Synthesis and thermal transformations of polyphosphosiloxane based on trimethyl phosphate and (3-aminopropyl)triethoxysilane |
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Authors: | S V Klement’eva N F Cherepennikova V V Semenov A I Kirillov M A Lopatin O V Kuznetsova Yu A Kurskii A A Zaitsev L G Klapshina V E Duglas G A Domrachev |
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Institution: | (1) G. A. Razuvaev Institute of Organometallic Chemistry, Russian Academy of Sciences, 49 ul. Tropinina, 603950 Nizhny Novgorod, Russian Federation;(2) Montpellier II University, Chemical Laboratory of Molecular Organization of Solid State, French Academy of Sciences, 34095 Montpellier, France |
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Abstract: | A method for the synthesis of polyphosphosiloxane by the thermal condensation of an equimolar mixture of trimethyl phosphate
and (3-aminopropyl)triethoxysilane at 200 °C was developed. The reaction affords ethanol and polyphosphosiloxane-{Si(OEt)(CH2)3NR1R2]-O-P(O)(OMe)-O}n-(R1 = H, Me; R2 = Me), whose composition and structure were confirmed by 1H, 13C, and 31P NMR spectroscopy, IR spectroscopy, and elemental analysis. The scheme of polymerization involving the intermediate formation
of methyl-and dimethylphosphoric acids and their condensation with ethoxysilanes was proposed. The calcination of the obtained
polyphosphosiloxane in vacuo at 350 °C results in the elimination of the amino groups and alkoxide substituents, and a spatially cross-linked polymer
is formed as an amorphous powder. Its further thermolysis at 600 and 1000 °C gives crystalline phosphosilicates Si5O(PO4)6 or SiP2O7. Their amorphous and crystalline samples were characterized by IR spectroscopy, X-ray diffraction analysis, and solid-state
13C and 31P spectroscopy.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2138–2148, November, 2007. |
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Keywords: | trimethyl phosphate (3-aminopropyl)triethoxysilane condensation polyphosphosiloxane phosphosilicates thermal transformations amorphous and crystalline phases organosilicon compounds |
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