Challenges of Mechanochemistry: Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation | Sciact - CRIS-система Института катализа

Challenges of Mechanochemistry: Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation Научная публикация

Журнал

Advanced Science
, E-ISSN: 2198-3844

Вых. Данные

Год: 2017, Том: 4, Номер: 9, Номер статьи : 1700132, Страниц : 7 DOI: 10.1002/advs.201700132

Ключевые слова

kinetics, mechanochemistry, organic salts, X-ray powder diffraction

Авторы

Michalchuk Adam A.L. ^1,2,3 , Tumanov Ivan A. ^1,4 , Konar Sumit ² , Kimber Simon A.J. ⁵ , Pulham Colin R. ^2,3 , Boldyreva Elena V. ^1,4

Организации

1	REC-008 Novosibirsk State University ul. Pirogova 2, 630090 Novosibirsk, Russian Federation
2	EaStChem School of Chemistry and Centre for Science at Extreme Conditions (CSEC) University of Edinburgh Edinburgh EH9 3FJ, UK
3	EPSRC Centre for Continuous Manufacturing and Crystallisation (CMAC), Joseph Black Building, King’s Buildings, David Brewster Rd. Edinburgh EH9 3FJ, UK
4	Institute of Solid State Chemistry and Mechanochemistry SB RAS Kutateladze 18, 630128 Novosibirsk, Russian Federation
5	European Synchrotron Radiation Facility 71 avenue des Martyrs, 38000 Grenoble, France

Информация о финансировании (5)

1	Министерство образования и науки Российской Федерации	1828
2	Российский фонд фундаментальных исследований	16-33-60086 (АААА-А15-115121840103-1)
3	Федеральное агентство научных организаций России	0301-2014-0002
4	Engineering and Physical Sciences Research Council	CMAC 1/1033459/1
5	The University of Edinburgh

Mechanochemical methods offer unprecedented academic and industrial opportunities for solvent‐free synthesis of novel materials. The need to study mechanochemical mechanisms is growing, and has led to the development of real‐time in situ X‐ray powder diffraction techniques (RI‐XRPD). However, despite the power of RI‐XRPD methods, there remain immense challenges. In the present contribution, many of these challenges are highlighted, and their effect on the interpretation of RI‐XRPD data considered. A novel data processing technique is introduced for RI‐XRPD, through which the solvent‐free mechanochemical synthesis of an organic salt is followed as a case study. These are compared to ex situ studies, where notable differences are observed. The process is monitored over a range of milling frequencies, and a nonlinear correlation between milling parameters and reaction rate is observed. Kinetic analysis of RI‐XRPD allows, for the first time, observation of a mechanistic shift over the course of mechanical treatment, resulting from time evolving conditions within the mechanoreactor.

Michalchuk A.A.L. , Tumanov I.A. , Konar S. , Kimber S.A.J. , Pulham C.R. , Boldyreva E.V.
Challenges of Mechanochemistry: Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation

Advanced Science. 2017. V.4. N9. 1700132 :1-7. DOI: 10.1002/advs.201700132 WOS Scopus РИНЦ CAPlus OpenAlex

Полный текст от издателя

Поступила в редакцию:	22 мар. 2017 г.
Опубликована online:	8 мая 2017 г.
Опубликована в печати:	1 сент. 2017 г.

Web of science:	WOS:000411148100014
Scopus:	2-s2.0-85019110441
РИНЦ:	31021610
Chemical Abstracts:	2017:1512933
OpenAlex:	W2612038360

БД	Цитирований
Scopus	50
Web of science	53
OpenAlex	64