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In this study, the synthesis and characterization of permanently porous polymeric microspheres was presented. The microspheres were obtained via suspension polymerization using diverse functional monomers, such as 4,4′-bis(methacryloyloxymethylphenyl)sulphone, 1,4-bis(methacryloyloxymethyl)benzene, 4,4′-bis(methacryloyloxymethylphenyl)methane,  N -vinylpyrrolidone, ethylene glycol dimethacrylate, and divinylbenzene as a co-monomer. As porogenic solvents, toluene and chlorobenzene were applied. The main aim of the research was to synthesize polymers having a highly developed internal structure and a good thermal stability. The synthesized materials were characterized by ATR-FTIR, scanning electron microscopy, a size distribution analysis, a low-temperature nitrogen adsorption–desorption method, differential scanning calorimetry, and thermogravimetry coupled with FTIR and inverse gas chromatography. It was found that, depending on the functional monomer, regular microspheres with a specific surface area in the range of 418–746 m 2 /g can be successfully synthesized. Moreover, all the synthesized copolymers showed a good thermal stability. In helium, they exhibited 5% mass losses at temperatures over 300 °C, whereas in air these values were only slightly lower. In addition, the presence of miscellaneous functional groups promoted diverse kinds of interactions. Therefore, the microspheres can be possibly use in many adsorption techniques including high temperature processes.

Regular Polymeric Microspheres with Highly Developed Internal Structure and Remarkable Thermal Stability