Abstract:The influence of phenylacetic acid hydrazide (NAPAH) derivative content, melt temperature (170−200°C) and cooling rate (1−20°C/min) on poly (L-lactide) (PLLA) nucleation were investigated. Increasing the content of NAPAH (0.5−3.0 wt.%) had a positive effect on PLLA crystallization, while an increase in the cooling rate and heating temperature had a negative effect. In the case of isothermal crystallization carried out for a long time (180 min), the melting process depended only on the crystallization temperatu… Show more
“…NCAPH's synthesis pathway is shown in Figure .1. The synthetic procedure is similar to that of other compounds reported by our research group [32,40], and there are two main reason steps, they are acylation and amination reaction. The resulting NCAPH is characterized by 1 H Nuclear Magnetic Resonance ( 1 H NMR) and Fourier Transform Infrared Spectrometer (FT-IR), the detailed characterization data are as follows: FT-IR (KBr) υ: 3379.9 cm -1 (the stretching vibrations absorption of N-H), 3257.7 cm -1 (C-H stretching vibration of 2-pyridine), 1678.1 cm -1 (the stretching vibration absorption of C=O which is near naphthalene), 1652.4 cm -1 (the stretching vibration absorption of C=O which is near 2-pyridine), 1590.7, 1570.3, 1490 and 1464.1 cm -1 (the vibration absorption of C-C of naphthalene and pyridine), 1515.6 cm −1 (N-H bending vibration absorption), 1328.7 cm −1 (the mixed absorption about bending vibration of N-H and stretching vibration of C-N), 1140.7 cm -1 (the stretching vibration of C-H of naphthalene), 998.5 cm -1 (the stretching vibrations absorption of C-C which located in C=O and naphthalene), 859.2 cm -1 (the out-of-plane bending vibration absorption of C-H of naphthalene).…”
Melt processing poly(L-lactide) (PLLA) with a nucleating agent has been thought to be one of the most effective route to enhance PLLA s crystallization and heat resistance. In the current work, a newly-developed organic nucleating agent named N, N -bis(2-picolinyl) 1, 4-naphthalenedicarboxylic acid dihydrazide (NCAPH) was synthesized to investigate its effects on PLLA�s crystallization and melting behaviors. It is proved that NCAPH as an organic crystallization nucleating agent could provide large number of crystallization nucleation sites to improve PLLA�s crystallization, as observed from DSC and POM measurements. The result from melt-crystallization processes further showed that the final melting temperature and cooling rate were two important factors for affecting PLLA�s melt-crystallization behaviors in cooling, and the theoretical calculation result of frontier orbital energy indicated there existed probable intermolecular interaction between N-H of NCAPH and C=O of PLLA, which was proposed as nucleation mechanism of NCAPH for promoting PLLA�s crystallization. The melting behaviors of PLLA/NCAPH after non-isothermal crystallization or isothermal crystallization further confirmed the positive effects of NCAPH and NCAPH�s loading for the crystallization of PLLA, meantime, the melting behaviors depended on the heating rate, crystallization temperature, crystallization time, etc.
“…NCAPH's synthesis pathway is shown in Figure .1. The synthetic procedure is similar to that of other compounds reported by our research group [32,40], and there are two main reason steps, they are acylation and amination reaction. The resulting NCAPH is characterized by 1 H Nuclear Magnetic Resonance ( 1 H NMR) and Fourier Transform Infrared Spectrometer (FT-IR), the detailed characterization data are as follows: FT-IR (KBr) υ: 3379.9 cm -1 (the stretching vibrations absorption of N-H), 3257.7 cm -1 (C-H stretching vibration of 2-pyridine), 1678.1 cm -1 (the stretching vibration absorption of C=O which is near naphthalene), 1652.4 cm -1 (the stretching vibration absorption of C=O which is near 2-pyridine), 1590.7, 1570.3, 1490 and 1464.1 cm -1 (the vibration absorption of C-C of naphthalene and pyridine), 1515.6 cm −1 (N-H bending vibration absorption), 1328.7 cm −1 (the mixed absorption about bending vibration of N-H and stretching vibration of C-N), 1140.7 cm -1 (the stretching vibration of C-H of naphthalene), 998.5 cm -1 (the stretching vibrations absorption of C-C which located in C=O and naphthalene), 859.2 cm -1 (the out-of-plane bending vibration absorption of C-H of naphthalene).…”
Melt processing poly(L-lactide) (PLLA) with a nucleating agent has been thought to be one of the most effective route to enhance PLLA s crystallization and heat resistance. In the current work, a newly-developed organic nucleating agent named N, N -bis(2-picolinyl) 1, 4-naphthalenedicarboxylic acid dihydrazide (NCAPH) was synthesized to investigate its effects on PLLA�s crystallization and melting behaviors. It is proved that NCAPH as an organic crystallization nucleating agent could provide large number of crystallization nucleation sites to improve PLLA�s crystallization, as observed from DSC and POM measurements. The result from melt-crystallization processes further showed that the final melting temperature and cooling rate were two important factors for affecting PLLA�s melt-crystallization behaviors in cooling, and the theoretical calculation result of frontier orbital energy indicated there existed probable intermolecular interaction between N-H of NCAPH and C=O of PLLA, which was proposed as nucleation mechanism of NCAPH for promoting PLLA�s crystallization. The melting behaviors of PLLA/NCAPH after non-isothermal crystallization or isothermal crystallization further confirmed the positive effects of NCAPH and NCAPH�s loading for the crystallization of PLLA, meantime, the melting behaviors depended on the heating rate, crystallization temperature, crystallization time, etc.
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