scholarly journals In situ monitoring of mechanochemical synthesis of calcium urea phosphate fertilizer cocrystal reveals highly effective water-based autocatalysis

2020 ◽  
Vol 11 (9) ◽  
pp. 2350-2355 ◽  
Author(s):  
Patrick A. Julien ◽  
Luzia S. Germann ◽  
Hatem M. Titi ◽  
Martin Etter ◽  
Robert E. Dinnebier ◽  
...  
Keyword(s):  
Mechanochemical Synthesis ◽  
Phosphate Fertilizer ◽  
In Situ Monitoring ◽  
Mechanochemical Reaction ◽  
Quantitative Investigation ◽  
Urea Phosphate ◽  
Water Based ◽  
Highly Effective ◽  
Effective Water

Using the mechanosynthesis of the fertilizer cocrystal calcium urea phosphate as a model, we provide a quantitative investigation of chemical autocatalysis in a mechanochemical reaction.

scholarly journals Tetrathiafulvalene: A Gate to the Mechanochemical Mechanisms of Electron Transfer Reactions

Crystals ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 482
Author(s):  
Richard Chen ◽  
Mehmet Kerem Gokus ◽  
Silvina Pagola
Keyword(s):  
Mechanochemical Synthesis ◽  
Amorphous Material ◽  
In Situ Monitoring ◽  
Ex Situ ◽  
Mechanochemical Reaction ◽  
Charge Transfer Complexes ◽  
Spectroscopic Techniques ◽  
Diffusion Controlled ◽  
Mechanochemical Reactions

This report describes aspects of our previous studies of the mechanochemical synthesis of charge transfer complexes of the electron donor tetrathiafulvalene, which are relevant to the use of laboratory X-ray powder diffraction for ex situ monitoring of mechanochemical reactions toward investigating their mechanisms. In particular, the reaction of tetrathiafulvalene and chloranil was studied under neat mechanochemical conditions and liquid-assisted grinding with diethyl ether (1 μL/mg). The product in both cases is the green tetrathiafulvalene chloranil polymorph and the mechanism of the redox reaction is presumably the same. However, while the kinetic profile of the neat mechanochemical synthesis was fitted with a second-order rate law, that of the overall faster liquid-assisted grinding reaction was fitted with the Ginstling-Brounshtein 3D diffusion-controlled model. Hence, the diffusional processes and mass transfer bringing the reactants together and separating them from products must be different. Diffraction measurements sensitive to crystalline phases and amorphous material, combined with in situ monitoring by spectroscopic techniques, will ultimately afford a better understanding of mechanochemical reaction mechanisms, a hot topic in mechanochemistry.

In Situ Monitoring of Mechanochemical Synthesis of Calcium Urea Phosphate Fertilizer Cocrystal Reveals Water-Based Autocatalysis

2019 ◽  
Author(s):  
Patrick Julien ◽  
Luzia S. Germann ◽  
Hatem M. Titi ◽  
Martin Etter ◽  
Robert E. Dinnebier ◽  
...  
Keyword(s):  
Direct Evidence ◽  
Phosphate Fertilizer ◽  
In Situ Monitoring ◽  
Mechanochemical Reaction ◽  
X Ray Diffraction ◽  
In Situ Raman Spectroscopy ◽  
X Ray ◽  
In Situ Raman ◽  
In Situ Investigation

Using the mechanosynthesis of the calcium phosphate and urea fertilizer cocrystal as a model, we provide the first in situ investigation of autocatalysis in a mechanochemical reaction. The application of in situ Raman spectroscopy and synchrotron X-ray diffraction provided the first direct evidence of a mechanochemical system in which a reaction product (water) mediates the rate of transformation and underpins positive feedback kinetics.

In Situ Monitoring of Mechanochemical Synthesis of Calcium Urea Phosphate Fertilizer Cocrystal Reveals Water-Based Autocatalysis

2019 ◽  
Author(s):  
Patrick Julien ◽  
Luzia S. Germann ◽  
Hatem M. Titi ◽  
Martin Etter ◽  
Robert E. Dinnebier ◽  
...  
Keyword(s):  
Direct Evidence ◽  
Phosphate Fertilizer ◽  
In Situ Monitoring ◽  
Mechanochemical Reaction ◽  
X Ray Diffraction ◽  
In Situ Raman Spectroscopy ◽  
X Ray ◽  
In Situ Raman ◽  
In Situ Investigation

Using the mechanosynthesis of the calcium phosphate and urea fertilizer cocrystal as a model, we provide the first in situ investigation of autocatalysis in a mechanochemical reaction. The application of in situ Raman spectroscopy and synchrotron X-ray diffraction provided the first direct evidence of a mechanochemical system in which a reaction product (water) mediates the rate of transformation and underpins positive feedback kinetics.

scholarly journals Real-Time in Situ Monitoring of Particle and Structure Evolution in Mechanochemical Synthesis of UiO-66 Metal-Organic Framework

2019 ◽  
Author(s):  
Luzia S. Germann ◽  
Athanassios D. Katsenis ◽  
Igor Huskić ◽  
Patrick A. Julien ◽  
Krunoslav Uzarevic ◽  
...  
Keyword(s):  
Metal Organic Framework ◽  
Model System ◽  
In Situ Monitoring ◽  
Mechanochemical Reaction ◽  
Structure Evolution ◽  
X Ray ◽  
Framework Model ◽  
Metal Organic ◽  
Organic Framework

Manuscript about monitoring the mechanochemical reaction of a metal-organic framework model system by in situ X-ray powder diffraction<br>

scholarly journals Real-Time in Situ Monitoring of Particle and Structure Evolution in Mechanochemical Synthesis of UiO-66 Metal-Organic Framework

2019 ◽  
Author(s):  
Luzia S. Germann ◽  
Athanassios D. Katsenis ◽  
Igor Huskić ◽  
Patrick A. Julien ◽  
Krunoslav Uzarevic ◽  
...  
Keyword(s):  
Metal Organic Framework ◽  
Model System ◽  
In Situ Monitoring ◽  
Mechanochemical Reaction ◽  
Structure Evolution ◽  
X Ray ◽  
Framework Model ◽  
Metal Organic ◽  
Organic Framework

Manuscript about monitoring the mechanochemical reaction of a metal-organic framework model system by in situ X-ray powder diffraction<br>

scholarly journals Synthesis, characterization and in situ monitoring of the mechanochemical reaction process of two manganese(II)-phosphonates with N-containing ligands

2018 ◽  
Vol 53 (19) ◽  
pp. 13390-13399 ◽  
Author(s):  
Irina Akhmetova ◽  
Konstantin Schutjajew ◽  
Manuel Wilke ◽  
Ana Buzanich ◽  
Klaus Rademann ◽  
...  
Keyword(s):  
In Situ Monitoring ◽  
Reaction Process ◽  
Mechanochemical Reaction

scholarly journals Tuning and in situ monitoring of surface-initiated, atom-transfer radical polymerization of acrylamide derivatives in water-based solvents

2019 ◽  
Vol 10 (29) ◽  
pp. 3933-3942 ◽  
Author(s):  
Joydeb Mandal ◽  
Rok Simic ◽  
Nicholas D. Spencer
Keyword(s):  
Atomic Force Microscopy ◽  
Quartz Crystal ◽  
Polymer Brush ◽  
In Situ Monitoring ◽  
Colloidal Probe ◽  
Force Microscopy ◽  
Atomic Force ◽  
Water Based ◽  
Kinetics Of

SI-ATRP kinetics of acrylamide derivatives is studied in situ using a quartz crystal microbalance with dissipation (QCM-D). The effect of growth kinetics on polymer-brush dispersity have been examined using colloidal-probe atomic force microscopy.

scholarly journals Real-Time in Situ Monitoring of Particle and Structure Evolution in the Mechanochemical Synthesis of UiO-66 Metal–Organic Frameworks

2019 ◽  
Vol 20 (1) ◽  
pp. 49-54 ◽  
Author(s):  
Luzia S. Germann ◽  
Athanassios D. Katsenis ◽  
Igor Huskić ◽  
Patrick A. Julien ◽  
Krunoslav Užarević ◽  
...  
Keyword(s):  
Real Time ◽  
Mechanochemical Synthesis ◽  
Metal Organic Frameworks ◽  
In Situ Monitoring ◽  
Structure Evolution ◽  
Metal Organic

scholarly journals Control of Pharmaceutical Cocrystal Polymorphism on Various Scales by Mechanochemistry: Transfer from the Laboratory Batch- to the Large-Scale Extrusion Processing

2018 ◽  
Author(s):  
Tomislav Stolar ◽  
Stipe Lukin ◽  
Martina Tireli ◽  
Irena Sović ◽  
Bahar Karadeniz ◽  
...  
Keyword(s):  
Vitamin C ◽  
Mechanochemical Synthesis ◽  
Large Scale ◽  
Antioxidant Properties ◽  
In Situ Monitoring ◽  
Human Consumption ◽  
Continuous Manufacturing ◽  
X Ray Diffraction ◽  
X Ray

<p>We demonstrate a controllable mechanochemical synthesis of cocrystal polymorphs of ascorbic acid (vitamin C) and nicotinamide (vitamin B3) on different scales and without using bulk solvents. Next to the previously described polymorph of the 1:1 cocrystal, which is one of the first cocrystals approved for human consumption, we report here a new, thermodynamically more stable polymorph detected during in situ synchrotron powder X-ray diffraction monitoring of milling reactions. The new polymorph is currently available exclusively by mechanochemical synthesis, and its crystal structure was determined from powder X-ray diffraction data. Laboratory in situ monitoring by Raman spectroscopy provided direct insight into the cocrystals formation and was further used to optimize the manufacturing procedure. Sub-gram synthesis using laboratory mixer mill was transferred to the 10 g scale on a planetary ball mill and continuous manufacturing using a twin-screw extruder. Both cocrystal polymorphs perform excellently in tableting, thus alleviating the notoriously poor compactible properties of vitamin C, while the mechanochemical cocrystallization does not harm its antioxidant properties.<b></b></p>

scholarly journals Control of Pharmaceutical Cocrystal Polymorphism on Various Scales by Mechanochemistry: Transfer from the Laboratory Batch- to the Large-Scale Extrusion Processing

2018 ◽  
Author(s):  
Tomislav Stolar ◽  
Stipe Lukin ◽  
Martina Tireli ◽  
Irena Sović ◽  
Bahar Karadeniz ◽  
...  
Keyword(s):  
Vitamin C ◽  
Mechanochemical Synthesis ◽  
Large Scale ◽  
Antioxidant Properties ◽  
In Situ Monitoring ◽  
Human Consumption ◽  
Continuous Manufacturing ◽  
X Ray Diffraction ◽  
X Ray

<p>We demonstrate a controllable mechanochemical synthesis of cocrystal polymorphs of ascorbic acid (vitamin C) and nicotinamide (vitamin B3) on different scales and without using bulk solvents. Next to the previously described polymorph of the 1:1 cocrystal, which is one of the first cocrystals approved for human consumption, we report here a new, thermodynamically more stable polymorph detected during in situ synchrotron powder X-ray diffraction monitoring of milling reactions. The new polymorph is currently available exclusively by mechanochemical synthesis, and its crystal structure was determined from powder X-ray diffraction data. Laboratory in situ monitoring by Raman spectroscopy provided direct insight into the cocrystals formation and was further used to optimize the manufacturing procedure. Sub-gram synthesis using laboratory mixer mill was transferred to the 10 g scale on a planetary ball mill and continuous manufacturing using a twin-screw extruder. Both cocrystal polymorphs perform excellently in tableting, thus alleviating the notoriously poor compactible properties of vitamin C, while the mechanochemical cocrystallization does not harm its antioxidant properties.<b></b></p>

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