Determination of the Intra- and Intermolecular Microstructure of Bulk and Emulsion Copolymers of Styrene and 2-Hydroxyethyl Methacrylate by Means of Proton NMR and Gradient Polymer Elution Chromatography

Schoonbrood, Harold A. S.; Aerdts, Annemieke M.; German, Anton L.; Velden, G. P. M. Van der

doi:10.1021/ma00120a016

Cited by 30 publications

(24 citation statements)

References 19 publications

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“…The composition drift was analysed by following the average terpolymer composition as a function of conversion using 1 H NMR. [23,24] In Fig. 3 a and 3 b, the 1 H NMR spectra at l 70% conversion are shown for terpolymers prepared by COPhBF and DDM, respectively; very similar spectra were obtained during the entire course of polymerization in both systems.…”

Section: Composition Driftmentioning

confidence: 77%

Preparation and characterization of oligomeric terpolymers of styrene, methyl methacrylate and 2-hydroxyethyl methacrylate: A comparison of conventional and catalytic chain transfer

Heuts

Muratore

Davis

2000

Macromol. Chem. Phys.

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Batch solution terpolymerizations of styrene, methyl methacrylate and 2‐hydroxyethyl methacrylate were carried out at 70°C in the presence of either dodecanethiol or bis[(difluoroboryl)diphenylglyoximato]cobalt‐(II) (COPhBF), to yield polymer products with a number average molecular weight of about 2 500. Conversion, molecular weight distribution and overall composition were monitored during the reaction, and the final products were investigated using differential scanning calorimetry and thermogravimetric analysis. It was found that the overall rates of polymerization do not differ significantly in the two systems, but that the molecular weight distribution of the polymer formed in the presence of the thiol becomes increasingly broader during the polymerization, whereas the COPhBF‐mediated polymerization produces a relatively uniform product during the course of the reaction. The polymer product formed with COPhBF was found to be slightly less thermally stable than the product formed by the thiol, which can be explained by the formation of unsaturated endgroups in the case of the former product.

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Section: Composition Driftmentioning

confidence: 77%

Preparation and characterization of oligomeric terpolymers of styrene, methyl methacrylate and 2-hydroxyethyl methacrylate: A comparison of conventional and catalytic chain transfer

Heuts

Muratore

Davis

2000

Macromol. Chem. Phys.

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“…Several works focused on the study of acrylic copolymers, widely used as resins for coatings, appeared recently in the literature. In particular, the free radical copolymerization kinetics was investigated to get a good understanding of the mechanism of copolymer chain‐growth [1–7]. Copolymers based on 2‐hydroxyethyl acrylate (HEA) were reported by copolymerization with ethers, acrylates, or methacrylates [8–13].…”

Section: Introductionmentioning

confidence: 99%

A quantum chemistry study of the free‐radical copolymerization propagation kinetics of styrene and 2‐hydroxyethyl acrylate

Dossi

Storti

Moscatelli

2011

Polymer Engineering & Sci

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Several difficulties are reported in literature about the experimental analysis of polymerizations involving 2‐hydroxyethyl acrylate (HEA), mainly due to transfer reactions that characterize the system. In particular, major problems are emerged in the study of free radical copolymerization kinetics of HEA. In this work, free‐radical copolymerization propagation kinetics of HEA and styrene (ST) are investigated through a computational approach based on density functional theory. Monomer reactivity ratios for HEA/ST copolymerization are calculated at 50°C and 125°C, obtaining values that exhibit a weak dependence on temperature. In particular, HEA reactivity ratio, rHEA, equal to 0.14 and ST reactivity ratio, rST, equal to 0.31 at 50°C, whereas rHEA = 0.17 and rST = 0.29 at 125°C. Moreover, the reliability of such parameters has been tested by analyzing copolymer composition data as a function of monomer feed composition, at the same temperatures indicated above. Experimental values proposed in literature are well predicted by the terminal copolymerization model using the kinetic parameters computationally determined. POLYM. ENG. SCI., 2011. © 2011 Society of Plastics Engineers

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“…For HEMA/S copolymerizations, the effect of solvent was pronounced . In DMF solution, the monomer reactivity ratios for HEMA/S were 0.45/0.53 ( r s / r HEMA , 90.0 °C, 50 vol% DMF), compared to the values of 0.27/0.49, respectively, reported in bulk ( r s / r HEMA , 50.0 °C) . Table summarized the related kinetic data for copolymerization of HEMA with S and of MMA with S. The 〈 k p 〉〈 K 〉 value could be estimated from the apparent rate constant.…”

Section: Resultsmentioning

confidence: 99%

Nitroxide‐Mediated Polymerization of 2‐Hydroxyethyl Methacrylate (HEMA) Controlled with Low Concentrations of Acrylonitrile and Styrene

Mei

Marić

2017

Macro Reaction Engineering

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Nitroxide‐mediated controlled radical polymerization of 2‐hydroxyethyl methacrylate (HEMA) is achieved using the copolymerization method with a small initial concentration of acrylonitrile (AN, 5–16 mol%)) or styrene (S, 5–10 mol%). The polymerization is mediated by N‐tert‐butyl‐N‐(1‐diethyl phosphono‐2,2‐dimethyl propyl) nitroxide (SG1)‐based BlocBuilder unimolecular alkoxyamine initiator modified with an N‐succinimidyl ester group (N‐hydroxysuccinimide‐BlocBuilder). As little as 5% molar feed of acrylonitrile results in a controlled polymerization, as evidenced by a linear increase in number average molecular weight Mn with conversion and dispersities (Đ) as low as 1.30 at 80% conversion in N,N‐dimethylformamide (DMF) at 85 °C. With S as the controlling comonomer, higher initial S composition (≈10 mol%) is required to maintain the controlled copolymerization. Poly(HEMA‐ran‐AN)s with Mn ranging from 5 to 20 kg mol−1 are efficiently chain extended using n‐butyl methacrylate/styrene mixtures at 90.0 °C in DMF, thereby showing a route to HEMA‐based amphiphilic block copolymers via nitroxide‐mediated polymerization.

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Determination of the Intra- and Intermolecular Microstructure of Bulk and Emulsion Copolymers of Styrene and 2-Hydroxyethyl Methacrylate by Means of Proton NMR and Gradient Polymer Elution Chromatography

Cited by 30 publications

References 19 publications

Preparation and characterization of oligomeric terpolymers of styrene, methyl methacrylate and 2-hydroxyethyl methacrylate: A comparison of conventional and catalytic chain transfer

Preparation and characterization of oligomeric terpolymers of styrene, methyl methacrylate and 2-hydroxyethyl methacrylate: A comparison of conventional and catalytic chain transfer

A quantum chemistry study of the free‐radical copolymerization propagation kinetics of styrene and 2‐hydroxyethyl acrylate

Nitroxide‐Mediated Polymerization of 2‐Hydroxyethyl Methacrylate (HEMA) Controlled with Low Concentrations of Acrylonitrile and Styrene

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