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  1. Article ; Online: Coordinative Chain Transfer and Chain Shuttling Polymerization.

    Mundil, Robert / Bravo, Catarina / Merle, Nicolas / Zinck, Philippe

    Chemical reviews

    2023  Volume 124, Issue 1, Page(s) 210–244

    Abstract: Coordinative chain transfer polymerization, CCTP, is a degenerative chain transfer polymerization process that has a wide range of applications. It allows a highly controlled synthesis of polyolefins, stereoregular polydienes, and stereoregular ... ...

    Abstract Coordinative chain transfer polymerization, CCTP, is a degenerative chain transfer polymerization process that has a wide range of applications. It allows a highly controlled synthesis of polyolefins, stereoregular polydienes, and stereoregular polystyrene, including (stereo)block as well as statistical copolymers thereof. It also shows a green character by allowing catalyst economy during the synthesis of such polymers. CCTP notably allows the end functionalization of both the commodity and stereoregular specialty polymers aforementionned, control of the composition of statistical copolymers without adjusting the feed, and quantitative formation of 1-alkenes from ethene. A one-pot one-step synthesis of the original multiblock microstructures and architectures by chain shuttling polymerization (CSP) is also an asset of CCTP. This methodology takes advantage of the simultaneous presence of two catalysts of different selectivity toward comonomers that produce blocks of different composition/microstructure, while still allowing the chain transfer. This affords the production of highly performant functional polymers, such as thermoplastic elastomers and adhesives, among others. This approach has been extended to cyclic esters' and ethers' ring-opening polymerization, providing new types of multiblock microstructure. The present Review provides the state of the art in the field with a focus on the last 10 years.
    Language English
    Publishing date 2023-12-12
    Publishing country United States
    Document type Journal Article ; Review
    ZDB-ID 207949-5
    ISSN 1520-6890 ; 0009-2665
    ISSN (online) 1520-6890
    ISSN 0009-2665
    DOI 10.1021/acs.chemrev.3c00440
    Database MEDical Literature Analysis and Retrieval System OnLINE

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  2. Article: Organocatalytic sequential ring-opening polymerization of a cyclic ester and anionic polymerization of a vinyl monomer

    Mundil, Robert / Kayser, Franck / Favrelle-Huret, Audrey / Stoclet, Grégory / Zinck, Philippe

    Chemical communications. 2020 July 21, v. 56, no. 58

    2020  

    Abstract: Organocatalysis has provided new tools for making block copolymers, in particular active species able to polymerize monomers of different chemical nature such as cyclic esters, cyclic carbonates and epoxides. We report herein the first example of an ... ...

    Abstract Organocatalysis has provided new tools for making block copolymers, in particular active species able to polymerize monomers of different chemical nature such as cyclic esters, cyclic carbonates and epoxides. We report herein the first example of an organocatalytic active species able to polymerize sequentially a cyclic ester, ε-decalactone, and a vinyl monomer, methyl methacrylate. The resulting block copolymer shows the properties of thermoplastic elastomers.
    Keywords carbonates ; catalytic activity ; composite polymers ; epoxides ; lactones ; polymerization ; thermoplastics
    Language English
    Dates of publication 2020-0721
    Size p. 8067-8070.
    Publishing place The Royal Society of Chemistry
    Document type Article
    ZDB-ID 1472881-3
    ISSN 1364-548X ; 1359-7345 ; 0009-241X
    ISSN (online) 1364-548X
    ISSN 1359-7345 ; 0009-241X
    DOI 10.1039/d0cc02906h
    Database NAL-Catalogue (AGRICOLA)

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  3. Article ; Online: Organocatalytic sequential ring-opening polymerization of a cyclic ester and anionic polymerization of a vinyl monomer.

    Mundil, Robert / Kayser, Franck / Favrelle-Huret, Audrey / Stoclet, Grégory / Zinck, Philippe

    Chemical communications (Cambridge, England)

    2020  Volume 56, Issue 58, Page(s) 8067–8070

    Abstract: Organocatalysis has provided new tools for making block copolymers, in particular active species able to polymerize monomers of different chemical nature such as cyclic esters, cyclic carbonates and epoxides. We report herein the first example of an ... ...

    Abstract Organocatalysis has provided new tools for making block copolymers, in particular active species able to polymerize monomers of different chemical nature such as cyclic esters, cyclic carbonates and epoxides. We report herein the first example of an organocatalytic active species able to polymerize sequentially a cyclic ester, ε-decalactone, and a vinyl monomer, methyl methacrylate. The resulting block copolymer shows the properties of thermoplastic elastomers.
    Language English
    Publishing date 2020-06-16
    Publishing country England
    Document type Journal Article
    ZDB-ID 1472881-3
    ISSN 1364-548X ; 1359-7345 ; 0009-241X
    ISSN (online) 1364-548X
    ISSN 1359-7345 ; 0009-241X
    DOI 10.1039/d0cc02906h
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  4. Article: Topology Analysis of Chain Walking Polymerized Polyethylene: An Alternative Approach for the Branching Characterization by Thermal FFF

    Geisler, Martin / Smith, William C / Plüschke, Laura / Mundil, Robert / Merna, Jan / Williams, S. Kim Ratanathanawongs / Lederer, Albena

    Macromolecules. 2019 Nov. 05, v. 52, no. 22

    2019  

    Abstract: Thermal field-flow fractionation (ThFFF) was designed to investigate the retention behavior of a series of dendritic polyethylenes synthesized using a chain walking catalyst (cwPE) with variations in the branching architecture. The retention behavior of ... ...

    Abstract Thermal field-flow fractionation (ThFFF) was designed to investigate the retention behavior of a series of dendritic polyethylenes synthesized using a chain walking catalyst (cwPE) with variations in the branching architecture. The retention behavior of these macromolecules correlates with their branching. Based on differences in the Soret coefficient, a new model has been developed for the application of ThFFF as an alternative to the branching calculation approach based on light scattering or viscosity for the branching analysis of novel short-chain branched PEs.
    Keywords catalysts ; chemical structure ; fractionation ; light scattering ; models ; polyethylene ; polymerization ; topology ; viscosity
    Language English
    Dates of publication 2019-1105
    Size p. 8662-8671.
    Publishing place American Chemical Society
    Document type Article
    ZDB-ID 1491942-4
    ISSN 1520-5835 ; 0024-9297
    ISSN (online) 1520-5835
    ISSN 0024-9297
    DOI 10.1021/acs.macromol.9b01410
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  5. Article ; Online: High Temperature Quadruple-Detector Size Exclusion Chromatography for Topological Characterization of Polyethylene.

    Plüschke, Laura / Mundil, Robert / Sokolohorskyj, Anatolij / Merna, Jan / Sommer, Jens-Uwe / Lederer, Albena

    Analytical chemistry

    2018  Volume 90, Issue 10, Page(s) 6178–6186

    Abstract: Modifying material properties in simple macromolecules such as polyethylene (PE) is achieved by different connection modes of ethylene monomers resulting in a plurality of possible topologies-from highly linear to dendritic species. However, the ... ...

    Abstract Modifying material properties in simple macromolecules such as polyethylene (PE) is achieved by different connection modes of ethylene monomers resulting in a plurality of possible topologies-from highly linear to dendritic species. However, the challenge still lies within the experimental identification of the topology and conformation of the isolated macromolecules because of their low solubility, which demands methods with specific solvents and high operating temperatures. Additionally, a separation technique has to be coupled to different detection methods to meet the specific demands of the respective characterization goal. In this work, we report a quadruple-detector high temperature size exclusion chromatography (HT-SEC) system which contains online multiangle laser light scattering, dynamic light scattering, differential viscometry, and differential refractometry detectors. Quadruple-detector HT-SEC was successfully applied to explore the full range of physical parameters of various PE samples with different branching topologies ranging from highly linear macromolecules, polymers with moderate level of branching, to highly branched PEs with hyperbranched structure. This method is a useful tool not only to investigate molecular weight, mass distribution, and size but also to enable access to important factors which describe the conformation in dilute solution and branching density.
    Language English
    Publishing date 2018-05-04
    Publishing country United States
    Document type Journal Article ; Research Support, Non-U.S. Gov't
    ZDB-ID 1508-8
    ISSN 1520-6882 ; 0003-2700
    ISSN (online) 1520-6882
    ISSN 0003-2700
    DOI 10.1021/acs.analchem.8b00619
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  6. Article ; Online: Polyolefins Formed by Chain Walking Catalysis-A Matter of Branching Density Only?

    Dockhorn, Ron / Plüschke, Laura / Geisler, Martin / Zessin, Johanna / Lindner, Peter / Mundil, Robert / Merna, Jan / Sommer, Jens-Uwe / Lederer, Albena

    Journal of the American Chemical Society

    2019  Volume 141, Issue 39, Page(s) 15586–15596

    Abstract: Recently developed chain walking (CW) catalysis is an elegant approach to produce materials with controllable structure and properties. However, there is still a lack in understanding of how the reaction mechanism influences the macromolecular structures. ...

    Abstract Recently developed chain walking (CW) catalysis is an elegant approach to produce materials with controllable structure and properties. However, there is still a lack in understanding of how the reaction mechanism influences the macromolecular structures. In this study, a series of dendritic polyethylenes (PE) synthesized by Pd-α-diimine-complex through CW catalysis (CWPE) is investigated by means of theory and experiment. Thereby, the exceptional ability of in situ tailoring polymer structure by varying synthesis parameters was exploited to tune the branching architecture, which allowed us to establish a precise relationship between synthesis, structure, and solution properties. The systematically produced polymers were characterized by state-of-the-art multidetector separation and neutron scattering experiments as well as atomic force microscopy to access molecular properties of CWPE. On a global scale, the CWPE appear in a worm-like conformation independently on the synthesis conditions. However, severe differences in their contraction factors suggested that CWPE differ substantially in topology. These observations were verified by NMR studies that showed that CWPE possess a constant total number of branches but varying branching distribution. Small angle neutron scattering experiments gave access to structural characteristics from global to segmental scale and revealed the unique heterogeneity of CWPE, which is predominantly based on differences in their dendritic side chains. The experimental data were compared to theoretical CW structures modeled with different reaction-to-walking probabilities. Simple theoretical arguments predict a crossover from dendritic to linear topologies yielding a structural range from purely linear to dendritic chain growth. Yet, comparison of theoretical and empirical scattering curves gave the first evidence that a transition state to worm-like topologies is actually experimentally accessible. This crossover regime is characterized by linear global features and dendritic local substructures contrary to randomly hyperbranched systems. Instead, the obtained CWPE systems have characteristics of disordered dendritic bottle brushes and can be adjusted by the walking rate/reaction probability of the catalyst.
    Language English
    Publishing date 2019-09-03
    Publishing country United States
    Document type Journal Article
    ZDB-ID 3155-0
    ISSN 1520-5126 ; 0002-7863
    ISSN (online) 1520-5126
    ISSN 0002-7863
    DOI 10.1021/jacs.9b06785
    Database MEDical Literature Analysis and Retrieval System OnLINE

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  7. Article: Polyolefins Formed by Chain Walking Catalysis—A Matter of Branching Density Only?

    Dockhorn, Ron / Geisler, Martin / Lederer, Albena / Lindner, Peter / Merna, Jan / Mundil, Robert / Plüschke, Laura / Sommer, Jens-Uwe / Zessin, Johanna

    Journal of the American Chemical Society. 2019 Aug. 23, v. 141, no. 39

    2019  

    Abstract: Recently developed chain walking (CW) catalysis is an elegant approach to produce materials with controllable structure and properties. However, there is still a lack in understanding of how the reaction mechanism influences the macromolecular structures. ...

    Abstract Recently developed chain walking (CW) catalysis is an elegant approach to produce materials with controllable structure and properties. However, there is still a lack in understanding of how the reaction mechanism influences the macromolecular structures. In this study, a series of dendritic polyethylenes (PE) synthesized by Pd-α-diimine-complex through CW catalysis (CWPE) is investigated by means of theory and experiment. Thereby, the exceptional ability of in situ tailoring polymer structure by varying synthesis parameters was exploited to tune the branching architecture, which allowed us to establish a precise relationship between synthesis, structure, and solution properties. The systematically produced polymers were characterized by state-of-the-art multidetector separation and neutron scattering experiments as well as atomic force microscopy to access molecular properties of CWPE. On a global scale, the CWPE appear in a worm-like conformation independently on the synthesis conditions. However, severe differences in their contraction factors suggested that CWPE differ substantially in topology. These observations were verified by NMR studies that showed that CWPE possess a constant total number of branches but varying branching distribution. Small angle neutron scattering experiments gave access to structural characteristics from global to segmental scale and revealed the unique heterogeneity of CWPE, which is predominantly based on differences in their dendritic side chains. The experimental data were compared to theoretical CW structures modeled with different reaction-to-walking probabilities. Simple theoretical arguments predict a crossover from dendritic to linear topologies yielding a structural range from purely linear to dendritic chain growth. Yet, comparison of theoretical and empirical scattering curves gave the first evidence that a transition state to worm-like topologies is actually experimentally accessible. This crossover regime is characterized by linear global features and dendritic local substructures contrary to randomly hyperbranched systems. Instead, the obtained CWPE systems have characteristics of disordered dendritic bottle brushes and can be adjusted by the walking rate/reaction probability of the catalyst.
    Keywords atomic force microscopy ; brushes ; catalysts ; catalytic activity ; neutron diffraction ; nuclear magnetic resonance spectroscopy ; polyethylenes ; probability ; reaction mechanisms ; topology
    Language English
    Dates of publication 2019-0823
    Size p. 15586-15596.
    Publishing place American Chemical Society
    Document type Article
    ZDB-ID 3155-0
    ISSN 1520-5126 ; 0002-7863
    ISSN (online) 1520-5126
    ISSN 0002-7863
    DOI 10.1021/jacs.9b06785
    Database NAL-Catalogue (AGRICOLA)

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    In stock of ZB MED Bonn / Germany

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