Chemical dehydrochlorination of polytrichlorobutadienes—A new route to carbynes

Vointseva, I.I.; Gil'man, L. M.; Kudryavtsev, Yu. P.; Evsyukov, S. E.; Песин, Л. А.; Gribov, I.V.; Moskvina, N. A.; Khvostov, V. V.

doi:10.1016/0014-3057(95)00104-2

Cited by 23 publications

(10 citation statements)

References 10 publications

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“…In order to obtain wt.% PVC and wt.% PMMA based on a 50% : 50% bulk stoichiometry, the mass% O for PMMA and mass% Cl for PVC are utilized %PMMA D %O ð 3.13/ %Cl ð 1.76 C %O ð 3. 13 1…”

Section: Survey Quantificationmentioning

confidence: 99%

Quantification of PVC–PMMA polymer blend compositions by XPS in the presence of x‐ray degradation effects

Artyushkova

Fulghum

2001

Surface & Interface Analysis

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X-ray photoelectron spectroscopy is widely used for the quantitative surface analysis of polymer blends. The compositions of some polymers can change under x-ray exposure, influencing peak intensities and positions in survey spectra and, in addition, the peak shapes in high-energy resolution spectra. In order to quantify spectra acquired after prolonged (>15 min) x-ray exposure, polymer decomposition may need to be taken into account. Calculating the surface composition of a polymer blend using survey and high-resolution core-level spectra is thus not always straightforward.Halogenated compounds, especially chlorinated, are known to degrade with x-ray exposure, resulting in a decrease in the Cl 2p photopeak intensity and an increase in C 1s intensity. In this work, 50 : 50 PVC-PMMA blends are used to evaluate quantitative methods that correct for PVC degradation, based upon either survey or high-resolution spectra. For survey quantification, degradation data were acquired from both blends and pure polymers in order to measure the rate of change of the photoelectron signal intensity. Correction factors were developed based on changes in C 1s, O 1s and Cl 2p intensities as a function of analysis time. High-resolution C 1s spectra were curve-fit using photopeak shapes acquired from PVC and PMMA standards. After degradation, an additional peak attributed to hydrocarbon (HC), which is the product of PVC dehydrochlorination, is required in the curve-fit. Non-uniform HC contamination present initially in some of the PVC-PMMA blends complicates the quantification. The determination of PVC and PMMA concentrations based upon different approaches to the C 1s curve-fitting is presented.The influence of PVC degradation on image appearance and analysis has also been investigated. Principal component analysis (PCA) and classification methods are used to extract maps of the pure components from a degradation image data set. The maps are compared with elemental XPS images and maps of the pure components extracted from an images-to-spectra data set. Analysis of the image data provides insight into the difficulties in basing quantification on the C 1s photopeak curve-fits.

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“…In order to obtain wt.% PVC and wt.% PMMA based on a 50% : 50% bulk stoichiometry, the mass% O for PMMA and mass% Cl for PVC are utilized %PMMA D %O ð 3.13/ %Cl ð 1.76 C %O ð 3. 13 1…”

Section: Survey Quantificationmentioning

confidence: 99%

Quantification of PVC–PMMA polymer blend compositions by XPS in the presence of x‐ray degradation effects

Artyushkova

Fulghum

2001

Surface & Interface Analysis

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“…Chemical or electrochemical reduction dechlorination of PVC/PVDC is the effective method to obtain carbyne carbon [8][9][10][11][19][20][21][22][23]. But it must be performed in toxic liquid environment and special strong reductive agents, such as alkali metal amalgam.…”

Section: The Formation Of Carbinementioning

confidence: 99%

Behavior and products of mechano-chemical dechlorination of polyvinyl chloride and poly (vinylidene chloride)

Xiao

Zeng

Songwen

2008

Journal of Hazardous Materials

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“…239 Poly(vinyl halides) are, however, chemically dehydrohalogenated in alkaline media: [251][252][253][254][255] An analogous reaction proceeds with a copolymer of vinylidene fluoride and tetrafluoroethylene 256 and poly(trichlorobutadienes). 257 The carbonization (35) accelerates in the presence of phase-transfer catalysts (quaternary ammonium or phosphonium halides), 207,255,256,258 but it can be also driven electrochemically. Shirakawa et al 33 found that reductive carbonization of PVDF dissolved in dimethylformamide + NBu 4 ClO 4 takes place at a Pt cathode, provided tert-butyl alcohol (BuOH) is added to the electrolyte solution.…”

Section: F Other Halogenated Polymersmentioning

confidence: 99%