scholarly journals Synthesis of polystyrene-block-poly(iso-butyl vinyl ether) by dinuclear half-metallocene catalyst and atom transfer radical polymerization

2015 ◽  
Vol 18 (3) ◽  
pp. 189-199
Author(s):  
Thanh Thi Le Nguyen ◽  
Nhon Thi Le Nguyen

The synthesis of polystyrene-block-poly(iso-butyl vinyl ether) by using the combination of metallocene catalyst and atom transfer radical polymerization (ATRP) has been tried. This synthetic method takes advantages of both metallocene catalyst to form stereoregular polymer with high activity and ATRP with the controlled molecular weights and low polydispersity. The recent dinuclear half-sandwich complexes of titanium with xylene bridge, [Ti(η5-cyclopentadienyl)Cl2L]2-ortho, meta-[CH2-C6H4-CH2] (L = Cl, L = O-2,6-iPr2C6H3 ) were successfully synthesized. These catalysts were characterized by 1H NMR, 13C NMR and elemental analysis. Copolymers have been characterized by using gel permeation chromatography (GPC) and nuclear magnetic resonance (NMR). The collected copolymers have got narrow molecular weight distribution (≤1.8) and the improvement of stereoregularity (racemo dyads, r, are from 45 % to 56 %).

2018 ◽  
Vol 18 (3) ◽  
pp. 537 ◽  
Author(s):  
Melahat Göktaş ◽  
Guodong Deng

Poly(methyl methacrylate)-b-poly(N-isopropylacrylamide) [PMMA-b-PNIPAM] block copolymers were obtained by a combination of redox polymerization and atom transfer radical polymerization (ATRP) methods in two steps. For this purpose, PMMA macroinitator (ATRP-macroinitiator) was synthesized by redox polymerization of methyl methacrylate and 3-bromo-1-propanol using Ce(NH4)2(NO3)6 as a catalyst. The synthesis of PMMA-b-PNIPAM block copolymers was carried out by means of ATRP of ATRP-macroinitiator and NIPAM at 60 °C. The block copolymers were obtained in high yield and high molecular weight. The characterization of products was accomplished by using multi instruments and methods such as nuclear magnetic resonance spectroscopy, Fourier transform infrared spectroscopy, gel permeation chromatography, and thermogravimetric analysis.


1999 ◽  
Vol 32 (2) ◽  
pp. 290-293 ◽  
Author(s):  
Kenji Yamada ◽  
Masayuki Miyazaki ◽  
Kohji Ohno ◽  
Takeshi Fukuda ◽  
Masahiko Minoda

e-Polymers ◽  
2007 ◽  
Vol 7 (1) ◽  
Author(s):  
Aihua Zhu ◽  
Zhi Wang ◽  
Meiran Xie ◽  
Yiqun Zhang

AbstractThe synthesis of imidazole end-capped poly(n-butyl methacrylate)s via atom transfer radical polymerization (ATRP) is reported. n-Butyl methacrylate (n- BMA) was polymerized in isopropyl alcohol (IPA) at different temperatures via ATRP using a new N-heterocyclic functional initiator (1-α-bromoisobutylimidazole, BrBI) in the presence of CuBr/2,2’-bipyridine (bpy) as the catalyst. With this new initiating system, a successful ATRP of n-BMA was carried out, and imidazole endcapped polymers with predetermined molecular weights and low polydispersities (1.1<PDI<1.3) were obtained at low polymerization temperature (below 80 °C). Furthermore, the dependence of both the rate of polymerization and PDI on temperature gave the optimal reaction temperature (50 °C). However, at elevated temperature (especially above 80 °C), some different phenomena appeared in the polymerization: the conversion of monomer remains constant after reaching a maximum value (20%-30%), and the higher the temperature, the lower the conversion obtained.


2015 ◽  
Vol 1 (6) ◽  
pp. 874-881 ◽  
Author(s):  
Linlin Duan ◽  
Qianqian Zhao ◽  
Jindun Liu ◽  
Yatao Zhang

Poly(4-vinylpyridine) (P4VP) with various molecular weights was grafted onto halloysite nanotubes (HNTs) via reverse atom transfer radical polymerization (RATRP).


2013 ◽  
Vol 295-298 ◽  
pp. 3-7
Author(s):  
Guo Bin Yi ◽  
Ying Wu ◽  
Ping Ke Ai

The reverse atom transfer radical polymerization (RATRP) of N-vinylpyrrolidone (NVP) using azobisisobutyronitrile (AIBN)/FeCl3/triphenylphosphine(PPh3) as the initiating system, was successfully carried out in bulk at 80°C. Plots of In ([M]0/[M]) vs time and molecular weight evolution vs monomer conversion presented a linear dependence and the polymerization was proved to accord with the first-order kinetics. After 10 hours’ reaction, the monomer conversion was up to 84%. Gel permeation chromatography (GPC) was used in testing the molecular weight of polymer and molecular weight distribution, the results showed that polymer molecular weight distribution was as low as 1.018 (Mn=3288 g/mol). Moreover, the resultant polymer was characterized by 1H-NMR, 13C-NMR spectroscopy and Pyrolysis GC-MS, and the results showed that the polymerization mechanism is consistent with RATRP.


e-Polymers ◽  
2006 ◽  
Vol 6 (1) ◽  
Author(s):  
Huiqi Zhang ◽  
Caroline H. Abeln ◽  
Martin W. M. Fijten ◽  
Ulrich S. Schubert

AbstractCombinatorial chemistry and high-throughput experimentation have drawn great attention in recent years because of their significant advantages in increasing the research productivity. One of the emerging fields is their application in polymer science. Herein we describe the high-throughput optimization of purification conditions for polymers prepared via atom transfer radical polymerization using an automated synthesizer. The effects of the column materials, column lengths and eluent volumes on the purification efficiency as well as the molecular weights of the obtained purified polymers were systematically investigated for the first time. The optimum purification conditions for the removal of copper catalysts are provided. As a result an online high-throughput purification workflow using SPE cartridges is now available for the utilization in automated parallel synthesizers for ATRP screening experiment.


Polymers ◽  
2020 ◽  
Vol 12 (4) ◽  
pp. 763 ◽  
Author(s):  
Sibo Li ◽  
Mengying Tian ◽  
Jirong Wang ◽  
Feipeng Du ◽  
Liang Li ◽  
...  

The Br-terminated poly (ethylene oxide) (PEO-Br) is used as a green and efficient macroinitiator in bulk Fe-catalyzed atom transfer radical polymerization (ATRP) without the addition of any organic ligands. The polymerization rate is able to be mediated by PEO-Br with various molecular weights, and the decrease in redox potential of FeBr2 in cyclic voltammetry (CV) curves indicates that an increased coordination effect is deteriorated with the depressing reaction activity in the longer ethylene oxide (EO) chain in PEO-Br. In combination with the study of different catalysts and catalytic contents, the methyl metharylate (MMA) or poly (ethylene glycol) monomethacrylate (PEGMA) was successfully polymerized with PEO-Br as an initiator. This copolymer obtained from PEGMA polymerization can be further employed as a polymer matrix to form the polymer electrolyte (PE). The higher ionic conductivity of PE was obtained by using a high molecular weight of copolymer.


2012 ◽  
Vol 535-537 ◽  
pp. 1516-1519
Author(s):  
Ying Gang Jia ◽  
Peng Tian ◽  
Kun Ming Song ◽  
Bao Yan Zhang

Atom transfer radical polymerization (ATRP) of methacrylate liquid crystal monomer M (4-((4-(2-(acryloyloxy)ethoxy)benzoyl)oxy)phenyl 4-propylbenzoate) was carried out using CuBr/PMDETA complex as catalyst and 2-bromo-2-methyl-propionic acid ester as initiator. The obtained monomer M and polymer P was characterized via infrared spectroscopy and1H NMR. The phase behavior and mesomorphism were investigated by differential scanning calorimetry (DSC), polarizing optical microscopy (POM), and x-ray diffraction (XRD). The molecular weight and the structure of the polymers were identified with gel permeation chromatography and nuclear magnetic resonance.


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