Vibrational and NMR spectroscopic studies of a thiolsulphonate produced from the non-catalytic hydrogenation of polybutadiene

Edwards, Howell G. M.; Johnson, A. F.; Lewis, Ian R.; Maitland, Derek J.; Webb, Ned C.

doi:10.1016/0022-2860(92)80223-5

Cited by 9 publications

(5 citation statements)

References 10 publications

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“…As a result of hydrogenation, the bands associated with the C-O-C ring vibration of epoxide groups disappeared. Additionally, two distinct extra bands at 1152 and 1592 cm 1 are observed and can be assigned to the symmetric -C-SO 2 -C-vibration mode and the C C bond stretching mode of the aromatic ring of the TSOH by-product, respectively, as found by Edwards et al 19 Epoxide ring opening of the ENR was confirmed by the disappearance of the signals in the IR spectrum at 870 and 1250 cm 1 characteristic of the C-O-C vibrations of epoxide groups. The band at 3460 cm 1 assigned to the O-H stretching of the hydroxy group was also detected as shown in Fig.…”

Section: Raman Spectroscopic Analysissupporting

confidence: 54%

Raman spectroscopic study of non‐catalytic hydrogenation of unsaturated rubbers

Samran

Phinyocheep

Daniel

et al. 2004

J Raman Spectroscopy

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The non-catalytic hydrogenation of natural rubber (NR) and two epoxidized NRs (ENRs) i.e. ENR-22 and ENR-40 containing 22 and 40 mol% of epoxide, respectively, was carried out using ptoluenesulfonylhydrazide (TSH) as a hydrogenating agent. A two-fold molar excess of TSH compared with unsaturated units of the rubber was used. The evidence of hydrogenation is a decrease in the intensity of the characteristic signal of the carbon-carbon double bond stretching vibration of the rubber in both the Raman and FT-IR spectra. The percentage hydrogenation was successfully determined by Raman spectroscopy since the vibrational mode of the carbon-carbon unsaturation is strongly Raman active. The progress of the hydrogenation could be monitored by means of the techniques mentioned above as a function of reaction time. The maximum degree of hydrogenation of NR is ∼89% whereas in the case of ENR-22 and ENR-40 it reaches 94 and 96%, respectively. Solid-state 13 C NMR spectroscopy was also used to confirm the microstructure characteristics of the hydrogenated rubbers. 13 C NMR analysis showed that cis-trans isomerization of carbon-carbon unsaturations occur during hydrogenation.

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Section: Raman Spectroscopic Analysissupporting

confidence: 54%

Raman spectroscopic study of non‐catalytic hydrogenation of unsaturated rubbers

Samran

Phinyocheep

Daniel

et al. 2004

J Raman Spectroscopy

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“…If reduced polyethylene products were not washed thoroughly on the filter with MeOH, they sometimes contained small amounts of the byproduct MeC 6 H 4 SO 2 SC 6 H 4 Me. This compound has been reported as a byproduct of p -toluenesulfonohydrazide reduction of polybutadiene …”

Section: Methodsmentioning

confidence: 95%

“…This compound has been reported as a byproduct of p-toluenesulfonohydrazide reduction of polybutadiene. 10 Molecular Weight Characterization. Several of the fluoroalkyl-ended polymers have been characterized by gel permeation chromatography (GPC) vs polystyrene standards.…”

Section: Methodsmentioning

confidence: 99%

Surface Properties and Metathesis Synthesis of Block Copolymers Including Perfluoroalkyl-Ended Polyethylenes

1996

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Linear polyethylene with fluoroalkyl end groups has been prepared by ring-opening metathesis polymerization of cyclododecene in the presence of partially fluorinated acyclic olefins (chain transfer agents), followed by reduction of the double bonds in the backbone. Melt surface tensions (γ) were obtained for samples with one or both ends terminated by F(CF2)10 or F(CF2)4 groups at different molecular weights (MWs) of the hydrocarbon segments down to oligomeric sizes. The polyethylenes with two perfluorinated ends, i.e., PE(C10F21)2, were the most effective at lowering γ. At only 10% atomic F in the bulk, values of γ were obtained which were even lower than those for pure poly(tetrafluoroethylene). The surfaces of films of selected fluoroalkyl-terminated polymers were also characterized by advancing and receding contact angle measurements and angle dependent X-ray photoelectron spectroscopy (XPS). Advancing contact angles in hexadecane were as high as 70°, indicating a high surface concentration of perfluorinated species. Comparison with model systems indicate that much of the surface is covered by close-packed CF3 groups. XPS profiling quantified the ratio of fluorocarbon to hydrocarbon in the surface regions and also indicated a strong surface excess of oriented chain ends. The hexadecane contact angles of fluoroalkyl-ended metathesis polymers [PE(C10F21)2] decrease substantially as the molecular weight increases above ca. 40 000. In that range, the bulk concentration of chain ends becomes quite low and surface concentration of fluorocarbon chain ends at the surface is sharply reduced because of configurational entropic reasons. The surface properties of blends of a lower MW PE(C10F21)2 copolymer with a PE homopolymer were evaluated and compared to the series of pure PE(C10F21)2 copolymers where the high MW limit of the polyethylene center is approached. At similar bulk F levels in the blends and pure copolymer, the surface fluorocarbon content in the blends is significantly enhanced.

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“…The presence of sulfur groups in FMTnF-SO 3 H was revealed by the characteristic vibration of −SO 3 H at 1220 cm –1 . Also, the peaks at 1180 and 1068 cm –1 were attributed to symmetric and asymmetric stretching vibrations of C–SO 2 . The peak at 620 cm –1 was a characteristic frequency of the C–S group .…”

Section: Resultsmentioning

confidence: 93%

“…31 Also, the peaks at 1180 and 1068 cm −1 were attributed to symmetric and asymmetric stretching vibrations of C−SO 2 . 32 The peak at 620 cm −1 was a characteristic frequency of the C−S group. 31 The above mentioned evidence proved the successful preparation of FMTnF-SO 3 H and FMTnF-COOH.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

Preparation of Novel Bifunctional Magnetic Tubular Nanofibers and Their Application in Efficient and Irreversible Uranium Trap from Aqueous Solution

Ahmad

Cui

et al. 2020

ACS Sustainable Chem. Eng.

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A low-cost and efficient material is highly attractive for the removal of radioactive metal ions from aqueous solutions. However, it is highly required and still challenging. In this work, novel bifunctional magnetic tubular nanofibers (FMTnF) are prepared from α,α′-dichloro-p-xylene via self-polymerization by the two-oil-solvent method. The polymerized material is followed by carbonization. The carbonized material experienced bifunctionalization, first, grafting of sulphonic (−SO 3 H) and carboxylic (−COOH) groups and second, loading of Fe 3 O 4 for the preparation of sulphonic magnetic tubular nanofibers (FMTnF-SO 3 H) and carboxyl magnetic tubular nanofibers (FMTnF-COOH). The average diameter of FMTnF-SO 3 H and FMTnF-COOH is about 160 nm, and the saturation magnetization values are 21.61 and 19.44 emu g −1 , respectively. The adsorption performances of these two adsorbents are studied and compared for the removal of U(VI) from aqueous solution. Fourier transform infrared and X-ray photoelectron spectroscopy characterizations combined with isothermal studies confirmed that the interaction of U(VI) with active sites of FMTnF-SO 3 H and FMTnF-COOH is usually through coordination complexation. The maximum adsorption capacities of FMTnF-SO 3 H and FMTnF-COOH are 955.6993 and 980.3921 mg g −1 , respectively, at pH = 8. Moreover, the high adsorption efficiency can reach 85 ± 0.5% at low concentration (3 μg L −1 ). Excellent regeneration and reusability of FMTnF-SO 3 H and FMTnF-COOH offered long-term usage to decrease cost for U(VI) adsorption from seawater/wastewater treatment.

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Vibrational and NMR spectroscopic studies of a thiolsulphonate produced from the non-catalytic hydrogenation of polybutadiene

Cited by 9 publications

References 10 publications

Raman spectroscopic study of non‐catalytic hydrogenation of unsaturated rubbers

Raman spectroscopic study of non‐catalytic hydrogenation of unsaturated rubbers

Surface Properties and Metathesis Synthesis of Block Copolymers Including Perfluoroalkyl-Ended Polyethylenes

Preparation of Novel Bifunctional Magnetic Tubular Nanofibers and Their Application in Efficient and Irreversible Uranium Trap from Aqueous Solution

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