{"title":"微波辅助水热反应合成己酸酯簇的机理","authors":"Nattamon Panichakul , Hiroki Nagakari , Soichi Kikkawa , Shuntaro Tsubaki , Kotaro Higashi , Tomoya Uruga , Hideyuki Kawasoko , Seiji Yamazoe","doi":"10.1016/j.cattod.2025.115593","DOIUrl":null,"url":null,"abstract":"<div><div>Anionic hexaniobate clusters [Nb<sub>6</sub>O<sub>19</sub>]<sup>8 −</sup>, which act as a superbase catalyst, could be synthesized by the microwave-assisted hydrothermal method at 180℃ within 10 min with high purity, whereas the conventional hydrothermal synthesis method requires a long reaction time (>24 h). In this study, the mechanism of synthesizing [Nb<sub>6</sub>O<sub>19</sub>]<sup>8−</sup> by the microwave-assisted hydrothermal method was investigated by <em>in situ</em> quick-scan X-ray absorption fine structure and electrospray ionization time-of-flight mass spectroscopy. This revealed rapid [Nb<sub>6</sub>O<sub>19</sub>]<sup>8−</sup> nucleation along with dissolution of Nb<sub>2</sub>O<sub>5</sub>∙<em>n</em>H<sub>2</sub>O accompanied by the formation of mononuclear Nb species at 160℃. The unveiled mechanistic insights provide the controllability in products during microwave-assisted hydrothermal synthesis of polyoxoniobate clusters.</div></div>","PeriodicalId":264,"journal":{"name":"Catalysis Today","volume":"463 ","pages":"Article 115593"},"PeriodicalIF":5.3000,"publicationDate":"2025-10-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Mechanism of synthesizing hexaniobate cluster by microwave-assisted hydrothermal reaction\",\"authors\":\"Nattamon Panichakul , Hiroki Nagakari , Soichi Kikkawa , Shuntaro Tsubaki , Kotaro Higashi , Tomoya Uruga , Hideyuki Kawasoko , Seiji Yamazoe\",\"doi\":\"10.1016/j.cattod.2025.115593\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>Anionic hexaniobate clusters [Nb<sub>6</sub>O<sub>19</sub>]<sup>8 −</sup>, which act as a superbase catalyst, could be synthesized by the microwave-assisted hydrothermal method at 180℃ within 10 min with high purity, whereas the conventional hydrothermal synthesis method requires a long reaction time (>24 h). In this study, the mechanism of synthesizing [Nb<sub>6</sub>O<sub>19</sub>]<sup>8−</sup> by the microwave-assisted hydrothermal method was investigated by <em>in situ</em> quick-scan X-ray absorption fine structure and electrospray ionization time-of-flight mass spectroscopy. This revealed rapid [Nb<sub>6</sub>O<sub>19</sub>]<sup>8−</sup> nucleation along with dissolution of Nb<sub>2</sub>O<sub>5</sub>∙<em>n</em>H<sub>2</sub>O accompanied by the formation of mononuclear Nb species at 160℃. The unveiled mechanistic insights provide the controllability in products during microwave-assisted hydrothermal synthesis of polyoxoniobate clusters.</div></div>\",\"PeriodicalId\":264,\"journal\":{\"name\":\"Catalysis Today\",\"volume\":\"463 \",\"pages\":\"Article 115593\"},\"PeriodicalIF\":5.3000,\"publicationDate\":\"2025-10-07\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Catalysis Today\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0920586125004110\",\"RegionNum\":2,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"CHEMISTRY, APPLIED\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Catalysis Today","FirstCategoryId":"92","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0920586125004110","RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, APPLIED","Score":null,"Total":0}
Mechanism of synthesizing hexaniobate cluster by microwave-assisted hydrothermal reaction
Anionic hexaniobate clusters [Nb6O19]8 −, which act as a superbase catalyst, could be synthesized by the microwave-assisted hydrothermal method at 180℃ within 10 min with high purity, whereas the conventional hydrothermal synthesis method requires a long reaction time (>24 h). In this study, the mechanism of synthesizing [Nb6O19]8− by the microwave-assisted hydrothermal method was investigated by in situ quick-scan X-ray absorption fine structure and electrospray ionization time-of-flight mass spectroscopy. This revealed rapid [Nb6O19]8− nucleation along with dissolution of Nb2O5∙nH2O accompanied by the formation of mononuclear Nb species at 160℃. The unveiled mechanistic insights provide the controllability in products during microwave-assisted hydrothermal synthesis of polyoxoniobate clusters.
期刊介绍:
Catalysis Today focuses on the rapid publication of original invited papers devoted to currently important topics in catalysis and related subjects. The journal only publishes special issues (Proposing a Catalysis Today Special Issue), each of which is supervised by Guest Editors who recruit individual papers and oversee the peer review process. Catalysis Today offers researchers in the field of catalysis in-depth overviews of topical issues.
Both fundamental and applied aspects of catalysis are covered. Subjects such as catalysis of immobilized organometallic and biocatalytic systems are welcome. Subjects related to catalysis such as experimental techniques, adsorption, process technology, synthesis, in situ characterization, computational, theoretical modeling, imaging and others are included if there is a clear relationship to catalysis.