Synthesis of four‐arm star poly(L‐lactide) oligomers using an in situ‐generated calcium‐based initiator
Identifieur interne : 007D66 ( Main/Exploration ); précédent : 007D65; suivant : 007D67Synthesis of four‐arm star poly(L‐lactide) oligomers using an in situ‐generated calcium‐based initiator
Auteurs : Karina A. George [Australie] ; François Schué [France] ; Traian V. Chirila [Australie] ; Edeline Wentrup-Byrne [Australie]Source :
- Journal of Polymer Science Part A: Polymer Chemistry [ 0887-624X ] ; 2009-09-15.
Descripteurs français
- Pascal (Inist)
- Wicri :
English descriptors
- KwdEn :
- Alkoxide, Argon atmosphere, Bulk polymerization, Bulk polymerizations, Calcium, Calcium alkoxide, Calcium alkoxide initiator, Calcium compound, Calcium hydride, Carboxylated lactyl, Chem, Coadded scans, Coinitiator, Conversion plot, Crude polymers, Cyclic esters, Dalton trans, Early stages, Excellent agreement, Experimental study, Feed mixture, Feed mole ratio, Feed ratio, Feed ratios, Ftir spectroscopy, Full conversion, Heterogeneous polymerization, Huang, Hydride, Hydroxyl, Hydroxyl groups, Initial ratios, Initiator, Inorg chem, Kinetic data, Kinetic plots, Lactic acid polymer, Lactide, Lactoyllactic acid, Laser power, Linear relationship, Living polymer, Macromol chem phys, Macromolecule, Makromol chem, Molar ratio, Mole ratio, Molecular weight, Octoate, Oligomer, Optically active polymer, Peak area, Pentaerythritol, Pentaerythritol hydroxyl groups, Pentaerythritol molecules, Plla, Plla samples, Polym, Polym bull, Polym chem, Polymer, Polymer chemistry, Polymer science, Polymeric, Polymeric arms, Polymerization, Polymerization mixture, Preparation, Priming activity, Pure appl chem, Queensland, Queensland university, Raman microspectroscopy, Reaction mixture, Reaction scheme, Reference band, Reference spectra, Ring opening polymerization, Secondary hydroxyl groups, Small bands, Solid lines, Spectroscopy, Stannous, Stannous octoate, Star oligomers, Star plla, Star plla oligomers, Star plla polymers, Star polymer, Star polymers, Theoretical values, Trace impurities, Trace quantities, Unreacted calcium hydride, Wiley periodicals.
- Teeft :
- Alkoxide, Argon atmosphere, Bulk polymerizations, Calcium, Calcium alkoxide, Calcium alkoxide initiator, Calcium hydride, Carboxylated lactyl, Chem, Coadded scans, Coinitiator, Conversion plot, Crude polymers, Cyclic esters, Dalton trans, Early stages, Excellent agreement, Feed mixture, Feed mole ratio, Feed ratio, Feed ratios, Ftir spectroscopy, Full conversion, Huang, Hydride, Hydroxyl, Hydroxyl groups, Initial ratios, Initiator, Inorg chem, Kinetic data, Kinetic plots, Lactide, Lactoyllactic acid, Laser power, Linear relationship, Macromol chem phys, Macromolecule, Makromol chem, Molar ratio, Mole ratio, Molecular weight, Octoate, Peak area, Pentaerythritol, Pentaerythritol hydroxyl groups, Pentaerythritol molecules, Plla, Plla samples, Polym, Polym bull, Polym chem, Polymer, Polymer chemistry, Polymer science, Polymeric, Polymeric arms, Polymerization, Polymerization mixture, Pure appl chem, Queensland, Queensland university, Raman microspectroscopy, Reaction mixture, Reaction scheme, Reference band, Reference spectra, Secondary hydroxyl groups, Small bands, Solid lines, Spectroscopy, Stannous, Stannous octoate, Star oligomers, Star plla, Star plla oligomers, Star plla polymers, Star polymer, Star polymers, Theoretical values, Trace impurities, Trace quantities, Unreacted calcium hydride, Wiley periodicals.
Abstract
Using an in situ‐generated calcium‐based initiating species derived from pentaerythritol, the bulk synthesis of well‐defined four‐arm star poly(L‐lactide) oligomers has been studied in detail. The substitution of the traditional initiator, stannous octoate with calcium hydride allowed the synthesis of oligomers that had both low PDIs and a comparable number of polymeric arms (3.7–3.9) to oligomers of similar molecular weight. Investigations into the degree of control observed during the course of the polymerization found that the insolubility of pentaerythritol in molten L‐lactide resulted in an uncontrolled polymerization only when the feed mole ratio of L‐lactide to pentaerythritol was 13. At feed ratios of 40 and greater, a pseudoliving polymerization was observed. As part of this study, in situ FT‐Raman spectroscopy was demonstrated to be a suitable method to monitor the kinetics of the ring‐opening polymerization of lactide. The advantages of using this technique rather than FTIR‐ATR and 1H NMR for monitoring L‐lactide consumption during polymerization are discussed. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 4736–4748, 2009
Url:
DOI: 10.1002/pola.23527
Affiliations:
- Australie, France
- Languedoc-Roussillon, Occitanie (région administrative)
- Montpellier
- PRES Sud de France, Université Montpellier 2
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Le document en format XML
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<term>Bulk polymerizations</term>
<term>Calcium</term>
<term>Calcium alkoxide</term>
<term>Calcium alkoxide initiator</term>
<term>Calcium compound</term>
<term>Calcium hydride</term>
<term>Carboxylated lactyl</term>
<term>Chem</term>
<term>Coadded scans</term>
<term>Coinitiator</term>
<term>Conversion plot</term>
<term>Crude polymers</term>
<term>Cyclic esters</term>
<term>Dalton trans</term>
<term>Early stages</term>
<term>Excellent agreement</term>
<term>Experimental study</term>
<term>Feed mixture</term>
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<term>Feed ratios</term>
<term>Ftir spectroscopy</term>
<term>Full conversion</term>
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<term>Huang</term>
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<term>Hydroxyl</term>
<term>Hydroxyl groups</term>
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<term>Initiator</term>
<term>Inorg chem</term>
<term>Kinetic data</term>
<term>Kinetic plots</term>
<term>Lactic acid polymer</term>
<term>Lactide</term>
<term>Lactoyllactic acid</term>
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<term>Macromolecule</term>
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<term>Solid lines</term>
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<term>Alcoolate</term>
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<term>Lactique acide polymère</term>
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<term>Polymère optiquement actif</term>
<term>Polymère vivant</term>
<term>Polymère étoile</term>
<term>Polymérisation masse</term>
<term>Polymérisation ouverture cycle</term>
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<term>Argon atmosphere</term>
<term>Bulk polymerizations</term>
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<term>Calcium alkoxide</term>
<term>Calcium alkoxide initiator</term>
<term>Calcium hydride</term>
<term>Carboxylated lactyl</term>
<term>Chem</term>
<term>Coadded scans</term>
<term>Coinitiator</term>
<term>Conversion plot</term>
<term>Crude polymers</term>
<term>Cyclic esters</term>
<term>Dalton trans</term>
<term>Early stages</term>
<term>Excellent agreement</term>
<term>Feed mixture</term>
<term>Feed mole ratio</term>
<term>Feed ratio</term>
<term>Feed ratios</term>
<term>Ftir spectroscopy</term>
<term>Full conversion</term>
<term>Huang</term>
<term>Hydride</term>
<term>Hydroxyl</term>
<term>Hydroxyl groups</term>
<term>Initial ratios</term>
<term>Initiator</term>
<term>Inorg chem</term>
<term>Kinetic data</term>
<term>Kinetic plots</term>
<term>Lactide</term>
<term>Lactoyllactic acid</term>
<term>Laser power</term>
<term>Linear relationship</term>
<term>Macromol chem phys</term>
<term>Macromolecule</term>
<term>Makromol chem</term>
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<term>Mole ratio</term>
<term>Molecular weight</term>
<term>Octoate</term>
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<front><div type="abstract" xml:lang="en">Using an in situ‐generated calcium‐based initiating species derived from pentaerythritol, the bulk synthesis of well‐defined four‐arm star poly(L‐lactide) oligomers has been studied in detail. The substitution of the traditional initiator, stannous octoate with calcium hydride allowed the synthesis of oligomers that had both low PDIs and a comparable number of polymeric arms (3.7–3.9) to oligomers of similar molecular weight. Investigations into the degree of control observed during the course of the polymerization found that the insolubility of pentaerythritol in molten L‐lactide resulted in an uncontrolled polymerization only when the feed mole ratio of L‐lactide to pentaerythritol was 13. At feed ratios of 40 and greater, a pseudoliving polymerization was observed. As part of this study, in situ FT‐Raman spectroscopy was demonstrated to be a suitable method to monitor the kinetics of the ring‐opening polymerization of lactide. The advantages of using this technique rather than FTIR‐ATR and 1H NMR for monitoring L‐lactide consumption during polymerization are discussed. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 4736–4748, 2009</div>
</front>
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