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

Recycling of PVC wastes

Influence of aggressive ions on the degradation behavior of biomedical magnesium alloy in physiological environment.

This paper describes a hydrometallurgical process for recovering neodymium (Nd) and dysprosium (Dy) from a magnetic waste sludge generated from the Nd–Fe–B(–Dy) manufacturing process. Phase analysis by XRD study revealed Nd(OH)3 and Fe2O3 as main mineral phases, and chemical analysis by ICP showed the contents of 35.1 wt% Nd, 29.5 wt% Fe, 1.1 wt% Dy and 0.5 wt% B. A solution of 1 M HNO3 + 0.3 M H2O2 was used to dissolve up to 98 % Nd and 81 % Dy, while keeping Fe dissolution below 15 % within 10 min. Fe dissolved in solution was completely removed as Fe(OH)3 at pH 3 followed by precipitation of Nd and Dy with oxalic acid (H2C2O4) and recovered 91.5 % of Nd and 81.8 % of Dy from solution. The precipitate containing Nd and Dy was calcined at 800 °C to obtain Nd2O3 as final product with 68 % purity, and final recovery of 69.7 % Nd and 51 % of Dy was reported in this process.

Recovery of Nd and Dy from rare earth magnetic waste sludge by hydrometallurgical process

We have attempted to synthesize the meixnerite (Mg–Al–OH) type layered double hydroxide (LDH) by a two step milling operation of a mixture of Mg(OH)2 and Al(OH)3 with water. In the first-step, a mixture of the starting materials was milled for 1 h without water, and the product prepared in the first-step was milled for 2 h with water in the second-step milling operation. The milled products were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR), and thermo gravimetric-differential thermal analyses with mass spectroscopy (TG-DTA/MS). The surface morphology was characterized by scanning electron microscopy (SEM). Meixnerite with a small amount of carbonate was successfully synthesized mechanochemically at ambient conditions by milling for only 3 h in a planetary ball mill.

Preparation of meixnerite (Mg–Al–OH) type layered double hydroxide by a mechanochemical route

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

Simultaneous treatment of PVC and oyster-shell wastes by mechanochemical means

Mechanochemical decomposition of PVC by using La2O3 as additive

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