Table 1.
Composition of Organic and Aqueous Phases in a Typical Miniemulsion Polymerizationa
| component | weight (g) | comments |
|---|---|---|
| organic phase | ||
| BA | 7.12 | 20 vol% (18 wt%) to total |
| Ethyl α-bromoisobutyrate (EBiB) | 0.039b | [BA]/[EBiB] = 280/1 |
| Hexadecane (HD) | 0.77 | 10.8 wt% to BA |
| aqueous phase | ||
| Water | 32 | Distilled water |
| SDSc | 0.44 | 6.2 wt% to BA |
| NaBr | 0.41 | [NaBr] = 0.1 M |
| CuIIBr2 | 8.9×10−3 | 1 mM with respect to Vtot |
| TPMAc | 0.023 | [CuIIBr2]/[L] = 1/2 |
Polymerization conditions: T = 65 °C; working electrode = Pt mesh with area ≈ 6 cm2; counter electrode = Pt mesh separated from reaction mixture by methylcellulose gel saturated with (C2H5)4NBF4; reference electrode = Ag/AgI/0.1 M (n-C4H9)4NI;
Initiator concentration, [EBiB], was varied to target different degrees of polymerization (DP);
Other employed surfactants and copper ligands are listed in Scheme 2; tris(2-pyridylmethyl)amine (TPMA), 1-(4-methoxy-3,5-dimethylpyridin-2-yl)-N-((4-methoxy-3,5-dimethylpyridin-2-yl)methyl)-N-(pyridin-2-ylme-thyl)methanamine (TPMA*2), tris[2-(dimethylamino)ethyl]amine (Me6TREN), N,N-bis(2-pyri-dylmethyl)-2-hydroxyethylamine (BPMEA), and bis[2-(4-methoxy-3,5-dimethyl)pyridyl-methyl]octadecylamine (BPMODA*).