Evaluation of the formation pathways of cocrystal polymorphs in liquid-assisted syntheses

Fischer, Friedrich; Scholz, Gudrun; Benemann, Sigrid; Rademann, Klaus; Emmerling, Franziska

doi:10.1039/c4ce00472h

Cited by 45 publications

(59 citation statements)

References 41 publications

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“…[11] Neat grinding of CAFF and AA produced the thermodynamic polymorphic form (form I) [11] of the cocrystal ( Figure 5). [11] Neat grinding of CAFF and AA produced the thermodynamic polymorphic form (form I) [11] of the cocrystal ( Figure 5).…”

Section: Methodsmentioning

confidence: 99%

“…These are both important issues when the aims are [17] b) calculated PHE, [18] c) PHE-MA cocrystal prepared in neat conditions, d) calculated PHE-MA, [9] e), f),a nd h) PHE-MA cocrystal prepared using 2.5, 5a nd 10 wt %o fPEG 10 000 respectively. PXRD pattern of:a )calculated CAFF-AAform I, [11] b) CAFF-AA form Iprepared by neat grinding, c) calculated CAFF-AAform II, [11] d) CAFF-AAprepared by LAG with acetonitrile;C AFF-AAprepared by POLAG using 1wt% of e) PEG 200 and f) PEG 10 000. PXRD pattern of:a )calculated CAFF-AAform I, [11] b) CAFF-AA form Iprepared by neat grinding, c) calculated CAFF-AAform II, [11] d) CAFF-AAprepared by LAG with acetonitrile;C AFF-AAprepared by POLAG using 1wt% of e) PEG 200 and f) PEG 10 000.…”

Section: Methodsmentioning

confidence: 99%

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Cocrystal Formation through Mechanochemistry: from Neat and Liquid‐Assisted Grinding to Polymer‐Assisted Grinding

et al. 2015

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Mechanochemistry is an effective method for the preparation of multicomponent crystal systems. In the present work, we propose an alternative to the established liquid-assisted grinding (LAG) approach. Polymer-assisted grinding (POLAG) is demonstrated to provide a new class of catalysts for improving reaction rate and increasing product diversity during mechanochemical cocrystallization reactions. We demonstrate that POLAG provides advantages comparable to the conventional liquid-assisted process, whilst eliminating the risk of unwanted solvate formation as well as enabling control of resulting particle size. It represents a new approach for the development of functional materials through mechanochemistry, and possibly opens new routes toward the understanding of the mechanisms and pathways of mechanochemical cocrystal formation.

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Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Cocrystal Formation through Mechanochemistry: from Neat and Liquid‐Assisted Grinding to Polymer‐Assisted Grinding

et al. 2015

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“…[11] Neat grinding of CAFF and AA produced the thermodynamic polymorphic form (form I) [11] of the cocrystal ( Figure 5). Instead, POLAGe xperiments using 1wt% of PEG 200 and PEG 10 000 gave CAFF-AA form II ( Figure 5).…”

Section: Methodsmentioning

confidence: 99%

“…[4,11] Thepolymer selected as acatalyst was polyethylene glycol (PEG). PEG is obtained by the polymerization of ethylene oxide under alkaline catalysis,a nd has aw ide range of applications both in the chemical and pharmaceutical industries.…”

mentioning

confidence: 99%

Cocrystal Formation through Mechanochemistry: from Neat and Liquid‐Assisted Grinding to Polymer‐Assisted Grinding

et al. 2015

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Mechanochemistry is an effective method for the preparation of multicomponent crystal systems.I nt he present work, we propose an alternative to the established liquidassisted grinding (LAG) approach.P olymer-assisted grinding (POLAG) is demonstrated to provide an ew class of catalysts for improving reaction rate and increasing product diversity during mechanochemical cocrystallization reactions.W edemonstrate that POLAGp rovides advantages comparable to the conventional liquid-assisted process,whilst eliminating the risk of unwanted solvate formation as well as enabling control of resulting particle size. It represents an ew approachf or the development of functional materials through mechanochemistry,and possibly opens new routes towardthe understanding of the mechanisms and pathwayso fm echanochemical cocrystal formation.

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“…Mechanochemistry is an effective solid‐state approach for the rapid synthesis of materials in high yields . Extensive reviews of mechanosyntheses are available, highlighting their particular benefit of avoiding solvent waste.…”

Section: Introductionmentioning

confidence: 99%

Mechanistic Insights into a Sustainable Mechanochemical Synthesis of Ettringite

et al. 2019

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Mechanochemistry offers an environmentally benign and facile synthesis method for a variety of cement paste constituents. In addition, these methods can be used to selectively tune the properties of cement components. The mineral ettringite is an important component of cementitious materials and has additional technological potential due to its ion exchange properties. Synthesis of ettringite via mechanochemistry is an environmentally friendly alternative to conventional wet‐chemical synthesis established in industry. This contribution explores the mechanism of a two‐step mechanochemical synthesis of ettringite, which was previously found to greatly improve the reaction conversion as compared with one‐pot synthesis. The crystallinity of Al(OH) 3 was found to decrease during the first stage of this mechanochemical synthesis. This was correlated to a significant decrease in the particle size of Al(OH) 3 in this stage. No other significant changes were found for the other components, suggesting that mechanochemical activation of Al(OH) 3 is responsible for the enhanced formation of ettringite by the two‐step approach. The environmentally friendly approach developed for ettringite synthesis offers a versatile synthetic strategy, which can be applied to synthesise further cementitious materials.

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Evaluation of the formation pathways of cocrystal polymorphs in liquid-assisted syntheses

Abstract: Small but important: the kind of solvent added in liquid-assisted grinding syntheses of cocrystals influences the final product and the reaction rate.

Cited by 45 publications

References 41 publications

Cocrystal Formation through Mechanochemistry: from Neat and Liquid‐Assisted Grinding to Polymer‐Assisted Grinding

Cocrystal Formation through Mechanochemistry: from Neat and Liquid‐Assisted Grinding to Polymer‐Assisted Grinding

Cocrystal Formation through Mechanochemistry: from Neat and Liquid‐Assisted Grinding to Polymer‐Assisted Grinding

Mechanistic Insights into a Sustainable Mechanochemical Synthesis of Ettringite

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