligand upon silica gel was confirmed from the two carbonyl stretching frequencies at 1735 cm<sup>−1</sup> and 1619 cm<sup>−1</sup> in the FTIR spectrum and carbonyl carbon atom signal at 170 ppm in <sup>13</sup>C (CP/MAS) solid state NMR spectrum. Thermo gravimetric measurement showed 17.3 ± 0.2 % (W/W) weight loss corresponding to the ligand loading value of 425 µmol/g. The resin showed very high uptake of trivalent lanthanide and actinide ions from 4.0 M HNO<sub>3</sub> medium and very low distribution of Cs & Sr; K<sub>d</sub> ∼ 1.1×10<sup>3</sup> mL/g for Am(III), ∼ 1.41×10<sup>3</sup> mL/g for Eu(III), ∼2.5 mL/g for Sr and 1.53 mL/g for Cs. FTIR spectroscopic study of the Eu<sup>3+</sup> adsorbed resin showed single carbonyl stretching frequency at 1654 cm<sup>−1</sup>, instead of the two carbonyl stretching frequencies in fresh silica-DGA(2EH) resin indicating complexation through carbonyl oxygen. Very low K<sub>d</sub> of ∼1.2–5.1 mL/g for lanthanides/actinides from 4.0 M HNO<sub>3</sub> containing water soluble DGA namely N, N, N, N, Tetraethyldiglycolamide (TEDGA) in the concentration range 0.3–0.1 M indicates 99 % back adsorption feasibility.</p></div>","PeriodicalId":10019,"journal":{"name":"Chemical Engineering Research & Design","volume":null,"pages":null},"PeriodicalIF":3.7000,"publicationDate":"2024-08-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Chemical Engineering Research & Design","FirstCategoryId":"5","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0263876224004702","RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"ENGINEERING, CHEMICAL","Score":null,"Total":0}
引用次数: 0
Abstract
A novel diglycolamide resin with 2-ethylhexyl terminal alkyl chain functionalised to silica gel was synthesised and characterised by ATR-FTIR, SEM, TG/DSC, & 13C (CP/MAS) solid state NMR techniques. Effective functionalization of the organic ligand upon silica gel was confirmed from the two carbonyl stretching frequencies at 1735 cm−1 and 1619 cm−1 in the FTIR spectrum and carbonyl carbon atom signal at 170 ppm in 13C (CP/MAS) solid state NMR spectrum. Thermo gravimetric measurement showed 17.3 ± 0.2 % (W/W) weight loss corresponding to the ligand loading value of 425 µmol/g. The resin showed very high uptake of trivalent lanthanide and actinide ions from 4.0 M HNO3 medium and very low distribution of Cs & Sr; Kd ∼ 1.1×103 mL/g for Am(III), ∼ 1.41×103 mL/g for Eu(III), ∼2.5 mL/g for Sr and 1.53 mL/g for Cs. FTIR spectroscopic study of the Eu3+ adsorbed resin showed single carbonyl stretching frequency at 1654 cm−1, instead of the two carbonyl stretching frequencies in fresh silica-DGA(2EH) resin indicating complexation through carbonyl oxygen. Very low Kd of ∼1.2–5.1 mL/g for lanthanides/actinides from 4.0 M HNO3 containing water soluble DGA namely N, N, N, N, Tetraethyldiglycolamide (TEDGA) in the concentration range 0.3–0.1 M indicates 99 % back adsorption feasibility.
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