Characterization of thermal properties of porous microspheres bearing pyrrolidone units

Journal of Thermal Analysis and Calorimetry, Nov 2014

Porous microspheres of glycidyl methacrylate(GMA) cross-linked with trimethylolpropane trimethacrylate (TRIM) were prepared with toluene as porogen by suspension–emulsion polymerization. In order to obtain adsorbents bearing functional groups, the porous methacrylate network was modified by subsequent reaction with pyrrolidone. The thermal behavior of the obtained material was studied using TG and DSC. It was found that the process of modification considerably changed the textural and thermal properties of the polymers.

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Characterization of thermal properties of porous microspheres bearing pyrrolidone units

M. Maciejewska 0 Porous polymers TG DSC 0 0 M. Maciejewska (&) Faculty of Chemistry, Maria Curie-Skodowska University , Pl. M. Curie-Skodowskiej 3, 20-031 Lublin , Poland Porous microspheres of glycidyl methacrylate(GMA) cross-linked with trimethylolpropane trimethacrylate (TRIM) were prepared with toluene as porogen by suspension-emulsion polymerization. In order to obtain adsorbents bearing functional groups, the porous methacrylate network was modified by subsequent reaction with pyrrolidone. The thermal behavior of the obtained material was studied using TG and DSC. It was found that the process of modification considerably changed the textural and thermal properties of the polymers. DBJH Microstructure Solubility parameter/(MPa)1/2 Pore diameter/A Temperature of final decomposition/ C Initial decomposition temperature/ C Pyrrolidone Specific surface area/m2g-1 Temperature of the first maximum rate of mass loss/ C Temperature of the second maximum rate of mass loss/ C Temperature of 20 % mass loss/ C Temperature of 50 % mass loss/ C The parent copolymer, molar ratio of trimethylolpropane trimethacrylate to glycidyl methacrylate equal 1:1 TRIM GMA2 TRIM GMA3 TRIM GMA4 TRIM GMA5 TRIM GMA1 ? P TRIM GMA2 ? P TRIM GMA3 ? P TRIM GMA4 ? P TRIM GMA5 ? P The parent copolymer, molar ratio of trimethylolpropane trimethacrylate to glycidyl methacrylate equal 1:2 The parent copolymer, molar ratio of trimethylolpropane trimethacrylate to glycidyl methacrylate equal 1:3 The parent copolymer, molar ratio of trimethylolpropane trimethacrylate to glycidyl methacrylate equal 1:4 The parent copolymer, molar ratio of trimethylolpropane trimethacrylate to glycidyl methacrylate equal 1:5 The copolymer modified with pyrrolidone, molar ratio of trimethylolpropane trimethacrylate to glycidyl methacrylate equal 1:1 The copolymer modified with pyrrolidone, molar ratio of trimethylolpropane trimethacrylate to glycidyl methacrylate equal 1:2 The copolymer modified with pyrrolidone, molar ratio of trimethylolpropane trimethacrylate to glycidyl methacrylate equal 1:3 The copolymer modified with pyrrolidone, molar ratio of trimethylolpropane trimethacrylate to glycidyl methacrylate equal 1:4 The copolymer modified with pyrrolidone, molar ratio of trimethylolpropane trimethacrylate to glycidyl methacrylate equal 1:5 Pore volume/cm3g-1 Porous polymers possess a number of distinguishing properties like highly developed internal structure, hydrophobic/ hydrophilic character, and the presence of various functional groups on the surface. These features make them very attractive from scientific and industrial point of view. Consequently, porous polymers are subject of many scientific investigations and have attracted the attention of producers. They are used as effective materials for many separation processes and various kinds of sorbents [19]. They can be obtained from numerous types of monomers as well as by modification of copolymers that contain reactive groups [1018]. One of the convenient routes to incorporate new functional group into polymer matrix is ring-opening reaction of oxirane ring with required agent. Widespread practice is reaction of epoxy group with amines [1922]. This process leads not only to the introduction of the active pendant group to the network but also to the changes in the textural and thermal properties of the newly obtained materials. Recently, we have described the synthesis and some properties of porous microspheres of glycidyl methacrylate (GMA) cross-linked with trimethylolpropane trimethacrylate (TRIM) modified with pyrrolidone [23]. It was of interest to investigate in detail, how the process of modification influences the thermal resistance of the newly formed copolymers. To achieve this goal, a set of ten copolymers was synthesized. The thermal properties of the parent and modified copolymers were evaluated by the means of TG and DSC. Additionally, the textural characterization was carried out on the basis of the low-temperature nitrogen adsorption on the studied copolymers. Experimental 2,3-Epoxypropyl methacrylate (GMA) and TRIM (Sigma Aldrich, Steinheim, Germany) were washed with 5 % aqueous sodium hydroxide in order to remove inhibitors. Pyrrolidone bis(2-ethylhexyl) sulfosuccinate sodium salt (DAC,BP) and a,a0-azoisobutyronitrile (AIBN), purchased from Fluka AG (Buchs, Switzerland), were used without purification. Toluene, n-dodecane, acetone, and methanol (reagent grade) were from POCh (Gliwice, Poland). Preparation of the GMATRIM microspheres Copolymerization was performed in an aqueous suspension medium. In a typical experiment, 195 mL of distilled water and 2.2 g of bis(2-ethylhexyl)sulfosuccinate sodium salt were stirred for 2 h at 80 C in order to dissolve the surfactant. Then the solution containing 15 g of monomers (GMA and TRIM), and 0.2 g of a,a0-azoisobutyronitrile dissolved in 22.5 mL of toluene was prepared and added while stirring to the aqueous medium. Molar ratios of GMA (...truncated)


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M. Maciejewska. Characterization of thermal properties of porous microspheres bearing pyrrolidone units, Journal of Thermal Analysis and Calorimetry, 2014, pp. 1147-1155, Volume 119, Issue 2, DOI: 10.1007/s10973-014-4250-0