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See detailPrecision synthesis of poly(ionic liquid)-based block copolymers by cobalt-mediated radical polymerization and preliminary study of their self-assembling properties
Coupillaud, Paul; Fèvre, Maréva; Wirotius, Anne-Laure et al

in Macromolecular Rapid Communications (2014), 35(4), 422-430

A poly(ionic liquid)-based block copolymer (PIL BCP), namely, poly(vinyl acetate)-b-poly(N-vinyl-3-butylimidazolium bromide), PVAc-b-PVBuImBr, is synthesized by sequential cobalt-mediated radical ... [more ▼]

A poly(ionic liquid)-based block copolymer (PIL BCP), namely, poly(vinyl acetate)-b-poly(N-vinyl-3-butylimidazolium bromide), PVAc-b-PVBuImBr, is synthesized by sequential cobalt-mediated radical polymerization (CMRP). A PVAc precursor is first prepared at 30 °C in bulk by CMRP of VAc, using bis(acetylacetonato)cobalt(II), Co(acac)2, and a radical source (V-70). Growth of PVBuImBr from PVAc-Co(acac)2 is accomplished by CMRP in DMF/MeOH (2:1, v/v). This PIL BCP self-assembles in the sub-micron size range into aggregated core–shell micelles in THF, whereas polymeric vesicles are observed in water, as evidenced by dynamic light scattering (DLS) and transmission electron microscopy (TEM). Thin-solid sample cut from raw materials analyzed by TEM shows an ordered lamellar organization by temperature-dependent synchrotron small-angle X-ray scattering (SAXS). Anion exchange can be accomplished to achieve the corresponding PIL BCP with bis(trifluorosulfonyl)imide (Tf2N−) anions, which also gives rise to an ordered lamellar phase in bulk samples. A complete suppression of SAXS second-order reflection suggests that this compound has a symmetric volume fraction (f ≈ 0.5). SAXS characterization of both di- and triblock PIL BCP analogues previously reported also shows a lamellar phase of very similar behavior, with only an increase of the period by about 8% at 60 °C. [less ▲]

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See detailThermoreversibly crosslinked poly(ε-caprolactone) as recyclable shape-memory polymer network
Defize, Thomas ULg; Riva, Raphaël ULg; Raquez, Jean-Marie et al

in Macromolecular Rapid Communications (2011), 32(16), 1264-1269

A new concept to build shape memory polymers (SMP) combining outstanding fixity and recovery ratios (both above 99% after only one training cycle) typical of chemically crosslinked SMPs with ... [more ▼]

A new concept to build shape memory polymers (SMP) combining outstanding fixity and recovery ratios (both above 99% after only one training cycle) typical of chemically crosslinked SMPs with reprocessability restricted to physically crosslinked SMPs is demonstrated by covalently bonding, through thermoreversible Diels–Alder (DA) adducts, star-shaped poly(epsilon-caprolactones) (PCL) end-functionalized by furan and maleimide moieties. A PCL network is easily prepared by melt-blending complementary end-functional star polymers in retro DA regime, then by curing at lower temperature to favour the DA cycloaddition. Such covalent network can be reprocessed when heated again at the retro DA temperature. The resulting SMP shows still excellent shape memory properties attesting for its good recyclability. [less ▲]

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See detail"Clip" and "click" chemistries combination: toward easy PEGylation of degradable aliphatic polyesters
Freichels, Hélène; Pourcelle, Vincent; Le Duff, Cécile S. et al

in Macromolecular Rapid Communications (2011), 32(7), 616-621

The combination of “clip” and “click” reactions provides a versatile and straightforward pathway for the synthesis of functional amphiphilic and degradable copolymers valuable for biomedical applications ... [more ▼]

The combination of “clip” and “click” reactions provides a versatile and straightforward pathway for the synthesis of functional amphiphilic and degradable copolymers valuable for biomedical applications such as targeted drug-delivery vehicles. [less ▲]

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See detailPolymeric Micelles Induced by Interpolymer Complexation
Lefèvre, Nathalie ULg; Fustin, Charles-André; Gohy, Jean-François

in Macromolecular Rapid Communications (2009), 30(22), 1871-88

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See detailMacromolecular engineering of biodegradable polyesters by ring-opening polymerization and 'Click' chemistry
Lecomte, Philippe ULg; Riva, Raphaël ULg; Jérôme, Christine ULg et al

in Macromolecular Rapid Communications (2008), 29(12-13), 982-997

Biodegradability makes aliphatic polyesters valuable candidates for biomaterials and environmentally friendly thermoplastics. Nevertheless, their chemical modification, which is mandatory for a series of ... [more ▼]

Biodegradability makes aliphatic polyesters valuable candidates for biomaterials and environmentally friendly thermoplastics. Nevertheless, their chemical modification, which is mandatory for a series of potential applications, is usually a problem because it must be carried out under very mild conditions in order to prevent degradation by hydrolysis and/or transesterification from occurring. In this review, the copper(i) -catalyzed azide-alkyne cycloaddition, which is a click reaction, is shown to be very efficient to bypass these problems and to tailor the macromolecular architecture and functionality of those polyesters without facing undesired degradation reactions. [less ▲]

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See detailNew monomers tailored for direct electrografting onto carbon in water
Cecius, Michaël ULg; Jérôme, Robert ULg; Jérôme, Christine ULg

in Macromolecular Rapid Communications (2007), 28(8), 948-954

Electrografting, which is an electropolymerization technique dedicated to the chemisorption of polyacrylates onto conductive surfaces, was actively studied in anhydrous organic media until now. This ... [more ▼]

Electrografting, which is an electropolymerization technique dedicated to the chemisorption of polyacrylates onto conductive surfaces, was actively studied in anhydrous organic media until now. This communication aims at extending this technique to aqueous media for the grafting of polyacrylates onto carbon. The key criterion for the successful electrografting under these not very demanding experimental conditions (water vs. anhydrous organic solvents) is the use of amphiphilic acrylic monomers. The impact of the chemical structure of these new monomers on the coating properties was investigated. Composition of the coatings was analyzed by FT-IR ATR and XPS, whereas film thickness and morphology were analyzed by ellipsometry and AFM, respectively. [less ▲]

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See detailFast controlled radical polymerization of styrene mediated by oligomeric nitroxides formed in situ
Sciannamea, Valérie; Catala, Jean-Marie; Jérôme, Robert ULg et al

in Macromolecular Rapid Communications (2007), 28(2), 147-151

In the presence of an oligomeric hindered secondary amine added with peracetic acid as the oxidant, radical polymerization of styrene is fast and controlled at 110 degrees C. Under these experimental ... [more ▼]

In the presence of an oligomeric hindered secondary amine added with peracetic acid as the oxidant, radical polymerization of styrene is fast and controlled at 110 degrees C. Under these experimental conditions, an oligomeric nitroxide is formed in situ. This polymerization is 2.5 faster than polymerization mediated by the alkoxyamine derivated from TIPNO (2,2,5-trimethyl-4- phenyl-3-azahexane-3-nitroxide), which generates a low molar mass nitroxide. Similarly, substitution of a low molar mass secondary amine, 2,2,6, 6-tetramethylpiperidone (4-oxo-TMP), for the oligomeric secondary amine maintains the control on the polymerization, which is however 4.6 times slower, all the other conditions being the same. The in situ formation of the oligomeric nitroxide has been confirmed by electron spin resonance (ESR). [less ▲]

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See detailSingle-mode microwave-assisted atom transfer radical polymerization catalyzed by [RuCl2(p-cymene)(PCy3)]
Delfosse, Sebastien; Borguet, Yannick ULg; Delaude, Lionel ULg et al

in Macromolecular Rapid Communications (2007), 28(4), 492-503

In the atom transfer radical polymerization (ATRP) of methyl methacrylate in the presence of [RuCl2(p-cymene)(PCy3)] (p-cymene=4-isopropyltoluene, PCy3=tricyclohexylphosphine), a microwave effect is noted ... [more ▼]

In the atom transfer radical polymerization (ATRP) of methyl methacrylate in the presence of [RuCl2(p-cymene)(PCy3)] (p-cymene=4-isopropyltoluene, PCy3=tricyclohexylphosphine), a microwave effect is noted which strikingly depends on both the temperature and the method used (conventional microwave synthesis (CMS, i.e., without simultaneous cooling) or enhanced microwave synthesis (EMS, with simultaneous cooling)). Thus, between 85 and 120 degrees C under CMS conditions, microwave-assisted polymerizations take place in a controlled fashion, and at 120 degrees C the microwave-assisted polymerization is three times faster than the conventionally heated protocol. However, from 130 degrees C, microwave irradiation has a deleterious effect and the polymerizations are no longer controlled. Likewise, using the EMS method in the temperature range of 85-120 degrees C results in uncontrolled processes, as indicated by the unsuccessful resumption of the polymerizations. These failures might be attributed to a significantly high concentration of radical species, which results in enhanced propagation and termination - mostly disproportionation - rates. [less ▲]

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See detailPreparation of well-defined PVOH/C60 nanohybrids by cobalt-mediated radical polymerization of vinyl acetate
Detrembleur, Christophe ULg; Stoilova, Olya; Bryaskova, Rayna ULg et al

in Macromolecular Rapid Communications (2006), 27(7), 498-504

Poly(vinyl acetate) chains end-capped by a Co(acac)(2) complex [PVAc-Co(acac)(2)] were prepared by bulk cobalt-mediated radical polymerization (CMRP) of vinyl acetate and used for grafting fullerene (C60 ... [more ▼]

Poly(vinyl acetate) chains end-capped by a Co(acac)(2) complex [PVAc-Co(acac)(2)] were prepared by bulk cobalt-mediated radical polymerization (CMRP) of vinyl acetate and used for grafting fullerene (C60) with four PVAc arms at low temperature (30 degrees C). A photoactive water-soluble poly(vinyl alcohol)/C60 nanohybrid was then prepared by hydrolysis of the PVAc arms of the nanohybrid. Because of photoactivity and very low cytotoxicity, this type of water-soluble nanohybrid is very promising for the photodynamic cancer therapy. [less ▲]

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See detailCobalt-mediated radical polymerization of vinyl acetate in miniemulsion: Very fast formation of stable poly(vinyl acetate) latexes at low temperature
Detrembleur, Christophe ULg; Debuigne, Antoine ULg; Bryaskova, Rayna ULg et al

in Macromolecular Rapid Communications (2006), 27(1), 37-41

Poly(vinyl acetate) macroinitiators end-capped by a Co(acac)(2) complex (PVAc-Co(acac)(2)), prepared in bulk by cobalt-mediated radical polymerization (CMRP), are used for the controlled radical ... [more ▼]

Poly(vinyl acetate) macroinitiators end-capped by a Co(acac)(2) complex (PVAc-Co(acac)(2)), prepared in bulk by cobalt-mediated radical polymerization (CMRP), are used for the controlled radical polymerization of vinyl acetate in miniemulsion to give high-molecular-weight polymers and high monomer conversion. Stable poly(vinyl acetate) latexes with solid contents ranging from 25 to 30 wt.-% are prepared within unusually short reaction times (similar to 1 h) at low temperatures (0-30 degrees C). [less ▲]

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See detailSequential electrografting and ring opening metathesis polymerization: a strategy for the tailoring of conductive surfaces
Voccia, Samuel; Claes, Michael; Jérôme, Robert ULg et al

in Macromolecular Rapid Communications (2005), 26(10), 779-783

An electrografting technique has been combined with ring-opening metathesis polymerization (ROMP). Poly(allyl methacrylate) chains have been chemisorbed onto steel and carbon plates under an appropriate ... [more ▼]

An electrografting technique has been combined with ring-opening metathesis polymerization (ROMP). Poly(allyl methacrylate) chains have been chemisorbed onto steel and carbon plates under an appropriate cathodic potential in N,N-dimethylformamide. The allyl moieties have been converted into Ru catalysts active in ROMP of norbornene and its derivatives. Initiation of ROMP from the surface is an efficient strategy to prepare strongly adhering coatings of tunable thickness and hydrophilic/hydrophobic balance, depending on the norbornene derivative polymerized at the surface. [less ▲]

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See detailSegregation of coronal chains in micelles formed by supramolecular interactions
Gohy, Jean-François; Khousakoun, Eric; Willet, Nicolas ULg et al

in Macromolecular Rapid Communications (2004), 25(17), 1536-1539

Spherical micelles have been formed by mixing, in DMF, a poly(styrene)-block-poly(2-vinylpyridine)-block-poly(ethylene oxide) (PS-block-P2VP-block-PEO) triblock copolymer with either poly(acrylic acid ... [more ▼]

Spherical micelles have been formed by mixing, in DMF, a poly(styrene)-block-poly(2-vinylpyridine)-block-poly(ethylene oxide) (PS-block-P2VP-block-PEO) triblock copolymer with either poly(acrylic acid) (PAA) or a tapered triblock copolymer consisting of a PAA central block and PEO macromonomer-based outer blocks. Noncovalent interactions between PAA and P2VP result in the micellar core while the outer corona contains both PS and PEO chains. Segregation of the coronal chains is observed when the tapered copolymer is used. [less ▲]

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See detailFunctionalization of multi-walled carbon nanotubes by electrografting of polyacrylonitrile
Petrov, Petar; Lou, Xudong; Pagnoulle, Christophe et al

in Macromolecular Rapid Communications (2004), 25(10), 987-990

As a result of their unique architecture and remarkable mechanical and electrical properties[1,2] carbon nanotubes (CNTs)[3] have great potential that remains, however, un-exploited because of poor ... [more ▼]

As a result of their unique architecture and remarkable mechanical and electrical properties[1,2] carbon nanotubes (CNTs)[3] have great potential that remains, however, un-exploited because of poor dispersibility in liquids and problems of processability, Major efforts have, therefore, been devoted towards any modification of the CNTs that could improve their handling[4,5] Typically, chemical modification of CNTs is based on severe oxidation processes that often damage the tubes[5] Mild and single-step electrochemical modification of CNTs is a valuable alternative to the oxidative treatment. There are several reports in the scientific literature on the electrochemical functionalization of CNTs by electroreduction of diazonium salts,[6-8] and on the halogenation of MWNTs by electrolysis However, the grafting of polymers instead of low-molecular-weight compounds onto CNTs by an electrochemical process is a possible strategy for dispersing CNTs in polymer matrices and improving the mechanical properties of CNT-based nanocomposites.. For the past few years, we have been interested in the electiografting of insulating polymer films onto cathodic surfaces, for example, nickel and glassy carbon, provided that the potential and solvent are properly selected.[10-15] These films are designated as "grafted films", because they have the unique property of remaining attached to the electrode surface even when they are prepared and kept in a solvent in which the polymer is highly soluble. The extension of this technique to CNTs has been explored with acrylonitrile as monomer. This communication aims at reporting the functionaliza-tion of multi-walled carbon nanotubes (MWNTs) by the electropolymerization of acrylonitrile. [less ▲]

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See detailExfoliated polylactide/clay nanocomposites by in-situ coordination-insertion polymerization
Paul, Marie-Amélie; Alexandre, Michaël ULg; Degée, Philippe et al

in Macromolecular Rapid Communications (2003), 24(9), 561-566

Poly(L-lactide)/layered aluminosilicate nanocomposites were synthesized in bulk by ring-opening polymerization in the presence of two organo-modified montmorillonites. When the organo-modifier consisted ... [more ▼]

Poly(L-lactide)/layered aluminosilicate nanocomposites were synthesized in bulk by ring-opening polymerization in the presence of two organo-modified montmorillonites. When the organo-modifier consisted of an ammonium cation bearing primary hydroxyl groups, polymerization was initiated by the alcohol functions after adequate activation. The growing polymer chains were directly "grafted" onto the clay surface through the hydroxyl-functionalized ammonium cations yielding exfoliated nano-composites with enhanced thermal stability. [less ▲]

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See detailNovel aliphatic polyesters based on functional cyclic (di)esters
Lou, Xudong; Detrembleur, Christophe ULg; Jérôme, Robert ULg

in Macromolecular Rapid Communications (2003), 24(2), 161-172

Recent progress in the chemical synthesis of novel aliphatic polyesters via ring-opening polymerization of functional cyclic (di)esters are reviewed in this article. Syntheses of these functional ... [more ▼]

Recent progress in the chemical synthesis of novel aliphatic polyesters via ring-opening polymerization of functional cyclic (di)esters are reviewed in this article. Syntheses of these functional aliphatic polyesters are being classified into three groups according to the structure of the cyclic monomers: (i) cyclic diesters, (ii) morpholine-2,5-dione derivatives, and (iii) cyclic esters. Progress in the synthesis and polymerization of monomers in each category is reported with an emphasis on controlled synthesis. The recent achievements have enabled the synthesis of a variety of novel aliphatic polyesters, including hydrophilic, halogenated, and unsaturated polyesters. [less ▲]

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See detailTwo-step backbiting reaction in the ring-opening polymerization of gamma-acryloyloxy-epsilon-caprolactone initiated with aluminium isopropoxide
Lou, Xudong; Detrembleur, Christophe ULg; Lecomte, Philippe ULg et al

in Macromolecular Rapid Communications (2002), 23(2), 126-129

gamma-Acryloyloxyethyl-gamma-butyrolactone is formed as a byproduct when the polymerization of gamma-acryloyloxy-epsilon-caprolactone is initiated with aluminium isopropoxide in toluene. The extent of ... [more ▼]

gamma-Acryloyloxyethyl-gamma-butyrolactone is formed as a byproduct when the polymerization of gamma-acryloyloxy-epsilon-caprolactone is initiated with aluminium isopropoxide in toluene. The extent of this side reaction decreases with decreasing temperature and is dependent on whether the reaction is stopped as soon as monomer conversion is complete or not. A two-step backbiting mechanism is proposed for this intramolecular transesterification reaction. [less ▲]

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See detailAssociation of telechelic ionomers in apolar solvents
Chassenieux, Christophe; Nicolai, Taco; Tassin, Jean-François et al

in Macromolecular Rapid Communications (2001), 22

The associative properties of well-defined halatotelechelic ionomers in an apolar solvent were studied by means of dynamic mechanical spectroscopy, small-angle X-ray scattering, as well as static and ... [more ▼]

The associative properties of well-defined halatotelechelic ionomers in an apolar solvent were studied by means of dynamic mechanical spectroscopy, small-angle X-ray scattering, as well as static and dynamic light scattering. The effect of end-functionalisation was investigated by comparing results on polystyrene (PS) and polyisoprene (PI) precursors using PS and PI of the same molar mass modified at one or both ends with sulfonate groups. The molar-mass dependence was investigated by comparing difunctionalised samples with different molar masses and the influence of the backbone by comparing polystyrene and polyisoprene. Experimental data suggest a relatively simple model for the association of this material. At low concentrations, the polymer chains organise themselves into well-defined reversed micelles, so-called flowers. Above a certain concentration C+, the flowers associate into larger aggregates according to an open association mechanism. At a critical concentration Cgel, the aggregates fill the whole space and a transient network is formed most likely by a percolation process. A semi-quantitative description of the associating process can be obtained by considering an open association mechanism properly combined with inter-particle interactions. [less ▲]

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See detailPreparation and properties of layered silicate nanocomposites based on ethylene vinyl acetate copolymers
Alexandre, Michaël ULg; Beyer, Günter; Henrist, Catherine ULg et al

in Macromolecular Rapid Communications (2001), 22(8), 643-646

(Nano)composites based on ethylene vinyl acetate copolymers (EVA) and montmorillonite modified by various alkylammonium cations were processed by mechanical kneading. Polymer intercalation and filler ... [more ▼]

(Nano)composites based on ethylene vinyl acetate copolymers (EVA) and montmorillonite modified by various alkylammonium cations were processed by mechanical kneading. Polymer intercalation and filler exfoliation were evidenced by X-ray diffraction and transmission electron microscopy, respectively. Nano-composites tensile properties showed that Young's modulus increases significantly even at very low content of the organo-modified filler while preserving high ultimate elongation and tensile stress. The matrix thermal stability in air was increased by 40°C and, interestingly, the obtained nanocomposites present flame retardant properties. TEM micrograph of the nanocomposite based on EVA3 filled with 5 wt.-% of Mont-2CN2C18. [less ▲]

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See detailReverse atom-transfer radical polymerization at room temperature
Wang, Wenxin; Yan, Deyue; Jiang, Xuling et al

in Macromolecular Rapid Communications (2001), 22(6), 439-443

This paper aims at reporting on the living/controlled radical polymerization of methyl methacrylate initiated with the benzoyl peroxide (BPO)/CuIX (X=Br,Cl)/2,2'-bipyridine (bpy) redox system at room ... [more ▼]

This paper aims at reporting on the living/controlled radical polymerization of methyl methacrylate initiated with the benzoyl peroxide (BPO)/CuIX (X=Br,Cl)/2,2'-bipyridine (bpy) redox system at room temperature. No control is observed for the polymerization conducted in bulk and in toluene, whereas a polymer with predetermined molecular weight and rather narrow molecular weight distribution is formed in butanone. The solvent has thus a decisive effect on the reverse atom-transfer radical polymerization of methyl methacrylate initiated with the BPO/CuIX (X = Br,Cl)/bpy ternary system at 25°C. [less ▲]

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See detailUse of metallocenes in the polymerization-filling technique with production of polyolefin-based composites
Alexandre, Michaël ULg; Martin, Eric; Dubois, Philippe ULg et al

in Macromolecular Rapid Communications (2000), 21(13), 931-936

In an updated version of the polymerization-filling technique, the surface of particulate fillers has been activated by metallocenes. Homogeneously filled polyolefins have accordingly been produced by the ... [more ▼]

In an updated version of the polymerization-filling technique, the surface of particulate fillers has been activated by metallocenes. Homogeneously filled polyolefins have accordingly been produced by the in situ copolymerization of ethylene and α-olefins, e.g., 1-octene and 1,9-decadiene. Different fillers have been successfully used, including inorganic particles with either an acidic surface (kaolin, glass beads, silica) or a basic surface (magnesium hydroxide, wollastonite), graphite and nickel particles. Hydrogen has proved to be efficient in reducing the molecular weight of the produced polymers. [less ▲]

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