<i>In situ</i> investigation of controlled polymorphism in mechanochemistry at elevated temperature

Linberg, Kevin; Sander, Philipp C.; Emmerling, Franziska; Michalchuk, Adam A. L.

doi:10.1039/d3mr00019b

Cited by 5 publications

(1 citation statement)

References 57 publications

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“…Indeed, the recent coupling of milling with various energy sources has led to unique reactions not achievable solely by conventional milling techniques . In particular, regulating the temperature of the milling vessel affects the reaction rate, its mechanisms, and selectivity. − Developing a milling reactor operating at temperatures >100 °C opens the possibility of employing mechanochemistry for previously unexplored systems …”

Section: Introductionmentioning

confidence: 99%

Mechanochemically Induced OSDA-Free Interzeolite Conversion

Jakupec,

Ardila-Fierro,

Martinez

et al. 2024

ACS Sustainable Chem. Eng.

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Zeolites are versatile materials widely used in various aspects of modern society and are some of the most relevant industrial catalysts. Regardless of such ubiquity, the conventional hydrothermal synthesis of zeolite materials with predetermined properties is challenging and in some instances not feasible, motivating a constant search for new synthesis avenues to expand their application potential. Here, thermally controlled mechanochemistry results in rapid, controllable, and energyefficient organic structures directing agent-free (OSDA-free) interzeolite conversions. Milling under elevated temperatures yielded pure solid phases distinct from the parent commercial zeolite Y. In situ synchrotron X-ray diffraction monitoring revealed a strong effect of the composition of the reaction mixture on the reaction pathways and interconversion outcome. The properties of the formed material arise as an outcome of the subtle interplay of the kinetic and thermodynamic factors. The findings reported here afford directions for broader zeolite mechanosynthesis.

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Section: Introductionmentioning

confidence: 99%

Mechanochemically Induced OSDA-Free Interzeolite Conversion

Jakupec,

Ardila-Fierro,

Martinez

et al. 2024

ACS Sustainable Chem. Eng.

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Mechanochemical Transformations of Pharmaceutical Cocrystals: Polymorphs and Coformer Exchange

Trzeciak,

Dudek,

Potrzebowski

2024

Chemistry A European J

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Transformations of solid samples under solvent‐free or minimal solvent conditions set the future trend and define a modern strategy for the production of new materials. Of the various technologies tested in recent years, the mechanochemical approach seems to be the most promising. The aim of this review article is to present the current state of art in solid state research on binary systems, which have found numerous applications in the pharmaceutical and materials science industries. This article is divided into three sections. In the first part, we describe the new equipment improvements. A brief description of techniques dedicated to ex‐situ and in‐situ studies of progress and the mechanism of solid matter transformation is presented. In the second section, we discuss the problem of cocrystal polymorphism highlighting the issue related with correlation between mechanochemical parameters (time, temperature, energy, molar ratio, liquid assistant, surface energy, crystal size, crystal shape) and preference for the formation of requested polymorph. The last part is devoted to the description of the processes of coformer exchange in binary systems forced by mechanical and/or thermal stimuli. The influence of the thermodynamic factor on the selection of the best‐suited partner for the formation of a two‐component structure is presented.

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Terahertz-Raman spectroscopy for in situ benchtop monitoring of changes to extended, supramolecular structure in milling mechanochemistry

Borchers,

Topić,

Arhangelskis

et al. 2024

Chem

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In situ investigation of controlled polymorphism in mechanochemistry at elevated temperature

Abstract: Through thermo-mechanochemical conditions it is possible to generate metastable crystal forms below equilibrium thermodynamic transition temperatures, making thermo-mechanical conditions an exciting new direction for solid form control.

Cited by 5 publications

References 57 publications

Mechanochemically Induced OSDA-Free Interzeolite Conversion

Mechanochemically Induced OSDA-Free Interzeolite Conversion

Mechanochemical Transformations of Pharmaceutical Cocrystals: Polymorphs and Coformer Exchange

Terahertz-Raman spectroscopy for in situ benchtop monitoring of changes to extended, supramolecular structure in milling mechanochemistry

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