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Record W194745401 · doi:10.53846/goediss-3860

Investigations into the Propagation and Termination Kinetics of the Radical Polymerization of Polar Monomers in Aqueous Solution

2013· dissertation· en· W194745401 on OpenAlex

Why this work is in the frame

A frame that forgets how it found something cannot be audited. These are the routes that admitted this work.

fundA Canadian funder is recorded on the work.
no affNo Canadian affiliation: this work is invisible to an affiliation-only frame.
No Canadian affiliation. An affiliation-only frame, the usual design, would never have seen this work. It is one of the works that make the case for inverting the frame.

Bibliographic record

Venuenot available
Typedissertation
Languageen
FieldChemistry
TopicPhotopolymerization techniques and applications
Canadian institutionsnot available
FundersÉcole Polytechnique Fédérale de LausanneQueen's UniversitySlovenská Akadémia Vied
KeywordsMonomerChemistryArrhenius equationActivation energyIntermolecular forcePolymerizationAqueous solutionKineticsPhysical chemistryPolymer chemistryMoleculeAnalytical Chemistry (journal)Organic chemistryPolymer

Abstract

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Propagation and termination rate coefficients of radical polymerizations in aqueous solution were determined from pulsed-laser induced polymerizations and chemically initiated polymerizations. Pulsed-laser induced polymerizations of <i>N</i>,2&#8209;dimethylprop&#8209;2&#8209;enamide, <i>N</i>,<i>N</i>&#8209;dimethylprop&#8209;2&#8209;enamide, 2&#8209;methylprop&#8209;2&#8209;enamide, and prop&#8209;2&#8209;enamide were performed. Subsequent analysis of the products by size-exclusion chromatography provided access to propagation rate coefficients. The obtained variation of the propagation rate coefficients with monomer concentration may be explained by the degree to which internal rotations and vibrations in the transition state of the propagation step are hindered. The dependence of the degree of hindrance on monomer concentration may be ascribed to an increase of intermolecular interactions of the transition-state structure with solvating molecules towards higher monomer content. Pressure and temperature were varied from ambient pressure to 2&nbsp;000&nbsp;bar and from 10&nbsp;&deg;C to 80&nbsp;&deg;C, respectively, to allow for determination of volumes of activation and Arrhenius activation energies for propagation. The activation energy and the absolute value of the volume of activation in case of 2&#8209;methylprop&#8209;2&#8209;enamide are larger compared to <i>N</i>,<i>N</i>&#8209;dimethylprop&#8209;2&#8209;enamide. This finding may be ascribed to the circumstance that <i>N</i>,<i>N</i>&#8209;dimethylprop&#8209;2&#8209;enamide lacks an &alpha;&#8209;methyl group. Both activation parameters in case of <i>N</i>,2&#8209;dimethylprop&#8209;2&#8209;enamide are close to the ones of <i>N</i>,<i>N</i>&#8209;dimethylprop&#8209;2&#8209;enamide. This is unexpected because <i>N</i>,2&#8209;dimethylprop&#8209;2&#8209;enamide exhibits an &alpha;&#8209;methyl group. Differences between both monomers regarding the conformation of the carbon&ndash;carbon double bond relative to the carbon&ndash;oxygen double bond may explain this observation.<br> Initiation of a polymerization by a single laser pulse and subsequent detection of monomer-to-polymer conversion by time-resolved near-infrared spectroscopy was used to measure termination rate coefficients. The time resolution has been improved to 0.33&nbsp;&mu;s. Repetitive application of laser pulses in conjunction with near-infrared spectroscopic analysis yields termination rate coefficients as a function of the degree of monomer conversion. Investigations into the termination kinetics of prop&#8209;2&#8209;enamide, 2&#8209;methylprop&#8209;2&#8209;enamide, <i>N</i>,2&#8209;dimethylprop&#8209;2&#8209;enamide, <i>N</i>,<i>N</i>&#8209;dimethylprop&#8209;2&#8209;enamide, and 1&#8209;vinylpyrrolidin&#8209;2&#8209;one were performed at 2&nbsp;000&nbsp;bar because of the better signal-to-noise ratio at high pressure. Additional measurements were conducted at pressures of 500&nbsp;bar, 1&nbsp;000&nbsp;bar, and 1&nbsp;500&nbsp;bar in case of most prop&#8209;2&#8209;enamides. The so-obtained volumes of activation may be used to estimate termination rate coefficients at ambient pressure. The volumes of activation amount to 12.4&nbsp;cm<sup>3</sup>&middot;mol<sup>&minus;1</sup> and 14.3&nbsp;cm<sup>3</sup>&middot;mol<sup>&minus;1</sup> for the termination rate coefficients of <i>N</i>,2&#8209;dimethylprop&#8209;2&#8209;enamide and prop&#8209;2&#8209;enamide, respectively. The volume of activation in case of <i>N</i>,<i>N</i>&#8209;dimethylprop&#8209;2&#8209;enamide (4.9&nbsp;cm<sup>3</sup>&middot;mol<sup>&minus;1</sup>) is lower than expected. Termination rate coefficients of 1&#8209;vinylpyrrolidin&#8209;2&#8209;one could be obtained for a large range of initial monomer concentrations and degrees of monomer conversion. This information allows for a detailed analysis of the parameters used to describe the monomer-conversion dependence of the termination rate coefficient. Within the monomer-conversion ranges under investigation the termination rate coefficient is assumed to be controlled by segmental, translational, and reaction diffusion.<br> In case of <i>N</i>,<i>N</i>&#8209;dimethylprop&#8209;2&#8209;enamide and 1&#8209;vinylpyrrolidin&#8209;2&#8209;one, dynamic viscosities of monomer&ndash;water mixtures were determined at ambient pressure to assist the understanding of termination kinetics. A large set of termination rate coefficients in dependence on initial monomer concentration was obtained for these two monomers by pulsed-laser induced polymerization.<br> Chemically initiated polymerizations of prop&#8209;2&#8209;enamide were conducted to determine termination rate coefficients at ambient pressure as a function of the degree of monomer conversion. The obtained data are in good agreement with data determined by pulsed-laser induced polymerizations.<br> Investigations into the binary copolymerization of 1&#8209;vinylpyrrolidin&#8209;2&#8209;one and sodium acrylate revealed a strong incorporation of sodium acrylate into the copolymer, as was measured by nuclear magnetic resonance spectroscopy. Monomer reactivity ratios were determined by means of the Mayo&ndash;Lewis equation.

Fetched live from OpenAlex and de-inverted. Abstracts are not stored in this database: the inverted indexes are 8.6 GB of the frame’s 9.3 GB of text, and the host has 13 GB free.

Full frame distilled prediction

Teacher imitation

Not calibrated prevalence, not ground truth. Human validation pending. Learned from the 10,348 direct Codex labels and 10,348 direct Gemma labels. Candidate is the union of thresholded teacher heads; consensus is their intersection. These outputs are machine_predicted_unvalidated and are not human labels or direct frontier model labels.

metaresearch head score (Codex)0.000
metaresearch head score (Gemma)0.000
Version: codex-gemma-dda1882f352aValidation status: machine_predicted_unvalidated
Candidate categoriesnone
Consensus categoriesnone
DomainCandidate signal: none · Consensus signal: none
Study designCandidate signal: Bench or experimental · Consensus signal: Bench or experimental
GenreCandidate signal: Empirical · Consensus signal: Empirical
Teacher disagreement score0.012
Threshold uncertainty score0.544

Codex and Gemma teacher scores by category

CategoryCodexGemma
Metaresearch0.0000.000
Meta-epidemiology (narrow)0.0000.000
Meta-epidemiology (broad)0.0000.000
Bibliometrics0.0000.000
Science and technology studies0.0000.000
Scholarly communication0.0000.000
Open science0.0000.000
Research integrity0.0000.000
Insufficient payload (model declined to judge)0.0000.000

Machine scores (provisional)

The two teacher heads of the student model, read on this work. A score orders the frame for review; it never asserts a category, and the validation status ships verbatim with every row.

Baseline scores from an immature model (maturity gate not passed, 7 training rounds). Scores rank; they never assert a category.

Opus teacher head0.006
GPT teacher head0.233
Teacher spread0.227 · how far apart the two teachers sit on this one work
Validation statusscore_only:v0-immature-baseline · verbatim from the scoring run: score_only means the number may rank works, and no category label ships from it