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See detailSynthesis of poly(vinyl acetate)-b-poly(vinyl chloride) block copolymers by cobalt-mediated radical polymerization (CMRP)
Piette, Yasmine; Debuigne, Antoine ULg; Bodart, Vinent et al

in Polymer Chemistry (2013), 4(5), 1685-1693

The synthesis of poly(vinyl acetate)-b-poly(vinyl chloride) (PVAc-b-PVC) block copolymers by Cobalt-Mediated Radical Polymerization (CMRP) is investigated for the first time in this paper. A PVAc–Co(acac ... [more ▼]

The synthesis of poly(vinyl acetate)-b-poly(vinyl chloride) (PVAc-b-PVC) block copolymers by Cobalt-Mediated Radical Polymerization (CMRP) is investigated for the first time in this paper. A PVAc–Co(acac)2 macroinitiator is prepared by CMRP using the V-70/Co(acac)2 binary system or a preformed alkylcobalt(III) compound. Then, the block copolymerization occurs in the bulk at 40 °C by the addition of VC. The addition of water to the polymerization medium or the slow generation of alkyl radicals during the whole polymerization is beneficial to the process by consuming part of the excess of deactivator (Co(acac)2) that blocks the polymer chains into the dormant form. Dynamic light scattering (DLS) measurements and AFM analyses evidence that the PVAc-b-PVC forms core–shell micelles in a selective solvent of the PVAc block, i.e. methanol, evidencing the blocky structure of the copolymer. PVAc-b-P(VC-co-VAc) copolymers are also successfully prepared by initiating the radical copolymerization of VC and VAc at 40 °C from a PVAc–Co(acac)2 macroinitiator. [less ▲]

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See detailFunctional nanogels as platforms for imparting antibacterial, antibiofilm, and antiadhesion activities to stainless steel
Faure, Emilie ULg; Falentin, Céline ULg; Svaldo Lanero, Tiziana ULg et al

in Advanced Functional Materials (2012), 22(24), 5271-5282

In this work, long-term antibacterial, antiadhesion, and antibiofilm activities are afforded to industrial stainless steel surfaces following a green and bio-inspired strategy. Starting from catechol ... [more ▼]

In this work, long-term antibacterial, antiadhesion, and antibiofilm activities are afforded to industrial stainless steel surfaces following a green and bio-inspired strategy. Starting from catechol bearing synthetic polymers, the film cross-linking and the grafting of active (bio)molecules are possible under environmentally friendly conditions (in aqueous media and at room temperature). A bio-inspired polyelectrolyte, a polycation-bearing catechol, is used as the film-anchoring polymer while a poly(methacrylamide)-bearing quinone groups serves as the cross-linking agent in combination with a polymer bearing primary amine groups. The amine/quinone reaction is exploited to prepare stable solutions of nanogels in water at room temperature that can be easily deposited to stainless steel. This coating provides quinonefunctionalized surfaces that are then used to covalently anchor active (bio) molecules (antibiofi lm enzyme and antiadhesion polymer) through thiol/ quinone reactions. [less ▲]

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See detailCobalt-mediated radical (co)polymerization of vinyl chloride and vinyl acetate
Piette, Yasmine; Debuigne, Antoine ULg; Jérôme, Christine ULg et al

in Polymer Chemistry (2012), 3(10), 2880-2891

The cobalt mediated radical polymerization (CMRP) of vinyl chloride (VC) in the presence of bis(acetylacetonato)cobalt(II) (Co(acac)2) as a controlling agent is presented for the first time. Using an ... [more ▼]

The cobalt mediated radical polymerization (CMRP) of vinyl chloride (VC) in the presence of bis(acetylacetonato)cobalt(II) (Co(acac)2) as a controlling agent is presented for the first time. Using an alkyl-Co(III) compound (R0–(CH2–CHOAc)<4–Co(acac)2; R0 = (H3C)2(OCH3)C–CH2–C(CH3)(CN)–) as an initiator, the bulk polymerization under non-isotherm conditions is controlled. 1H NMR spectra of the resulting PVC show that the CMRP process does not significantly affect the level of defects compared to a PVC prepared by a conventional free radical polymerization at the same temperature. Using the same alkyl-cobalt(III) compound, the copolymerization of VC and VAc is controlled at 40 °C provided that enough VAc (about 40 mol%) is present in the polymerization medium to moderate the VC polymerization. In line with reactivity ratios, VC is preferentially incorporated in the polymer at the early stages of the polymerization, leading to copolymers with a high VC content at moderate conversions. This is the first report of a CMRP of VC and of the synthesis of well-defined statistical PVC-co-PVAc copolymers by this technique. [less ▲]

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See detailEffects of cellular morphology on electricalconductivity of carbon nanotubes containing nanocomposites foams
Tran, Minh Phuong ULg; Detrembleur, Christophe ULg; Thomassin, Jean-Michel ULg et al

Conference (2012, September 13)

In the last few years, polymer carbon nanotubes (CNTs) nanocomposites foams have received increasing attention due to their potential applications in electrostatic dissipation (ESD) and in electromagnetic ... [more ▼]

In the last few years, polymer carbon nanotubes (CNTs) nanocomposites foams have received increasing attention due to their potential applications in electrostatic dissipation (ESD) and in electromagnetic interferences (EMI) shielding. To be efficient, these foams must exhibit appropriate electrical conductivity (> 1 S/m) and dielectric constant. A good understanding of the influence of the foam structural parameters on the electrical properties of the foam will ultimately enable the optimum design of these materials for the targeted applications. A wide range of poly(methyl methacrylate) (PMMA)/CNTs nanocomposites foams were synthesized using the supercritical CO2 technology. Different foaming parameters, such as the temperature, impregnation pressure, time and rate of depressurization were varied to modify the foam structure. The amount of carbon nanotubes in PMMA plays the most important role in increasing the electrical conductivity. Nanocomposite foams show higher electrical conductivity than non-foamed nanocomposites at the same volume content of CNTs. Effects of foam morphology such as cell-density; pore size, volume expansion, and cell-wall thickness on electrical conductivity were comprehensively assessed. High electrical conductivity can be achieved with nanocomposite foams that have high volume expansion, small pore size, high cell density, and thin cell-walls [less ▲]

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See detailStimuli-responsive Magnetic Nanohybrids for Triggered Drug Release and Potential Tumor Treatment via Hyperthermia
Liu, Ji ULg; Detrembleur, Christophe ULg; Mornet, Stéphane et al

Poster (2012, September 13)

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See detailMechanistic investigation and selectivity of the grafting onto C60 of macroradicals prepared by cobalt-mediated radical polymerization
Hurtgen, Marie ULg; Debuigne, Antoine ULg; Gigmes, Didier et al

in Polymer (2012), 53(20), 4353-4358

The grafting mechanism of poly(vinyl acetate) macroradicals prepared by cobalt-mediated radical polymerization onto C60 is investigated. The experimental conditions directly impact the nature and ... [more ▼]

The grafting mechanism of poly(vinyl acetate) macroradicals prepared by cobalt-mediated radical polymerization onto C60 is investigated. The experimental conditions directly impact the nature and stability of the PVAc/C60 adducts. In the presence of residual initiating radicals that can compete with PVAc! macroradicals for addition onto C60, mixtures of PVAc/C60 adducts having between one and eight polymer chains per C60 are formed. PVAc/C60 adducts prepared with low [PVAc]:[C60] ratios may contain weak C60-C60 bonds that further dissociate and account for the instability of the products. The formation of such dimers can be lessened by increasing the temperature from 30 !C to 100 !C. The temperature increase also allows a complete dissociation of the PVAc-Co dormant species into PVAc! macroradicals and an almost quantitative grafting of eight PVAc chains onto C60, leading to well-de!ned C60(PVAc)8 octa-adducts. These results might shed new light on the grafting onto C60 of macroradicals prepared by other CRP techniques. [less ▲]

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See detailThermally induced coupling of poly(thiophene)-based block copolymers prepared by Grignard metathesis polymerization: a straightforward route toward highly regioregular multiblock conjugated copolymers
Ouhib, Farid ULg; Desbief, Simon; Lazzaroni, Roberto et al

in Macromolecules (2012), 45(17), 6796-6806

We report on a convenient and simple process to prepare highly regioregular poly(thiophene)-based multiblock copolymers by a novel thermally induced coupling reaction. Diblock copolymers of 3 ... [more ▼]

We report on a convenient and simple process to prepare highly regioregular poly(thiophene)-based multiblock copolymers by a novel thermally induced coupling reaction. Diblock copolymers of 3-hexylthiophene (3HT) and 2,5-dibromo-3-(2-(2-tetrahydropyranyl-2-oxy)ethyl)thiophene (THPET) end-capped by a nickel complex (Br-P3HT-b-PTHPET-Ni(dppp)Br) are first prepared using Ni(dppp)Cl2 as catalyst at 30 °C by Grignard metathesis polymerization (GRIM process). The coupling of these α-bromo, ω-Ni(dppp)Br telechelic diblock copolymers then occurs by heating the solution of the copolymer at 80 °C for a few hours without adding any additional reagent. Reactions are complete in only 10 min when heating the copolymer at 120 °C using microwaves. The deprotection of the alcohol groups of PTHPET blocks allows further modifications such as the incorporation of acrylates by esterification. AFM analysis on thin films shows the influence of the nature of side chains (protected alcohol or acrylate), the molecular weight, and the architecture (diblock or multiblock) of the copolymer on the supramolecular organization of the polythiophene chains. [less ▲]

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See detailSINGLE-MOLECULE AFM STUDY OF ADHESIVE POLYMERS PREPARED BY COBALT-MEDIATED RADICAL POLYMERIZATION AND NITRONE-MEDIATED RADICAL COUPLING
Willet, Nicolas ULg; Sluysmans, Damien ULg; Delvaux, Cédric ULg et al

Scientific conference (2012, September 10)

Well-defined poly(vinyl acetate) (PVAc) chains prepared by CMRP (cobalt-mediated radical polymerization) were coupled using an alkyne-functional nitrone via NMRC (nitrone-mediated radical coupling).1 In ... [more ▼]

Well-defined poly(vinyl acetate) (PVAc) chains prepared by CMRP (cobalt-mediated radical polymerization) were coupled using an alkyne-functional nitrone via NMRC (nitrone-mediated radical coupling).1 In all the cases, the coupling efficiencies were close to 90% or higher. The polymers mid-chain functionalized with an alkyne group were then reacted with azide-functionalized atomic force microscopy (AFM) tips via copper-catalyzed azide-alkyne cycloaddition (CuAAC). As a result, polymers having a double-branch architecture were linked to AFM tips via a short linker. The structure and the molecular parameters of the polymers were determined by NMR and GPC, whereas the ‘click’ step onto AFM tips was assessed by performing the same CuAAC reaction onto macroscopic surfaces and characterizing them by ATR FT-IR. The adhesive properties of these double-branched polymers were studied by AFM single-molecule force spectroscopy. By performing approach-retraction cycles in solution upon a glass surface, the interaction between single PVAc chains and the surface was investigated. The effect of the double-branch architecture on the adhesion forces was under focus. Setting a residence time of the tip on the surface before retraction was found to have a beneficial influence on the adhesion forces. Signs of multiple interactions acting in parallel were detected in the experimental force-distance traces. [less ▲]

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See detailOrganometallic-mediated radical polymerization of vinyl amides: Effect of metal coordination
Kermagoret, Anthony ULg; Morin, A.; Hurtgen, Marie ULg et al

Poster (2012, September 04)

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See detailOrganometallic-mediated radical polymerization of vinyl amides: Effect of metal coordination
Kermagoret, Anthony ULg; Morin, A.; Hurtgen, Marie ULg et al

Conference (2012, September 04)

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See detailOnline monitoring of heterogeneous polymerizations in supercritical carbon dioxide by Raman spectroscopy
Grignard, Bruno ULg; Gilbert, Bernard ULg; Malherbe, Cédric ULg et al

in Chemphyschem : A European Journal of Chemical Physics and Physical Chemistry (2012), 13(11), 2666-2670

A novel setup is described to monitor the kinetics of homogeneous and heterogeneous reactions online using Raman spectroscopy under high pressure. The arrangement is based on a high-pressure reactor ... [more ▼]

A novel setup is described to monitor the kinetics of homogeneous and heterogeneous reactions online using Raman spectroscopy under high pressure. The arrangement is based on a high-pressure reactor equipped with a sapphire window in combination with a mobile probe that allows the collection of the back-scattered Raman signal at 360°. [less ▲]

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See detailA green and bio-inspired process to afford durable anti-biofilm properties to stainless steel
Faure, Emilie; Vreuls, Christelle; Falentin-Daudré, Céline et al

in Biofouling (2012), 28(7), 719-728

A bio-inspired durable anti-biofilm coating was developed for industrial stainless steel (SS) surfaces. Two polymers inspired from the adhesive and cross-linking properties of mussels were designed and ... [more ▼]

A bio-inspired durable anti-biofilm coating was developed for industrial stainless steel (SS) surfaces. Two polymers inspired from the adhesive and cross-linking properties of mussels were designed and assembled from aqueous solutions onto SS surfaces to afford durable coatings. Trypsin, a commercially available broad spectrum serine protease, was grafted as the final active layer of the coating. Its proteolytic activity after long immersion periods was demonstrated against several substrata, viz. a synthetic molecule, N-a-benzoyl-DL-arginine-p-nitroanilide hydrochloride (BAPNA), a protein, FTC-casein, and Gram-positive biofilm forming bacterium Staphylococcus epidermidis. [less ▲]

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See detailSynthetic and mechanistic inputs of photochemistry into the bisacetylacetonatocobalt- mediated radical polymerization of n-butyl acrylate and vinyl acetate
Detrembleur, Christophe ULg; Versace, Davy-Louis; Piette, Yasmine et al

in Polymer Chemistry (2012), 3(7), 1856-1866

The input of photochemistry to the Co(acac)2 mediated radical polymerization (CMRP) of n-butyl acrylate and vinyl acetate is investigated for the first time. Upon UV irradiation, photoinitiators are able ... [more ▼]

The input of photochemistry to the Co(acac)2 mediated radical polymerization (CMRP) of n-butyl acrylate and vinyl acetate is investigated for the first time. Upon UV irradiation, photoinitiators are able to initiate the n-butyl acrylate polymerization that remains controlled up to very high molar masses (>4 × 106 g mol−1) with low polydispersities. The photoinitiator as well as the irradiation time must be appropriately chosen to reach acceptable initiator efficiencies while maintaining an optimal control over the polymerization. Laser flash photolysis experiments were then carried out to evidence the addition of alkyl and phosphonyl radicals onto Co(acac)2 and to determine the rate constants (kdeact) of these addition reactions that were still lacking. Finally, both kinetics of polymerization and spin-trapping experiments have evidenced that the C–Co bond at the extremity of the dormant polymer chains can be easily photocleaved. UV irradiation can therefore be considered as an additional lever for tuning the reactivity of the CMRP process mediated by Co(acac)2. [less ▲]

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See detailInterpolymer radical coupling: A toolbox complementary to controlled radical polymerization
Debuigne, Antoine ULg; Hurtgen, Marie ULg; Detrembleur, Christophe ULg et al

in Progress in Polymer Science (2012), 37(7), 1004-1030

The current review focuses on the relevance and practical benefit of interpolymer radical coupling methods. The latter are developing rapidly and constitute a perfectly complementary macromolecular ... [more ▼]

The current review focuses on the relevance and practical benefit of interpolymer radical coupling methods. The latter are developing rapidly and constitute a perfectly complementary macromolecular engineering toolbox to the controlled radical polymerization techniques (CRP). Indeed, all structures formed by CRP are likely to be prone to radical coupling reactions, which multiply the available synthetic possibilities. Basically, the coupling systems can be divided in two main categories. The first one, including the atom transfer radical coupling (ATRC), silane radical atom abstraction (SRAA) and cobalt-mediated radical coupling (CMRC), relies on the recombination of macroradicals produced from a dormant species. The second one, including atom transfer nitroxide radical coupling (ATNRC), single electron transfer nitroxide radical coupling (SETNRC), enhanced spin capturing polymerization (ESCP) and nitrone/nitroso mediated radical coupling (NMRC), makes use of a radical scavenger in order to promote the conjugation of the polymer chains. More than a compilation of macromolecular engineering achievements, the present review additionally aims to emphasize the particularities, synthetic potential and present limitations of each system. [less ▲]

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See detailControlled radical polymerization of halogenated monomers
Bodart, Vincent; Piette, Yasmine; Detrembleur, Christophe ULg et al

Patent (2012)

Process for the preparation of a halogenated polymer comprising a controlled radical polymerization step of at least one monomer containing at least one halogen-carbon bond performed in the presence of an ... [more ▼]

Process for the preparation of a halogenated polymer comprising a controlled radical polymerization step of at least one monomer containing at least one halogen-carbon bond performed in the presence of an organo-cobalt complex, said polymerization step being further carried out in the presence of at least one ligand. [less ▲]

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See detailControlled radical polymerization of halogenated monomers
Bodart, Vincent; Piette, Yasmine; Detrembleur, Christophe ULg et al

Patent (2012)

Process for the preparation of a halogenated polymer comprising a controlled radical polymerization step of at least one monomer containing at least one halogen-carbon bond, performed in the presence of ... [more ▼]

Process for the preparation of a halogenated polymer comprising a controlled radical polymerization step of at least one monomer containing at least one halogen-carbon bond, performed in the presence of an organo-cobalt complex, said polymerization step being further carried out in non-isotherm conditions. [less ▲]

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