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A series of novel multifunctional initiators derived from adamantane-based derivatives have been used in the syntheses of various styrenic and (meth)acrylic star polymers by atom transfer radical polymerization (ATRP). Conditions were identified in each system to produce star polymers with nearly monomodal molecular distributions. These synthesized star polymers have glass transition temperatures...
Atom transfer radical suspension polymerization (suspension ATRP) of methyl methacrylate (MMA) was carried out using 1-chloro-1-phenylethane (1-PECl) as initiator, copper chloride/bipyridine (CuCl/bpy) as catalyst. The polymerization was accomplished with a mechanical agitator under the protection of nitrogen atmosphere. Apart from the dispersing agent (1% PVA), NaCl was also used in the water phase...
We report on the synthesis of an azobenzene-containing inimer 6-{4-[4-(2-(2-bromoisobutyryloxy)hexyloxy)phenylazo]phenoxy}hexyl methacrylate (I) and used it to prepare hyperbranched homopolymer and copolymers by self-condensing vinyl polymerization (SCVP) and copolymerization (SCVCP) with its precursor 6-{4-[4-(6-hydroxyhexyloxy)phenylazo]phenoxy}hexyl methacrylate (M) using atom transfer radical...
The ATRP of methyl methacrylate (MMA) with the system of FeCl 2 .4H 2 O, N,N,N',N'',N''-penta(methyl acylate)diethylenetriamine (MA 5 -DETA) and ethyl 2-bromoisobutyrate (EBiB) showed high activity and is not well-controlled. The addition of a certain amount of FeCl 3 .6H 2 O as the additive into the above system results in the decrease of the polymerization...
A series of P[(HEMA-TMS)-co-PEOMA] graft copolymers with different amounts of incorporated macromonomer grafts were prepared by copolymerization of a PEO macromonomer (PEOMA, MW av =1100g/mol, DP PEO =23) with 2-(trimethylsilyloxy)ethyl methacrylate (HEMA-TMS) using various initial ratios of the comonomers via atom transfer radical polymerization. After transformation of the HEMA-TMS...
This communication describes a novel strategy to synthesize binary mixed homopolymer brushes from mixed self-assembled monolayers (SAMs) on silica substrates by combining atom transfer radical polymerization (ATRP) and nitroxide-mediated radical polymerization (NMRP). Mixed SAMs terminated by ATRP and NMRP initiators were prepared by coadsorption of two corresponding organotrichlorosilanes from toluene...
A convenient, one-pot synthesis of telechelic and semi-telechelic polyacrylates with unsaturated end-groups has been developed. Atom transfer radical polymerization of methyl or n-butyl acrylate was initiated with either ethyl α-bromomethylacrylate or methyl dichloroacetate, as a monofunctional or difunctional initiator, respectively, and mediated with various Cu/amine complexes. Addition of excess...
Block copolymers, poly(LLA-b-St)s and triblock copolymes, poly(LLA-b-St-b-MMA)s have been synthesized by the combination of the atom transfer radical polymerization (ATRP) with ring-opening polymerization (ROP) using bifunctional initiator β-hydroxylethyl α-bromoisobutyrate (HEBIB) without intermediate function transformation. The molecular weight (MW) and the molecular weight distribution (MWD) can...
A series of diblock, triblock and star-block copolymers composed of polystyrene and poly(acrylic acid) were synthesized by ATRP. The structure of the copolymers, the size of the blocks and the composition were varied, keeping however a short polystyrene block and a poly(acrylic acid) content larger than 60mol% to allow solubility in alkaline water. Their micellization was studied by static and dynamic...
Star-polymers with arm numbers ranging from 3 to 10 have been synthesized and characterized by conventional GPC and GPC-light-scattering. The GPC elution behavior of the stars was studied and compared with predictions from computer simulations. The comparison of simulated and experimental data shows reasonable agreement if the arms are sufficiently long. Thus, using computer simulations GPC calibration...
Fluorescent PMMAs containing a phthalic anhydride (PA) group at the chain ends were prepared using the newly developed initiator 7 by atom transfer radical polymerization and subsequent pyrolysis. These polymers allowed for the detection of inter-macromolecular reaction in reactive polymer blends at a low concentration by the use of fluorescence-gel permeation chromatography. The PA-amine coupling...
A multifunctional initiator for ATRP has been synthesized by reacting a hyperbranched polyether, based on 3-ethyl-3-(hydroxymethyl)oxetane, with 2-bromo-isobutyrylbromide. The macroinitiator contained approximately 25 initiating sites per molecule. It was used for the atom transfer radical polymerization of methyl acrylate mediated by Cu(I)Br and tris(2-(dimethylamino)ethyl)amine (Me 6 -TREN)...
Two series of semifluorinated fluorocarbon diblock copolymer poly(butyl methacrylate-co-perfluoroalkyl acrylate) have been synthesized by atom transfer radical polymerization (ATRP). The 1 H NMR, F-EA, GPC and FTIR were used to characterize copolymer structure. Contact angle measurements on the thin polymer films showed low critical surface tensions and low dispersion force contributions to...
Patterned films of a low-polydispersity polymer densely end-grafted on a silicon substrate were fabricated for the first time by the combined use of electron beam (EB) lithography and living radical polymerization; a focused EB was scanned on an initiator-immobilized substrate to selectively bombard and decompose the initiator, and then the EB-induced pattern was amplified by the atom transfer radical...
The synthesis of poly{2,5-bis[(4-methoxyphenyl)oxycarbonyl]styrene} (PMPCS) with different molecular weight and low polydispersity was achieved by atom transfer radical polymerization in methoxybenzene solution using 1-bromoethylbenzene as an initiator and CuBr/sparteine complex as a catalyst. The concentration of the living centers throughout the polymerization was found to be constant. The liquid-crystalline...
Novel asymmetric difunctional initiators 2-phenyl-2-[(2,2,6,6-tetramethylpiperidino)oxy]ethyl 2-bromo-2-methyl propanoate and of 2-phenyl-2-[(2,2,6,6-tetramethylpiperidino)oxy]ethyl 2-bromo propanoate were synthesized in a three-step reaction sequence and used in atom transfer radical polymerization (ATRP) of methyl methacrylate or tert-butyl acrylate leading to corresponding polymer with tempo moiety...
The atom transfer radical polymerization (ATRP) technique using the copper halide/sparteine complexes was applied to the graft polymerization of methyl methacrylate on a porous glass filter on which the initiator, 2-(4-chlorosulfonylphenyl) ethyltrichlorosilane, was immobilized by chemisorption. The graft chains were cleaved from the glass filter by the HF treatment in the presence of a phase transfer...
A series of semifluorinated fluorocarbon/hydrocarbon di- and triblock copolymers were prepared by atom transfer radical polymerization (ATRP). The mono- and difunctional macroinitiators, which were obtained from bulk ATRP of styrene, butyl acrylate and methyl acrylate, initiated solution ATRP of 2-[(perfluorononenyl)oxy]ethyl methacrylate and ethylene glycol mono-methacrylate mono-perfluorooctanoate,...
The atom transfer radical polymerization (ATRP) of styrene and methyl methacrylate with differently substituted model and macroinitiators was performed, in order to evaluate qualitatively the structural features which affect the efficiency of the initiation step. It was found that substituents which stabilize radicals enhance the dissociation of the halogen atom and lead to high initiation efficiencies...
The synthesis of poly(styrene-dimethylsiloxane) block and graft copolymers is described. Commercially available difunctional poly(dimethylsiloxane) (PDMS) containing either vinylsilyl or hydrosilyl terminal species was reacted with the corresponding hydrosilyl or vinylsilyl attachable initiators containing the benzyl chloride species. The attachment of the initiators to PDMS was achieved by hydrosilation...
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