Characterization of thermal properties of porous microspheres bearing pyrrolidone units

Maciejewska, Małgorzata

doi:10.1007/s10973-014-4250-0

Cited by 8 publications

(5 citation statements)

References 22 publications

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“…Next, the mixture of monomer/monomers (DVB, GMA, BM), pore forming diluent (toluene) and the initiator (AIBN) was prepared and poured to the dispersion medium, all details are collected in Table 1. The reaction mixture was stirred at 250 rpm for 18 h at 80 °C (Maciejewska 2015b). The obtained copolymers were washed in an ultrasonic bath successively with distilled water, methanol, hexane and again methanol (each solvent for half an hour).…”

Section: Synthesis Of Polymeric Microspheresmentioning

confidence: 99%

Analysis of structure and properties of DVB–GMA based porous polymers

Sobiesiak

2018

Adsorption

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Polar porous polymeric microspheres divinylbenzene-glycidyl methacrylate (DVB-GMA) were synthesized with a suspension method. Two kinds of polymers differing in chemical composition and physical properties were obtained. The molar ratios of monomers in the polymers were 50:50 and 75:25, respectively. Next, the prepared materials were chemically treated with phosphoric or sulphuric acid in order to additionally modify their surface. Consequently, the polymers gained acidic character and cation exchange properties. The prepared materials were characterized by: elemental analysis, ATR-FTIR, DSC, low temperature nitrogen sorption and SPE experiments. CHN and ATR-FTIR confirmed the chemical structures of the polymers. The DSC analyses revealed their network was highly cross-linked. Porous structure parameters of the studied materials strongly depended on their chemical composition. All the materials were mesoporous with bimodal pore size distribution (3.7 nm and 5.5-7.5 nm). Highly cross-linked DVB-GMA 75:25 and its acidic derivatives had twice higher specific surface areas (320-370 m 2 /g) than their less cross-linked counterparts DVB-GMA 50:50 (140-190 m 2 /g). The prepared materials were tested for the sorption of phenolic compounds (phenol, 2-chlorophenol, 2,4-dichlorophenol and 2,4,6-trichlorophenol) and popular pharmaceuticals-aspirin, paracetamol and ibuprofen. The process of dynamic sorption of phenols depended on both porous structure and surface chemistry of the polymers. And the less polar character of the polymeric surface was balanced by its higher porosity to maintain the sorption ability on the same level. In case of pharmaceuticals dependence of sorption properties on porosity and/or surface chemistry was more diversified and additionally chemical nature of adsorbate had to be taken into account.

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Section: Synthesis Of Polymeric Microspheresmentioning

confidence: 99%

Analysis of structure and properties of DVB–GMA based porous polymers

Sobiesiak

2018

Adsorption

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“…Such monomers include aliphatic methacrylates, like ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate (TRIM), or aromatic monomers, like the widely used divinylbenzene (DVB) [ 6 , 7 , 8 , 9 , 10 , 11 ]. On the other hand, the oxirane group introduced to the polymer structure by GMA can react with strong and weak nucleophiles, e.g., amines [ 12 , 13 , 14 , 15 ], which are reagents that allow the introduction of carboxyl groups [ 16 , 17 ], pyrrolidone [ 18 , 19 ] and many others. The modification with a reactive oxirane group is more demanding, but some functional groups, like a thiol group (-SH), can only be introduced into the microsphere structure in this way.…”

Section: Introductionmentioning

confidence: 99%

Thermal Characterization of Crosslinked Polymeric Microspheres Bearing Thiol Groups Studied by TG/FTIR/DSC under Non-Oxidative Conditions

Maciejewska,

Łastawiecka,

Grochowicz

2024

Materials

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This paper presents the thermal behavior of polymer microspheres based on glycidyl methacrylate (GMA) and crosslinking agents benzene-1,4-diylbis(2-methylprop-2-enoate) (1,4DMB) and trimethylolpropane trimethacrylate (TRIM) before and after functionalization with thioglycolic acid (TGA). The thermal stability of the polymers was determined using thermogravimetric analysis and differential scanning calorimetry under non-oxidizing conditions. The evolved gases were detected by FTIR and NMR spectroscopy, and the chemical structure of solid residues after preheating was assessed by FTIR/ATR spectroscopy. The post-functionalized microspheres showed higher thermal stability (within 270–290 °C) than the initial copolymers (within 240–250 °C). In this paper, examples of decomposition patterns of polymer microspheres before and after functionalization are presented. The decomposition of the initial microspheres starts with the emission of GMA monomers, acrolein, carbon dioxide, and the formation of unsaturated bonds in the solid residue. In the case of functionalized microspheres, degradation involves the transesterification of ester groups with the -SH groups, resulting in the emission of carbonyl sulfide, acrolein and carbon dioxide. Furthermore, lactone groups are created in the solid residue. The degradation of the functionalized copolymers is a complex process due to their crosslinked structure, rendering the identification of all the degradation products unattainable.

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“…In the case of polymers, the porosity is created already on an early stage of a synthesis by, e.g. control of crosslinking degree [36], using appropriate porogenic solvents [37,38] or hybrid monomer [7] or template [39]. The formation of the porous structure of carbon materials depends on the technique of their synthesis.…”

Section: Introductionmentioning

confidence: 99%

Investigations of the carbonization process of hybrid polymer microspheres using the TGA-EGA method: assessment of the impact of sulphanilic acid on the process

Sobiesiak,

Podkościelna,

Mazur

2024

J Therm Anal Calorim

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The TGA-EGA technique was used to study the influence of sulphanilic acid (SA) on the carbonisation process of the hybrid terpolymeric precursors composed of methacrylamide, divinylbenzene, and trimethoxyvinylsilane. The pristine polymers were impregnated with saturated solution of SA, dried, and carbonized at 600 °C under N2 atmosphere. The characteristic properties of both the pristine hybrid polymers and the resulting carbons were based on FTIR, Raman, and PXRD analyses, which revealed the materials were composed of amorphous polymeric or carbon phase interpenetrated by silica/silicate disordered network. The porosimetric analysis showed the resulted carbons possessed homogeneous supermicropores with the average pore width of 0.7 nm and reduced number of mesopores compared to pristine precursors. From the TGA results, it was followed that impregnated polymers decomposed in two stages, instead of one like pristine precursors did. Moreover, IDT of impregnated polymers was reduced by about 100 °C, and their Tmax was increased by 2–5.5 °C. Their decomposition proceeded slower by 22–37% that caused increase in efficiency of the process by 10–48%. The EGA showed the decomposition of the impregnated precursors started from the degradation of the amide groups, then SA destruction took place, followed by further decomposition of the polymer. The studies led to the conclusion that SA had the protective effect on the surface of the carbonized polymers. During impregnation and thermal treatment, SA produced a deposit in pores of the precursors. This resulted in narrowing of the pore width, delaying and slowing down the polymer thermal decomposition process, as well as increasing its efficiency.

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Characterization of thermal properties of porous microspheres bearing pyrrolidone units

Cited by 8 publications

References 22 publications

Analysis of structure and properties of DVB–GMA based porous polymers

Analysis of structure and properties of DVB–GMA based porous polymers

Thermal Characterization of Crosslinked Polymeric Microspheres Bearing Thiol Groups Studied by TG/FTIR/DSC under Non-Oxidative Conditions

Investigations of the carbonization process of hybrid polymer microspheres using the TGA-EGA method: assessment of the impact of sulphanilic acid on the process

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