Synthesis of thermoplastic poly(ester-olefin) elastomers
A series of thermoplastic poly(ester-olefin) elastomers, based on poly(ethylene-stat-butylene), HO-PEB-OH, as the soft segment and poly (butylene terephthalate), PBT, as the hard segment, were synthesized by a catalyzed transesterification reaction in solution. The incorporation of soft hydrogenated...
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| Format: | Article |
| Language: | English |
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Association of Chemical Engineers of Serbia
2004-01-01
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| Series: | Hemijska Industrija |
| Subjects: | |
| Online Access: | http://www.doiserbia.nb.rs/img/doi/0367-598X/2004/0367-598X0410444T.pdf |
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| author | Tanasijević Branka Elkhaseh Salem F.K. Nikolić Marija S. Đonlagić Jasna A. |
| author_facet | Tanasijević Branka Elkhaseh Salem F.K. Nikolić Marija S. Đonlagić Jasna A. |
| author_sort | Tanasijević Branka |
| collection | DOAJ |
| description | A series of thermoplastic poly(ester-olefin) elastomers, based on poly(ethylene-stat-butylene), HO-PEB-OH, as the soft segment and poly (butylene terephthalate), PBT, as the hard segment, were synthesized by a catalyzed transesterification reaction in solution. The incorporation of soft hydrogenated poly(butadiene) segments into the copolyester backbone was accomplished by the polycondensation of α, ω-dihydroxyl telechelic HO-PEB-OH, (PEB Mn = 3092 g/mol) with 1,4-butanediol (BD) and dimethyl terephthalate (DMT) in the presence of a 50 wt-% high boiling solvent i.e., 1,2,4-trichlorobenzene. The molar ratio of the starting comonomers was selected to result in a constant hard to soft weight ratio of 60:40. The synthesis was optimized in terms of both the concentration of catalyst, tetra-n-butyl-titanate (Ti(OBu)4), and stabilizer, N,N'-diphenyl-p-phenylenediamine (DPPD), as well as the reaction time. It was found that the optimal catalyst concentration (Ti(OBu)4) for the synthesis of these thermoplastic elastomers was 1.0 mmol/mol ester and the optimal DPPD concentration was 1.0 wt-%. The extent of the reaction was followed by measuring the inherent viscosity of the reaction mixture. The effectiveness of the incorporation of the soft segments into the copolymer chains was proved by Soxhlet extraction with chloroform. The molecular structures, composition and the size of the synthesized poly(ester-butylene)s were verified by 1H NMR spectroscopy, viscometry of dilute solutions and the complex dynamic melt viscosity. The thermal properties of poly(ester-olefin)s were investigated by differential scanning calorimetry (DSC). The degree of crystallinity was also determined by DSC. The thermal and thermo-oxidative stability were investigated by thermogravimetric analysis (TGA). The rheological properties of poly(ester-olefin)s were investigated by dynamic mechanical spectroscopy in the melt and solid state. |
| first_indexed | 2024-12-22T22:26:20Z |
| format | Article |
| id | doaj.art-084a3ebc26e54147b9170848c956f3e0 |
| institution | Directory Open Access Journal |
| issn | 0367-598X |
| language | English |
| last_indexed | 2024-12-22T22:26:20Z |
| publishDate | 2004-01-01 |
| publisher | Association of Chemical Engineers of Serbia |
| record_format | Article |
| series | Hemijska Industrija |
| spelling | doaj.art-084a3ebc26e54147b9170848c956f3e02022-12-21T18:10:32ZengAssociation of Chemical Engineers of SerbiaHemijska Industrija0367-598X2004-01-01581044444910.2298/HEMIND0410444TSynthesis of thermoplastic poly(ester-olefin) elastomersTanasijević BrankaElkhaseh Salem F.K.Nikolić Marija S.Đonlagić Jasna A.A series of thermoplastic poly(ester-olefin) elastomers, based on poly(ethylene-stat-butylene), HO-PEB-OH, as the soft segment and poly (butylene terephthalate), PBT, as the hard segment, were synthesized by a catalyzed transesterification reaction in solution. The incorporation of soft hydrogenated poly(butadiene) segments into the copolyester backbone was accomplished by the polycondensation of α, ω-dihydroxyl telechelic HO-PEB-OH, (PEB Mn = 3092 g/mol) with 1,4-butanediol (BD) and dimethyl terephthalate (DMT) in the presence of a 50 wt-% high boiling solvent i.e., 1,2,4-trichlorobenzene. The molar ratio of the starting comonomers was selected to result in a constant hard to soft weight ratio of 60:40. The synthesis was optimized in terms of both the concentration of catalyst, tetra-n-butyl-titanate (Ti(OBu)4), and stabilizer, N,N'-diphenyl-p-phenylenediamine (DPPD), as well as the reaction time. It was found that the optimal catalyst concentration (Ti(OBu)4) for the synthesis of these thermoplastic elastomers was 1.0 mmol/mol ester and the optimal DPPD concentration was 1.0 wt-%. The extent of the reaction was followed by measuring the inherent viscosity of the reaction mixture. The effectiveness of the incorporation of the soft segments into the copolymer chains was proved by Soxhlet extraction with chloroform. The molecular structures, composition and the size of the synthesized poly(ester-butylene)s were verified by 1H NMR spectroscopy, viscometry of dilute solutions and the complex dynamic melt viscosity. The thermal properties of poly(ester-olefin)s were investigated by differential scanning calorimetry (DSC). The degree of crystallinity was also determined by DSC. The thermal and thermo-oxidative stability were investigated by thermogravimetric analysis (TGA). The rheological properties of poly(ester-olefin)s were investigated by dynamic mechanical spectroscopy in the melt and solid state.http://www.doiserbia.nb.rs/img/doi/0367-598X/2004/0367-598X0410444T.pdfthermoplastic elastomerspoly(ester-olefin)shydroxyl-terminated poly(ethylenestat-butylene)polycondensationthermal analysisrheology |
| spellingShingle | Tanasijević Branka Elkhaseh Salem F.K. Nikolić Marija S. Đonlagić Jasna A. Synthesis of thermoplastic poly(ester-olefin) elastomers Hemijska Industrija thermoplastic elastomers poly(ester-olefin)s hydroxyl-terminated poly(ethylenestat-butylene) polycondensation thermal analysis rheology |
| title | Synthesis of thermoplastic poly(ester-olefin) elastomers |
| title_full | Synthesis of thermoplastic poly(ester-olefin) elastomers |
| title_fullStr | Synthesis of thermoplastic poly(ester-olefin) elastomers |
| title_full_unstemmed | Synthesis of thermoplastic poly(ester-olefin) elastomers |
| title_short | Synthesis of thermoplastic poly(ester-olefin) elastomers |
| title_sort | synthesis of thermoplastic poly ester olefin elastomers |
| topic | thermoplastic elastomers poly(ester-olefin)s hydroxyl-terminated poly(ethylenestat-butylene) polycondensation thermal analysis rheology |
| url | http://www.doiserbia.nb.rs/img/doi/0367-598X/2004/0367-598X0410444T.pdf |
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