ACCELERATING EFFECT OF 3-AMINOPROPYLOLIGOMERIC SILSESQUIOXANE ON FORMATION KINETICS OF THERMOSTABLE HYBRID NANOCOMPOSITES BASED ON POLYCYANURATE NETWORK.
In this work, reactive 3-aminopropyloligomeric silsesquioxane (AP-OSS) was synthesized and studied, and the effect of AP-OSS depending on its content (0.1–1.0 wt.%) on the kinetics of polycyclotrimerization of dicyanate ester of bisphenol E (DCBE) was determined using the dynamic DSC method. AP-OS...
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| Дата: | 2024 |
|---|---|
| Автори: | , , , , , , |
| Формат: | Стаття |
| Мова: | English |
| Опубліковано: |
V.I.Vernadsky Institute of General and Inorganic Chemistry
2024
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| Онлайн доступ: | https://ucj.org.ua/index.php/journal/article/view/665 |
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| Назва журналу: | Ukrainian Chemistry Journal |
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oai:ojs2.1444248.nisspano.web.hosting-test.net:article-6652025-01-28T08:26:28Z ACCELERATING EFFECT OF 3-AMINOPROPYLOLIGOMERIC SILSESQUIOXANE ON FORMATION KINETICS OF THERMOSTABLE HYBRID NANOCOMPOSITES BASED ON POLYCYANURATE NETWORK. Shulzhenko, Diana Grigoryeva, Olga Gumenna, Mariana Polunkin, Evgen Gorelov, Borys Fainleib, Alexander Grande, Daniel cyanate ester resins, oligomeric silsesquioxane, polycyanurates, synthesis kinetics, accelerating effect. In this work, reactive 3-aminopropyloligomeric silsesquioxane (AP-OSS) was synthesized and studied, and the effect of AP-OSS depending on its content (0.1–1.0 wt.%) on the kinetics of polycyclotrimerization of dicyanate ester of bisphenol E (DCBE) was determined using the dynamic DSC method. AP-OSS was prepared in high yield by the hydrolysis and polycondensation of 3-aminopropyltrimethoxysilane in a mixture of acetonitrile and ethanol, with tetrabutylammonium hydroxide (But4NOH) as a catalyst. The chemical structure of the synthesized AP-OSS was confirmed by the results of FTIR and 1H NMR spectroscopies, as well as by MALDI-TOF method. The FTIR spectra showed broad and intensive stretching absorption bands centered at ν≈ 3431 and ν≈ 3378 cm–1 and bending absorption bands centered at δ≈ 1638 and δ≈ 1599 cm-1 of the N–H in NH2 groups, as well as the absorption bands centered at ν≈1027 and δ≈859 cm–1, attributed to the special characteristic vibrations of the silsesquioxane cage Si–O–Si. MALDI-TOF spectroscopy detected predominantly singly charged protonatedions, indicating that the degree of oligomerization in this silsesquioxane is between n = 3 and 10. It was found that AP-OSS accelerated the DCBE polycyclotrimerization allowing decreasing the final temperature and time of polycyanurate network (PCN) synthesis, the higher content of the AP-OSS the higher acceleration effect has been observed. It was supposed that during the in situ synthesis of the hybrid PCN/AP-OSS nanocomposites, the amino groups on a surface of AP-OSS nanoparticles chemically interact with –O–C≡N-groups of DCBE with formation of isourea fragments providing the covalent embedding of AP-OSS into the growing PCN matrix. Using DSC method, it was found that all synthesized hybrid PCN/AP-OSS nanocomposites possessed high glass transition temperatures (Tg>280oC) and can be classified as thermally stable polymer materials. V.I.Vernadsky Institute of General and Inorganic Chemistry 2024-06-28 Article Article Organic chemistry Органическая xимия Органічна xімія application/pdf https://ucj.org.ua/index.php/journal/article/view/665 10.33609/2708-129X.90.5.2024.28-43 Ukrainian Chemistry Journal; Vol. 90 No. 5 (2024): Ukrainian Chemistry Journal; 28-43 Украинский химический журнал; Том 90 № 5 (2024): Ukrainian Chemistry Journal; 28-43 Український хімічний журнал; Том 90 № 5 (2024): Ukrainian Chemistry Journal; 28-43 2708-129X 2708-1281 en https://ucj.org.ua/index.php/journal/article/view/665/331 |
| institution |
Ukrainian Chemistry Journal |
| baseUrl_str |
|
| datestamp_date |
2025-01-28T08:26:28Z |
| collection |
OJS |
| language |
English |
| topic_facet |
cyanate ester resins oligomeric silsesquioxane polycyanurates synthesis kinetics accelerating effect. |
| format |
Article |
| author |
Shulzhenko, Diana Grigoryeva, Olga Gumenna, Mariana Polunkin, Evgen Gorelov, Borys Fainleib, Alexander Grande, Daniel |
| spellingShingle |
Shulzhenko, Diana Grigoryeva, Olga Gumenna, Mariana Polunkin, Evgen Gorelov, Borys Fainleib, Alexander Grande, Daniel ACCELERATING EFFECT OF 3-AMINOPROPYLOLIGOMERIC SILSESQUIOXANE ON FORMATION KINETICS OF THERMOSTABLE HYBRID NANOCOMPOSITES BASED ON POLYCYANURATE NETWORK. |
| author_facet |
Shulzhenko, Diana Grigoryeva, Olga Gumenna, Mariana Polunkin, Evgen Gorelov, Borys Fainleib, Alexander Grande, Daniel |
| author_sort |
Shulzhenko, Diana |
| title |
ACCELERATING EFFECT OF 3-AMINOPROPYLOLIGOMERIC SILSESQUIOXANE ON FORMATION KINETICS OF THERMOSTABLE HYBRID NANOCOMPOSITES BASED ON POLYCYANURATE NETWORK. |
| title_short |
ACCELERATING EFFECT OF 3-AMINOPROPYLOLIGOMERIC SILSESQUIOXANE ON FORMATION KINETICS OF THERMOSTABLE HYBRID NANOCOMPOSITES BASED ON POLYCYANURATE NETWORK. |
| title_full |
ACCELERATING EFFECT OF 3-AMINOPROPYLOLIGOMERIC SILSESQUIOXANE ON FORMATION KINETICS OF THERMOSTABLE HYBRID NANOCOMPOSITES BASED ON POLYCYANURATE NETWORK. |
| title_fullStr |
ACCELERATING EFFECT OF 3-AMINOPROPYLOLIGOMERIC SILSESQUIOXANE ON FORMATION KINETICS OF THERMOSTABLE HYBRID NANOCOMPOSITES BASED ON POLYCYANURATE NETWORK. |
| title_full_unstemmed |
ACCELERATING EFFECT OF 3-AMINOPROPYLOLIGOMERIC SILSESQUIOXANE ON FORMATION KINETICS OF THERMOSTABLE HYBRID NANOCOMPOSITES BASED ON POLYCYANURATE NETWORK. |
| title_sort |
accelerating effect of 3-aminopropyloligomeric silsesquioxane on formation kinetics of thermostable hybrid nanocomposites based on polycyanurate network. |
| description |
In this work, reactive 3-aminopropyloligomeric silsesquioxane (AP-OSS) was synthesized and studied, and the effect of AP-OSS depending on its content (0.1–1.0 wt.%) on the kinetics of polycyclotrimerization of dicyanate ester of bisphenol E (DCBE) was determined using the dynamic DSC method. AP-OSS was prepared in high yield by the hydrolysis and polycondensation of 3-aminopropyltrimethoxysilane in a mixture of acetonitrile and ethanol, with tetrabutylammonium hydroxide (But4NOH) as a catalyst. The chemical structure of the synthesized AP-OSS was confirmed by the results of FTIR and 1H NMR spectroscopies, as well as by MALDI-TOF method. The FTIR spectra showed broad and intensive stretching absorption bands centered at ν≈ 3431 and ν≈ 3378 cm–1 and bending absorption bands centered at δ≈ 1638 and δ≈ 1599 cm-1 of the N–H in NH2 groups, as well as the absorption bands centered at ν≈1027 and δ≈859 cm–1, attributed to the special characteristic vibrations of the silsesquioxane cage Si–O–Si. MALDI-TOF spectroscopy detected predominantly singly charged protonatedions, indicating that the degree of oligomerization in this silsesquioxane is between n = 3 and 10. It was found that AP-OSS accelerated the DCBE polycyclotrimerization allowing decreasing the final temperature and time of polycyanurate network (PCN) synthesis, the higher content of the AP-OSS the higher acceleration effect has been observed. It was supposed that during the in situ synthesis of the hybrid PCN/AP-OSS nanocomposites, the amino groups on a surface of AP-OSS nanoparticles chemically interact with –O–C≡N-groups of DCBE with formation of isourea fragments providing the covalent embedding of AP-OSS into the growing PCN matrix. Using DSC method, it was found that all synthesized hybrid PCN/AP-OSS nanocomposites possessed high glass transition temperatures (Tg>280oC) and can be classified as thermally stable polymer materials. |
| publisher |
V.I.Vernadsky Institute of General and Inorganic Chemistry |
| publishDate |
2024 |
| url |
https://ucj.org.ua/index.php/journal/article/view/665 |
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2025-09-24T17:43:56Z |
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2025-09-24T17:43:56Z |
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