Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO4/2
Identifieur interne : 000791 ( Main/Exploration ); précédent : 000790; suivant : 000792Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO4/2
Auteurs : Jerzy J. Chru Ciel [Pologne] ; Marzena Fejdy ; Witold FortuniakSource :
- Polymers [ 2073-4360 ] ; 2018.
Abstract
Six liquid branched poly(methylhydrosiloxanes) of new random structures (PMHS-Q), containing quadruple branching units SiO4/2 (Q), both MeHSiO (DH) and Me2SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me3SiO0.5 (M) were prepared by a hydrolytic polycondensation method of appropriate organic chlorosilanes and tetraethyl ortosilicate (TEOS), in diethyl ether medium at temperature below 0 °C. Volatile low molecular weight siloxanes were removed by a vacuum distillation at 150–155 °C. Yields of PMHS-Q reached from 55–69 wt%. Their dynamic viscosities were measured in the Brookfield HBDV+IIcP cone-plate viscometer and ranged from 10.7–13.1 cP. Molecular weights (MW) of PMHS-Q (Mn = 2440–6310 g/mol, Mw = 5750–10,350 g/mol) and polydispersities of MW (Mw/Mn = 2.0–2.8) were determined by a size exclusion chromatography (SEC). All polymers were characterized by FTIR, 1H- and 29Si-NMR, and an elemental analysis. A microstructure of siloxane chains was proposed on a basis of 29Si-NMR results and compared with literature data.
Url:
DOI: 10.3390/polym10050484
PubMed: 30966518
PubMed Central: 6415389
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO<sub>4/2</sub></title><author><name sortKey="Chru Ciel, Jerzy J" sort="Chru Ciel, Jerzy J" uniqKey="Chru Ciel J" first="Jerzy J." last="Chru Ciel">Jerzy J. Chru Ciel</name><affiliation wicri:level="1"><nlm:aff id="af1-polymers-10-00484">Textile Research Institute, Brzezińska Str. 5/15, 92-103 Łódź, Poland</nlm:aff><country xml:lang="fr">Pologne</country><wicri:regionArea>Textile Research Institute, Brzezińska Str. 5/15, 92-103 Łódź</wicri:regionArea><wicri:noRegion>92-103 Łódź</wicri:noRegion></affiliation></author><author><name sortKey="Fejdy, Marzena" sort="Fejdy, Marzena" uniqKey="Fejdy M" first="Marzena" last="Fejdy">Marzena Fejdy</name><affiliation><nlm:aff id="af2-polymers-10-00484">The Institute of Security Technologies “MORATEX”, Marii Skłodowskiej-Curie Str. 3, 90-505 Łódź, Poland;<email>mfejdys@moratex.eu</email></nlm:aff></affiliation></author><author><name sortKey="Fortuniak, Witold" sort="Fortuniak, Witold" uniqKey="Fortuniak W" first="Witold" last="Fortuniak">Witold Fortuniak</name><affiliation><nlm:aff id="af3-polymers-10-00484">Centre of Molecular and Macromolecular Studies, Polish Academy of Sciences, Sienkiewicza Str. 112, 90-363 Łódź, Poland;<email>wfortuni@cbmm.lodz.pl</email></nlm:aff></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">PMC</idno><idno type="pmid">30966518</idno><idno type="pmc">6415389</idno><idno type="url">http://www.ncbi.nlm.nih.gov/pmc/articles/PMC6415389</idno><idno type="RBID">PMC:6415389</idno><idno type="doi">10.3390/polym10050484</idno><date when="2018">2018</date><idno type="wicri:Area/Pmc/Corpus">001125</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Corpus" wicri:corpus="PMC">001125</idno><idno type="wicri:Area/Pmc/Curation">001125</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Curation">001125</idno><idno type="wicri:Area/Pmc/Checkpoint">000455</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Checkpoint">000455</idno><idno type="wicri:source">PubMed</idno><idno type="RBID">pubmed:30966518</idno><idno type="wicri:Area/PubMed/Corpus">000578</idno><idno type="wicri:explorRef" wicri:stream="PubMed" wicri:step="Corpus" wicri:corpus="PubMed">000578</idno><idno type="wicri:Area/PubMed/Curation">000578</idno><idno type="wicri:explorRef" wicri:stream="PubMed" wicri:step="Curation">000578</idno><idno type="wicri:Area/PubMed/Checkpoint">000751</idno><idno type="wicri:explorRef" wicri:stream="Checkpoint" wicri:step="PubMed">000751</idno><idno type="wicri:Area/Ncbi/Merge">002179</idno><idno type="wicri:Area/Ncbi/Curation">002179</idno><idno type="wicri:Area/Ncbi/Checkpoint">002179</idno><idno type="wicri:Area/Main/Merge">000794</idno><idno type="wicri:Area/Main/Curation">000791</idno><idno type="wicri:Area/Main/Exploration">000791</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en" level="a" type="main">Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO<sub>4/2</sub></title><author><name sortKey="Chru Ciel, Jerzy J" sort="Chru Ciel, Jerzy J" uniqKey="Chru Ciel J" first="Jerzy J." last="Chru Ciel">Jerzy J. Chru Ciel</name><affiliation wicri:level="1"><nlm:aff id="af1-polymers-10-00484">Textile Research Institute, Brzezińska Str. 5/15, 92-103 Łódź, Poland</nlm:aff><country xml:lang="fr">Pologne</country><wicri:regionArea>Textile Research Institute, Brzezińska Str. 5/15, 92-103 Łódź</wicri:regionArea><wicri:noRegion>92-103 Łódź</wicri:noRegion></affiliation></author><author><name sortKey="Fejdy, Marzena" sort="Fejdy, Marzena" uniqKey="Fejdy M" first="Marzena" last="Fejdy">Marzena Fejdy</name><affiliation><nlm:aff id="af2-polymers-10-00484">The Institute of Security Technologies “MORATEX”, Marii Skłodowskiej-Curie Str. 3, 90-505 Łódź, Poland;<email>mfejdys@moratex.eu</email></nlm:aff></affiliation></author><author><name sortKey="Fortuniak, Witold" sort="Fortuniak, Witold" uniqKey="Fortuniak W" first="Witold" last="Fortuniak">Witold Fortuniak</name><affiliation><nlm:aff id="af3-polymers-10-00484">Centre of Molecular and Macromolecular Studies, Polish Academy of Sciences, Sienkiewicza Str. 112, 90-363 Łódź, Poland;<email>wfortuni@cbmm.lodz.pl</email></nlm:aff></affiliation></author></analytic><series><title level="j">Polymers</title><idno type="eISSN">2073-4360</idno><imprint><date when="2018">2018</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en"><p>Six liquid branched poly(methylhydrosiloxanes) of new random structures (PMHS-Q), containing quadruple branching units SiO<sub>4/2</sub> (Q), both MeHSiO (D<sup>H</sup>) and Me<sub>2</sub>SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me<sub>3</sub>SiO<sub>0.5</sub> (M) were prepared by a hydrolytic polycondensation method of appropriate organic chlorosilanes and tetraethyl ortosilicate (TEOS), in diethyl ether medium at temperature below 0 °C. Volatile low molecular weight siloxanes were removed by a vacuum distillation at 150–155 °C. Yields of PMHS-Q reached from 55–69 wt%. Their dynamic viscosities were measured in the Brookfield HBDV+IIcP cone-plate viscometer and ranged from 10.7–13.1 cP. Molecular weights (MW) of PMHS-Q (M<sub>n</sub> = 2440–6310 g/mol, M<sub>w</sub> = 5750–10,350 g/mol) and polydispersities of MW (M<sub>w</sub>/M<sub>n</sub> = 2.0–2.8) were determined by a size exclusion chromatography (SEC). All polymers were characterized by FTIR, <sup>1</sup>H- and <sup>29</sup>Si-NMR, and an elemental analysis. A microstructure of siloxane chains was proposed on a basis of <sup>29</sup>Si-NMR results and compared with literature data.</p></div></front><back><div1 type="bibliography"><listBibl><biblStruct><analytic><author><name sortKey="Eaborn, C" uniqKey="Eaborn C">C. Eaborn</name></author></analytic></biblStruct><biblStruct><analytic><author><name sortKey="Noll, W" uniqKey="Noll W">W. 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