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then used as an initiator (the macroinitiator) together with CuX to polymerize monomer B. RAn X is usually isolated by precipitation with a nonsolvent or some other technique. The halogen-terminated macroinitiator is typically quite stable and can be stored for long periods prior to use in forming the second block. Both methods require that the polymerization of the rst monomer not be carried to completion, usually 90% conversion is the maximum conversion, because the extent of normal bimolecular termination increases as the monomer concentration decreases. This would result in loss of polymer chains with halogen end groups and a corresponding loss of the ability to propagate when the second monomer is added. The nal product would be a block copolymer contaminated with homopolymer A. Similarly, the isolated macroinitiator method requires isolation of RAn X prior to complete conversion so that there is a minimum loss of functional groups for initiation. Loss of functionality is also minimized by adjusting the choice and amount of the components of the reaction system (activator, deactivator, ligand, solvent) and other reaction conditions (concentration, temperature) to minimize normal termination. The one-pot sequential method has the disadvantage that the propagation of the second monomer involves a mixture of the second monomer plus unreacted rst monomer. The second block is actually a random copolymer. The isolated macroinitiator method is the method of choice to avoid this contamination of the second block. The isolated macroinitiator
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method often stops the conversion of the rst monomer at much less than 90%, sometimes as low as 50%, to save time. To go to the higher conversion, one needs to have more deactivator present to completely minimize normal termination, but this results in slower polymerization rates. Isolation of the macroinitiator at lower conversions allows the use of lower deactivator concentrations and faster polymerizations. Tri- and higher block copolymers, such as ABA, ABC, ABCB, can be synthesized by a continuation of the processes with the successive additions of the appropriate monomers. A symmetric block copolymer such as ABA or CABAC can be made ef ciently by using a difunctional initiator, such as, a, a-dichloro-p-xylene or dimethyl 2,6-dibromoheptanedioate, instead of the monofunctional initiator. For the ABA block copolymer only two, instead of three, monomer charges are needed:
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The exact sequence of monomer addition may be critical to success in producing the desired block copolymer. For example, does one add A rst or B rst to produce an AB block copolymer The answer depends on the reactivity of an AX chain end toward monomer B compared to the reactivity of a BX chain end toward monomer A:
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Either addition sequence works if the two monomers are in the same family (e.g., methyl acrylate and butyl acrylate or methyl methacrylate and butyl methacrylate or styrene and 4-acetoxystyrene), because the equilibrium constants (for activation) for both types of chain ends have about the same value. The situation is usually quite different for pairs of monomers from different families. Chain ends from monomers with large equilibium constants can initiate the polymerization of monomers with lower equilibrium constants; thus, cross-propagation is ef cient. Methacrylate works well as the rst monomer to form methacrylate acrylate and methacrylate styrene blocks. However, styrene or acrylate monomers are inef cient as the rst monomer to form those block copolymers. The problem is that there is a slow activation of styrene or acrylate chain ends, cross-propagation is fast (because methacrylate is very reactive), and subsequent activation of methacrylate chain ends is fast, resulting in considerable conversion of the second monomer before all the styrene or acrylate chain ends are activated all of which leads to increased polydispersity in methacrylate block lengths and molecular weight. If styrene or acrylate rst is the desired sequence for some reason, for instance, as the prelude to some other block sequence, it may be possible to achieve it by employing a halogen exchange. One starts polymerization of the acrylate or styrene monomer with a bromo initiator and CuBr. Prior to the addition of methacrylate, CuCl is added to convert bromo-terminated chain ends to chloro-terminated chain ends. The equilibrium constant for the latter is lower, activation and cross-propagation are slowed suf ciently that complete activation and crosspropagation are achieved before signi cant conversion of methacrylate occurs. Styrene acrylate block copolymers can be synthesized with either monomer as the rst monomer because the equilibium constants for acrylate and styrene chain ends are similar.
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