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Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO4/2.

Identifieur interne : 000578 ( PubMed/Corpus ); précédent : 000577; suivant : 000579

Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO4/2.

Auteurs : Jerzy J. Chru Ciel ; Marzena Fejdy ; Witold Fortuniak

Source :

RBID : pubmed:30966518

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.

DOI: 10.3390/polym10050484
PubMed: 30966518

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pubmed:30966518

Le document en format XML

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<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>
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<nlm:affiliation>Textile Research Institute, Brzezińska Str. 5/15, 92-103 Łódź, Poland. jchrusci@p.lodz.pl.</nlm:affiliation>
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<name sortKey="Fejdy, Marzena" sort="Fejdy, Marzena" uniqKey="Fejdy M" first="Marzena" last="Fejdy">Marzena Fejdy</name>
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<nlm:affiliation>The Institute of Security Technologies "MORATEX", Marii Skłodowskiej-Curie Str. 3, 90-505 Łódź, Poland. mfejdys@moratex.eu.</nlm:affiliation>
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<div type="abstract" xml:lang="en">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 Me₂SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me₃SiO
<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, ¹H- 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.</div>
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<Title>Polymers</Title>
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<sub>4/2</sub>
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<sub>4/2</sub>
(Q), both MeHSiO (D
<sup>H</sup>
) and Me₂SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me₃SiO
<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, ¹H- 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.</AbstractText>
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<Language>eng</Language>
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<GrantID>a grant Nr 3 T08E 053 30</GrantID>
<Agency>The Ministry of Science and Higher Education (Poland)</Agency>
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<Keyword MajorTopicYN="N">29Si-NMR</Keyword>
<Keyword MajorTopicYN="N">hydrolytic polycondensation</Keyword>
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