A novel method for synthesizing microspheres from lignin or lignin acrylate derivatives through copolymerization with styrene (St) and divinylbenzene (DVB) has been developed. The copolymers were obtained by the emulsion-suspension polymerization with a constant molar ratio of DVB to St of 1:1 (w/w) and different amounts of lignin or its derivatives. The morphologies of the obtained materials were examined by scanning electron microscopy. Two types of lignin modifications were performed to introduce vinyl groups into the lignin molecules: modification with acrylic acid and modification with epichlorohydrin plus acrylic acid. The course of modification was confirmed by attenuated total reflectance Fourier transform infrared spectroscopy. The thermal stability and degradation behavior of the obtained microspheres were investigated by thermogravimetric analysis, and the pore structure was characterized via nitrogen sorption experiments. Owing to the presence of specific functional groups and the well-developed pore structure, the obtained Lignin-St-DVB microspheres may have potential application as specific sorbents for the removal of phenolic pollutants from water, as demonstrated by the solid-phase extraction technique.
Nanoporous microspheres with divinylbenzene (DVB), styrene (St), and lignin were synthesized by an emulsion-suspension polymerization method. Several types of lignins were used: (1) kraft lignin before (L-unmod) and after modification with methacryloyl chloride (L-Met) and (2) low-molecularweight kraft lignin unmodified (LWL-unmod) and modified with methacrylic anhydride (LWL-Met). LWL was prepared by ultrafiltration of industrial black liquor using a ceramic membrane with a molecular weight (Mw) cut-off of 5 kDa. The synthesis was optimized by addition of different amounts of lignins. The microsphere texture was characterized using low-temperature nitrogen adsorption and small angle X-ray scattering analyses. The microspheres were nano-and mesoporous with a specific surface area in the range of 0.1-409 m 2 /g. The morphology of the copolymers was studied using field emission scanning electron microscopy and atomic force microscopy. The thermal properties were studied using differential scanning calorimetry and thermogravimetric analysis methods. A significant difference in the microsphere roughness is affected by lignins due to the presence of lignin nanoparticles at the surface of the microspheres. Molecular modeling was used to predict the sorption properties of the copolymers affected by various fields around the particles. The particle size, polydispersity and zeta potential of the St ? DVB, L-Met ? St ? DVB and L-unmod ? St ? DVB samples were measured by dynamic light scattering. Additionally, the point of zero charge of the samples was determined using potentiometric titration. The materials studied have a great potential for sorption processes due to their developed porosity and the presence of a number of active surface functionalities.
In this study, a novel method for the synthesis of hybrid, porous microspheres, including divinylbenzene (DVB), triethoxyvinylsilane (TEVS) and methacrylated lignin (L-Met), is presented. The methacrylic derivatives of kraft lignin were obtained by reaction with methacryloyl chloride according to a new experimental protocol. The course of the modification of lignin was confirmed by attenuated total reflectance (ATR-FTIR) and nuclear magnetic resonance (NMR) spectroscopy. The emulsion-suspension polymerization method was employed to obtain copolymers of DVD, TEVS and L-Met in spherical forms. The porous structures and morphologies of the obtained lignin-containing functionalized microspheres were investigated by low-temperature nitrogen adsorption data and scanning electron microscopy (SEM). The microspheres are demonstrated to be mesoporous materials with specific surface areas in the range of 430–520 m2/g. The effects of the lignin component on the porous structure, shape, swelling and thermal properties of the microspheres were evaluated.
Synthesis, copolymerization, and physicochemical properties of new, of different degrees of crosslinker tetrafunctional bis[4(2-hydroxy-3-methacryloyloxypropoxy)phenyl]sulfide and glycidyl methacrylate copolymers are presented. The monomers were used for the synthesis of porous microspheres in the presence of pore-forming diluents, decan-1-ol, and toluene. Influence of diluents composition on their porous structures was studied. Porous structure of the obtained microspheres in dry (from nitrogen adsorption-desorption measurements) states was studied. Their chemical structures were studied by the use of Fourier transform infrared. The number of epoxy groups of the obtained copolymers, their thermal properties (thermogravimetric analysis), and swelling characteristics in 10 solvents of different chemical nature were examined. Selected copolymers were modified by amines in the epoxide ring-opening reaction. V C 2011 Wiley Periodicals, Inc. J Appl Polym Sci 120: [3020][3021][3022][3023][3024][3025][3026] 2011
The synthesis, thermal, and mechanical properties of epoxy resin composites incorporating waste fibers of hemp were studied. Five different systems with increasing quantity of the eco-filler were obtained. For the synthesis of polymeric materials, the commercial epoxy resins Epidian® 5 and triethylenetetramine (TETA) were applied as crosslinking agents. The composites were obtained based on the polyaddition reaction of an amine group with an epoxide ring. ATR/FT-IR (Attenuated Total Reflection-Fourier Transform Infrared) analysis was used to confirm the chemical structure of the composites and the course of curing processes. Moreover, the influence of the eco-friendly components on the mechanical properties was determined, while thermal properties of the materials were investigated by thermogravimetry analysis (TGA) and differential scanning calorimetry (DSC). Dynamic mechanical studies (DMA) and Shore hardness tests of the obtained polymers were also carried out. The DSC curves and DMA analysis revealed that all materials were characterized by a similar glass transition range. Furthermore, the DMA and hardness measurements of the composites demonstrated an increasing elasticity with the increase in the amount of eco-filler present in the compositions.
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