Synthesis and dilute solution properties of branched poly(benzyl methacrylate) using na‐clay supported aqueous‐phase catalysis

Aggarwal, Ravi; Baskaran, Durairaj

doi:10.1002/pola.29193

Title: Synthesis and dilute solution properties of branched poly(benzyl methacrylate) using na‐clay supported aqueous‐phase catalysis

Abstract

ABSTRACT The supported aqueous‐phase catalysis (SAPC) using hydrated interface has been used to synthesize branched polymers (star and graft) of benzyl methacrylate (BnMA) via atom‐transfer radical polymerization (ATRP) in the presence of Na‐clay supported catalyst in anisole at ambient temperature. The propagation of star poly(BnMA)s using diPENDTA‐Br ₆ , as hexa ‐functional initiator is confined at the hydrated interface between the support and the liquid medium as evident from the obtained polymers that are catalyst contamination‐free, and exhibited moderately narrow molecular weight distributions ( M _w / M _n ≤ 1.33). The hexa ‐functionality of synthesized stars is verified by ¹ H NMR, the measurement of their intrinsic viscosity ([ η ]), and radius of gyration ( R _g ). The polymerization was also recycled up to 5 times to produce star PBnMAs with high initiator efficiency. The star polymers prepared using hydrated Na‐clay supported is compared with star prepared using covalent silica supported catalyst system. The star polymer obtained from covalently supported catalyst gave broad M _w / M _n and poor initiator efficiency. The polystyrene‐ graft ‐PBnMA (PS‐ g ‐PBnMA) copolymer is also prepared using hydrated Na‐clay supported catalyst system in anisole at ambient temperature. The graft ‐copolymermore »« less

Authors:

Aggarwal, Ravi ^[1];

^[1]

Department of Chemistry University of Tennessee Knoxville Tennessee 37996

Publication Date:: Sun Sep 09 00:00:00 EDT 2018

Sponsoring Org.:: USDOE

OSTI Identifier:: 1469228

Grant/Contract Number:: De‐AC05‐00OR22725

Resource Type:: Publisher's Accepted Manuscript

Journal Name:: Journal of Polymer Science. Part A, Polymer Chemistry

Additional Journal Information:: Journal Name: Journal of Polymer Science. Part A, Polymer Chemistry Journal Volume: 56 Journal Issue: 19; Journal ID: ISSN 0887-624X

Publisher:: Wiley Blackwell (John Wiley & Sons)

Country of Publication:: United States

Language:: English

Citation Formats


                    Aggarwal, Ravi, and Baskaran, Durairaj. Synthesis and dilute solution properties of branched poly(benzyl methacrylate) using na‐clay supported aqueous‐phase catalysis.  United States: N. p., 2018. 
Web.  doi:10.1002/pola.29193.

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                    Aggarwal, Ravi, & Baskaran, Durairaj. Synthesis and dilute solution properties of branched poly(benzyl methacrylate) using na‐clay supported aqueous‐phase catalysis.  United States.  https://doi.org/10.1002/pola.29193

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                    Aggarwal, Ravi, and Baskaran, Durairaj. Sun .  
"Synthesis and dilute solution properties of branched poly(benzyl methacrylate) using na‐clay supported aqueous‐phase catalysis".  United States.  https://doi.org/10.1002/pola.29193.

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@article{osti_1469228,

  title        = {Synthesis and dilute solution properties of branched poly(benzyl methacrylate) using na‐clay supported aqueous‐phase catalysis},

  author       = {Aggarwal, Ravi and Baskaran, Durairaj},

  abstractNote = {ABSTRACT The supported aqueous‐phase catalysis (SAPC) using hydrated interface has been used to synthesize branched polymers (star and graft) of benzyl methacrylate (BnMA) via atom‐transfer radical polymerization (ATRP) in the presence of Na‐clay supported catalyst in anisole at ambient temperature. The propagation of star poly(BnMA)s using diPENDTA‐Br 6 , as hexa ‐functional initiator is confined at the hydrated interface between the support and the liquid medium as evident from the obtained polymers that are catalyst contamination‐free, and exhibited moderately narrow molecular weight distributions ( M w / M n ≤ 1.33). The hexa ‐functionality of synthesized stars is verified by 1 H NMR, the measurement of their intrinsic viscosity ([ η ]), and radius of gyration ( R g ). The polymerization was also recycled up to 5 times to produce star PBnMAs with high initiator efficiency. The star polymers prepared using hydrated Na‐clay supported is compared with star prepared using covalent silica supported catalyst system. The star polymer obtained from covalently supported catalyst gave broad M w / M n and poor initiator efficiency. The polystyrene‐ graft ‐PBnMA (PS‐ g ‐PBnMA) copolymer is also prepared using hydrated Na‐clay supported catalyst system in anisole at ambient temperature. The graft ‐copolymer had narrow M w / M n and was confirmed using 1 H NMR and atomic force microscopy. © 2018 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2018 , 56 , 2225–2237},

  doi          = {10.1002/pola.29193},

  journal      = {Journal of Polymer Science. Part A, Polymer Chemistry},

  number       = 19,

  volume       = 56,

  place        = {United States},

  year         = {Sun Sep 09 00:00:00 EDT 2018},

  month        = {Sun Sep 09 00:00:00 EDT 2018}

}

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Title: Synthesis and dilute solution properties of branched poly(benzyl methacrylate) using na‐clay supported aqueous‐phase catalysis

Abstract

Citation Formats

Feasibility Analysis of Surface Mediation in Supported Atom Transfer Radical Polymerization journal, July 2006

Fundamentals and development of high-efficiency supported catalyst systems for atom transfer radical polymerization journal, January 2007

Metal-Catalyzed Living Radical Polymerization journal, December 2001

Newly Designed Star-Shaped Polystyrene: Synthesis and Characterization journal, October 1998

Synthesis and Dilute-Solution Behavior of Model Star-Branched Polymers journal, July 1978

Initiation Efficiency in the Synthesis of Molecular Brushes by Grafting from via Atom Transfer Radical Polymerization journal, February 2005

Preparation and Characterization of Four-Branched Star Polystyrene journal, July 1972

The Synthesis of Densely Grafted Copolymers by Atom Transfer Radical Polymerization journal, December 1998

An Immobilized/Soluble Hybrid Catalyst System for Atom Transfer Radical Polymerization journal, July 2001

Preparation and characterization of H-shaped polystyrene journal, September 1981

Investigation of Methyl Methacrylate and Vinyl Acetate Polymerization Promoted by Al( i Bu) 3 /2,2‘-Bipyridine and Al( i Bu) 3 /2,2‘-Bipyridine/TEMPO Complexes journal, October 1998

Anionic Copolymerization of Styrene with p-Divinylbenzene journal, September 1970

Effect of arm number and arm molecular weight on the solid-state morphology of poly(styrene-isoprene) star block copolymers journal, January 1986

Characterization of branched polymers by SEC coupled with a multiangle light scattering detector. II. Data processing and interpretation journal, January 2001

Atom Transfer Radical Polymerization of Styrene Using a Novel Octafunctional Initiator: Synthesis of Well-Defined Polystyrene Stars journal, October 1998

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Angular distribution of intensity of rayleigh scattering from comblike branched molecules journal, December 1966

Calixarene-Core Multifunctional Initiators for the Ruthenium-Mediated Living Radical Polymerization of Methacrylates 1 journal, October 1998

Chain Architecture and Asymmetry in Copolymer Microphases journal, April 1994

Synthesis of Amphiphilic PS- b -PEG- b -PS by Atom Transfer Radical Polymerization journal, January 1998

Dilute solution properties of branched macromolecules journal, January 1992

Polymers with Complex Architecture by Living Anionic Polymerization journal, December 2001

Synthesis and characterization of multiarm star polybutadienes journal, July 1989

Preparation of Six-Branched Polystyrene. Thermodynamic and Hydrodynamic Porperties of Four- and Six-Branched Star Polystyrenes journal, July 1974

Novel double hydrophilic block copolymers based on poly(p-hydroxystyrene) derivatives and poly(ethylene oxide) journal, January 2007

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Effect of Ligand Structure on Activation Rate Constants in ATRP journal, July 2006

Controlled/"living" radical polymerization. atom transfer radical polymerization in the presence of transition-metal complexes journal, May 1995

Living Polymerization Methods journal, February 1991

Synthesis and Characterization of Star Polymers with Varying Arm Number, Length, and Composition from Organic and Hybrid Inorganic/Organic Multifunctional Initiators journal, October 1999

Multifunctional Initiators for the Ruthenium-Mediated Living Radical Polymerization of Methyl Methacrylate: Di- and Trifunctional Dichloroacetates for Synthesis of Multiarmed Polymers 1 journal, February 1998

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Feasibility Analysis of Surface Mediation in Supported Atom Transfer Radical Polymerization
journal, July 2006

Fundamentals and development of high-efficiency supported catalyst systems for atom transfer radical polymerization
journal, January 2007

Metal-Catalyzed Living Radical Polymerization
journal, December 2001

Newly Designed Star-Shaped Polystyrene: Synthesis and Characterization
journal, October 1998

Synthesis and Dilute-Solution Behavior of Model Star-Branched Polymers
journal, July 1978

Initiation Efficiency in the Synthesis of Molecular Brushes by Grafting from via Atom Transfer Radical Polymerization
journal, February 2005

Preparation and Characterization of Four-Branched Star Polystyrene
journal, July 1972

The Synthesis of Densely Grafted Copolymers by Atom Transfer Radical Polymerization
journal, December 1998

An Immobilized/Soluble Hybrid Catalyst System for Atom Transfer Radical Polymerization
journal, July 2001

Preparation and characterization of H-shaped polystyrene
journal, September 1981

Investigation of Methyl Methacrylate and Vinyl Acetate Polymerization Promoted by Al( ⁱ ^{Bu) ₃ /2,2‘-Bipyridine and Al( ⁱ ^{Bu) ₃ /2,2‘-Bipyridine/TEMPO Complexes}}
journal, October 1998

Anionic Copolymerization of Styrene with p-Divinylbenzene
journal, September 1970

Effect of arm number and arm molecular weight on the solid-state morphology of poly(styrene-isoprene) star block copolymers
journal, January 1986

Characterization of branched polymers by SEC coupled with a multiangle light scattering detector. II. Data processing and interpretation
journal, January 2001

Atom Transfer Radical Polymerization of Styrene Using a Novel Octafunctional Initiator: Synthesis of Well-Defined Polystyrene Stars
journal, October 1998

Scope of the Copper Halide/Bipyridyl System Associated with Calixarene-Based Multihalides for the Synthesis of Well-Defined Polystyrene and Poly(meth)acrylate Stars
journal, October 2000

Angular distribution of intensity of rayleigh scattering from comblike branched molecules
journal, December 1966

Calixarene-Core Multifunctional Initiators for the Ruthenium-Mediated Living Radical Polymerization of Methacrylates ¹
journal, October 1998

Chain Architecture and Asymmetry in Copolymer Microphases
journal, April 1994

Synthesis of Amphiphilic PS- b -PEG- b -PS by Atom Transfer Radical Polymerization
journal, January 1998

Dilute solution properties of branched macromolecules
journal, January 1992

Polymers with Complex Architecture by Living Anionic Polymerization
journal, December 2001

Synthesis and characterization of multiarm star polybutadienes
journal, July 1989

Preparation of Six-Branched Polystyrene. Thermodynamic and Hydrodynamic Porperties of Four- and Six-Branched Star Polystyrenes
journal, July 1974

Novel double hydrophilic block copolymers based on poly(p-hydroxystyrene) derivatives and poly(ethylene oxide)
journal, January 2007

Cylindrical polymer brushes
journal, January 2005

Double-Grafted Cylindrical Brushes: Synthesis and Characterization of Poly(lauryl methacrylate) Brushes
journal, August 2007

Effect of Ligand Structure on Activation Rate Constants in ATRP
journal, July 2006

Controlled/"living" radical polymerization. atom transfer radical polymerization in the presence of transition-metal complexes
journal, May 1995

Living Polymerization Methods
journal, February 1991

Synthesis and Characterization of Star Polymers with Varying Arm Number, Length, and Composition from Organic and Hybrid Inorganic/Organic Multifunctional Initiators
journal, October 1999

Multifunctional Initiators for the Ruthenium-Mediated Living Radical Polymerization of Methyl Methacrylate: Di- and Trifunctional Dichloroacetates for Synthesis of Multiarmed Polymers ¹
journal, February 1998

Atom Transfer Radical Polymerization
journal, September 2001

Highly efficient recyclable hydrated-clay supported catalytic system for atom transfer radical polymerization
journal, January 2009

Synthesis of Molecular Brushes by “Grafting onto” Method: Combination of ATRP and Click Reactions
journal, May 2007

Star polymers by ATRP of styrene and acrylates employing multifunctional initiators
journal, January 2005

Nickel-Mediated Living Radical Polymerization of Methyl Methacrylate ¹
journal, April 1997

Hydration Mediation in Supported Aqueous-Phase Catalysis for Atom Transfer Radical Polymerization
journal, November 2011

Amphiphilic Cylindrical Core−Shell Brushes via a “Grafting From” Process Using ATRP
journal, September 2001

Controlled/"Living" Radical Polymerization. Halogen Atom Transfer Radical Polymerization Promoted by a Cu(I)/Cu(II) Redox Process
journal, November 1995

Supported atom transfer radical polymerization of methyl methacrylate mediated by CuBr-tetraethyldiethylenetriamine grafted onto silica gel
journal, January 2001

Analysis and dilute solution properties of 12- and 18-arm-star polystyrenes
journal, March 1983

Synthesis of Molecular Brushes with Block Copolymer Side Chains Using Atom Transfer Radical Polymerization
journal, June 2001

New Stars: Eight Polyisobutylene Arms Emanating from a Calixarene Core ^†
journal, January 1996

“Green” Atom Transfer Radical Polymerization: From Process Design to Preparation of Well-Defined Environmentally Friendly Polymeric Materials
journal, June 2007

?Living? and controlled radical polymerization
journal, April 1995

Polymers with Very Low Polydispersities from Atom Transfer Radical Polymerization
journal, May 1996

Effects of hydration and hydrophilicity on Na-Clay-supported aqueous-phase catalysis for atom transfer radical polymerization
journal, September 2011

The Dimensions of Chain Molecules Containing Branches and Rings
journal, December 1949

Polymerization of Methyl Methacrylate with the Carbon Tetrachloride/Dichlorotris- (triphenylphosphine)ruthenium(II)/Methylaluminum Bis(2,6-di-tert-butylphenoxide) Initiating System: Possibility of Living Radical Polymerization
journal, September 1995