A <sup>13</sup>C Nuclear Magnetic Resonance Study of Covalently Cross-Linked Gels. Effect of Chemical Composition, Degree of Cross-Linking, and Temperature to Chain Mobility

Yokota, Kazumichi; Abe, Akira; Hosaka, Shuntaro; Sakai, Ikuo; Saitô, Hazime

doi:10.1021/ma60061a017

Cited by 70 publications

(18 citation statements)

References 8 publications

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“…This is because ␤ is a measure not only of chemical crosslinking but also of physical interactions between the chains when the values are greater than unity. 39 It is of interest to observe that the crosslinked copolymers by electron-beam irradiation at an 80-kGy dose rate have lower ␤ values than those crosslinked by chemical initiator.…”

Section: ϫ3mentioning

confidence: 99%

Swelling and network parameters of high oil‐absorptive network based on 1‐octene and isodecyl acrylate copolymers

Atta

Arndt

2005

J of Applied Polymer Sci

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Crosslinked 1-octene-isodecyl acrylate copolymers were synthesized and evaluated for oil-absorbency applications. The copolymer was crosslinked at different concentrations of ethylene glycol diacrylate (EGDA) and EG dimethacrylate (EGDMA) crosslinkers via catalytic initiation or by electron-beam irradiation at a dose rate 80 kGy. The concentration of both crosslinkers was varied from 0.5 to 2%. The effects of the crosslinking conditions such as crosslinker concentration, method of polymerization and monomer concentrations on the conversion and gel fraction were examined through oil-absorption tests using petroleum crude oil. It was found that the oil absorbency was influenced mainly by the degree of crosslinking and the hydrophobicity of the copolymer units. The final equilibrium oil content, volume fraction of the polymer, and swelling capacity were determined at 298 K. The effective crosslinking density, average molecular weight between the crosslinks, and polymer-toluene interaction parameter were determined from stress-strain measurements. The crosslinking efficiencies of EGDA and EGDMA toward copolymers were determined.

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Section: ϫ3mentioning

confidence: 99%

Swelling and network parameters of high oil‐absorptive network based on 1‐octene and isodecyl acrylate copolymers

Atta

Arndt

2005

J of Applied Polymer Sci

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“…The assignment is made by off-resonance 1 H decoupling experiments and by reference of the spectrum of its monomer. 5 Upon the addition of Cu(II), neither apparent chemical shift change nor line-broadening/nar- 0)). Upon the addition of Cu(II), no appreciable change of relaxation rate is observed for the C2 carbon ( Figure 2).…”

Section: Resultsmentioning

confidence: 98%

“…g and /3 are the g-factor and the Bohr magneton of the electron spin, respectively. The correlation time of the electron-i 3 C dipolar interaction of the complex •c can be given as: (5) where "R is the correlation time of tumbling motion of Cu(II)---carbon bond of the complex. where •Ro is the correlation time at infinite temperature and E!…”

Section: Resultsmentioning

confidence: 99%

13C NMR Study of Poly(N-vinylpyrrolidone)–Cu(II) Complex in Aqueous Solution

Tsuchiya

Takegoshi

Hikichi

1994

Polym J

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ABSTRACT:Structural and dynamic properties of the poly(N-vinylpyrrolidone}-Cu(II) complex in aqueous solution are studied by 13 C NMR relaxation measurements. At pH 4, the spinlattice relaxation rate of the carbonyl carbon increases remarkably with increasing Cu(II) concentration. This indicates that Cu(Il) interacts with the carbonyl group at low pH. The temperature dependence of relaxation rate is explained in terms of the electron-13 C dipolar interaction, the 1 H-13 C dipolar interaction, and the chemical shift anisotropy interaction. The distance between Cu(II) and the carbonyl carbon is evaluated to be 4.0 A at pH 4.Since the paramagnetic metal ion has a large electronic magnetic moment, the spin-lattice relaxation of nuclei in the neighborhood of the metal ion is greatly enhanced. One can investigate structural and dynamic properties of polymer-metal complex by examining such effects. So far, we examined the interaction of Cu(II) and Mn(II) ions with poly(amino acid)s in aqueous solution. 1 -4 It was shown that Cu(II) interacts with the side-chain carboxyl group, 1 • 3 the side-chain amino group,2 and the main-chain amide group 1 ofpoly(amino acid)s, and that Mn(II) interacts with the side-chain carboxyl group and the main-chain carbonyl group. 4 The oxygen atom of carbonyl group can interact with Cu(II); for example, bis(acetylacetonato )Cu(II) is a well-known complex. In this work, we study the interaction of Cu(II) with poly(N-vinylpyrrolidone) (PVP) which has a carbonyl group in the side-chain pyrrolidone ring and is water soluble. EXPERIMENTAL

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“…It causes an up field shift of the line due to resonance of the carbonyl carbon atom caused by enhanced interactions between the functional groups of the monomers. Peak of lactam carbonyl of PVP split into a doublet [27] . Splitting of singlet to doublet is due to the existence of different configurational sequences, low field component refers to syndiotactic triad C=O at 174.6 d ppm and high field component corresponds to the heterotactic traid at 174.3 d ppm.…”

Section: Characterization Of Copolymersmentioning

confidence: 99%

Synthesis and Characterization of Methylmethacrylate-alt-N-vinyl-2-pyrrolidone Initiated by Phosphorus Containing 1,2 Dipolar Compound

Prajapati

Varshney

2007

Polymer-Plastics Technology and Engineering

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Copolymerization of methylmethacrylate (MMA) with 1-vinyl-2-pyrrolidone (N-VP), initiated by p-nitrobenzyl triphenyl phosphonium ylide in dioxane at 60 C for 60 min under inert atmosphere of nitrogen yields alternating copolymer as evidenced by the values of r 1 ¼ 0.01 and r 2 ¼ 0.02. The kinetic expression was R p / [I] 0.75 [MMA] 1.2 [VP] 1.2 . The overall activation energy is 45.4 kJ/mol. The FTIR bands of OCH 3 of MMA at 1725 cm À1 and ÀC=O of N-VP at 1679 cm À1 , confirms the incorporation of both the monomers in the copolymer. The glass transition temperature of the copolymer is 133 C. The GPC data shows the polydispersity index at about 1.5. The ESR spectroscopy confirm phenyl radical responsible for initiation.

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A ¹³C Nuclear Magnetic Resonance Study of Covalently Cross-Linked Gels. Effect of Chemical Composition, Degree of Cross-Linking, and Temperature to Chain Mobility

Cited by 70 publications

References 8 publications

Swelling and network parameters of high oil‐absorptive network based on 1‐octene and isodecyl acrylate copolymers

Swelling and network parameters of high oil‐absorptive network based on 1‐octene and isodecyl acrylate copolymers

13C NMR Study of Poly(N-vinylpyrrolidone)–Cu(II) Complex in Aqueous Solution

Synthesis and Characterization of Methylmethacrylate-alt-N-vinyl-2-pyrrolidone Initiated by Phosphorus Containing 1,2 Dipolar Compound

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A 13C Nuclear Magnetic Resonance Study of Covalently Cross-Linked Gels. Effect of Chemical Composition, Degree of Cross-Linking, and Temperature to Chain Mobility

Cited by 70 publications

References 8 publications

Swelling and network parameters of high oil‐absorptive network based on 1‐octene and isodecyl acrylate copolymers

Swelling and network parameters of high oil‐absorptive network based on 1‐octene and isodecyl acrylate copolymers

13C NMR Study of Poly(N-vinylpyrrolidone)–Cu(II) Complex in Aqueous Solution

Synthesis and Characterization of Methylmethacrylate-alt-N-vinyl-2-pyrrolidone Initiated by Phosphorus Containing 1,2 Dipolar Compound

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A ¹³C Nuclear Magnetic Resonance Study of Covalently Cross-Linked Gels. Effect of Chemical Composition, Degree of Cross-Linking, and Temperature to Chain Mobility