Synthesis of poly-2-hydroxyethyl methacrylate–montmorillonite nanocomposite via in situ atom transfer radical polymerization

2008 ◽  
Vol 23 (12) ◽  
pp. 3316-3322 ◽  
Author(s):  
Ayhan Oral ◽  
Talal Shahwan ◽  
Çetin Güler
Keyword(s):  
Atom Transfer Radical Polymerization ◽  
Radical Polymerization ◽  
Interlayer Spacing ◽  
Solvent System ◽  
Polymerization Reaction ◽  
Atom Transfer ◽  
Scanning Calorimetry ◽  
Copper Bromide ◽  
Transmission Electron

The poly-2-hyroxyethyl methacrylate (PHEMA)/clay nanocomposite was synthesized by in situ atom transfer radical polymerization (ATRP) from initiator moieties immobilized within the silicate galleries of the clay particles. To produce organically modified montmorillonite (MMT) that has ATRP initiator moiety, a new catalyst that consists of quaternary ammonium salt moiety and an initiator moiety was synthesized. This initiator was intercalated into the interlayer spacing of the MMT. The polymerization reaction was carried out in a mixed solvent system consisting of methyl ethyl ketone and 1-propanol at 50 °C, using the initiator that has been already synthesized with a copper bromide catalyst. The 2, 2′-bipyridyl (bpy) complex was used as ligand. The products were characterized via Fourier transform infrared, nuclear magnetic resonance (1H NMR, 12C NMR), transmission electron microscopy, x-ray diffraction, thermogravimetric analysis, and differential scanning calorimetry.

scholarly journals In Situ Surface-Initiated Atom-Transfer Radical Polymerization Utilizing the Nonvolatile Nature of Ionic Liquids: A First Attempt

Polymers ◽  
2020 ◽  
Vol 13 (1) ◽  
pp. 61
Author(s):  
Ryo Satoh ◽  
Saika Honma ◽  
Hiroyuki Arafune ◽  
Ryo Shomura ◽  
Toshio Kamijo ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Liquid Film ◽  
Atom Transfer Radical Polymerization ◽  
Radical Polymerization ◽  
Silicon Wafer ◽  
Thin Liquid Film ◽  
Average Molecular Weight ◽  
Polymerization Reaction ◽  
Atom Transfer

In this paper, in situ surface-initiated atom-transfer radical polymerization (SI-ATRP) based on both an open and a coated system, without using volatile reagents, was developed to overcome the limited usage of ATRP due to the necessity of sealing. Nonvolatile ionic liquid (IL)-type components were used, specifically N,N-diethyl-N-(2-methacryloylethyl)-N-methylammonium bis(trifluoromethylsulfonyl)imide as the polymerizable monomer and N,N-diethylmethyl(2-methoxyethyl)ammonium bis(trifluoromethylsulfonyl)imide as the polymerization solvent. In the experiment, the reversible-deactivation radical polymerization characteristics are properly ensured in nonvolatile ATRP solution coated on silicon wafer as thin liquid film, to form concentrated polymer brushes (CPBs). The average molecular weight and molecular-weight distribution of the polymer produced in the liquid film and formed on silicon wafer were measured by gel permeation chromatography, which confirms that the polymerization reaction occurred as designed. Furthermore, it is clarified that the surface of the polymer brush synthesized in situ swollen by IL also exhibited low friction characteristics, comparable to that synthesized in a typical immersion process. This paper is the first to establish the effectiveness of in situ preparation for CPBs by using the coating technique.

Preparation, characterization, and properties of polystyrene/Na-montmorillonite composites

2018 ◽  
Vol 32 (8) ◽  
pp. 1078-1091 ◽  
Author(s):  
Sibel Erol Dağ ◽  
Pınar Acar Bozkurt ◽  
Fatma Eroğlu ◽  
Meltem Çelik
Keyword(s):  
Electron Microscopy ◽  
Interlayer Spacing ◽  
Decomposition Temperature ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Sem Images ◽  
Specific Pore Volume ◽  
Transmission Electron ◽  
Thermal Stability Of

A series of polystyrene (PS)/unmodified Na-montmorillonite (Na-MMT) composites were prepared via in situ radical polymerization. The prepared composites were characterized using various techniques. The presence of various functional groups in the unmodified Na-MMT and PS/unmodified Na-MMT composite was confirmed by Fourier transform infrared spectroscopy. Morphology and particle size of prepared composites was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). According to the XRD and TEM results, the interlayer spacing of MMT layers was expanded. SEM images showed a spongy and porous-shaped morphology of composites. TEM revealed the Na-MMT intercalated in PS matrix. The thermal stability of PS/unmodified Na-MMT composites was significantly improved as compared to PS, which is confirmed using thermogravimetric analysis (TGA). The TGA curves indicated that the decomposition temperature of composites is higher at 24–51°C depending on the composition of the mixture than that of pure PS. The differential scanning calorimetry (DSC) results showed that the glass transition temperature of composites was higher as compared to PS. The moisture retention, water uptake, Brunauer–Emmett–Teller specific surface area, and specific pore volume of composites were also investigated. Water resistance of the composites can be greatly improved.

Polystyrene–organoclay nanocomposites produced by in situ activators regenerated by electron transfer for atom transfer radical polymerization

2012 ◽  
Vol 32 (4-5) ◽  
pp. 235-243 ◽  
Author(s):  
Khezrollah Khezri ◽  
Vahid Haddadi-Asl ◽  
Hossein Roghani-Mamaqani ◽  
Mehdi Salami-Kalajahi
Keyword(s):  
Molecular Weight ◽  
Electron Transfer ◽  
Atom Transfer Radical Polymerization ◽  
Radical Polymerization ◽  
Polymer Matrix ◽  
Clay Content ◽  
Xrd Analysis ◽  
Size Exclusion ◽  
Atom Transfer ◽  
Scanning Calorimetry

Abstract A newly developed initiation system, activators regenerated by electron transfer (ARGET), was employed to synthesize polystyrene-organoclay nanocomposites via atom transfer radical polymerization (ATRP). ARGET ATRP was applied since it is carried out at significantly low concentrations of the catalyst and environmentally acceptable reducing agents. Conversion and molecular weight evaluations were performed using gravimetry and size exclusion chromatography (SEC), respectively. According to the findings, addition of clay content resulted in a decrease in conversion and molecular weight of nanocomposites. However, an increase of polydispersity index is observed by increasing nanoclay loading. The living nature of the polymerization is revealed by 1H NMR spectroscopy and extracted data from the SEC traces. X-ray diffraction (XRD) analysis shows that organoclay layers are disordered and delaminated in the polymer matrix and exfoliated morphology is obtained. Thermogravimetric analysis (TGA) shows that thermal stability of the nanocomposites is higher than the neat polystyrene. A decrease in glass transition temperature of the samples by increasing organoclay content is observed by differential scanning calorimetry (DSC). Transmission electron microscopy (TEM) reveals that clay layers are partially exfoliated in the polymer matrix containing 2 wt% of organomodified montmorillonite (PSON 2) and a dispersion of partially exfoliated clay stacks is formed.

Sign in / Sign up

Export Citation Format

Share Document