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TitleIn situ synthesis of polysulfides covalently bonded to silica
Publication TypeJournal Article
Year of Publication2002
AuthorsOssenkamp, G.C., Kemmitt T., and Johnston J.H.
JournalJournal of Colloid and Interface Science
Volume249
Issue2
Pagination464 - 470
Date Published2002
ISSN00219797 (ISSN)
Keywordsalcohol derivative, alkene derivative, article, bridged compound, catalysis, Chemical analysis, Chemical bonds, chemical modification, covalent bond, Esterification, mathematical analysis, microanalysis, nuclear magnetic resonance, nuclear magnetic resonance spectroscopy, Polysulfides, priority journal, Silica, silicon derivative, silicon dioxide, sulfide, sulfur, Sulphide bridges, surface property, synthesis, Synthesis (chemical), thermal analysis, Thermoanalysis, thiol derivative, Vulcanization, Zinc compounds, ziram
AbstractSilanol groups, ≡Si-OH, on the surface of silica were esterified with unsaturated alcohols and long-chain alcohols bearing thiol groups. The modified silicas obtained were used as substrates for a vulcanization-analogous reaction with sulfur catalyzed by zinc dimethyldithiocarbamate. Surface-esterified thiols could be smoothly converted to bridged polysulfides bonded to the silica surface, whereas the use of surface-esterified unsaturated alcohols led to removal of the surface-esterified alcohol from the silica surface. The materials were characterized by solid-state NMR and thermal and microanalytical analysis. The linking of surface-esterified alkenols and thiols by sulfide bridges was investigated by a numerical model for a flat surface. This showed that for a typical density of 3-4 μmol/m2 surface groups, a statistical maximum of 70-75% of groups could be linked by Sn bridges (n = 2-4). © 2002 Elsevier Science (USA).
URLhttp://www.scopus.com/inward/record.url?eid=2-s2.0-0036354790&partnerID=40&md5=2a309055fff24916b6b3df649382d8f3
DOI10.1006/jcis.2002.8294

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