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    Preparation and characterization of hydroxyapatite/poly(ethylene adipate) hybrid composites
    Hydroxyapatite/poly(ethylene adipate) (HAp/PEA) composites were prepared by in situ ring-opening polymerization of cyclic oligo(ethylene adipate) (C-OEA) within the porous HAp templates. HAp was firstly prepared by a co-precipitation method using calcium hydroxide and phosphoric acid and then shaped as a rectangular porous template. PEA precursor was synthesized by bulk polymerization of dimethyl adipate and ethylene glycol in the presence of tetraisopropyl orthotitanate. C-OEA was obtained by cyclo-depolymerization of the PEA precursor under high dilution condition using dibutyl tinoxide as a catalyst. The HAp/PEA composites were prepared by immersing the porous HAp templates in the mixture solution of C-OEA and dibutyl tinoxide catalyst overnight and ring-opening polymerizing at 180, 200 and 220°C for 24 h. The ring-opening polymerized PEA formed as a thin film coating on the surface of porous HAp template. The HAp/PEA composites contained PEA in the range of 20-26 wt%. The weight-average molecular weights of ring-opening polymerized PEA were in the range of 3800-4450 g/mol. Compressive strength of the HAp/PEA composite was significantly increased from 25 MPa in the porous HAp template to 140 MPa in the composite. © 2008 VSP.
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    Synthesis of poly(ethylene adipate) and poly(ethylene adipate-co-terephthalate) via ring-opening polymerization
    (2007-08-01) ;
    Loungvanidprapa, Pittaya
    Syntheses of poly(ethylene adipate) (ROP-PEA) and poly(ethylene adipate-co-terephthalate) (ROP-PEA-co-PET) were achieved via ring-opening polymerization of corresponding cyclic oligoesters. In case of ROP-PEA, cyclic oligo(ethylene adipate) (C-OEA) was equilibrated in the presence of di-n-butyltin oxide as a catalyst under high-concentration conditions at 180 and 200 °C for 1-24 h. The polymer products were obtained in yields up to 100% with the over(M, -)<inf>n</inf> and over(M, -)<inf>w</inf> in the ranges of 3000-23 000 g/mol and 5000-60 000 g/mol, respectively. The ROP-PEA-co-PET was prepared by equilibrating an equimolar amount of C-OEA and cyclic oligo(ethylene terephthalate) (C-OET) using di-n-butyltin oxide catalyst under high-concentration conditions at 250 °C for 24 h. The copolyester produced was obtained in yield of 97% with the over(M, -)<inf>n</inf> and over(M, -)<inf>w</inf> of 18 000 and 46 000 g/mol, respectively. <sup>1</sup>H NMR spectrum of ROP-PEA-co-PET showed two new proton signals of ethylene unit representing the existence of heterolinkage with different chemical environment in the copolymer. This indicated the random transesterification of C-OEA and C-OET resulting in random structure in copolyester. In addition, the result of ROP-PEA-co-PET from DSC showed the glass transition temperature in the values of -8 °C with no melting temperature indicating thermoplastic elastomeric behavior. © 2007 Elsevier Ltd. All rights reserved.