An ultrasonic condition assisted phase transfer catalyzed radical polymerization of methyl methacrylate was investigated in an ethyl acetate/water two phase system at 60±1°C and 25kHz, 300W under inert atmosphere. The influence of monomer, initiator, catalyst and temperature, volume fraction of aqueous phase on the rate of polymerization was examined in detail. The reaction order was found to be unity for monomer, initiator and catalyst. Generally, the reaction rate was relatively fast in two phase system, when a catalytic amount of phase transfer catalyst was used. The combined approach, use of ultrasonic and PTC condition was significantly enhances the rate of polymerization. An ultrasonic and phase transfer catalyzed radical polymerization of methyl methacrylate has shown about three fold enhancements in the rate compared with silent polymerization of MMA using cetyltrimethylammonium bromide as PTC. The resultant kinetics was evaluated with silent polymerization and an important feature was discussed. The activation energy and other thermodynamic parameters were computed. Based on the obtained results an appropriate radical mechanism has been derived. TGA showed the polymer was stable up to 150°C. The FT-IR and DSC analysis validates the atactic nature of the obtained polymer. The XRD pattern reveals the amorphous nature of polymer was dominated.
This work establishes the kinetics of radical polymerization of methyl methacrylate in an aqueous-organic two-phase system using 1,4-bis (triethylmethylammonium) benzene dichloride (TEMABDC) as multi-site phase transfer catalyst and potassium peroxydisulphate (K 2 S 2 O 8 ) as water-soluble initiator at 60 ± 1°C under nitrogen atmosphere. The role of concentrations of monomer, initiator, catalyst, acid and ionic strength, temperature and volume fraction of aqueous phase on the rate of polymerization (R p ) was investigated. . The rate of polymerization increases with an increase in the concentration of monomer, initiator, catalyst and temperature. A generalized reaction model was developed to explain the phase transfer catalyzed polymerization reaction. Based on the kinetic results, radical mechanism has been derived. The activation energy and other thermodynamic parameters were calculated. The FT-IR spectroscopy validates a band of 1732 cm -1 of ester group of the obtained polymer. The viscosity average molecular weight of the PMMA was found 1.6955 9 10 4 g/mol.
An ultrasound condition associated with phasetransfer catalyst (PTC) has great diverse applications in synthesis of various organic and polymeric materials because of its fast reaction and high yield in short period of time. Phase transfer catalyst (cetyltrimethylammonium bromide as PTC) extracts the reactive radical anion from aqueous phase and transfer to organic phase whilst ultrasound condition enhances the radical formation; consequently, acrylonitrile was polymerized in ethyl acetate/ water two-phase system at 60 ± 1°C under ultrasound (25 kHz/300 W) and silent condition. The rate of polymerization (R p ) was doubled under ultrasound compare to silent condition. The various experimental parameters such as monomer, initiator, catalyst and temperature, solvent polarity on the rate of polymerization was studied in both conditions. The activation energy (E a ) and other thermodynamic parameters were calculated. The E a value of ultrasound condition supports the enhancement of rate of polymerization. On the basis of observed results, a suitable kinetic model, mechanism and effect of ultrasound in the rate of polymerization were discussed. The obtained polymer was analyzed by TG/DTA and FT-IR. The viscosity average molecular weight of the polymer was found to be 6.8526 9 10 4 g mol -1 .
Methyl and ethyl methacrylate was polymerized in heterogeneous system with the help of newly synthesized multi-site phase-transfer catalyst and using water-soluble initiator at 60 ± 1 °C under unstirred inert atmospheric condition. Polymer yield was increased with increasing molar concentrations of monomer, initiator, catalyst and temperature. Polymerization follows first-order kinetics with respect to monomer and half-order with respect to catalyst and initiator, respectively. PTC has myriads of applications in the synthesis of various organic and polymeric materials because of its fast reaction and high yield in short period of time. Without addition of PTC, polymerization did not occur; this indicates that catalyst plays the pivotal role on initiation of polymerization. It extracts the reactive radical anion from aqueous phase and transfers to the organic phase where acrylates were polymerized. Polymerization reactivity of methyl and ethyl methacrylate under PTC conditions was studied by various parameters. The activation energy (Ea) and other thermodynamic parameters were calculated. The Ea value supports the reactivity of acrylates. The results obtained from this investigation were used for inferring the radical mechanism of phase-transfer-catalyzed polymerization. The obtained polymers were analyzed by spectral and thermal analyses.
Carbazole-containing motifs are of most desired materials because of its wide range of applications due to π-extended systems, molecular and optical properties was easily tunable via diverse structural modifications. Herein, we reported an efficient and facile polymerization of N-vinyl carbazole (NVK) using multi-site phase transfer catalyst with and without ultrasound condition. The rate of polymerization (Rp) was effectively improved with ultrasound in short time on compare with silent condition. Role of different parameters such as variation of frequency, monomer, initiator, catalyst and temperature, solvents, aqueous and pH on the rate of polymerization of NVK was explored under silent and ultrasound condition (45 kHz/550 W). Activation energy of polymerization was supported for an enhancement of rate under ultrasound condition. From the experimental results, an appropriate kinetic model and role of various parameters in polymerization reaction was discussed. The obtained poly (N-vinyl carbazole) was confirmed and characterized by FT-IR, 1 H NMR, TGA and XRD techniques.
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