The Properties of Poly(l-Lactide) Prepared by Different Synthesis Procedure

• Published in: Journal of polymers and the environment 2011-06, Vol.19 (2), p.419-430
• Main Authors: Ristic, Ivan S, Tanasic, Ljiljana, Nikolic, Ljubisa B, Cakic, Suzana M, Ilic, Olivera Z, Radicevic, Radmila, Budinski-simendic, Jaroslava K
• Format: Article
• Language: English
• Subjects: Biodegradable materials; Calorimetry; Chemical synthesis; Chemistry; Chemistry and Materials Science; Environmental Chemistry; Environmental Engineering/Biotechnology; Fourier transforms; High pressure; Industrial Chemistry/Chemical Engineering; Infrared; Initiators; Materials Science; Microwaves; NMR; Nuclear magnetic resonance; Original Paper; Polymer Sciences; Polymerization; Polymers; Reactors; Synthesis; Thermal properties; Vessels
• ISSN: 1566-2543; 1572-8919; 1572-8900
• DOI: 10.1007/s10924-011-0297-1

Different synthesis methods were applied to determine optimal conditions for polymerization of ( 3S )- cis -3,6-dimethyl-1,4-dioxane-2,5-dione ( l -lactide), in order to obtain poly( l -lactide) (PLLA). Bulk polymerizations (in vacuum sealed vessel, high pressure reactor and in microwave field) were performed with tin(II) 2-ethylhexanoate as the initiator. Synthesis in the vacuum sealed vessel was carried out at the temperature of 150 °C. To reduce the reaction time second polymerization process was carried out in the high pressure reactor at 100 °C and at the pressure of 138 kPa. The third type of rapid synthesis was done in the microwave reactor at 100 °C, using frequency of 2.45 GHz and power of 150 W at the temperature of 100 °C. The temperature in this method was controlled via infrared system for in-bulk measuring. The solution polymerization (with trifluoromethanesulfonic acid as initiator) was possible even at the temperature of 40 °C, yielding PLLA with narrow molecular weight distribution in a very short period of time (less than 6 h). The obtained polymers had the number-average molecular weights ranging from 43,000 to 178,000 g mol −1 (polydispersity index ranging from 1 to 3) according to the gel permeation chromatography measurements. The polymer structure was characterized by Fourier transform infrared and NMR spectroscopy. Thermal properties of the obtained polymers were investigated using thermogravimetry and differential scanning calorimetry.