Synthesis and Investigation of the Properties of a Branched Phthalonitrile Containing Cyclotriphosphazene
To study the properties of cyclotriphosphazene (CTP)-containing phthalonitriles, a branched phthalonitrile containing CTP (CTP–PN) with self-catalytic behavior was designed and synthesized. The structure of CTP–PN was characterized by FT–IR (Fourier transform infrared spectroscopy), MS (mass spectro...
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2024-11-01
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| Series: | Molecules |
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| author | Dengxun Ren Zexu Fan Jiaqu Zhang Yi Xu Xianzhong Tang Mingzhen Xu |
| author_facet | Dengxun Ren Zexu Fan Jiaqu Zhang Yi Xu Xianzhong Tang Mingzhen Xu |
| author_sort | Dengxun Ren |
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| description | To study the properties of cyclotriphosphazene (CTP)-containing phthalonitriles, a branched phthalonitrile containing CTP (CTP–PN) with self-catalytic behavior was designed and synthesized. The structure of CTP–PN was characterized by FT–IR (Fourier transform infrared spectroscopy), MS (mass spectroscopy), <sup>1</sup>H–NMR (proton nuclear magnetic resonance spectroscopy), and <sup>13</sup>C–NMR (carbon nuclear magnetic resonance spectroscopy). Then, the curing reaction of CTP–PN was studied using DSC (differential scanning calorimetry) and DRA (dynamic rheological analysis). The results show that the curing reaction of CTP–PN is initiated at 200 °C. Additionally, the change in the viscosity of CTP–PN as a function of the temperature was investigated. After curing at different temperatures, the generated structures were characterized by FT–IR. The fracture morphology and thermomechanical properties of cured CTP–PN were scanned and studied using SEM (scanning electron microscopy) and TMA (thermomechanical analysis), respectively. The results demonstrate that CTP–PN exhibits a smooth fracture surface and possesses a relatively low CTE (coefficient of linear thermal expansion) of approximately 25 ppm/°C at 285 °C. A <i>T</i><sub>d5%</sub> (temperature at which 5% weight loss occurs) of as high as 405 °C can be obtained for cured CTP–PN, and its char yield at 800 °C exceeds 70% in N<sub>2</sub>. FT–IR and XPS (X-ray photoelectron spectroscopy) were used to study the thermal decomposition of cured CTP–PN, indicating that it remains stable below 350 °C. With an increasing temperature, there is decomposition first of CTP and P–NH–Ph and C–O–C bonds (>350 °C) and then nitrogen-containing aromatic heterocycles (>500 °C), ultimately resulting in the formation of P-containing residual char. |
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| institution | Kabale University |
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| language | English |
| publishDate | 2024-11-01 |
| publisher | MDPI AG |
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| series | Molecules |
| spelling | doaj-art-b74e9dac0acf439581e37fe4e9f36a782024-12-13T16:28:39ZengMDPI AGMolecules1420-30492024-11-012923566810.3390/molecules29235668Synthesis and Investigation of the Properties of a Branched Phthalonitrile Containing CyclotriphosphazeneDengxun Ren0Zexu Fan1Jiaqu Zhang2Yi Xu3Xianzhong Tang4Mingzhen Xu5School of Materials and Energy, University of Electronic Science and Technology of China, Chengdu 610054, ChinaSchool of Materials and Energy, University of Electronic Science and Technology of China, Chengdu 610054, ChinaSchool of Materials and Energy, University of Electronic Science and Technology of China, Chengdu 610054, ChinaSchool of Materials and Energy, University of Electronic Science and Technology of China, Chengdu 610054, ChinaSchool of Materials and Energy, University of Electronic Science and Technology of China, Chengdu 610054, ChinaSchool of Materials and Energy, University of Electronic Science and Technology of China, Chengdu 610054, ChinaTo study the properties of cyclotriphosphazene (CTP)-containing phthalonitriles, a branched phthalonitrile containing CTP (CTP–PN) with self-catalytic behavior was designed and synthesized. The structure of CTP–PN was characterized by FT–IR (Fourier transform infrared spectroscopy), MS (mass spectroscopy), <sup>1</sup>H–NMR (proton nuclear magnetic resonance spectroscopy), and <sup>13</sup>C–NMR (carbon nuclear magnetic resonance spectroscopy). Then, the curing reaction of CTP–PN was studied using DSC (differential scanning calorimetry) and DRA (dynamic rheological analysis). The results show that the curing reaction of CTP–PN is initiated at 200 °C. Additionally, the change in the viscosity of CTP–PN as a function of the temperature was investigated. After curing at different temperatures, the generated structures were characterized by FT–IR. The fracture morphology and thermomechanical properties of cured CTP–PN were scanned and studied using SEM (scanning electron microscopy) and TMA (thermomechanical analysis), respectively. The results demonstrate that CTP–PN exhibits a smooth fracture surface and possesses a relatively low CTE (coefficient of linear thermal expansion) of approximately 25 ppm/°C at 285 °C. A <i>T</i><sub>d5%</sub> (temperature at which 5% weight loss occurs) of as high as 405 °C can be obtained for cured CTP–PN, and its char yield at 800 °C exceeds 70% in N<sub>2</sub>. FT–IR and XPS (X-ray photoelectron spectroscopy) were used to study the thermal decomposition of cured CTP–PN, indicating that it remains stable below 350 °C. With an increasing temperature, there is decomposition first of CTP and P–NH–Ph and C–O–C bonds (>350 °C) and then nitrogen-containing aromatic heterocycles (>500 °C), ultimately resulting in the formation of P-containing residual char.https://www.mdpi.com/1420-3049/29/23/5668cyclotriphosphazenebranched phthalonitrilecuring reactionthermomechanical propertiesthermal decomposition analysis |
| spellingShingle | Dengxun Ren Zexu Fan Jiaqu Zhang Yi Xu Xianzhong Tang Mingzhen Xu Synthesis and Investigation of the Properties of a Branched Phthalonitrile Containing Cyclotriphosphazene Molecules cyclotriphosphazene branched phthalonitrile curing reaction thermomechanical properties thermal decomposition analysis |
| title | Synthesis and Investigation of the Properties of a Branched Phthalonitrile Containing Cyclotriphosphazene |
| title_full | Synthesis and Investigation of the Properties of a Branched Phthalonitrile Containing Cyclotriphosphazene |
| title_fullStr | Synthesis and Investigation of the Properties of a Branched Phthalonitrile Containing Cyclotriphosphazene |
| title_full_unstemmed | Synthesis and Investigation of the Properties of a Branched Phthalonitrile Containing Cyclotriphosphazene |
| title_short | Synthesis and Investigation of the Properties of a Branched Phthalonitrile Containing Cyclotriphosphazene |
| title_sort | synthesis and investigation of the properties of a branched phthalonitrile containing cyclotriphosphazene |
| topic | cyclotriphosphazene branched phthalonitrile curing reaction thermomechanical properties thermal decomposition analysis |
| url | https://www.mdpi.com/1420-3049/29/23/5668 |
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