tert-Butyl hydroperoxide → Butyl prop-2-enoate;styrene

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Sixteen stable free radical polymerization (SFRP) were carried out under aqueous emulsion conditions. Each polymerization was set up with a total volume 0.7 mL, with 10 weight % styrene (monomer). The amount of surfactant (sodium alpha (C14-C16) olefin sulfonate—sold by Rhodia as Rhodacal A-246/L) added was 1 weight % to monomer, and two different amounts of initiator were added: 0.001 and 0.002 mole equivalence to monomer. The initiator that was used was water soluble and was tert-butylhydroperoxide (TBHP). For each initiator concentration the series of seven polymerizations differed in the amount of control agent added, with the first well getting 0.6 mole equivalence control agent and the last well getting 1.2 mole equivalence of control agent, with even steps of 0.1 mole equivalence (the control agent used was 2,2,5-trimethyl-4-phenyl-3-azahexane-3-nitroxide—“α-hydrido-nitroxide”). In addition a polymerization reaction without control agent was conducted for each amount of initiator. After the predetermined heating and agitation time of 90° C. and 30 h the reactor vessels were opened and a small aliquot was taken from each vessel for analysis. Subsequently, an amount of n-butylacrylate equal to the amount of styrene previously added (10 wt %) was dispensed to each vessel. The vessels were then resealed and heated at 90° C. and mixed for an additional 30 h. Subsequently the reaction mixtures were worked up and characterized using the standard procedure outlined for polymerization experiments at the beginning of the Example section.

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