The aim of this critical review is to provide a broad but digestible overview of mechanochemical synthesis, i.e. reactions conducted by grinding solid reactants together with no or minimal solvent. Although mechanochemistry has historically been a sideline approach to synthesis it may soon move into the mainstream because it is increasingly apparent that it can be practical, and even advantageous, and because of the opportunities it provides for developing more sustainable methods. Concentrating on recent advances, this article covers industrial aspects, inorganic materials, organic synthesis, cocrystallisation, pharmaceutical aspects, metal complexes (including metal–organic frameworks), supramolecular aspects and characterization methods. The historical development, mechanistic aspects, limitations and opportunities are also discussed (314 references).

/pdf/mechanochemistry-opportunities-for-new-and-cleaner-synthesis-15fcwynvnd.pdf

Mechanochemistry: opportunities for new and cleaner synthesis

In the last few decades, mechanochemistry has become rapidly established as a powerful tool enabling environmentally-benign and sustainable chemical syntheses. Not only have these techniques been demonstrated as viable alternatives to traditional solution-based syntheses, but they have also received attention for their ability to enable new reactivity and "unlocking" novel compounds inaccessible by conventional methods. Reflecting the rising popularity of mechanochemistry, many excellent reviews highlighting its benefits have recently been published. Whilst the scope of most of these focuses on organic chemistry, transition-metal catalysis, porous framework materials, coordination compounds and supramolecular synthesis, few have addressed the use of mechanochemical ball milling for the synthesis of compounds containing s- and p-block elements. This tutorial review turns the spotlight towards mechanochemical research in the field of inorganic main group chemistry, highlighting significant advantages that solid-state inorganic reactions often possess, and the potential for these to drive the development of greener methodologies within the modern main group arena.

/pdf/main-group-mechanochemistry-from-curiosity-to-established-2cwx9ttjlv.pdf

Main group mechanochemistry: from curiosity to established protocols.

Mechanochemistry means mechanical breakage of intramolecular bonds by external force and must be differentiated from molecular solid-state chemistry, where contacts between micronized molecular solids are created by the mechanical action for mutual approach of the reacting centers. After an outline of the mechanistic differences, the varied mechanochemistry is discussed. Grinding, milling, shearing, scratching, polishing, and rapid friction (for polymers also cutting, kneading, extruding) provide the mechanical impact for mechanochemistry, while sonication and shock waving for intramolecular bond breaking are generally described as thermal processes. The various types of mechanophysics (e.g., mechanoelectricity, conformational changes, thixotropy, rheopexy, stirring of Newtonian liquids or suspensions, etc.) are not treated here. Mechanochemistry covers solid-state reactions of infinitely covalent crystals, brittle metals, polymers, molecular solids with weak covalent bonds, strong intramolecular bond breakage in shearing Bridgman's anvil or by friction at lubrication of rapidly moving cold contacting surfaces, and single bond breaking or cutting. The diverse wealth of practical applications of mechanochemistry is outlined with typical examples for ceramics, mechanical alloying, hydrogen storage, organic syntheses, waste remediation, leachings, surface plasmas, radical formation, explosives, nanotube formation, nanoparticles grafting, polymer technology, radical initiation, scratch-less polishing, wear protection, lubrication, mechanochromism, nano-dissection, and many more.

http://webpages.iust.ac.ir/naimi/Lectures/Current%20Topics%20in%20Synthetic%20Organic,%20PhD/Kaupp,%20MechanochemistryReprint.pdf

Mechanochemistry: the varied applications of mechanical bond-breaking

In recent years, the application of mechanical energy to chemical systems has repeatedly proven beneficial to facilitate chemical transformations in various areas in chemistry. Today, a systematic body of evidence indicates that mechanochemistry holds great promise to become a game-changer in chemical synthesis. Not only does mechanochemistry permit access to products that are inaccessible by established means (e.g. purely thermal activation), mechanochemical reactions often outperform their solution-based counterparts in terms of sustainability. Most mechanochemical reactions carried out by ball milling techniques involve transformations of solids and liquids, but the number of mechanochemical reactions with gaseous reactants is increasing. The aim of this Minireview is to provide an overview of recent chemical reactions involving gaseous samples by ball milling techniques and to highlight advances in ball milling technology for the safe handling of gaseous reagents. Examples of reactions proceeding at the interface of solid-/liquid-/gas-gas systems that led to significant improvements in reactivity or selectivity will also be highlighted.

Mechanochemistry of Gaseous Reactants.

The low or lack of solubility of fullerenes, carbon nanotubes and graphene/graphite in organic solvents and water severely hampers the study of their chemical functionalizations and practical applications. Covalent and noncovalent functionalizations of fullerenes and related materials via mechanochemistry seem appealing to tackle these problems. In this review article, we provide a comprehensive coverage on the mechanochemical reactions of fullerenes, carbon nanotubes and graphite, including dimerizations and trimerizations, nucleophilic additions, 1,3-dipolar cycloadditions, Diels–Alder reactions, [2 + 1] cycloadditions of carbenes and nitrenes, radical additions, oxidations, etc. It is intriguing to find that some reactions of fullerenes can only proceed under solvent-free conditions or undergo different reaction pathways from those of the liquid-phase counterparts to generate completely different products. We also present the application of the mechanical milling technique to complex formation, nanocomposite formation and enhanced hydrogen storage of carbon-related materials.

Mechanochemistry of fullerenes and related materials

Mechanochemical synthesis of kaolin–KH2PO4 and kaolin–NH4H2PO4 complexes for application as slow release fertilizer

This paper reviews mechanochemical (MC) syntheses of functional materials by means of dry grinding operation without heating. First of all, the authors have shown that the MC reaction is dependent on not only material function such as Gibbs free energy change of formation (Δ G G AB O 3 , where A and B trivalent oxides, respectively. Then, another type of complex ones such as AB O 4 from A 2 B 3 and B 2 O 5 , where B is pentavalent oxides, were shown. In these reactions, the structure of the starting samples are very important to determine the reaction completion or not. A reaction/non-reaction map has been introduced in this paper, and it is seen from the data that the radius ( r A , r B and r O ) of the each metal elements in the reaction systems are crucial parameters in the reaction systems. The paper has extended to the synthesis of halides and sulfides conversion, and final example is a doping with non-ferrous metal element into oxide like TiO 2 , attempting the improvement of its visible light photoreactivity. These information would be helpful to understand and estimate the MC solid-state reaction of the starting materials.

A Review on Mechanochemical Syntheses of Functional Materials

This article introduces a mechanochemical (MC) process for the synthesis of KMgPO4 and NH4MgPO4 by milling starting materials in a planetary ball mill. First, KMgPO4 was prepared by milling KHPO4 a...

Mechanochemical route for synthesizing KMgPO4 and NH4MgPO4 for application as slow-release fertilizers

Mechanochemical synthesis of rare earth orthovanadates from R2O3 (R = rare earth elements) and V2O5 powders

Synthesis of potassium/ammonium phosphates and alumina composites through a mechanochemical approach is presented for the first time. γ-alumina and the phosphate are coground and the ground products are characterized by X-ray diffraction and infrared spectroscopy. Quantitative evaluation of the remaining soluble part of the prepared amorphous phase at a low percentage around 10% demonstrates a potential use of the ground samples as slow-release fertilizers.

Mechanochemical Synthesis of Slow‐Release Fertilizers through Incorporation of Alumina Composition into Potassium/Ammonium Phosphates

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