Aliphatic polyesters based on 1,4-butanediol and even numbered C4-C20 dicarboxylic acids-synthesis and properties including after surface treatment by VUV photo-oxidation

被引:2
|
作者
Demyttenaere, Shao M. [1 ]
Samonte, Jewel R. [1 ]
Reilly, Liam T. [1 ]
Andelija, Amina [1 ]
Strohm, Brian M. [1 ]
Kovach, Timothy [1 ]
Oakes, Sarah A. [1 ]
Keeley, Ryan P. [1 ]
Takacs, Gerald A. [1 ]
Miri, Massoud J. [1 ]
机构
[1] Rochester Inst Technol, Sch Chem & Mat Sci, Rochester, NY 14623 USA
关键词
Sustainable polymers; Renewable polymers; Biodegradable polymers; Polyester synthesis; LIPASE-CATALYZED SYNTHESIS; POLY(BUTYLENE SUCCINATE); MOLECULAR-WEIGHT; 1,12-DODECANEDIOIC ACID; ENZYMATIC DEGRADATION; POLYMORPHIC CRYSTALS; POLYCONDENSATION; TRANSFORMATION; HYDROLYSIS; POLYMERS;
D O I
10.1007/s10965-023-03693-8
中图分类号
O63 [高分子化学(高聚物)];
学科分类号
070305 ; 080501 ; 081704 ;
摘要
Aliphatic polyesters were synthesized from 1,4-butanediol and predominantly renewable dicarboxylic acids containing even numbered carbons from 4 to 20 (succinic acid to eicosanedioic acid). Melt polymerizations were conducted up to 220 ? with titanium tetrabutoxide as polymerization catalyst. Two polymerization methods were applied: (1) stoichiometrically equivalent amounts of diol and diacid with 14 hours under argon followed by 10 hours under reduced pressure, (2) a 10 mol % excess of diol, with 6 hours under the inert gas and 6 hours under reduced pressure. Molecular weight properties were determined by size exclusion chromatography in chloroform and polystyrene as calibration standards. For the polyesters with the C6 to C20 diacids, M-w obtained by Method 1 lied between 15,800 to 31,200 g/mol, and for Method 2 between 27,000 and 180,400 g/mol (average of M-w for PBS was 194,000 g/mol). H-1 NMR and C-13 NMR spectra of all polymers were obtained, peak assignments were made and the microstructure of the polymers was verified. In addition, peaks associated with end-groups were identified. Thermal properties of the polymers were determined by differential scanning calorimetry, dynamic mechanical analysis and thermal gravimetric analysis. For the polyesters obtained with C6 to C20 diacids, the highest T-g was 1.25 ? (from tan d) and the highest T-m was 88.8 ?, both with the C20 diacid. The polymers were also treated by vacuum ultraviolet (VUV) photo-oxidation as a plasma surface modification. The wettability of the original polymers and after their VUV photo-oxidation was measured by contact angle goniometry with water.
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  • [1] Aliphatic polyesters based on 1,4-butanediol and even numbered C4 - C20 dicarboxylic acids - synthesis and properties including after surface treatment by VUV photo-oxidation
    Shao M. Demyttenaere
    Jewel R. Samonte
    Liam T. Reilly
    Amina Andelija
    Brian M. Strohm
    Timothy Kovach
    Sarah A. Oakes
    Ryan P. Keeley
    Gerald A. Takacs
    Massoud J. Miri
    Journal of Polymer Research, 2023, 30