Atom transfer radical polymerization of n-butyl methacrylate in an aqueous dispersed system: A miniemulsion approach

High Molecular Weight Poly(butyl methacrylate) by Reverse Atom Transfer Radical Polymerization in Miniemulsion Initiated by a Redox System

“…The weight-average particle diameter was 82 nm with a standard deviation of 34 nm. The evolution of the molecular weight and the rate of the polymerization is consistent with earlier reports of copper-mediated ATRP in aqueous dispersed systems using nonionic surfactants. − ,−

1 Evolution of number-average molecular weight ( M n , filled symbols) and polydispersity index (PDI, open symbols) with conversion (a) and the kinetic plots (b) for the reverse atom transfer radical polymerization of butyl methacrylate (BMA) at 60 °C in miniemulsion. [Brij 98]:[hexadecane] = 10:3.8 wt % based on monomer; 15% solid content; [BMA] 0 :[copper(II) bromide tris[2-di(2-ethylhexyl acrylate)aminoethyl]amine (CuBr 2 -EHA 6 TREN)] 0 = 400:1; experiment 1: [CuBr 2 -EHA 6 TREN] 0 :[2,2‘-azobis[2-(2-imidazolin-2-yl)propane] dihydrochloride] 0 = 1:1; experiment 4: [CuBr 2 -EHA 6 TREN] 0 :[hydrogen peroxide (HPO)] 0 :[ascorbic acid (AA)] 0 = 1:0.25:0.25; experiment 5: [CuBr 2 -EHA 6 TREN] 0 :[HPO] 0 :[AA] 0 = 1:0.5:0.25; experiment 6: [CuBr 2 -EHA 6 TREN] 0 :[HPO] 0 :[AA] 0 = 1:1:0.25.

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High Molecular Weight Poly(butyl methacrylate) by Reverse Atom Transfer Radical Polymerization in Miniemulsion Initiated by a Redox System

“…The weight-average particle diameter was 82 nm with a standard deviation of 34 nm. The evolution of the molecular weight and the rate of the polymerization is consistent with earlier reports of copper-mediated ATRP in aqueous dispersed systems using nonionic surfactants. − ,−

1 Evolution of number-average molecular weight ( M n , filled symbols) and polydispersity index (PDI, open symbols) with conversion (a) and the kinetic plots (b) for the reverse atom transfer radical polymerization of butyl methacrylate (BMA) at 60 °C in miniemulsion. [Brij 98]:[hexadecane] = 10:3.8 wt % based on monomer; 15% solid content; [BMA] 0 :[copper(II) bromide tris[2-di(2-ethylhexyl acrylate)aminoethyl]amine (CuBr 2 -EHA 6 TREN)] 0 = 400:1; experiment 1: [CuBr 2 -EHA 6 TREN] 0 :[2,2‘-azobis[2-(2-imidazolin-2-yl)propane] dihydrochloride] 0 = 1:1; experiment 4: [CuBr 2 -EHA 6 TREN] 0 :[hydrogen peroxide (HPO)] 0 :[ascorbic acid (AA)] 0 = 1:0.25:0.25; experiment 5: [CuBr 2 -EHA 6 TREN] 0 :[HPO] 0 :[AA] 0 = 1:0.5:0.25; experiment 6: [CuBr 2 -EHA 6 TREN] 0 :[HPO] 0 :[AA] 0 = 1:1:0.25.

…”

Reverse atom transfer radical polymerization of butyl methacrylate in a miniemulsion stabilized with a cationic surfactant

“…Similarly to the experiment in which Brij 98 was used to stabilize the systems, all the experiments using CTAB (experiments 2-6) showed a rapid increase in the molecular weight at the beginning of the polymerization, a trend that is commonly reported in the reverse ATRP literature. 20,22,24 As expected, the amount of the surfactant influences the particle diameter in these systems. A decrease in the amount of CTAB results in an increase in the particle diameter of the final latex (Table 1, experiments 2-4).…”

“…The evolution of the molecular weight showed little dependence on the amount of CTAB added to the system. Similarly to the experiment in which Brij 98 was used to stabilize the systems, all the experiments using CTAB (experiments 2–6) showed a rapid increase in the molecular weight at the beginning of the polymerization, a trend that is commonly reported in the reverse ATRP literature 20, 22, 24. As expected, the amount of the surfactant influences the particle diameter in these systems.…”

Miniemulsion Living Free Radical Polymerization by RAFT

“…LRP in emulsion − and miniemulsion of different monomers was also reported by Matyjaszewski and co-workers, using ATRP as living mechanism. It was shown that, by a suitable choice of surfactant (nonionic) and initiator, it is possible to obtain stable latexes exhibiting a living behavior, as indicated by the almost linear growth of M n with conversion and the low P d values.…”

High Molecular Weight Poly(butyl methacrylate) by Reverse Atom Transfer Radical Polymerization in Miniemulsion Initiated by a Redox System

“…The weight-average particle diameter was 82 nm with a standard deviation of 34 nm. The evolution of the molecular weight and the rate of the polymerization is consistent with earlier reports of copper-mediated ATRP in aqueous dispersed systems using nonionic surfactants. − ,−

1 Evolution of number-average molecular weight ( M n , filled symbols) and polydispersity index (PDI, open symbols) with conversion (a) and the kinetic plots (b) for the reverse atom transfer radical polymerization of butyl methacrylate (BMA) at 60 °C in miniemulsion. [Brij 98]:[hexadecane] = 10:3.8 wt % based on monomer; 15% solid content; [BMA] 0 :[copper(II) bromide tris[2-di(2-ethylhexyl acrylate)aminoethyl]amine (CuBr 2 -EHA 6 TREN)] 0 = 400:1; experiment 1: [CuBr 2 -EHA 6 TREN] 0 :[2,2‘-azobis[2-(2-imidazolin-2-yl)propane] dihydrochloride] 0 = 1:1; experiment 4: [CuBr 2 -EHA 6 TREN] 0 :[hydrogen peroxide (HPO)] 0 :[ascorbic acid (AA)] 0 = 1:0.25:0.25; experiment 5: [CuBr 2 -EHA 6 TREN] 0 :[HPO] 0 :[AA] 0 = 1:0.5:0.25; experiment 6: [CuBr 2 -EHA 6 TREN] 0 :[HPO] 0 :[AA] 0 = 1:1:0.25.

…”

Reverse atom transfer radical polymerization of butyl methacrylate in a miniemulsion stabilized with a cationic surfactant

“…Similarly to the experiment in which Brij 98 was used to stabilize the systems, all the experiments using CTAB (experiments 2-6) showed a rapid increase in the molecular weight at the beginning of the polymerization, a trend that is commonly reported in the reverse ATRP literature. 20,22,24 As expected, the amount of the surfactant influences the particle diameter in these systems. A decrease in the amount of CTAB results in an increase in the particle diameter of the final latex (Table 1, experiments 2-4).…”

“…The evolution of the molecular weight showed little dependence on the amount of CTAB added to the system. Similarly to the experiment in which Brij 98 was used to stabilize the systems, all the experiments using CTAB (experiments 2–6) showed a rapid increase in the molecular weight at the beginning of the polymerization, a trend that is commonly reported in the reverse ATRP literature 20, 22, 24. As expected, the amount of the surfactant influences the particle diameter in these systems.…”

Miniemulsion Living Free Radical Polymerization by RAFT

“…LRP in emulsion − and miniemulsion of different monomers was also reported by Matyjaszewski and co-workers, using ATRP as living mechanism. It was shown that, by a suitable choice of surfactant (nonionic) and initiator, it is possible to obtain stable latexes exhibiting a living behavior, as indicated by the almost linear growth of M n with conversion and the low P d values.…”

High Molecular Weight Poly(butyl methacrylate) by Reverse Atom Transfer Radical Polymerization in Miniemulsion Initiated by a Redox System

“…The weight-average particle diameter was 82 nm with a standard deviation of 34 nm. The evolution of the molecular weight and the rate of the polymerization is consistent with earlier reports of copper-mediated ATRP in aqueous dispersed systems using nonionic surfactants. − ,−

1 Evolution of number-average molecular weight ( M n , filled symbols) and polydispersity index (PDI, open symbols) with conversion (a) and the kinetic plots (b) for the reverse atom transfer radical polymerization of butyl methacrylate (BMA) at 60 °C in miniemulsion. [Brij 98]:[hexadecane] = 10:3.8 wt % based on monomer; 15% solid content; [BMA] 0 :[copper(II) bromide tris[2-di(2-ethylhexyl acrylate)aminoethyl]amine (CuBr 2 -EHA 6 TREN)] 0 = 400:1; experiment 1: [CuBr 2 -EHA 6 TREN] 0 :[2,2‘-azobis[2-(2-imidazolin-2-yl)propane] dihydrochloride] 0 = 1:1; experiment 4: [CuBr 2 -EHA 6 TREN] 0 :[hydrogen peroxide (HPO)] 0 :[ascorbic acid (AA)] 0 = 1:0.25:0.25; experiment 5: [CuBr 2 -EHA 6 TREN] 0 :[HPO] 0 :[AA] 0 = 1:0.5:0.25; experiment 6: [CuBr 2 -EHA 6 TREN] 0 :[HPO] 0 :[AA] 0 = 1:1:0.25.

…”

Reverse atom transfer radical polymerization of butyl methacrylate in a miniemulsion stabilized with a cationic surfactant

“…Similarly to the experiment in which Brij 98 was used to stabilize the systems, all the experiments using CTAB (experiments 2-6) showed a rapid increase in the molecular weight at the beginning of the polymerization, a trend that is commonly reported in the reverse ATRP literature. 20,22,24 As expected, the amount of the surfactant influences the particle diameter in these systems. A decrease in the amount of CTAB results in an increase in the particle diameter of the final latex (Table 1, experiments 2-4).…”

“…The evolution of the molecular weight showed little dependence on the amount of CTAB added to the system. Similarly to the experiment in which Brij 98 was used to stabilize the systems, all the experiments using CTAB (experiments 2–6) showed a rapid increase in the molecular weight at the beginning of the polymerization, a trend that is commonly reported in the reverse ATRP literature 20, 22, 24. As expected, the amount of the surfactant influences the particle diameter in these systems.…”

Miniemulsion Living Free Radical Polymerization by RAFT

“…LRP in emulsion − and miniemulsion of different monomers was also reported by Matyjaszewski and co-workers, using ATRP as living mechanism. It was shown that, by a suitable choice of surfactant (nonionic) and initiator, it is possible to obtain stable latexes exhibiting a living behavior, as indicated by the almost linear growth of M n with conversion and the low P d values.…”