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Novel Calix[4]arene based Ligands: Complexation, Extraction and Functional Materials. Sebastian haupt René Schnorr, Steve Ullmann prof. dr. b. kersting leipzig university. macrocyclic hexaaza-bis ( thiophenolate ) ligand. calix[4] arenes. Working group of Prof. Dr. B. Kersting. 15 Å.
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Novel Calix[4]arene based Ligands: Complexation, Extraction and Functional Materials Sebastian haupt René Schnorr, Steve Ullmann prof.dr. b. kersting leipziguniversity
macrocyclichexaaza-bis(thiophenolate)ligand • calix[4]arenes Working group of Prof. Dr. B. Kersting 15 Å Au(111) 1 Kersting, B., Steinfeld, G., Fritz, T., and Hausmann, J. Eur. J. Inorg. Chem. 1999, 12, 2167 2J. Lach,A . Jeremies, F. Lungwitz, B. Kersting, submitted. . Sebastian Haupt Leipzig University
BMBF-project, 02NUK014C TU Dresden Karsten Gloe – HZDR Gert Bernhard Steuerung des Migrationsverhaltens von Radionukliden mit Hilfe makrozyklischer, multifunktionaler Chelatliganden Working group of Prof. Dr. B. Kersting • binding sites for alkaline and alkaline earth and/or • d- and f-elements • coordination chemistry • binary interactions in liquid-liquid and solid-liquid • systems • cooperation with HZDR – research site Leipzig and TU Dresden . Sebastian Haupt Leipzig University
calix[4]arenes upperrim n = 4 - 14 Introduction lowerrim • four conformations 1 C. D. Gutsche, M. Iqbal, Org. Synth.1990, 68, 234–237. 2C. D. Gutsche, Calixarenes. An introduction, RSC Publ., Cambridge, 2008. Sebastian Haupt Leipzig University
a Zn(II)-complex supported by a novel salicylidene-linked double-calix[4]arene Coordination chemistry of calix[4]arenes - CHEF-effect 1 S.Ullmann Sebastian Haupt Leipzig University
H2Lbandit, a calix[4]arene in partial-cone conformation Coordination chemistry of calix[4]arenes • anion driven self-assembly -2:1 complexeswithnitrateandchloride -2:3 complexeswithacetate 1 R. Schnorr Sebastian Haupt Leipzig University
liquid-liquid extraction of divalent metals Starting point • focus of interest Sr2+ 1Ungaro et al., J. Chem. Soc., Chem. Commun. 1984,981. 2Ungaro et al., J. lncl. Phen.1984, 199. Sebastian Haupt Leipzig University
systematic use of derivates simple CHCl3 / water system radiometric determination: 85Sr2+ investigation of influences New tricks for an old dog • pH value, counter ion, temperature, time, concentration • pH = 9 • 1 h shaking • room temperature • ligand/strontium 5/1 over 95 % extracted strontium Sebastian Haupt Leipzig University 1 S. Haupt, R. Schnorr, M. Poetsch (in preperation) 2 A. Mansel, S. Gruhne,K. Franke,S. Fischer, Production of 85Sr at a 18 MeV-cyclotron and purification for geochemical investigations2012 (Submitted )
Synthetic groundwater over 90 % extracted strontium • 1 P. Mellet al.Journal of Radioanalytical and Nuclear Chemistry2006, 268, 405-410. • 2 B. Torstenfelt, K. Andersson, B. Allard Chemical Geology1982, 36, 123-137. Sebastian Haupt Leipzig University
joint linker calix[4]arene solid support joint -triazole, tetrazole -ester, aminoacid -imine, amine -ether -C-C coupling Immobilization on mesoporous CPG-silica radicalthioladdition 1 R. Brindle, K. Albert, J. D. Glennon, Journal of Chromatography A1996, 731, 41–46. 2 J. D. Glennon, E. Horne, K. Hall, D. Cocker, M. A. McKervey, Journal of Chromatography A1996, 731, 47–55. Sebastian Haupt Leipzig University
Immobilization on mesoporous CPG-silica 1 S. Haupt, M. Handke (in preparation) Sebastian Haupt Leipzig University
13C CP/MAS NMR Immobilization on mesoporous CPG-silica • DTA thermal stability to 300 °C • elemental analyses up to 0.5 mmol ligand / g CPG • Raman no SH vibration Sebastian Haupt Leipzig University
batch experiments strontium salt buffer, ph = 9 Solid-liquid-extraction filtration gamma counter 1 M. Poetsch Sebastian Haupt Leipzig University
see poster number 6 and 28 Posters encapsulation of amino acids gold nanoparticles 1 A. Jeremies, R. Schnitter, M. Börner Sebastian Haupt Leipzig University
Thankyouforyourattention. Das diesem Vortrag zugrundeliegende Vorhaben wurde mit Mitteln des Bundesministeriums für Bildung und Forschung unter dem Förderkennzeichen 02NUK014C gefördert.
Anhang Sebastian Haupt Leipzig University
CPG-SiO2: OF ~ 100m2/g, Porengröße 30nm (groß), Körnung 100-400µm, OH-dichte 4-6/nm2 max 1 mmol OH/g (mit 6 OH gerechnet) Anhang Sebastian Haupt Leipzig University