Ternary composites by an <i>in situ</i> hydrolytic polymerization process

Nagel, Kevin; Kaßner, Lysann; Seifert, Andreas; Grützner, Rolf-Egbert; Cox, Gerhard; Spange, Stefan

doi:10.1039/c8ra02402b

Cited by 4 publications

(2 citation statements)

References 39 publications

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“…13 C NMR : δ = 183.4 (C=O), 45.1 (C ε ), 38.3 (C α ), 30.2 (C δ ), 29.7 (C γ ), 23.5 (C β ), –0.4 (SiMe) ppm. 29 Si NMR : δ = –19.2 ppm (–19.2 ppm). RAMAN : ν̃ = 2978 (w), 2934 (vs), 2857 (m), 2791 (vw), 2699 (vw), 2631 (vw), 1628 (vw), 1445 (w), 1401 (vw), 1337 (vw), 1295 (vw), 1237 (vw), 1088 (vw), 1029 (vw), 967 (vw), 849 (vw), 786 (vw), 714 (vw), 616 (vw), 543 (vw), 439 (vw), 361 (vw), 317 (vw), 259 (vw), 213 (vw), 165 (vw), 122 (vw) cm –1 .…”

Section: Methodsunclassified

Lactamomethylsilanes – Synthesis, Structures, and Reactivity towards CO₂ and Phenylisocyanate

Herbig

Böhme

Kroke

2019

Zeitschrift anorg allge chemie

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Lactamomethylsilanes of γ-butyrolactam, δ-valerolactam, ε-caprolactam, and 1-isoindolinone (phthalimidine) with up to three methyl moieties were synthesized according to the chemical formula Me x SiLac (4-x) (x = 0, 1, 2, and 3). Using the lactams as starting materials four synthetic routes were tested: salt elimination, transsilylation, transamination, and metallation of the lactames followed by reaction 377 with methylchlorosilanes. All products were analyzed by NMR ( 1 H, 13 C and 29 Si) and RAMAN spectroscopy. Selected solid products were crystallized and the molecular structure was determined by single-crystal X-ray diffraction. The reactivity of the lactamomethylsilanes towards phenylisocyanate and CO 2 was studied.Si-O bond but less reactive than a Si-Cl bond. The Si-N bond is prone towards hydrolysis and alkoholysis. Additionally, some substances containing Si-N bonds react with heteroallenes like CO 2 and isocyanates via insertion reactions yielding useful products such as ureas, carbamates, and polysiloxanes, among others. [23][24][25][26] Therefore, in the presented study we have synthesized lactamomethylsilanes of the type Me x SiLac (4-x) (x = 0, 1, 2, and 3) [Lac = γ-butyrolactam, δ-valerolactam, εcaprolactam, and 1-isoindolinone (phthalimidine)] in order to investigate their structures and reactivities.

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Section: Methodsunclassified

Lactamomethylsilanes – Synthesis, Structures, and Reactivity towards CO₂ and Phenylisocyanate

Herbig

Böhme

Kroke

2019

Zeitschrift anorg allge chemie

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“…The obtained spectra are presented in Figure 3. The signals in the 1 H- 13 C CP/MAS NMR spectra (Figure 3a) corresponding to the PA6 sample, as well as to the PA6/ED, PA6/NED, and PA6/PHED samples, can be assigned to the typical signals of the PA6 in α-crystalline form [35,36]. No significant differences could be observed in the solid state 1 H- 13 C CP/MAS NMR spectra corresponding to the reference PA6, PA6/ED, PA6/NED, and PA6/PHED samples.…”

Section: Structure Characterizationmentioning

confidence: 98%

Effect of Different Flame-Retardant Bridged DOPO Derivatives on Properties of in Situ Produced Fiber-Forming Polyamide 6

et al. 2020

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The production of sustainable and effective flame retardant (FR) polyamide 6 (PA6) fibrous materials requires the establishment of a novel approach for the production of polyamide 6/FR nanodispersed systems. This research work explores the influence of three different flame-retardant bridged 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) derivatives on the comprehensive properties of in situ produced PA6/FR systems. To this end, in situ water-catalyzed ring-opening polymerization of ε-caprolactam was conducted in the presence of three different bridged DOPO derivatives, e.g., one P−N bond phosphonamidate derivative and two P−C bond phosphinate derivatives. The selected bridged DOPO derivatives mainly act in the gas phase at the temperatures that relatively match the PA6 pyrolysis specifics. The effects of the FRs on the dispersion state, morphological, molecular, structural, melt-rheological, and thermal properties of the in situ synthesized PA6 were evaluated. The specific advantage of this approach is one-step production of PA6 with uniformly distributed nanodispersed FR, which was obtained in the case of all three applied FRs. However, the applied FRs differently interacted with monomer and polymer during the polymerization, which was reflected in the length of PA6 chains, crystalline structure, and melt-rheological properties. The applied FRs provided a comparable effect on the thermal stability of PA6 and stabilization of the PA6/FR systems above 450 °C in the oxygen-assisted pyrolysis. However, only with the specifically designed FR molecule were the comprehensive properties of the fiber-forming PA6 satisfied for the continuous conduction of the melt-spinning process.

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Synthesis and characterisation of nickel oxide-carboxylated multiwalled carbon nanotube polymer nanocomposites

Meenatchi,

Velraj

2023

J Mater Sci: Mater Electron

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Ternary composites by an in situ hydrolytic polymerization process

Abstract: Polyamide 6/silica/polysiloxane composites have been prepared in a one-step process using lactam-substituted silicon monomers.

Cited by 4 publications

References 39 publications

Lactamomethylsilanes – Synthesis, Structures, and Reactivity towards CO₂ and Phenylisocyanate

Lactamomethylsilanes – Synthesis, Structures, and Reactivity towards CO₂ and Phenylisocyanate

Effect of Different Flame-Retardant Bridged DOPO Derivatives on Properties of in Situ Produced Fiber-Forming Polyamide 6

Synthesis and characterisation of nickel oxide-carboxylated multiwalled carbon nanotube polymer nanocomposites

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Ternary composites by an in situ hydrolytic polymerization process

Abstract: Polyamide 6/silica/polysiloxane composites have been prepared in a one-step process using lactam-substituted silicon monomers.

Cited by 4 publications

References 39 publications

Lactamomethylsilanes – Synthesis, Structures, and Reactivity towards CO2 and Phenylisocyanate

Lactamomethylsilanes – Synthesis, Structures, and Reactivity towards CO2 and Phenylisocyanate

Effect of Different Flame-Retardant Bridged DOPO Derivatives on Properties of in Situ Produced Fiber-Forming Polyamide 6

Synthesis and characterisation of nickel oxide-carboxylated multiwalled carbon nanotube polymer nanocomposites

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Lactamomethylsilanes – Synthesis, Structures, and Reactivity towards CO₂ and Phenylisocyanate

Lactamomethylsilanes – Synthesis, Structures, and Reactivity towards CO₂ and Phenylisocyanate