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Synthesis and characterisation of novel polymeric materials for high temperature composite applications.

Pullinger, Mark A. (2002) Synthesis and characterisation of novel polymeric materials for high temperature composite applications. Doctoral thesis, University of Surrey (United Kingdom)..

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Attempts have been made to synthesise a novel siloxane-containing dicyanate ester, 1,3-bis(4-cyanatophenyl)-1,1,3,3-tetramethyldisiloxane, commencing from 4-bromophenol or 4-methoxyphenol. Most of these syntheses have involved the use of a Grignard reaction to form a disiloxane group, followed up subsequent cleavage of an alkyl-protecting group to yield a free phenol. Several different ethers have been attempted, but none was successful. The extreme susceptibility of the aryl silicon-carbon bond to cleavage under acidic conditions has been demonstrated by these reactions. A novel phosphazene-containing dicyanate ester, 1,3-bis(4-cyanatophenyl)-1,3,5,5-tetraphenoxycyclotriphosphazene has been successfully synthesised in a four-step procedure with an overall yield of ca. 35%. The cyanate ester has been characterised by differential scanning calorimetry (DSC), thermogravimetric (TG) analysis, thermomechanical analysis (TMA), 1H, 13C and 13P NMR spectroscopy, and Fourier-Transform Infra-red (FT-IR) and Raman spectroscopy. The thermal data collected showed a surprisingly low glass transition temperature (59 °C) and enthalpy of polymerisation (ca. 36-5 kJ mol-1 of cyanate). The former figure was confirmed by TMA and modulated DSC. However, the cured cyanate showed reasonably high thermal stability: no mass loss was observed before 300 °C. Total decomposition did not occur until about 650 °C.

Item Type: Thesis (Doctoral)
Divisions : Theses
Authors :
Pullinger, Mark A.
Date : 2002
Contributors :
Depositing User : EPrints Services
Date Deposited : 09 Nov 2017 12:15
Last Modified : 20 Jun 2018 10:56

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