Synthesis of tri-block copolymer based on polyisobutylene and poly(ethylene glycol)

Gao, Bo; Kops, Jørgen

doi:10.1007/bf00294145

Cited by 18 publications

(14 citation statements)

References 18 publications

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“…The other alternative method of block copolymer synthesis is the coupling of functional polymers, which allows combining the polymers obtained by different mechanisms. However, the yield of polymer linkage with each other via functional group is usually low due to shielding of functionalities by long polymer chains 3…”

Section: Introductionmentioning

confidence: 99%

Synthesis of poly(glycidol)‐block‐poly(N‐isopropylacrylamide) copolymers using new hydrophilic poly(glycidol) macroinitiator

Mendrek

Adler

et al. 2008

J. Polym. Sci. A Polym. Chem.

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New, water soluble poly(glycidol) (PGl) macroinitiators for atom transfer radical polymerization (ATRP) were synthesized. This new class of macroinitiators were prepared in a three‐step process. First, series of well‐defined ω‐hydroxyl functional poly(glycidol acetal)s with different molecular weights was synthesized via anionic polymerization followed by quantitative termination of anionically growing active sites. End capping was achieved by treatment of living chain ends with water. The living nature of the system and termination reaction is discussed. In the second stage, monofunctional poly(glycidol acetal)s were functionalized by esterification with 2‐chloropropionyl chloride. Finally, selective deprotection (hydrolysis) of acetal protective groups was performed. As simultaneous partial cleavage of ester bond of attached ATRP moieties was unavoidable, the final functionality of macroinitiator calculated from 1H NMR varied in the range 85–95%. The obtained (2‐chloropropionyl) poly(glycidol) macroinitiator with DP = 55 and 90% functionality was successfully used in ATRP polymerization of N‐isopropylacrylamide (NIPAAm) at room temperature in the DMF/water mixture. Linear block copolymers with relatively narrow molecular weight distribution and controlled composition were obtained and characterized with 1H NMR and SEC‐MALLS measurements. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 2488–2499, 2008

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Section: Introductionmentioning

confidence: 99%

Synthesis of poly(glycidol)‐block‐poly(N‐isopropylacrylamide) copolymers using new hydrophilic poly(glycidol) macroinitiator

Mendrek

Adler

et al. 2008

J. Polym. Sci. A Polym. Chem.

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“…In the first step of the synthesis of MPEG-b-PS diblock copolymer (Figure 1), the macroinitiator is prepared by reacting MPEG with chloroacetyl chloride. In order to avoid the cleavage of the MPEG polymer chains, as found in case of other derivatizations of PEG, 26 the reaction was carried out at 0°C in THF in the presence of TEA and DMAP.…”

Section: Resultsmentioning

confidence: 99%

Synthesis and characterization of amphiphilic methoxypoly(ethylene glycol)-polystyrene diblock copolymer by ATRP and NMRP techniques

Abbasian

Bonab

Shoaeifar

et al. 2011

Journal of Elastomers & Plastics

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Amphiphilic block copolymers are used in a variety of applications, for example, as stabilizers for emulsions and dispersions or as compatibilizers in polymer blends. Amphiphilic diblock copolymer composed of methoxypoly(ethylene glycol) and polystyrene (MPEG-b-PS) was synthesized using atom transfer radical polymerization (ATRP) and nitroxide-mediated radical polymerization (NMRP). In order to synthesize MPEG-b-PS diblock copolymer using ATRP, monofunctional MPEG macroinitiator (chloroacetylated MPEG [MPEG-Cl]) was prepared from monohydroxyfunctional poly(ethylene glycol) and initiated end group on the basis of chloroacetyl chloride. ATRP was carried out in bulk using MPEG-Cl as the macroinitiator, copper chloride (CuCl)/2,2 0 -bipyridine (bipy) as the catalyst ([MPEG-Cl]/[CuCl]/[bipy] ¼ 1:1:3), and styrene as the monomer. For preparation of MPEG-b-PS by means of NMRP, firstly, 1-hydroxy-2,2,6,6-tetramethylpiperidine (TEMPO-OH) was obtained by reduction of 2,2,6,6-tetramethyl-piperidinyl-1oxy (TEMPO) with sodium ascorbat. Then, TEMPO-OH was coupled with chloroacetylated MPEG (MPEG-Cl) to yield the macroinitiator MPEG terminated with a TEMPO unit

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“…Material. The triblock copolymer, poly(ethylene oxide)−poly(isobutylene)−poly(ethylene oxide), PEO−PIB−PEO or EIBE, was synthesized using a two-step process in which poly(isobutylene), PIB, was functionalized with phenol at both ends, using boron triflouride etherate (BF 3 · OEt 2 ) as catalyst, and then coupled with tosylated monomethoxy poly(ethylene oxide), PEO …”

Section: Methodsmentioning

confidence: 99%

Structural Properties of Bulk and Aqueous Systems of PEO−PIB−PEO Triblock Copolymers As Studied by Small-Angle Neutron Scattering and Cryo-Transmission Electron Microscopy

et al. 1997

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The phase behavior of a low molecular weight (M w = 6000) symmetric triblock copolymer of poly(ethylene oxide) and poly(isobutylene), PEO−PIB−PEO, in the bulk as well in aqueous, D2O, solutions has been studied using small-angle neutron scattering and cryo-transmission electron microscopy. In aqueous solutions PEO−PIB−PEO self-associates into micelles. At low polymer concentration, the micelles predominantly have threadlike form, with lengths of typically 1−2000 Å. Those coexist, however, with spheroidal micelles of similar diameter. For a polymer concentration above roughly 20% the aggregates probably have a more disclike shape, as the micelles organize in lamellar structure. The 30% solution forms a bulk lamellar structure which, upon shear, organizes in a monodomain crystal. The bulk, PEO−PIB−PEO block copolymer forms at low temperatures a lamellar ordered phase induced by the PEO crystallization into lamellar sheets of PEO chains, presumably in helical form with a single fold. In a temperature regime near the transition temperature of T c ≈ 45 °C, the PEO chains unfold, giving rise to significant swelling of the lamellar. Above T c ≈ 45 °C, a strong correlation peak is observed corresponding to that observed in amorphous block copolymer systems, but it is still not clear whether this peak reflects strong concentration fluctuations of a disordered phase or the Bragg scattering of an ordered mesophase of amorphous blocks.

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Synthesis of tri-block copolymer based on polyisobutylene and poly(ethylene glycol)

Cited by 18 publications

References 18 publications

Synthesis of poly(glycidol)‐block‐poly(N‐isopropylacrylamide) copolymers using new hydrophilic poly(glycidol) macroinitiator

Synthesis of poly(glycidol)‐block‐poly(N‐isopropylacrylamide) copolymers using new hydrophilic poly(glycidol) macroinitiator

Synthesis and characterization of amphiphilic methoxypoly(ethylene glycol)-polystyrene diblock copolymer by ATRP and NMRP techniques

Structural Properties of Bulk and Aqueous Systems of PEO−PIB−PEO Triblock Copolymers As Studied by Small-Angle Neutron Scattering and Cryo-Transmission Electron Microscopy

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