Experimental Investigation of AGET ATRP Polymerization of Butyl Methacrylate in an Emulsion Stirred Tank Reactor

This study investigates ATRP emulsion polymerization of butyl methacrylate (BMA) in a 2-L stirred tank reactor using AGET as the initiation technique with ascorbic acid. The polymerization is performed in two step procedure using surfactant (Brij 98) in distilled water. The reaction is initiated by the catalyst CuBr2/dNbpy and initiator EBiB under a blanket of nitrogen to minimize air presence. An experimental design is performed to investigate the effects of the key variables: temperature, catalyst complex, surfactant and reducing agent. For reaction temperatures of 50°C, 60°C and 70°C, BMA conversion obtained is 63.9%, 70.2% and 85.8%, respectively. All other nine tests are done at 70°C for appropriate amounts of reactants. The results concluded that BMA conversion improves to 90% and the PDI increases slightly from 1.15 to 1.29 for more ascorbic acid. BMA conversion and PDI improve with less surfactant, but more ligand narrows MWD and reduces the catalyst activity.

Experimental Investigation of AGET ATRP Polymerization of Butyl Methacrylate in an Emulsion Stirred Tank Reactor

This study investigates ATRP emulsion polymerization of butyl methacrylate (BMA) in a 2-L stirred tank reactor using AGET as the initiation technique with ascorbic acid. The polymerization is performed in two step procedure using surfactant (Brij 98) in distilled water. The reaction is initiated by the catalyst CuBr2/dNbpy and initiator EBiB under a blanket of nitrogen to minimize air presence. An experimental design is performed to investigate the effects of the key variables: temperature, catalyst complex, surfactant and reducing agent. For reaction temperatures of 50°C, 60°C and 70°C, BMA conversion obtained is 63.9%, 70.2% and 85.8%, respectively. All other nine tests are done at 70°C for appropriate amounts of reactants. The results concluded that BMA conversion improves to 90% and the PDI increases slightly from 1.15 to 1.29 for more ascorbic acid. BMA conversion and PDI improve with less surfactant, but more ligand narrows MWD and reduces the catalyst activity.

Experimental Investigation of Emulsion AGET ATRP of MMA in a Stirred Tank Reactor

This study investigates the emulsion AGET ATRP of MMA in a 2-L reactor using the reactants: surfactant (Brij 98), catalyst complex (CuBr2/dNbpy), initiator (EBiB) and reducing agent (ascorbic acid). Preliminary trials demonstrate that the two-step procedure preserves the ATRP living features much better than the single-step procedure. An experimental design and statistical analysis were performed to investigate the main effects and two-factor interaction effects of temperature, surfactant, catalyst complex, initiator and reducing agent on the monomer conversion, average molecular weights and polydispersity index of the polymer. The input-output model predictions agree with experimental data. The results revealed that the temperature was the most influential factor for all three-process responses with 71.34%, 32.78% and 27.76 % contribution. However, the initiator was the least influential factor for both conversion and PDI with 0.035% and 0.13% contribution, whereas the surfactant was the least influential factor for molecular weight with 0.068% contribution

Experimental Investigation of Emulsion AGET ATRP of MMA in a Stirred Tank Reactor

This study investigates the emulsion AGET ATRP of MMA in a 2-L reactor using the reactants: surfactant (Brij 98), catalyst complex (CuBr2/dNbpy), initiator (EBiB) and reducing agent (ascorbic acid). Preliminary trials demonstrate that the two-step procedure preserves the ATRP living features much better than the single-step procedure. An experimental design and statistical analysis were performed to investigate the main effects and two-factor interaction effects of temperature, surfactant, catalyst complex, initiator and reducing agent on the monomer conversion, average molecular weights and polydispersity index of the polymer. The input-output model predictions agree with experimental data. The results revealed that the temperature was the most influential factor for all three-process responses with 71.34%, 32.78% and 27.76 % contribution. However, the initiator was the least influential factor for both conversion and PDI with 0.035% and 0.13% contribution, whereas the surfactant was the least influential factor for molecular weight with 0.068% contribution

Modelling and experimental investigation of ARGET/AGET atom transfer radical polymerization systems

Activators Generated by Electron Transfer (AGET) and Activators Regenerated by Electron Transfer (ARGET) Atom Transfer Radical Polymerization (ATRP) are emerging topics within the polymerization field. These techniques allow for better control over polymer structure and polymer size distributions than conventional polymerizations. However, investigations into these processes are lacking, especially from a modelling point of view. Therefore, a kinetic model of the ARGET ATRP of butyl methacrylate (BMA) in a solution medium and Hybrid Monte Carlo model of the AGET ATRP of butyl acrylate (BA) in a dispersed system were developed and compared with data. In addition, an experimental investigation of the AGET ATRP of BA was carried out to study the kinetic aspects of this polymerization. The results of these studies demonstrate that both models have relatively strong predictive powers, and that different kinetic regimes appear to be available within the dispersed system studied experientially.

Modelling and experimental investigation of ARGET/AGET atom transfer radical polymerization systems

Activators Generated by Electron Transfer (AGET) and Activators Regenerated by Electron Transfer (ARGET) Atom Transfer Radical Polymerization (ATRP) are emerging topics within the polymerization field. These techniques allow for better control over polymer structure and polymer size distributions than conventional polymerizations. However, investigations into these processes are lacking, especially from a modelling point of view. Therefore, a kinetic model of the ARGET ATRP of butyl methacrylate (BMA) in a solution medium and Hybrid Monte Carlo model of the AGET ATRP of butyl acrylate (BA) in a dispersed system were developed and compared with data. In addition, an experimental investigation of the AGET ATRP of BA was carried out to study the kinetic aspects of this polymerization. The results of these studies demonstrate that both models have relatively strong predictive powers, and that different kinetic regimes appear to be available within the dispersed system studied experientially.

Experimental Investigation of Methyl Methacrylate in Stirred Batch Emulsion Reactor: AGET ATRP Approach

This study examines the ab initio emulsion atom transfer radical polymerization (ATRP) initiated by an eco-friendly reducing agent to produce poly(methyl methacrylate) (PMMA) polymer with controlled characteristics in a 2 L stirred batch reactor. The effect of the reaction temperature, surfactant concentration, monomer to water ratio, and stirring speed was thoroughly investigated. The results showed that PMMA coagulation becomes quite severe at a certain temperature threshold. However, the coagulation could be avoided at mild reaction temperature, since the outcomes showed that loading more surfactant to the system under high mixing speed has balanced the polymer mixture and yielded high monomer conversion. The PMMA product was analyzed by gravimetry and GPC measurements and after 5 h of polymerization at a reaction temperature of 50 °C, monomer conversion of 64.1% was obtained, and PMMA polymer samples produced had an average molar mass of 4.5 kg/mol and a polydispersity index of 1.17. The structure of the PMMA polymer was successfully proved by FTIR and nuclear magnetic resonance (NMR) spectroscopy. The results confirm the living feature of MMA AGET ATRP in emulsion medium and recommend further investigation for other types of surfactant.