Mechanochemical synthesis of crystalline U(vi) triperoxide solids

CrystEngComm ◽  
2022 ◽  
Author(s):  
Dmytro V. Kravchuk ◽  
Tori Z. Forbes
Keyword(s):  
Mechanochemical Synthesis ◽  
Mechanochemical Reaction

Mechanochemical reaction of UO3 with metal peroxides (M2O2) yields U(vi) triperoxide materials without producing radioactive solvent wastes.

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.

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.

Mechanochemical synthesis insights and solid-state characterization of quininium aspirinate, a glass-forming drug–drug salt

2021 ◽  
Vol 77 (9) ◽  
Author(s):  
Nehemiah Harris ◽  
Jubilee Benedict ◽  
Diane A. Dickie ◽  
Silvina Pagola
Keyword(s):  
Crystal Structure ◽  
Differential Scanning Calorimetry ◽  
Ir Spectroscopy ◽  
Mechanochemical Synthesis ◽  
Mechanochemical Reaction ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Quinine (an antimalarial) and aspirin (a nonsteroidal anti-inflammatory drug) were combined into a new drug–drug salt, quininium aspirinate, C20H25N2O2 +·C9H7O4 −, by liquid-assisted grinding using stoichiometric amounts of the reactants in a 1:1 molar ratio, and water, EtOH, toluene, or heptane as additives. A tetrahydrofuran (THF) solution of the mechanochemical product prepared using EtOH as additive led to a single crystal of the same material obtained by mechanochemistry, which was used for crystal structure determination at 100 K. Powder X-ray diffraction ruled out crystallographic phase transitions in the 100–295 K interval. Neat mechanical treatment (in a mortar and pestle, or in a ball mill at 20 or 30 Hz milling frequencies) gave rise to an amorphous phase, as shown by powder X-ray diffraction; however, FT–IR spectroscopy unambiguously indicates that a mechanochemical reaction has occurred. Neat milling the reactants at 10 and 15 Hz led to incomplete reactions. Thermogravimetry and differential scanning calorimetry indicate that the amorphous and crystalline mechanochemical products form glasses/supercooled liquids before melting, and do not recrystallize upon cooling. However, the amorphous material obtained by neat grinding crystallizes upon storage into the salt reported. The mechanochemical synthesis, crystal structure analysis, Hirshfeld surfaces, powder X-ray diffraction, thermogravimetry, differential scanning calorimetry, FT–IR spectroscopy, and aqueous solubility of quininium aspirinate are herein reported.

scholarly journals Preparation of Aluminium Hydroxide with Mechanochemical Synthesis in the Middle School Laboratory Lesson

2016 ◽  
Vol 21 (1-2) ◽  
pp. 53-59
Author(s):  
Anna Okálová ◽  
Jana Chrappová ◽  
Zuzana Haláková
Keyword(s):  
Mechanochemical Synthesis ◽  
Aluminium Hydroxide ◽  
Mechanochemical Reaction ◽  
Inorganic Synthesis ◽  
Water Release ◽  
Colour Changes ◽  
School Laboratory ◽  
Mechanochemical Reactions ◽  
Laboratory Lesson ◽  
Reaction Schemes

AbstractMechanochemical reactions proceed if solid reactants combine together by grinding, milling or kneading with no or minimal solvent. It is possible to observe changes: fizzing, foaming, colour changes, water release. This process is manually simple and there are several mechanochemical reactions which can be demonstrated during school laboratory lessons. For high school pupils there exist five possibilities of inorganic synthesis: mechanochemical synthesis, crystallisation, precipitation, filtration and decantation. The preparation of aluminium hydroxide in the school laboratory is described in this paper. Five mechanochemical reaction schemes were tested by pupils in their laboratories. The pupils conducted the experiments and filled in worksheets to accompany the practical. On the basis of their results, a suitable procedure for school use is suggested.

MECHANOCHEMICAL SYNTHESIS OF FLUORIDATED HYDROXYAPATITE NANOPOWDER

2008 ◽  
Vol 22 (18n19) ◽  
pp. 3099-3106 ◽  
Author(s):  
M. H. FATHI ◽  
E. MOHAMMADI ZAHRANI
Keyword(s):  
Grain Size ◽  
Ftir Spectroscopy ◽  
Mechanochemical Synthesis ◽  
Ball Mill ◽  
Rotation Speed ◽  
Mechanochemical Activation ◽  
Mechanochemical Reaction ◽  
Fluoridated Hydroxyapatite ◽  
Lower Solubility ◽  
Bone Apatite

Recently fluoridated hydroxyapatite (FHA) has been developed since it possesses lower solubility than pure hydroxyapatite (HA), while maintaining the comparable bioactivity and biocompatibility in dental and orthopedic application. The aim of this work was to synthesize and characterize the FHA nanopowder via mechanochemical activation method. Mechanochemical reaction was performed in the planetary ball mill at 300 rpm rotation speed by using 8 balls with 2 cm diameter. XRD technique was used to evaluate phase and composition and determine the grain size of prepared FHA nanopowder. FTIR spectroscopy was utilized to identify the functional groups and to compare obtained powder with bone apatite. The results showed that the synthesis of FHA after 6 hr ball milling at 300 rpm was completed. Fluorhydroxyapatite grain size was almost 37nm after 6 hr of milling.

scholarly journals Mechanochemical Synthesis of Nanocrystalline Hydroxyapatite from Ca(H2PO4)2.H2O, CaO, Ca(OH)2, and P2O5 Mixtures

Nanomaterials ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 2232
Author(s):  
Sneha Dinda ◽  
Ajay Bhagavatam ◽  
Husam Alrehaili ◽  
Guru Prasad Dinda
Keyword(s):  
Crystallite Size ◽  
Ball Milling ◽  
Mechanochemical Synthesis ◽  
Lattice Strain ◽  
Milled Powder ◽  
High Energy ◽  
Mechanochemical Reaction ◽  
Reactor Wall ◽  
Powder Mixtures ◽  
Nanocrystalline Hydroxyapatite

This paper reports the progress of the mechanochemical synthesis of nanocrystalline hydroxyapatite (HA) starting from six different powder mixtures containing Ca(H2PO4)2.H2O, CaO, Ca(OH)2, and P2O5. The reaction kinetics of HA phase formation during high-energy ball milling was systematically investigated. The mechanochemical reaction rate of the Ca(H2PO4)2.H2O–Ca(OH)2 powder mixture found to be very fast as the HA phase started to form at around 2 min and finished after 30 min of ball milling. All six powder mixtures were transformed entirely into HA, with the crystallite size between 18.5 and 20.2 nm after 1 h and between 22.5 and 23.9 nm after 2 h of milling. Moreover, the lattice strain was found to be 0.8 ± 0.05% in the 1 h milled powder and 0.6 ± 0.05% in all six powders milled for 2 h. This observation, i.e., coarsening of the HA crystal and gradual decrease of the lattice strain with the increase of milling time, is opposite to the results reported by other researchers. The gradual increase in crystallite size and decrease in lattice strain result from dynamic recovery and recrystallization because of an increase in the local temperature of the powder particles trapped between the balls and ball and reactor wall during the high-energy collision.

Comparative studies on conventional and solvent-free synthesis toward hydrazones: application of PXRD and chemometric data analysis in mechanochemical reaction monitoring

CrystEngComm ◽  
2018 ◽  
Vol 20 (13) ◽  
pp. 1804-1817 ◽  
Author(s):  
Jana Pisk ◽  
Tomica Hrenar ◽  
Mirta Rubčić ◽  
Gordana Pavlović ◽  
Vladimir Damjanović ◽  
...  
Keyword(s):  
Data Analysis ◽  
Mechanochemical Synthesis ◽  
Comparative Studies ◽  
Chemometric Analysis ◽  
Solvent Free ◽  
Mechanochemical Reaction ◽  
Reaction Monitoring ◽  
Solvent Free Synthesis

We describe the implementation of chemometric analysis for mechanochemical synthesis monitoring.

scholarly journals Mechanochemical synthesis of nanostructured metal nitrides, carbonitrides and carbon nitride: a combined theoretical and experimental study

2017 ◽  
Vol 19 (19) ◽  
pp. 12414-12424 ◽  
Author(s):  
Seyyed Amin Rounaghi ◽  
Danny E. P. Vanpoucke ◽  
Hossein Eshghi ◽  
Sergio Scudino ◽  
Elaheh Esmaeili ◽  
...  
Keyword(s):  
Experimental Study ◽  
Mechanochemical Synthesis ◽  
Carbon Nitride ◽  
Mechanochemical Reaction ◽  
Metal Nitrides ◽  
Nanostructured Metal

Mechanochemical reaction of metals with melamine: a versatile route to the synthesis of nanostructured metal nitrides, carbonitrides and carbon nitride.

Sign in / Sign up

Export Citation Format

Share Document