Anionic polymerization of ε-caprolactam and its copolymerization with ω-dodecanelactam in the presence of aromatic polyimides

Vygodskii, Ya. S.; Volkova, Тatyana V.; Пашкова, О. Н.; Batalova, T. L.; Dubovik, I. I.; Chekulaeva, L. A.; Garbuzova, I. A.

doi:10.1134/s0965545x06060010

Cited by 9 publications

(14 citation statements)

References 9 publications

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“…Later on Youlee5 used the same technique and synthesized copolymers based on polycaproamide (PCA) and PIs of the other type. However, copolymers prepared during this investigation and in Refs 2–4. differ from those obtained in Ref 5.…”

Section: Introductioncontrasting

confidence: 52%

“…Monomer, namely ε‐caprolactam, was recrystallized from benzene and dried thoroughly in high vacuum at 50°C before use 4…”

Section: Methodsmentioning

confidence: 99%

“…After the dissolution of aromatic PI in ε‐caprolactam at 150°C, the separately prepared solution of ε‐caprolactam magnesium bromide in ε‐caprolactam was quickly added. The reaction mass was stirred at 150°C for 1 min, then the temperature was raised to 180°C and finally the reaction mixture was kept at 180°C for 1.5 h 4. The obtained polymer solids were slowly cooled down to room temperature at a rate of 2.5°C/min.…”

Section: Methodsmentioning

confidence: 99%

“…Usually, the role of such macromolecular activators is carried out by the specially synthesized polymers having grafted acyllactam groups. In contrast to that, for the first time we had demonstrated2–4 the principle possibility of the utilization of common (without any grafted acyllactam side chains) aromatic polyimides (PI) as excellent activators for lactam anionic polymerization. Thus, a set of aromatic PIs, soluble in lactams melt, was successfully used in the polymerization of ε‐caprolactam.…”

Section: Introductionmentioning

confidence: 93%

“…Thus, a set of aromatic PIs, soluble in lactams melt, was successfully used in the polymerization of ε‐caprolactam. It was proved2–4 that polymerization activation occurred at 150–180 °C due to the opening of the imide cycles in PI backbone under the action of lactam anionic polymerization catalyst, namely ε‐caprolactam magnesium bromide. Along with this, it is necessary to mention that on the utilization of Na‐ε‐caprolactam as another popular catalyst the anionic polymerization of ε‐caprolactam (APC) with mentioned PIs did not proceed at elevated temperature.…”

Section: Introductionmentioning

confidence: 99%

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Synthesis and characterization of grafted copolymers of aromatic polyimides and ε‐caprolactam

Volkova

Vygodskii

Zabegaeva

et al. 2009

J of Applied Polymer Sci

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Anionic polymerization of e-caprolactam was performed in the presence of only 5 wt % of aromatic polyimides having five-and six-membered imide cycles and bearing hexafluoroisopropylidene, ether, fluorene, siloxane, phthalide, or SO 3 HA groups, both in the polymer backbone and as side moieties. The synthesized new copolymers were fully characterized by IR spectroscopy, thermomechanical analysis, dilatometry, and X-ray diffraction. Tough and frictional properties of the obtained copolymers were estimated as well. It was found that on the selection of polyimide activator it is possible to gain the desirable control over the polymer properties, namely the gel-fraction content, phase composition, compression modulus, notched Izod impact strength, temperature of frictional contact, friction coefficient, etc. These investigations will facilitate the choice of the optimum macromolecular activator for the modification of both the synthetic method and the properties of the commercial polycaproamide.

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Section: Introductioncontrasting

confidence: 52%

“…Monomer, namely ε‐caprolactam, was recrystallized from benzene and dried thoroughly in high vacuum at 50°C before use 4…”

Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 93%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Synthesis and characterization of grafted copolymers of aromatic polyimides and ε‐caprolactam

Volkova

Vygodskii

Zabegaeva

et al. 2009

J of Applied Polymer Sci

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Carbon nanotubes bearing imide groups for anionic polymerization of ε-caprolactam

et al. 2014

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Acyllactam groups and aromatic polyimides were grafted to the surface of single walled carbon nanotubes. The modified nanotubes were characterized by X ray photoelectron spectro scopy, scanning electron microscopy, thermogravimetric analysis, and elemental analysis. It was shown that the nanotubes with grafted acyllactam groups or polyimide macromolecules form homogeneous stable in time dispersions in a melt of  caprolactam.Efficience of using carbon nanotubes (CNTs) for the design of polyfunctional polymer materials mainly depends on the uniformity of the filler distribution in the polymer bulk and on the adhesion interaction of the CNT surface with the polymer matrix. 1-3 Functional groups grafted to CNTs provide a uniform dispersion of the latter in the solvent 4-6 or polymer 5,7 and also can favor the forma tion of a covalent bond with the polymer matrix, 8,9 which substantially affects the properties of the final nanocom posites. 10-14Polycaproamide (PCA) is a commercial polymer with high strength, tribological, and other performance char acteristics. Therefore, it is of considerable interest as an engineering plastic. The synthesis of PCA filled with CNTs was considered in a set of publications, 15-19 but only some of them report  caprolactam (CL) polymerization via the anionic mechanism using low molecular weight activa tors. 20,21 Meanwhile, the activated anionic polymeriza tion of  caprolactam (AAPCL) characterized by relative ly mild temperature conditions provides the high quality product by the method of reaction molding, which is most preferential for manufacturing engineering materials. 22 Recently, we have shown 23,24 that the introduction of 0.1-5 wt.% multiwalled CNTs into PCA at the stage of its synthesis substantially improves its thermal, strength, and tribological characteristics. It can be assumed that a more significant effect will be achieved by covalent bonding of the nanotube surface with the polymer ma trix. Nevertheless, the most methods for the preparation of PCA nanocomposites imply the improvement of the dispersability of CNTs in CL and PCA rather than the enhancement of the interaction between the matrix and filler. 25- 27 We discovered the activating effect on AAPCL of poly imides (PI) soluble in a CL melt that require no special functionalization. 28-30 This discovery stimulated us to de velop methods for synthesis of three component compos ites based on PCA and CNTs with grafted PI macromole cules. This approach will facilitate the covalent bonding of the PCA matrix with the filler. It should be noted that aromatic PI used by us are characterized by good solubili ty in a wide range of available organic solvents and in a series of monomers and high thermal and mechani cal characteristics 31 and thus favor the preparation of PCA co PI that significantly exceed homo PCA in ther mal and water resistance, impact strength, and other per formance parameters. 32, 33 To improve uniformity of the CNT distribution in the CL bulk and the subsequent covalent bonding with PCA, we functiona...

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Effect of single-walled carbon nanotubes with imide cycles on the synthesis and properties of polycaproamide

et al. 2016

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The anionic polymerization of ε-caprolactam in the presence of single-walled carbon nanotubes with grafted acyllactam groups or polyimide macromolecules is performed. It is shown that the polymerization of ε-caprolactam slows down with an increase in the filler concentration. The introduction of 0.01 wt % nanotubes with polyimide fragments into polycaproamide leads to a 25% increase in the compressive modulus. In this case, the Izod impact strength is 10 kJ/m 2 , that is, 150% higher than that for an unfilled polycaproamide or polycaproamide containing other types of nanotubes.

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Anionic polymerization of ε-caprolactam and its copolymerization with ω-dodecanelactam in the presence of aromatic polyimides

Cited by 9 publications

References 9 publications

Synthesis and characterization of grafted copolymers of aromatic polyimides and ε‐caprolactam

Synthesis and characterization of grafted copolymers of aromatic polyimides and ε‐caprolactam

Carbon nanotubes bearing imide groups for anionic polymerization of ε-caprolactam

Effect of single-walled carbon nanotubes with imide cycles on the synthesis and properties of polycaproamide

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