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Atom Transfer Radical Polymerization (ATRP) in Synthesis of Precisely Defined Polymers

A special issue of Materials (ISSN 1996-1944). This special issue belongs to the section "Polymeric Materials".

Deadline for manuscript submissions: closed (20 September 2022) | Viewed by 29810

Special Issue Editor

Prof. Dr. Paweł Chmielarz

E-Mail Website
Guest Editor
Department of Physical Chemistry, Faculty of Chemistry, Rzeszow University of Technology, Rzeszow, Poland
Interests: polymer synthesis and analysis; electrochemistry; atom transfer radical polymerization (ATRP); electrochemically mediated atom transfer radical polymerization (eATRP)
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

In the last decade, there have been increasing research activities in the use of atom transfer radical polymerization (ATRP) to prepare well-defined polymers. ATRP is one of the most rapidly developing areas of polymer science that allows easy control over molecular weight, preparation of polymers with narrow molecular weight distributions, incorporation of precisely placed functionalities, and fabrication of various architectures. Significant efforts have been dedicated to the green chemistry class of this approach, including low ppm ATRP techniques, which are based on improving regeneration processes of copper in the lower oxidation state using appropriate reducing agent or external stimuli.

This Special Issue is intended to cover the latest advances and developments in the synthesis of precisely defined polymers with different architecture with an emphasize on ATRP methods with diminished catalyst concentration, which offers a more environmentally benign and industrially relevant alternative for synthesizing polymers compared to normal ATRP. Topics include, but are not limited to, optimization of reaction setup, kinetics investigation of synthesis processes, characterization of ATRP macroinitiators, and received macromolecules including naturally-derived polymers.

It is my pleasure to invite you to submit a manuscript for this Special Issue. Original, high-quality research articles and reviews are all welcome.

Prof. Paweł Chmielarz
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Materials is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • Controlled polymerization
  • Well-defined polymers
  • Polymers with different architecture
  • Functional polymers
  • Bio-hybrid polymers
  • Naturally-derived macromolecules
  • Smart materials

Published Papers (7 papers)

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Research

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20 pages, 2360 KiB  
Article
Experimental Investigation of Methyl Methacrylate in Stirred Batch Emulsion Reactor: AGET ATRP Approach
by Mohammed Awad, Thomas Duever and Ramdhane Dhib
Materials 2020, 13(24), 5793; https://0-doi-org.brum.beds.ac.uk/10.3390/ma13245793 - 18 Dec 2020
Cited by 4 | Viewed by 2024
Abstract
This study examines the ab initio emulsion atom transfer radical polymerization (ATRP) initiated by an eco-friendly reducing agent to produce poly(methyl methacrylate) (PMMA) polymer with controlled characteristics in a 2 L stirred batch reactor. The effect of the reaction temperature, surfactant concentration, monomer [...] Read more.
This study examines the ab initio emulsion atom transfer radical polymerization (ATRP) initiated by an eco-friendly reducing agent to produce poly(methyl methacrylate) (PMMA) polymer with controlled characteristics in a 2 L stirred batch reactor. The effect of the reaction temperature, surfactant concentration, monomer to water ratio, and stirring speed was thoroughly investigated. The results showed that PMMA coagulation becomes quite severe at a certain temperature threshold. However, the coagulation could be avoided at mild reaction temperature, since the outcomes showed that loading more surfactant to the system under high mixing speed has balanced the polymer mixture and yielded high monomer conversion. The PMMA product was analyzed by gravimetry and GPC measurements and after 5 h of polymerization at a reaction temperature of 50 °C, monomer conversion of 64.1% was obtained, and PMMA polymer samples produced had an average molar mass of 4.5 kg/mol and a polydispersity index of 1.17. The structure of the PMMA polymer was successfully proved by FTIR and nuclear magnetic resonance (NMR) spectroscopy. The results confirm the living feature of MMA AGET ATRP in emulsion medium and recommend further investigation for other types of surfactant. Full article
(This article belongs to the Special Issue Atom Transfer Radical Polymerization (ATRP) in Synthesis of Precisely Defined Polymers)
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17 pages, 3578 KiB  
Article
Surface-Initiated Photoinduced Iron-Catalyzed Atom Transfer Radical Polymerization with ppm Concentration of FeBr3 under Visible Light
by Monika Słowikowska, Kamila Chajec, Adam Michalski, Szczepan Zapotoczny and Karol Wolski
Materials 2020, 13(22), 5139; https://0-doi-org.brum.beds.ac.uk/10.3390/ma13225139 - 14 Nov 2020
Cited by 13 | Viewed by 2593
Abstract
Reversible deactivation radical polymerizations with reduced amount of organometallic catalyst are currently a field of interest of many applications. One of the very promising techniques is photoinduced atom transfer radical polymerization (photo-ATRP) that is mainly studied for copper catalysts in the solution. Recently, [...] Read more.
Reversible deactivation radical polymerizations with reduced amount of organometallic catalyst are currently a field of interest of many applications. One of the very promising techniques is photoinduced atom transfer radical polymerization (photo-ATRP) that is mainly studied for copper catalysts in the solution. Recently, advantageous iron-catalyzed photo-ATRP (photo-Fe-ATRP) compatible with high demanding biological applications was presented. In response to that, we developed surface-initiated photo-Fe-ATRP (SI-photo-Fe-ATRP) that was used for facile synthesis of poly(methyl methacrylate) brushes with the presence of only 200 ppm of FeBr3/tetrabutylammonium bromide catalyst (FeBr3/TBABr) under visible light irradiation (wavelength: 450 nm). The kinetics of both SI-photo-Fe-ATRP and photo-Fe-ATRP in solution were compared and followed by 1H NMR, atomic force microscopy (AFM) and gel permeation chromatography (GPC). Brush grafting densities were determined using two methodologies. The influence of the sacrificial initiator on the kinetics of brush growth was studied. It was found that SI-photo-Fe-ATRP could be effectively controlled even without any sacrificial initiators thanks to in situ production of ATRP initiator in solution as a result of reaction between the monomer and Br radicals generated in photoreduction of FeBr3/TBABr. The optimized and simplified reaction setup allowed synthesis of very thick (up to 110 nm) PMMA brushes at room temperature, under visible light with only 200 ppm of iron-based catalyst. The same reaction conditions, but with the presence of sacrificial initiator, enabled formation of much thinner layers (18 nm). Full article
(This article belongs to the Special Issue Atom Transfer Radical Polymerization (ATRP) in Synthesis of Precisely Defined Polymers)
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21 pages, 3088 KiB  
Article
Stimuli-Responsive Rifampicin-Based Macromolecules
by Izabela Zaborniak, Angelika Macior and Paweł Chmielarz
Materials 2020, 13(17), 3843; https://0-doi-org.brum.beds.ac.uk/10.3390/ma13173843 - 31 Aug 2020
Cited by 5 | Viewed by 2825
Abstract
This paper presents the modification of the antibiotic rifampicin by an anionic polyelectrolyte using a simplified electrochemically mediated atom transfer radical polymerization (seATRP) technique to receive stimuli-responsive polymer materials. Initially, a supramolecular ATRP initiator was prepared by an esterification reaction of [...] Read more.
This paper presents the modification of the antibiotic rifampicin by an anionic polyelectrolyte using a simplified electrochemically mediated atom transfer radical polymerization (seATRP) technique to receive stimuli-responsive polymer materials. Initially, a supramolecular ATRP initiator was prepared by an esterification reaction of rifampicin hydroxyl groups with α-bromoisobutyryl bromide (BriBBr). The structure of the initiator was successfully proved by nuclear magnetic resonance (1H and 13C NMR), Fourier-transform infrared (FT-IR) and ultraviolet–visible (UV-vis) spectroscopy. The prepared rifampicin-based macroinitiator was electrochemically investigated among various ATRP catalytic complexes, by a series of cyclic voltammetry (CV) measurements, determining the rate constants of electrochemical catalytic (EC’) process. Macromolecules with rifampicin core and hydrophobic poly (n-butyl acrylate) (PnBA) and poly(tert-butyl acrylate) (PtBA) side chains were synthesized in a controlled manner, receiving polymers with narrow molecular weight distribution (Mw/Mn = 1.29 and 1.58, respectively). “Smart” polymer materials sensitive to pH changes were provided by transformation of tBA into acrylic acid (AA) moieties in a facile route by acidic hydrolysis. The pH-dependent behavior of prepared macromolecules was investigated by dynamic light scattering (DLS) determining a hydrodynamic radius of polymers upon pH changes, followed by a control release of quercetin as a model active substance upon pH changes. Full article
(This article belongs to the Special Issue Atom Transfer Radical Polymerization (ATRP) in Synthesis of Precisely Defined Polymers)
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Review

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16 pages, 2478 KiB  
Review
Low Ppm Atom Transfer Radical Polymerization in (Mini)Emulsion Systems
by Karolina Surmacz and Paweł Chmielarz
Materials 2020, 13(7), 1717; https://0-doi-org.brum.beds.ac.uk/10.3390/ma13071717 - 06 Apr 2020
Cited by 12 | Viewed by 3208
Abstract
In the last decade, unceasing interest in atom transfer radical polymerization (ATRP) has been noted, especially in aqueous dispersion systems. Emulsion or miniemulsion is a preferred environment for industrial polymerization due to easier heat dissipation and lower production costs associated with the use [...] Read more.
In the last decade, unceasing interest in atom transfer radical polymerization (ATRP) has been noted, especially in aqueous dispersion systems. Emulsion or miniemulsion is a preferred environment for industrial polymerization due to easier heat dissipation and lower production costs associated with the use of water as a dispersant. The main purpose of this review is to summarize ATRP methods used in emulsion media with different variants of initiating systems. A comparison of a dual over single catalytic approache by interfacial and ion pair catalysis is presented. In addition, future development directions for these methods are suggested for better use in biomedical and electronics industries. Full article
(This article belongs to the Special Issue Atom Transfer Radical Polymerization (ATRP) in Synthesis of Precisely Defined Polymers)
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15 pages, 2698 KiB  
Review
Surface Modifications of Poly(Ether Ether Ketone) via Polymerization Methods—Current Status and Future Prospects
by Monika Flejszar and Paweł Chmielarz
Materials 2020, 13(4), 999; https://0-doi-org.brum.beds.ac.uk/10.3390/ma13040999 - 23 Feb 2020
Cited by 35 | Viewed by 4981
Abstract
Surface modification of poly(ether ether ketone) (PEEK) aimed at applying it as a bone implant material aroused the unflagging interest of the research community. In view of the development of implantology and the growing demand for new biomaterials, increasing biocompatibility and improving osseointegration [...] Read more.
Surface modification of poly(ether ether ketone) (PEEK) aimed at applying it as a bone implant material aroused the unflagging interest of the research community. In view of the development of implantology and the growing demand for new biomaterials, increasing biocompatibility and improving osseointegration are becoming the primary goals of PEEK surface modifications. The main aim of this review is to summarize the use of polymerization methods and various monomers applied for surface modification of PEEK to increase its bioactivity, which is a critical factor for successful applications of biomedical materials. In addition, the future directions of PEEK surface modifications are suggested, pointing to low-ppm surface-initiated atom transfer radical polymerization (SI-ATRP) as a method with unexplored capacity for flat surface modifications. Full article
(This article belongs to the Special Issue Atom Transfer Radical Polymerization (ATRP) in Synthesis of Precisely Defined Polymers)
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15 pages, 2353 KiB  
Review
Ultrasound-Mediated Atom Transfer Radical Polymerization (ATRP)
by Izabela Zaborniak and Paweł Chmielarz
Materials 2019, 12(21), 3600; https://0-doi-org.brum.beds.ac.uk/10.3390/ma12213600 - 02 Nov 2019
Cited by 42 | Viewed by 5832
Abstract
Ultrasonic agitation is an external stimulus, rapidly developed in recent years in the atom transfer radical polymerization (ATRP) approach. This review presents the current state-of-the-art in the application of ultrasound in ATRP, including an initially-developed, mechanically-initiated solution with the use of piezoelectric nanoparticles, [...] Read more.
Ultrasonic agitation is an external stimulus, rapidly developed in recent years in the atom transfer radical polymerization (ATRP) approach. This review presents the current state-of-the-art in the application of ultrasound in ATRP, including an initially-developed, mechanically-initiated solution with the use of piezoelectric nanoparticles, that next goes to the ultrasonication-mediated method utilizing ultrasound as a factor for producing radicals through the homolytic cleavage of polymer chains, or the sonolysis of solvent or other small molecules. Future perspectives in the field of ultrasound in ATRP are presented, focusing on the preparation of more complex architectures with highly predictable molecular weights and versatile properties. The challenges also include biohybrid materials. Recent advances in the ultrasound-mediated ATRP point out this approach as an excellent tool for the synthesis of advanced materials with a wide range of potential industrial applications. Full article
(This article belongs to the Special Issue Atom Transfer Radical Polymerization (ATRP) in Synthesis of Precisely Defined Polymers)
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28 pages, 12950 KiB  
Review
Surface-Initiated Atom Transfer Radical Polymerization for the Preparation of Well-Defined Organic–Inorganic Hybrid Nanomaterials
by Monika Flejszar and Paweł Chmielarz
Materials 2019, 12(18), 3030; https://0-doi-org.brum.beds.ac.uk/10.3390/ma12183030 - 18 Sep 2019
Cited by 24 | Viewed by 6173
Abstract
Surface-initiated atom transfer radical polymerization (SI-ATRP) is a powerful tool that allows for the synthesis of organic–inorganic hybrid nanomaterials with high potential applications in many disciplines. This review presents synthetic achievements and modifications of nanoparticles via SI-ATRP described in literature last decade. The [...] Read more.
Surface-initiated atom transfer radical polymerization (SI-ATRP) is a powerful tool that allows for the synthesis of organic–inorganic hybrid nanomaterials with high potential applications in many disciplines. This review presents synthetic achievements and modifications of nanoparticles via SI-ATRP described in literature last decade. The work mainly focuses on the research development of silica, gold and iron polymer-grafted nanoparticles as well as nature-based materials like nanocellulose. Moreover, typical single examples of nanoparticles modification, i.e., ZnO, are presented. The organic–inorganic hybrid systems received according to the reversible deactivation radical polymerization (RDRP) approach with drastically reduced catalyst complex concentration indicate a wide range of applications of materials including biomedicine and microelectronic devices. Full article
(This article belongs to the Special Issue Atom Transfer Radical Polymerization (ATRP) in Synthesis of Precisely Defined Polymers)
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