Self-assembly and amphiphilic behavior of poly(ester)-block-poly(amide) diblock copolymer based on biodegradable poly(butylene succinate) and poly(2-pyrrolidone). (15th January 2022)

• Record Type: Journal Article
• Authors: Ono, Hideaki; Minamikawa, Hiroyuki; Nemoto, Koji; Yoshida, Masaru
• Is Part Of: European polymer journal. Volume 163(2022)
• Publication Date: 2022-01-15
• Subjects: Poly(butylene succinate) -- Polyamide 4 -- Diblock copolymer -- Lyotropic liquid crystal -- Self-assembly -- Emulsification; PBS-b-PA4 poly(butylene succinate)-block-poly(2-pyrrolidone) -- NMR nuclear magnetic resonance -- GPC gel permeation chromatography -- TG thermogravimetric -- DTA differential thermal analysis -- PBS polybutylene succinate -- PA4 poly(2-pyrrolidone) -- ROP ring-opening polymerization -- CLa ε-caprolactam -- PCLo poly(ε-caprolactone) -- PLA polylactides -- t-BuOK potassium tert-butoxide -- COMU (1-cyano-2-ethoxy-2-oxoethylidenaminooxy)dimethylamino-morpholinocarbenium hexafluorophosphate -- EDCIHCl 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride -- TEA triethylamine -- DMAP 4-dimethylaminopyridine -- TFA trifluoroacetic acid -- LiCl lithium chloride -- DMAc N, N-dimethylacetamide -- DIPEA N, N-diisopropylethylamine -- HFIP 1, 1, 1, 3, 3, 3-hexafluoro-2-propanol -- TCE 1, 1, 2, 2-tetrachloroethane -- DCM dichloromethane; Polymers -- Periodicals; Polymerization -- Periodicals; Polymères -- Périodiques; Polymérisation -- Périodiques; Polymerization; Polymers; Periodicals; Electronic journals; 547.705
• DOI: 10.1016/j.eurpolymj.2021.110961
• Languages: English
• ISSNs: 0014-3057

Abstract

Graphical abstract: Highlights: Designing and synthesizing poly(butylene succinate)-block-poly(2-pyrrolidone) Successful preparation and isolation of PBS- b -PA4 diblock copolymer confirmed. PBS- b -PA4 exhibited self-assembly and amphiphilic behavior. Promising candidate as a compatibilizer for PBS/PA4 resin binary blends. Abstract: In the present study, a novel poly(butylene succinate)-block-poly(2-pyrrolidone) (PBS- b -PA4 ) diblock copolymer was first designed and synthesized by condensing amino-terminal PBS and carboxyl-terminal PA4 at 100 °C under homogeneous conditions. The PBS- b -PA4 chemical structure was determined by combining nuclear magnetic resonance (NMR) spectroscopy and gel permeation chromatography (GPC) analysis, while the solid-state structure was investigated by wide-angle X-ray diffraction. In addition, the self-assembly behavior of the copolymer was studied by optical microscopy, NMR spectroscopy, and light scattering experiments using appropriate solvents. Both terminal groups of PBS- b -PA4 were well characterized, and the average molecular weight of PBS- b -PA4 was consistent with the sum of the precursors. The diffraction patterns also confirmed the presence of precursors. Micelle-like colloidal particles with an amide segment core and an ester segment corona were eventually observed in chloroform. Additionally, it was revealed that PBS- b -PA4 formed a birefringent and fluid liquid crystalline phase in 1, 1, 2, 2-tetrachloroethane. Thus, the emulsifying property was demonstrated in an immiscible two-liquid solution, indicating that the PBS- b -PA4 diblock copolymer is effective as an emulsifier at a comparable concentration of 1 g L -1 . Furthermore, the amphiphilic behavior of PBS- b -PA4 was attributed to the varying solubilities between the ester and amide segments. Thus, PBS- b -PA4 could be a promising candidate as a compatibilizer for PBS/PA4 resin binary blends.