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In situ ring-opening polymerization of hydroxyapatite/poly(ethylene adipate)-co-(ethylene terephthalate) biomimetic composites
(2013-02-01)
Siriphannon, Punnama
;
Monvisade, Pathavuth
Hydroxyapatite/poly(ethylene adipate)-co-poly(ethylene terephthalate) biomaterials (HAp/PEA-co-PET) have been prepared by ring opening polymerization (ROP) of cyclic oligo(ethylene adipate)-co-oligo(ethylene terephthalate) (C-OEA-co-C-OET) in the porous hydroxyapatite (HAp) scaffolds at 250 °C for 24 h under vacuum. The content of ROP-PEA-co-PET in the HAp/PEA-co-PET composite was about 20 wt% with the values of number average molecular weight (Mn) and weight average molecular weight (MW) of 3380 and 7160 g/mol, respectively. Compressive strength and modulus of the HAp/PEA-co-PET composites were about 29 and 246 MPa, respectively. These mechanical properties were higher than those of the porous HAp templates and natural cancellous bone. In vitro bioactivity of the HAp/PEA-co-PET composites was studied by soaking in simulated body fluid (SBF) under the flowing system at the rate of 130 mL/day for 7, 14, 21 and 28 days. The formation of hydroxyapatite nanocrystals was observed on the composite surfaces through the consumption of calcium and phosphorus from the SBF solution, indicating the bioactivity of these HAp/PEA-co-PET composites. These results indicated the competency of HAp/PEA-co-PET composites for biomedical applications. © Indian Academy of Sciences.
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Calcium silicate/poly(ethylene terephthalate) biomaterials via ring-opening polymerization
(2012-10-01)
Suebwongnat, Suebpong
;
Jianprasert, Apichaya
;
Siriphannon, Punnama
;
Monvisade, Pathavuth
Calcium silicate/poly(ethylene terephthalate) (CS/PET) composites were synthesized via ring-opening polymerization (ROP). CS raw material was synthesized by coprecipitation of calcium nitrate tetrahydrate and tetraethyl orthosilicate. Commercial grade PET was cyclodepolymerized under high dilution technique to cyclic oligo(ethylene terephthalate) (C-OET) raw material. The CS/PET precomposites were prepared by mixing 60:40 (C6P4) and 50:50 (C5P5) wt% of CS powder and C-OET with the presence of 3 mol% of dibutyl tinoxide catalyst (with respect to the cyclic) then shaped the pre-composites into cylindrical pellets. The presented C-OET in the pre-composites was ring-opening polymerized to obtain PET film covering on the CS grains with the different reaction temperatures as 180, 200 and 250 °C under vacuum for 24 h. Thermogravimetric analysis indicated that the ROP-PET content in the C5P5 and C6P4 composites were about 46-48 and 35-38 wt%, respectively. The melting points (T<inf>m</inf>) of ROP-PET of all composites were in a range of 233-246 °C. Compressive strength of the CS/ PET composites was significantly increased from 4.8 MPa of the neat CS to 31.0 MPa for the C5P5 composites at the ROP temperature of 250 °C. The CS/PET composites faster induced the continuous-phase formation of hydroxyapatite (HAp) nanocrystals on their surfaces than the HAp/polymer composites. The induction occurred within 7-day soaked in the simulated body fluid (SBF) solution, indicating the bioactivity of the CS/PET composites. © 2012 Springer Science+Business Media Dordrecht.
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Poly(ethylene terephthalate)/hydroxyapatite biomaterials: Preparation, characterization, and in vitro bioactivity
(2009-02-01)
Siriphannon, Punnama
;
Monvisade, Pathavuth
Poly(ethylene terephthalate)/hydroxyapatite (PET/HAp) composites were prepared by mixing HAp powder with a mixture solution of cyclic oligo(ethylene terephthalate) (C-OET) and dibutyl tinoxide catalyst in dichrolomethane, and then shaping the precomposites in cylindrical pellets. The C-OET in the precomposites was ring-opening polymerized (ROP) to PET under vacuum at 250°C for 24 h. The PET/HAp composites were formulated with HAp to PET ratios of 60:40 (H6P4) and 50:50 (H5P5). The ROP-PET in the composites was present as a thin-layer coating on the HAp grains and evenly distributed throughout the samples. Compressive strength of the PET/HAp composites was significantly increased from 8 MPa of the H10P0 to 17 and 29 MPa for H6P4 and H5P5, respectively. In vitro bioactivity of the PET/HAp composites was studied by soaking in simulated body fluid (SBF) at 36.5°C for 7-28 days. After prolonged soaking, the HAp nanocrystals precipitated from the SBF solution and formed as a layer of globular aggregates, coated on the composite surfaces. The H6P4 composite showed faster formation rate of nano-HAp than the H5P5 composite, indicating that the bioactivity of PET/HAp composites depended on the amount of HAp. © 2008 Wiley Periodicals, Inc.
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Synthesis of poly(ethylene terephthalate-co-isophthalate) via ring-opening polymerization of their cyclic oligomers
(2008-10-01)
Monvisade, Pathavuth
;
Loungvanidprapa, Pittaya
Syntheses of poly(ethylene terephthalate-co-isophthalate) (PET-co-PEI) were achieved via ring-opening copolymerization of corresponding cyclic oligoesters. The ring-opening polymerization (ROP)-PET-co-PEI were prepared by equilibrating an equimolar amount of cyclic oligo(ethylene terephthalate) and cyclic oligo(ethylene isophthalate) using di-n-butyltin oxide catalyst under high concentration conditions at 270 and 290°C for 8 and 12 h. The copolyesters were obtained in yields of up to 91% with the inherent viscosity (η <inf>inh</inf>) of up to 2.89 dl/g indicating the drastically high molecular weight compared with the conventional and ROP routes for the synthesis of PEI. The differential scanning calorimetry data of ROP-PET-co-PEI showed the melting temperatures above 400°C indicated the potential used in high temperature application. © 2008 Springer Science+Business Media B.V.
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Preparation and characterization of hydroxyapatite/poly(ethylene adipate) hybrid composites
(2008-06-01)
Siriphannon, Punnama
;
Monvisade, Pathavuth
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)
Monvisade, Pathavuth
;
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.
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Preparation and characterization of hydroxyapatite/poly(ethylene glutarate) biomaterials
(2007-05-01)
Siriphannon, Punnama
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Monvisade, Pathavuth
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Jinawath, Supatra
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Hemachandra, Khemchai
Hydroxyapatite/poly(ethylene glutarate) (HAp/PEG) biomaterial composites were prepared by ring-opening polymerization (ROP) of cyclic oligo(ethylene glutarate) (C-PEG) in porous HAp scaffolds. The HAp/C-PEG pre-composites were prepared by immersing the porous HAp scaffolds in the mixture solution of C-PEG and dibutyl tin-oxide catalyst overnight and polymerizing at 200°C for 24, 48, and 72 h under vacuum. The successful ROP of C-PEG in the porous HAp scaffolds was corroborated by the signals of hydroxyl end-group of PEG shown in the <sup>1</sup>H NMR spectrum of the ROP-products extracted from the composites. PEG in the composites was present as a thin layer coating on the HAp grains and was evenly distributed throughout the samples. The PEG content was about 13-16 wt % and decreased with increasing polymerization time. Its molecular weight (M̄<inf>w</inf>, weight average) measured by gel permeation chromatography was in the range of 4300-6800 g/mol. Compressive strength of the HAp/PEG composites was significantly increased from 3 MPa of the porous HAp scaffold to 11-15 MPa, depending on the PEG content in the composites. In vitro bioactivity of the HAp/ PEG composites was studied by soaking in simulated body fluid (SBF) at 36.5°C for 7-28 days. After prolonged soaking, the HAp nanocrystals precipitated from the SBF solution and formed as a layer of globular aggregates, coated on the composite surfaces. This result suggested that the HAp/PEG composite was a bioactive material. © 2006 Wiley Periodicals, Inc.

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