Carbon fabric reinforced propargyl ether/phthalonitrile composites produced by vacuum infusion

Bulgakov, Boris A.; Belsky, Kirill S.; Nechausov, Sergey; Afanaseva, Ekaterina S.; Babkin, Alexander V.; Кепман, А. В.; Авдеев, В. В.

doi:10.1016/j.mencom.2018.01.014

Cited by 29 publications

(8 citation statements)

References 23 publications

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“…Moreover, our previous results have shown the removal of the sizing during vacuum infusion process with the resin flow. 31 The formation of cracks in the composites during post-curing at 375 C (Figure 9), not only decreased the ILSS values for the native composites (Table 2), but also sufficiently increased the surfaces of the samples which accelerated the thermal oxidation. This resulted in complete destruction of the matrix during the aging of CFPN-375 at 330 C, while the lower post-cured samples retained ILSS values up to 23 MPa.…”

Section: Aging Of the Compositesmentioning

confidence: 98%

Effect of post‐curing temperature on the retention of mechanical strength of phthalonitrile thermosets and composites after a long‐term thermal oxidative aging

Lobanova,

Aleshkevich,

Babkin

et al. 2023

Polymer Composites

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This work concerns the thermal‐oxidative aging behavior of phthalonitrile thermosets and composites at 280–350°C. The easy‐to‐process resin containing bis(3‐[3,4‐dicyanophenoxy]phenyl)phenyl phosphate with APB as curing agent and the resin‐based composites post‐cured at 330°C, 350°C, and 375°C were studied. The phthalonitrile thermosets post‐cured at 330°C retained flexural strength of 77 MPa after 200 h of thermal aging at 280°C and 37 MPa (40%) after the same time at 300°C while the resins post‐cured at 350°C and 375°C lost over 80% of the flexural strength in these experiments. The same trend of faster oxidation of the samples post‐cured at higher temperatures was observed for the composites. For the first time, crosslinking reactions were observed during the aging, despite the aging temperatures being below the Tg of thermosets. Thus, the work shows a high long‐term thermal oxidative stability of the studied phthalonitrile resins at temperatures up to 300°C and fast destruction of the materials at 350°C despite the resin decomposition temperatures determined by dynamic TGA being over 500°C. The work has shown the negative effect of high‐temperature post‐curing on the operating properties of the phthalonitrile composites as constructive materials for long‐term application at elevated temperatures.Highlights Oxidation of phthalonitrile thermoset occurs at temperatures over 300°C in air. Increase in post‐curing temperature decreases thermal oxidation resistance. Thermosets retained up to 77% of flexural strength after 200 h aging at 300°C. Composites retained over 90% of ILSS after 200 h of aging at 300°C.

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Section: Aging Of the Compositesmentioning

confidence: 98%

Effect of post‐curing temperature on the retention of mechanical strength of phthalonitrile thermosets and composites after a long‐term thermal oxidative aging

Lobanova,

Aleshkevich,

Babkin

et al. 2023

Polymer Composites

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“…Thermal polymerization of phthalonitriles requires an initiator, such as aromatic amine or phenol, occurs with formation of isonoindoline, triazine, and phthalocyanine structures, and yields thermosets with extraordinarily high heat resistance ( T g up to 450 °C and T 5% > 500 °C), which are considered to be promising matrices for composites for operation under extreme conditions. − However, to the best of our knowledge, there have been no reports of utilizing PN resins for selective photocuring via 3D printing. Phthalonitrile resins are known for poor processability due to high melting points of the monomers, as well as high curing temperatures. ,,− High crystallinity (and, as a consequence, high melting points) might lead to low solubility in different solvents while it is necessary to dissolve solid phthalonitrile monomers in photopolymerizable comonomers to perform VP. − Moreover, phthalonitrile polymerization is typically initiated with an aromatic diamine, which can potentially act as an inhibitor for free-radical polymerization, hindering VP processing . Recently, our research group has successfully designed a low-melting and self-curing phthalonitrile monomer grafted with a maleimide group 4-[3-(2,5-dione-1 H -pyrrole-1-yl)phenoxy]benzene-1,2-dicarbonitrile (PNB-M) .…”

Section: Introductionmentioning

confidence: 99%

Heat-Resistant Phthalonitrile-Based Resins for 3D Printing via Vat Photopolymerization

Nechausov

Aleksanova

Morozov

et al. 2022

ACS Appl. Polym. Mater.

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In this study, a maleimide/phthalonitrile bifunctional monomer PNB-M was used in vat photopolymerization via the maleimide group to obtain phthalonitrile-containing polymers suitable for further thermal postcuring. A high concentration (40 wt %) and low viscosity (less than 500 mPa·s at 25 °C) photopolymer resin was prepared from the phthalonitrile monomer PNB-M with 4-acryloylmorpholine as comonomer and trimethylolpropane trimethacrylate as cross-linker. Photo-DSC, NMR, and FTIR tests revealed free-radical photoinduced copolymerization of the maleimide with the acrylic groups during 3D printing. Postprinting thermal curing of the phthalonitrile groups was performed with different curing agents as well as via self-initiation by PNB-M. The developed phthalonitrile-containing polymerizable compositions made it possible to increase glass transition temperatures of the 3D printed polymer materials up to 351 °C after additional thermal postcuring. Moreover, mechanical properties of the 3D printed materials have been improved after curing of the phthalonitrile monomer in the maleimide–acrylate copolymer.

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“…Наряду с легкоплавкими фосфорсодержащими мономерами [8][9][10] важным компонентом композиций фталонитрильных связующих для ПКМ [11][12][13][14] является 1,3-бис (3,4-дицианофенокси)бензол (ДФБ) (3), получаемый в результате взаимодействия 4-нитрофталонитрила (4НФН) (1) и резорцина (2) [15]. Термические свойства ДФБ и отвержденного полимера на его основе 1 представлены в табл.…”

Section: Introductionunclassified

Development of the technique for quality control of 1,3-bis(3,4-dicyanophenoxy)benzene by HPLC

Щеколдина

Bogolyubov

Zakharov

et al. 2021

Fine Chem. Technol.

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Objectives. Determination of target products and byproducts is necessary for the quality control of phthalonitrile monomer synthesis as well as production scaling and performing related kinetic studies. High-performance liquid chromatography (HPLC) is a simple and affordable method for quantitative chemical analysis, which also verifies the quality of raw materials. The objective of this study was to develop an HPLC technique for determining the composition of the reaction mixture in the synthesis of 1,3-bis(3,4-dicyanophenoxy)benzene (DPB).Methods. Reversed-phase HPLC was used to quantitatively analyze the reaction mixture.Results. A simple and rapid method for the quantitative HPLC analysis of phthalonitrile monomers and their mixtures with reagents was developed. Reaction times and the accumulation of byproducts were also studied.Conclusions. The successful performance of the developed technique allows us to recommend it for practical applications. The results obtained for reactors of different sizes have good convergence, and DPB synthesis was successfully scaled up to intermediate scale equipment.

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Carbon fabric reinforced propargyl ether/phthalonitrile composites produced by vacuum infusion

Cited by 29 publications

References 23 publications

Effect of post‐curing temperature on the retention of mechanical strength of phthalonitrile thermosets and composites after a long‐term thermal oxidative aging

Effect of post‐curing temperature on the retention of mechanical strength of phthalonitrile thermosets and composites after a long‐term thermal oxidative aging

Heat-Resistant Phthalonitrile-Based Resins for 3D Printing via Vat Photopolymerization

Development of the technique for quality control of 1,3-bis(3,4-dicyanophenoxy)benzene by HPLC

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