Analysis of Compositional Drift in Methyl Methacrylate and n-Butyl Acrylate Copolymers Synthesized by Atom Transfer Radical Polymerization Using 13C{1H} NMR Spectroscopy

Brar, A. S.; Kaur, Sukhdeep

doi:10.1295/polymj.37.316

Cited by 16 publications

(11 citation statements)

References 23 publications

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“…Their spectra were analyzed in deuterochloroform (CDCl3) solvent, and tetramethylsilane (TMS) was used as an internal reference. The mole fraction of MMA unit and n-BA unit in the copolymer was calculated from the 1 H-NMR spectra using the following equation 10,11 :…”

Section: Proton Nuclear Magnetic Resonance ( 1 H-nmr)mentioning

confidence: 99%

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Copolymerization of n-butyl acrylate/methyl methacrylate in xylene solvent

Linh

Duc²,

Phu

2019

Sci. Tech. Dev. J.

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Introduction: Copolymers are being used in a variety of fields because of their diversity and since any change could result in significant modifications. The butyl acrylate/methyl methacrylate copolymer is an extensively used polymer system with many advantages. This study aims to analyze some changes in copolymerization, from using different time or temperature of synthesis, in order to find an optimal process that can be applied in Vietnam. Methods: Copolymerization of butyl acrylate/methyl methacrylate copolymer with different butyl acrylate/methyl methacrylate monomer ratios was done using Xylene solvent. Copolymer compositions were determined from the Proton nuclear magnetic resonance spectra and Gel permeation chromatography. Results: The experimental results indicate that the copolymer was successfully synthesized. The highest molecular weight was 15,591 g/mol, with the lowest dispersity of 1.53 at 100 oC after 6 hours of copolymerization.

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Section: Proton Nuclear Magnetic Resonance ( 1 H-nmr)mentioning

confidence: 99%

“…The shift δ=4.04 ppm (3) represented the specialized methylene hydrogen (-CH2 -) in ester linkages (-COOCH2-) of the n-BA unit. The particular shifts on the 1 H-NMR spectrum were according to the de-shield effect and 1 H-NMR table 10,12 .…”

Section: Characteristics Of the N-ba/mma Copolymer Using 1 H-nmrmentioning

confidence: 99%

Copolymerization of n-butyl acrylate/methyl methacrylate in xylene solvent

Linh

Duc²,

Phu

2019

Sci. Tech. Dev. J.

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“…Due to large difference in the monomer reactivity ratios, any variation in the relative concentration of monomers may incorporate gradiency [42][43][44] in the copolymer chains. Figure 7 shows F C (molar fraction of C unit in the copolymer) as a function of the conversion for two different in-feed compositions (f C ).…”

Section: Copolymer Composition and Reactivity Ratio Determinationmentioning

confidence: 99%

Optimization of Atom Transfer Radical Copolymerization of Allyl Butyl Ether with Acrylonitrile

Brar

Saini

2007

Polym J

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ABSTRACT:The optimization of atom transfer radical polymerization (ATRP) conditions for the copolymerization of allyl butyl ether with acrylonitrile has been carried out with the aim of achieving control over molecular parameters. The influence of solvents, initiator concentration and in-feed molar compositions on the rate of copolymerization was also investigated. The molecular weight data as well as kinetic studies suggested conventional ATRP behavior of the copolymerization of acrylonitrile and allyl butyl ether. The variation of copolymer composition (F C ) with conversion indicated towards the synthesis of copolymers having significant changes in composition with conversion. The copolymer compositions obtained from 1 H NMR spectra were utilized to determine the reactivity ratios. With the help of DEPT (Distortionless Enhancement by Polarization Transfer) and 2D HSQC (Heteronuclear Single Quantum Coherence) NMR spectra, complete spectral assignments of 1 H and 13 C{

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“…The theoretical concentrations of various triads were calculated from the reactivity ratios using the methodology described elsewhere. 38 The experimentally observed M-centered triad fractions were estimated by determining the area under the resonance peaks using the Lorentzian curve-fitting. Curve fitting was done using an electronic integrator.…”

Section: D Hmbc Spectral Analysismentioning

confidence: 99%

“…taneous composition arising from these variations are reflected along all the chains, 28,29,37,38 resulting in the synthesis of gradient copolymers. The study of the arrangement of monomer units in these types of copolymers will be important as well as interesting, to understand the physical properties of copolymers 39 such as glass transition temperature, morphology, and the crystallinity, which are greatly influenced by the composition, molecular weight, molecular weight distribution, and sequence distribution.…”

mentioning

confidence: 99%

2D NMR Analysis of Acrylonitrile/2-Methoxyethyl Acrylate Copolymers Synthesized by Atom Transfer Radical Polymerization

Brar

Saini

2006

Polym J

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ABSTRACT:The copolymerization of acrylonitrile (A) and 2-methoxyethyl acrylate (M) at three different molar in-feed compositions was carried out under atom transfer radical polymerization (ATRP) conditions using 2-bromopropionitrile (BPN) as initiator and CuCl/2,2 0 -bipyridine (bpy) as catalyst system in ethylene carbonate at 60 C. Linear first order kinetics, linearly increasing molecular weight with conversion, and low polydispersities were observed for all the copolymerization. The copolymer compositions, obtained from 1 H NMR spectra, were utilized to determine the monomer reactivity ratios (r A ¼ 1:52 and r M ¼ 0:60) involved in ATRP. Two-dimensional NMR [Heteronuclear Single Quantum Correlation (HSQC) and Total Correlated Spectroscopy (TOCSY)] experiments in conjunction with onedimensional [ 1 H, 13 C{ 1 H}, and distortionless enhancement by polarization transfer (DEPT)] experiments were employed for assigning the complex and overlapping signals to various compositional and configurational sequences. The spectral assignments of carbonyl as well as nitrile carbons were done with the help of heteronuclear multiple bond correlation spectra.

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Analysis of Compositional Drift in Methyl Methacrylate and n-Butyl Acrylate Copolymers Synthesized by Atom Transfer Radical Polymerization Using 13C{1H} NMR Spectroscopy

Cited by 16 publications

References 23 publications

Copolymerization of n-butyl acrylate/methyl methacrylate in xylene solvent

Copolymerization of n-butyl acrylate/methyl methacrylate in xylene solvent

Optimization of Atom Transfer Radical Copolymerization of Allyl Butyl Ether with Acrylonitrile

2D NMR Analysis of Acrylonitrile/2-Methoxyethyl Acrylate Copolymers Synthesized by Atom Transfer Radical Polymerization

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