Mechanochemical reactors with a self-regulating thermal management system based on heat pipes

Abstract

A single- or multi-stage mechanochemical reactor (1) according to Figure 1, selected from the group consisting of ball mills, attritor ball mills, vibrating ball mills, resonant acoustic mixers, hammer mills, impact mills, pin mills, cutting mills, jet mills and twin-shaft extruders, equipped with a self-regulating thermal management system for a temperature range of -195°C to 1000°C, wherein - the self-regulating thermal management system comprises at least one heat pipe (2) and / or at least one flat heat pipe (3) and at least one heat source (4) and at least one heat sink (5) which are in thermally conductive contact with each other, - that at least one heat pipe (2) and / or at least one flat heat pipe (3) is or are installed in and / or a static component (1.1) of the reactor (1) and is or are in thermally conductive contact with the material to be ground (1.2) or the material to be ground (1.2) and the grinding media or grinding balls (1.4) in at least one grinding chamber (1.3) of the reactor (1) and - the static component (1.1) serves as a heat source (4) or as a heat sink (5) for the at least one heat pipe (2) and / or the at least one flat heat pipe (3); as well as its use in the fields of chemistry, biochemistry, nanotechnology, pharmacy, biology and microbiology, and environmental technology.

Description

Field of invention

[0001] The present invention relates to mechanochemical reactors with a self-regulating heat management system based on heat pipes.

[0002] Furthermore, the present invention relates to the use of the mechanochemical reactors with a self-regulating heat management system based on heat pipes in the fields of chemistry, biochemistry, nanotechnology, pharmaceuticals, medicine, biology and microbiology and environmental engineering under thermally controlled mechanochemical conditions, in particular for the grinding of materials, for carrying out chemical reactions for the production of suspensions and for the direct capture of carbon dioxide from gases by mineralization (Direct Gas Carbonization by Mechanochemical Mineralization; DGCMM) under thermally controlled mechanochemical conditions.

[0003] Furthermore, the present invention relates to a method for grinding materials, carrying out chemical reactions, producing suspensions and directly capturing carbon dioxide from gases (DGCMM) under thermally controlled mechanochemical conditions using mechanochemical reactors with a self-regulating heat management system. State of the art

[0004] The production of powders in the form of macro-, micro-, and nanoparticles in materials science, nanotechnology, the food industry, the pharmaceutical industry, and environmental technology through the grinding of solids of all kinds, such as stones, ores, cement, pigments, spices, grains, metals, chemical compounds, etc., is a fundamental operation in process engineering. A whole range of mechanochemical mills are available for this purpose, including ball mills, attritor ball mills, vibrating ball mills, resonant acoustic mixers, hammer mills, impact mills, pin mills, cutting mills, and jet mills, each adapted to the specific material being ground. These mechanochemical mills help to mix and homogenize materials uniformly, thereby achieving a consistent distribution of particle size and composition.

[0005] Thus, the primary function of these mills is the comminution of solids through mechanical forces. This comminution occurs particularly when... - by impact; the particles of the material being ground are broken up by rapid movements of the grinding media; - through friction: the particles rub against each other and against the grinding media, leading to further comminution; - through collision events in which the particles between the grinding media and the wall of the mills are crushed and broken down; - Piezoelectric effects (charge separation) and the emission of electrons.

[0006] This can lead to mechanochemical reactions, because the high energy input and release during comminution can trigger chemical reactions that would otherwise be difficult or only possible under extreme conditions. Examples include solid-state reactions between solid materials activated by mechanical energy, or reactions with gases introduced into the mills to react with the pulverized materials. The mechanical energy can also cause phase transitions in the materials, such as from crystalline to amorphous or from one crystalline phase to another. Mechanical processing can also alter the surface of the particles by creating new reaction sites or increasing the surface energy.

[0007] The specific physicochemical effects and mechanisms of mechanochemistry are the subject of numerous theoretical and experimental investigations, which are described, for example, in the articles by - VV Boldyrev, Mechanochemistry and mechanical activation of solids, in Russian Chemical Reviews, 75 (3) 177-189 (2006); - P. Yu. Butygain and AN Streletskii, The Kinetics and Energy Balance of Mechanochemical Transformations, in Physics of the Solid State, Vol. 47, No. 5, 2005, 856-852; - J. Fontaine et al. Tribochemistry between hydrogen and diamond-like carbon films, in Surface Coatings Technology 146-147 (2001) 286-291; - L. Takacs, Mechanochemistry and the Other Branches of Chemistry: Similarities and Differences, in Acta Physica PolonicaA, Vol. 121 (2012), 3, 711-714; - SA Steiner III et al., Circumventing the Mechanochemical Origins of Strength Loss in the Synthesis of Hierarchical Carbon Fibers, in Applied Materials & Interfaces, 2013, 4892-4903; or - Materialsgate Newsletter 12.9.2017, Tribology: Simulation reveals previously unknown friction mechanisms at the molecular level; or in the textbooks - by Gerhard Heinicke, Tribochemistry, Akademie-Verlag Berlin, 1984, or - Czeslaw Kajdas and Ken'ichi Hiratsuka, editors, Tribocatalysis, Tribochemistry, and Tribocorrosion, Pan Stanford Publishing, 2018, be described.

[0008] In recent years, the application of mechanochemical mills and reactors in the field of synthetic chemistry has developed rapidly. Besides the possibilities mentioned earlier, mechanochemistry offers the significant advantage that chemical reactions can be carried out without the use of solvents, especially volatile, flammable, toxic, non-biodegradable, and / or ozone-depleting solvents, and even achieve better yields than conventional methods. This is evidenced by the growing number of relevant scientific publications and review articles, such as... - SL James et al., Mechanochemistry: opportunities for new and cleaner synthesis, in Chem. Soc. Rev., 2012, 41, 413-447, which refers to syntheses of inorganic materials such as alloys, oxides, halides, sulfides, nitrides and composites, cocrystals such as charge-transfer cocrystals, acid-base cocrystals, ionic cocrystals and organic catalysis by cocrystallization, new forms of drugs such as pharmaceutical cocrystals and organic syntheses with carbon-carbon and carbon-X bond formation such as stoichiometric organic reactions, metal-catalyzed organic reactions, organocatalytic asymmetric reactions, syntheses of ligands and host-guest systems, the synthesis of metal complexes and the synthesis of coordination polymers (MOFs); - P. Balaz et al., Hallmarks of mechanochemistry: from nanoparticles to technology, in Chem. Soc. Rev., 42, 2013, 7571-7637; - D. Margetic and V. Strukil describe, among other things, continuous solid-state syntheses in twin-screw extruders in Recent Advances in Mechanochemical Organic Synthesis, DOI: http: / / dx.doi.org / 10.7772 / intecopen.90897; - Xu Sun et al. describe in Ultrafast green synthesis of sub-micron Silicate-1 zeolites by a grinding method, Journal of Solid State Chemistry, Volume 310, June 2022, 123016, the rapid synthesis of the material without the production of waste; - Tomislav Friscic, Supramolecular concepts and new techniques in mechanochemistry: cocrystals, cages, rotoxanes, open metal-organic frameworks, in Chem. Soc. Rev., 2012, 41, 3493-3510; - Junfeng Zhou et al. describe the mechanochemical depolymerization and repolymerization of polymers in Mechanochemical Degradation and Recycling of Synthetic Polymers, Angewandte Chemie Int. Ed., 2023, 62, e202300768; - C. Lennox et al. describe in Direct mechanocatalysis by resonant acoustic mixing (RAM), Chemical Sci, 2023 14, 7475-7481, the copper-catalyzed alkyne-azide click coupling (CuAAC) in an acoustomechanical reactor; - M. Wohlgemuth et al. compare resonant acoustic mixing processes with processes in ball mills using Suzuki cross couplings in Direct Mechanoctalysis without Milling Media - From Mixer Mill to Resonant Acoustic Mixer, Chemistry Europe, https: / / doi.org / 10.1002 / chem.202301714; - Huaizhou Yang et al. describe the depolymerization of lignin in a ball mill in Enhanced Catalytic Depolymerization of a Kraft Lignin by a Mechanochemical Approach, Energy Fuel 2022, 36, 12, 6606-6610, https: / / doi.org / 10.1002 / chem.202301714; - Läszlö Jicsinszky et al. give an overview of the mechanochemical depolymerization of biopolymers in Mechanochemical Degradation of Biopolymers, Molecules, 2023 Dec; 28(24): 8031, Matej Baláž, Academic Editor, Published online 2023 Dec 10. doi: 10.3390 / molecules28248031, PMCID: PMC10745761, PMID: 38138521; - SM Immohr investigates gas-phase reactions under mechanochemical conditions in her dissertation, Mechanocatalytic Effects in the Ball Mill, Faculty of Chemistry and Biochemistry, Ruhr University Bochum, 2015; - MAA Mohamed et al. describe the mechanochemical synthesis of cathode material in Mechanochemical synthesis of Li-rich (LiFe)SO cathode for Li-ion batteries, Green Chemistry, 2023, 10, https: / / pubs.rsc.org / en / content / articlelanding / 2023 / gc / d3qc00861d; - Tanja Butt, RETSCH GmbH, Haan, gives a brief overview of organic syntheses in ball mills in LABO, Mechanochemistry - a solvent-free synthesis method - reactions in ball mills, 2023; - Koji Kubota et al. provide an overview of the reactions in question in Redox reactions of small organic molecules using ball milling and piezoelectric materials, Science, Vol. 366, No. 6472, https: / / www.science.org / doi / 10.1126 / science.aay8224; -Gefei Wang et al. describe in Solid-state molecular oxygen activation using ball milling and a piezoelectric material for aerobic oxidation of thiols, DOI: 10.1039 / D2RA02255A (Paper) RSC Adv., 2022, 12, 18407-18411, https: / / pubs.rsc.org / en / content / article / 2022 / ra / d2ra02255a 1 / 12, the mechanochemical oxidation of thiols; - Yadong Pang et al. investigate the generation and reactions of trifluoromethyl radicals under mechanochemical conditions in Solid-State Radical CH Trifluoromethylation Reactions Using Ball Milling and Piezoelectric Materials, 2020, https: / / doi.org / 10.1002 / anie.202009844; - Mingjun Xuan et al. give an overview of the reactions of unsaturated and aromatic compounds under mechanochemical conditions in The Mechanochemical Synthesis and Activation of Carbon-Rich π-Conjugated Materials, Advanced Science Volume 9, Issue 19 2105497, 2022, https: / / doi.org / 10.1002 / advs.202105497; - F. Cavalierie and F. Padella show in Development of composite materials by mechanochemical treatment of post-consumer plastic waste, Waste Management, 22 (2002) 913-916, that a composite can be produced from mixtures of polypropylene and polyethylene by grinding in liquid carbon dioxide, which no longer shows any incompatibility between the two polymers and which has better properties than the starting polymers; - Haoliang Jia et al. describe in Formation of nanocrystalline TiC from titanium and different carbon sources by mechanical alloying, Journal of Alloys and Compounds, 472 (2009) 97-103, the production of nanocrystalline titanium carbide from titanium powders and different carbon sources; - Tan Xing et al. describe in Ball milling: a green approach for synthesis of nitrogen doped carbon nanoparticles in Nanoscale, 2013, 5, 7970-7976, an industrially applicable synthesis method for the production of nitrogen-doped carbon nanoparticles; - L. Borchardt et al. describe in Mechano-chemistry assisted synthesis of hierarchical porous carbon applied as supercapacitors, Beilstein Journal of Organic Chemistry, 2017, 13, 1332, the production of porous carbon from plant materials for use in capacitors and electrodes. - S. Motozuka et al. describe in Mechanochemical surface modification of carbon fibers using a simple rubbing method in Journal of Composite Materials 0 (0) 1-8, the surface modification of carbon fibers based on polyacrylonitrile by mechanical friction; - S. Grätz and L. Borchardt describe in Mechanochemical polymerization - controlling a polycondensation reaction between a diamine and a dialdehyde in a ball mill, RCS Adv., 2016, 6, 64799-64802, the mechanochemical polycondensation between a diamine and a dialdehyde, which offers an attractive alternative to conventional methods; - Federico Cuccu, Prof. Dr. Lidia De Luca, Prof. Dr. Francesco Delogu, Prof. Dr. Evelina Colacino, Prof. Dr. Niclas Solin, Dr. Rita Mocci, Prof. Dr. Andrea Porcheddu compare reactions in solvents and mechanochemical reactions in Mechanochemistry: New Tools to Navigate the Uncharted Territory of “Impossible” Reactions, ChemSusChem, 2022, https: / / doi.org / 10.1002 / cssc.202200362, comprehensively discussing reactions in solvents and mechanochemical reactions and demonstrating new synthetic methods; the publication also explicitly points out that the sometimes extreme heat generation during milling leads to problems in organic mechanochemical syntheses that still need to be solved; or - C. Hering-Junghans shows in Blickpunkt Inorganik. Mixen und Mahlen statt Lösen und Rühren, Nachrichten aus der Chemie, 72, April 2024, 68-72, that solventless syntheses of molecules such as tetraallyltin(IV) and of solid dispersions, which are considered impossible to produce in solution, are possible in ball mills and even in kitchen mixers.

[0009] In fact, it has also been possible to carry out a so-called "Dream Reaction" mechanochemically, namely the reaction of hydrogen and nitrogen at room temperature. See: - Gao-Feng Han et al., Mechanochemistry for ammonia synthesis under mild conditions, Nature Nanotechnology 16, 325-330 (2021); - Steffen Reichle et al., Mechanocatalytic Room-Temperature Synthesis of Ammonia from Its Elements Down to Atmospheric Pressure, 2021, https: / / doi.org / 10.1002 / anie.202112095; and - Ferdi Schüth, Ball mills as catalytic reactors: Ammonia synthesis at room temperature and atmospheric pressure, Research Report 2022 - Max Planck Institute for Coal Research.

[0010] Mechanochemistry is also gaining increasing importance in environmental technology, as the following exemplary scientific publications demonstrate. - In the conference report AIP Conference Proceedings, Volume 1664, Issue 1, 150008 (2015), Recycling and Processing of several typical crosslinked polymer scraps with enhanced mechanical properties based on solid state mechanochemical milling, the authors describe the milling of partially devulcanized or decrosslinked tire rubber scraps, revulcanized fluororubber scraps and crosslinked polyethylene scraps from cable waste, in which they obtain material with improved processability and better mechanical properties; - Kunlun Zhang et al. describe the mechanochemical degradation of these perennial chemicals in Destruction of Perfluorooctane Sulfonate (PFOS) and Perfluorooctanoic Acid (PFOA) by Ball Milling, Environ. Sci. Technol. 2013, 47, 12, 6471-6477, https: / / doi.org / 10.1021 / es400346n; - G. Cagnetta et al. describe in Mechanochemical conversion of brominated POPs into useful oxybromides: a greener approach, Sci. Rep., 2016, 6, 28394, the decomposition of brominated persistent organic pollutants by reaction with stoichiometric amounts of bismuth oxide or lanthanum oxide to form the corresponding oxybromides and amorphous carbon; - W. Tonganmp et al. describe in Simultaneous treatment of PVC and oyster-shell wastes by mechanochemical means, Waste Management 28 (2008) 484-488, the dechlorination of PVC with oyster shell waste, which yields calcium chloride and organic products with double bonds; - G. Cagnetta provides an overview of mechanochemical soil decontamination in "A mini-review on mechanochemical treatment of contaminated soil: From laboratory to large-scale", Critical Reviews in Environmental Science and Technology, August 2018, pages 1 to 51; and - Nanyang Yang et al. describe the 100% destruction of these persistent chemicals in the ball mill in Solvent-Free Nonthermal Destruction of PFAS Chemicals and PFAS in Sediment by Piezoelectric Ball Milling, Environ. Sci. Technol. Lett. 2023, 10, 2, 198-203, https: / / doi.org / 10.2021 / acs.estlett.2c00902.

[0011] The growing importance of mechanochemistry for chemical syntheses is also reflected in the increasing number of relevant patents, such as: - DE 601 17 922 T2, Mechanochemical synthesis of lithium-containing manganese dioxide; - DE 10 2021 104 059 A1, Mechanochemical synthesis process for the production of amides; - DE 10 2021 106 741 A1, Mechanochemical synthesis process using a catalytically active shaped body; - DE 10 2022 115 870 A1, Mechanochemical process for solvent-free Fries rearrangement; - EP 0 506 979 B1, Organic polymer compound and production thereof; - EP 1 830 824 B1, Nanoparticle composition and methods for synthesis thereof; - EP 4 253 398 A1, A mechanochemical method for obtaining cyclic peptides by solid state transformation; - US 10 947 120 B2, Production method of low dimensional nano material; - US 11 505 471 B2, Mechanochemical synthesis of rare earth sulfides; - US 2004 / 0092760 A1, Method for preparing pentaerythritol phosphate alcohol by mechanochemical synthesis; - US 2013 / 0266507 A1, Mechanochemical production of zeolites; or - WO 2018 / 104228 A1, Mechanochemical synthesis of radiographic agents intermediates.

[0012] While the milling of solids for powder production is carried out on a laboratory to industrial scale, syntheses are performed on a small scale in laboratory mills. The question of whether these syntheses can be carried out on a larger scale remains open. The same applies to environmental technology.

[0013] German patent application DE 10 2014 101 766 A1 discloses a process for the recovery and, if necessary, separation of lanthanides as chlorides or oxides from mineral waste and residues. In this process, powder particles are first produced, which are then mechanochemically activated.

[0014] The translation of European patent EP 0 963 825 B1, DE 699 11 502 T2, describes the mechanochemical treatment of plastics such as polyethylene terephthalate, polystyrene, polypropylene or polyethylene in the presence of liquid carbon dioxide for the compatibilization and recycling of heterogeneous plastics obtained from urban or commercial waste.

[0015] Another problem with recycling plastics, especially mixed-grade plastics and plastic laminates, is their high content of organically bound halogens, for example, when PVC, PVDF, PTFE, or chlorofluoropolymers are present in the plastic waste. Mechanochemistry also offers solutions here.

[0016] German patent DE 197 42 297 C2 discloses a mechanochemical process for the reductive dehalogenation of halogenated organic compounds, wherein the substance or mixture is ground in a single step with the addition of elemental alkali metal, alkaline earth metal, aluminum, or iron as a reducing agent and ethers, polyethers, ammonia, amines, amides, trialkylsilanes, polyalkylhydrogensiloxanes, or metal nitrides, individually or in combination, as a hydrogen source. In this way, sands or soils contaminated with PCBs or chlorophenes can be mechanochemically decontaminated.

[0017] However, not only the high organohalogen content of plastics like PVC, but also lower organohalogen content can cause problems in the recycling of plastics and plastic laminates. Even if the waste does not contain organically bound halogens, ubiquitous persistent organic pollutants (POPs) inevitably accumulate over time after prolonged outdoor use of the plastics and laminates. These include first-generation organochlorine insecticides such as chlordane, DDT, dieldrin, and toxaphene, industrially produced chemicals such as PCBs, and byproducts of manufacturing and combustion processes such as chlorinated and brominated dioxins and dibenzofurans. Representatives of these classes of compounds are also known as the "Dirty Dozen."POPs are semi-volatile and can occur in the gas phase as well as bound to dust particles, and are distributed worldwide via long-range transport mechanisms. Due to their lipophilicity, they bioaccumulate in the fatty tissues of animals and humans. Some POPs are considered endocrine disruptors or carcinogenic and are also associated with infertility, behavioral abnormalities, and immunodeficiency. They also contaminate, even in trace amounts, industrial products such as titanium dioxide nanoparticles, which are used as color pigments in cosmetics, inks, and plastics. While the quantities may appear small individually, they cannot be disregarded due to the amounts of titanium dioxide involved [see the article by Georgios Ctistis, Peter Schön, Wouter Bakker, and Gregor Luthe, "PCDDs, PCDFs, and PCBs cooccurence in TiO2 nanoparticles," in Environmental Science and Pollution Research, DOI 10.1007 / s11356-015-5628-7].

[0018] German patent DE 102 61 204 A1 discloses a process for the decontamination or detoxification of solid or liquid products contaminated with environmental toxins such as polyhalogenated compounds or organochlorine substances like dioxins, dibenzofurans and congeners, or PCBs. This process employs high-kinetic methods in which the contaminated products are subjected to high-kinetic fine comminution using tribomaterials and repeated impact or shear forces. Tribomaterials include all types of glass, from Duran / Solidex to window glass. Additionally, sand grains, granite particles, quartz porphyry particles, enamel (as shard particles), sodalite, or ceramics (possibly in mixtures) can be used. In these cases, the particles are up to 5 mm in size.However, oxides such as silicon dioxide, calcium oxide, magnesium oxide, titanium dioxide, iron oxides, zirconium oxide, or boron oxide, sulfides such as pyrite, iron sulfide, and antimony sulfide, nitrides such as boron nitride and silicon nitride, carbides such as boron carbide, silicon carbide, and tungsten carbide, silicides such as iron silicide and titanium silicide, or silicon and boron, possibly in mixtures, can also be used. The particle sizes range from 10 µm to 1 mm. In Example 3 of the patent application, 10 g of activated carbon, to which 0.17 g of TCDD (2,3,7,8-tetrachlorodibenzo[1,4]dioxin) and 0.23 g of congeners had absorbed, were ground with 200 g of Duran glass shards and 2 kg of steel balls (CR 6). After grinding, no toxins or volatile organic compounds could be detected.

[0019] Mechanochemical processes are also used in the sequestration of carbon dioxide, as exemplified by the following scientific publications: - Alexander M. Kalinkin et al., Mechanochemical interaction of Ca silicate and aluminosilicate minerals with carbon dioxide, Journal of Materials Science 39(16):5393-5398, DOI: 10.1023 / B: JMSC.0000039252.13062.63; - Sinkranth Mateti et al. , A mechanochemical process to capture and separate carbon dioxide from natural gas using boron nitride nanosheets, Materials Horizons, Issue 12, 2024', https: / / pubs.rsc.org / en / content / articlelanding / 2024 / mh / d4mh00188e; - Mark Stillings et al., Mechanochemical processing of silicate rocks to trap CO2, Nature Sustainability 6, 780-788 (2023), https: / / pubs.rsc.org / en / content / articlelanding / 2024 / mh / d4mh00188e; - Kai Wang et al., Mechanochemical synthesis of carbon from CO2: Mechanism for milling process-dependent morphology of carbon, Journal of Alloys and Compounds Volume 830, 25 July 2020, 154681, https: / / doi.org / 10. 1016 / j.jallcom.2020. 154681; - Michat K. Leszczyński et al., Mechanochemical vs Wet Approach for Directing CO Capture toward Various Carbonate and Bicarbonate Networks, ACS Sustainable Chem. Eng. 2022, 10, 14, 4374-4380, https: / / doi.org / 10.1021 / acssuschemeng.1c08402; - Prof. Dr. Christoph Müller, ETH Zürich, Laboratory of Energy Science and Engineering, Carbon Dioxide Capture and Chemical Looping, https: / / lese.mavt.ethz.ch / thegroup / person-detail.html?persid=169413; - Alexey Kurlov, Dr. Marcin Broda, Davood Hosseini, Dr. Sharon J. Mitchell, Prof.Dr. Javier Pérez-Ramírez, Prof.Dr. Christoph R. Müller, Mechanochemically Activated, Calcium Oxide-Based, Magnesium Oxide-Stabilized Carbon Dioxide Sorbents, ChemSusChem Volume 9, Issue 17, p. 2380-2390, https: / / doi.org / 10.1002 / - cssc.201600510; - Gábor Kozma et al., Mechanochemically induced solid-state CO2capture during the synthesis of SnO2 nanoparticles, Journal of Physics and Chemistry of Solids, Volume 167, August 2022, 110775 https: / / doi.org / 10.1016 / j.jpcs.2022.110775; - A. M. Kalinkin, Mechanosorption of carbon dioxide by Ca- and Mg-containing silicates and alumosilicates: Kinetic regularities and correlations with the dissolution of CO2 in silicate melts, Colloid Journal, Volume 71, pages 193-201, (2009); - Elena V Kalinkina et al., Sorption of atmospheric carbon dioxide and structural changes of Ca and Mg silicate minerals during grinding: I. Diopside, International Journal of Mineral Processing, Volume 61, Issue 4, April 2001, Pages 273-288, https: / / doi.org / 10.1016 / S0301-7516(00)00035-1; oder - Elena V Kalinkina et al., Sorption of atmospheric carbon dioxide and structural changes of Ca and Mg silicate minerals during grinding: II. Enstatite, äkermanite and wollastonite, International Journal of Mineral Processing, Volume 61, Issue 4, April 2001, Pages 289-299 https: / / doi.org / 10.1016 / S0301-7516(00)00038-7.

[0020] During grinding, very strong forces act on the material being ground and the grinding media. Temperatures can reach several hundred degrees Celsius in some places and 15,000 degrees Celsius in so-called hotspots.

[0021] This can lead to overheating of the mills, which is particularly problematic for industrial ball mills. If the temperature inside the ball mill exceeds 100°C, the air film insulating the surface of small particles is destroyed, leading to adhesion and reducing the grinding efficiency. To lower the temperature back below 50°C, a water mist is sprayed. However, if the material being ground becomes too moist, the ball mill can no longer operate [cf. FTM Fote Machinery 2023, https: / / www.ftmmachinery.com / blog / 17-signs-of-problems-with-ball-mills-quickly-remove-hidden-troubles.html]. Furthermore, this measure is unsuitable for moisture-sensitive materials.

[0022] To protect laboratory mills from overheating, it is recommended to grind the material only as finely as necessary, to take breaks during grinding, to reduce the grinding frequency, or to pre-cool manually [see Temperature control for ball mills - Cooling hot mills, including 5 tips against overheated ball mills, https: / / www.laborpraxis.vogel.de / heisse-muehlen-kuehlen-incl-5-tipps-gegen-ueberhitzte-kugelmuehlen-a-7b1a90e9febbbc4ba60b36939c4f9a36 / ]. However, these measures are disadvantageous for scaling up mills and continuous process control.

[0023] Cold or cryogenic milling with cryogenic cooling is used when thermally sensitive and / or highly reactive or even explosive materials, or soft, quickly softening or lubricating materials such as food, spices, pharmaceuticals, biological materials, base metals such as magnesium or aluminum, explosives such as TNT, waxes or plastics are to be milled.

[0024] Cold milling plays a vital role in various industries, including the food, chemical, pharmaceutical, and plastics sectors, as well as in materials research and development. This process enables the production of fine powders or particles required for diverse applications. Cold milling allows manufacturers to improve product quality and develop more efficient production methods. It also facilitates the processing of temperature-sensitive materials, as the process takes place at low temperatures.

[0025] Cold milling is used, for example, in the food industry to grind spices and herbs into fine powders. This allows the aromas to be released more effectively and results in a more even distribution of flavor in the products. In the chemical industry, cold milling is used to transform chemical substances into fine powders. This leads to improved solubility and reactivity of the substances.

[0026] In the pharmaceutical industry, cold milling is used to break down active ingredients into fine particles. This milling process allows the body to better absorb the active ingredients and improves the effectiveness of the medications.

[0027] In the plastics industry, cryogenic grinding is used to grind plastics into fine powder. This enables the reuse of plastic waste and the production of recycled plastic products.

[0028] In materials research and development, cryogenic grinding is also used to produce new materials with specific properties. By grinding and milling materials at low temperatures, new material combinations and structures can be created.

[0029] Typically, for cryogenic cooling, i.e., cooling to temperatures below -150°C, liquid nitrogen (sp. -195°C), methane (sp. -164°C), argon (sp. -185°C), or krypton (sp. -152°C), or dry ice is used as an internal coolant. The material being ground and the grinding media are brought into direct contact with the coolant. [See also:] - Cold grinding - comminution at low temperatures, https: / / www.refolution.de / de / anwendungen / materialbearbeitung / kaltmahlen; - Hemantkumar Junghare, Mayur Hamjade, CKPatil, SBGirase and Mandar M.Lele, A review on Cryogenic Grinding, International Journal of Current Engineering and Technology E-ISSN 2277 - 4106, P-ISSN 2347 - 516, http: / / inpressco.com / category / ijcet; - DE 10 2010 012 448 A1, Method and apparatus for cold grinding; - EP0 219 582 A1, Dispersion strengthened composite metal powders and a method of producing them; - EP 0 963 825 B1, Mechanochemical process for treating plastics; or - EP 2 366 638 B1, Method and apparatus for cold grinding].

[0030] A disadvantage is that chemical reactions are frozen at these low temperatures. Furthermore, refrigerant and energy consumption is high. In addition, the equipment and safety measures required are extensive. It is also possible to simply adjust the boiling points of the refrigerants.

[0031] Attempts have been made to solve these problems by pre-cooling a polymer milling material with liquid nitrogen [see also: - WO 2021 / 137086 A1, Thermoplastic powders and methods for producing the seed from foam pellets; or - US 9 518 178 B2, Milling process.]

[0032] However, this has the disadvantage that the temperature in the mill is not constant and also cannot be precisely adjusted.

[0033] Attempts have also been made to overcome the disadvantages by using a cooling jacket that surrounds the grinding chamber and through which a cooling fluid flows [see also: - EP 3 081 303 B1, stirred ball mill; or - JC Paredes Rojas, Research Article, Design, Construction, and Operation of a High-Energy Mill for Handling Magnesium Powder, Hindawi, Mathematical Problems in Engineering Volume 2019, Article ID 6278365, https: / / doi.org / 10. 1155 / 2019 / 6278365].

[0034] A disadvantage is that such cooling systems are prone to malfunctions and failures. For example, leaks can occur in the coolant lines, causing the entire cooling system to fail.

[0035] If the material being ground and the grinding media need to be heated for grinding or mechanochemical synthesis at higher temperatures, the mill can be heated in the grinding chamber area, for example, with a heating band. However, precautions must be taken to prevent overheating. If heat is generated within the material being ground itself through chemical reactions, it is difficult to dissipate this additional heat to maintain a constant temperature.

[0036] US Patent 11,919,007 B2 proposes an attritor ball mill with inductive heating of the grinding chamber. The inductors are located in the casing, and the susceptors in the agitator or attritor. However, the inductor coils must be cooled by a cooling jacket through which a cooling fluid flows. Furthermore, the grinding chamber wall must be made of an electrically and magnetically non-conductive material. The mill's design is therefore complex and prone to malfunctions.

[0037] Thermal management systems based on heat pipes and flat heat pipes (vapor chambers) are known.

[0038] A heat pipe consists of three components: a thin-walled tube, an insert called a wick, and a vapor chamber. This chamber is filled with a working fluid or heat transfer medium – liquid or gaseous, depending on the operating temperature range. When the heat pipe heats up at one end, the liquid part of the working fluid or heat transfer medium evaporates. This creates a pressure gradient that transports the vapor to the other – cooler – end of the heat pipe. There, it condenses and releases heat from the inside to the wall. From there, the heat is transferred to a heat sink or into the surrounding environment. The working fluid or heat transfer medium is now liquid again and flows back to the warm end of the heat pipe by gravity and capillary action. There, the cycle begins anew.

[0039] Because both the vaporous and liquid phases of the working fluid or heat transfer medium are contained within the heat pipe, and thus within a closed volume, a wet steam environment is created. The temperature differences along the heat pipe are therefore very small (virtually isothermal), resulting in low thermal resistance (ΔT). A heat pipe can thus transport heat over long distances with very little loss. The pipe itself is usually made of a highly thermally conductive material, such as high-purity copper. However, the key factors determining its functionality are the coil and the working fluid or heat transfer medium, the selection of which depends on the temperature range in which the heat pipe is to be used. The pipe material can also be adapted to this temperature range.

[0040] A vapor chamber operates on the same principle as a heat pipe, but in a flat form. It is therefore not a tubular component, but a flat one that also dissipates heat through evaporation. For this reason, it is often referred to as a flat heat pipe. Vapor chambers can also be constructed from two tightly bonded metal half-shells, such as copper, containing sintered and socketed structures. Because vapor chambers have a very large contact area, they are often called heat spreaders. Vapor chambers are used, for example, in laptops to evenly distribute the heat generated by a small chip as a thermal hot spot across a large heat sink.

[0041] Heat pipes and vapor chambers are used in the automotive industry, for example in LED headlights or powertrains, in batteries for electric vehicles (infotainment, e-mobility in general), in industrial technology, for example in industrial notebooks, in high-performance computers and processors, servers and graphics cards, in gaming, IoT products (Internet of Things), camera systems, and high-performance LEDs, in power supply systems, for example in voltage converters, in consumer electronics, in defense and armaments, in aerospace, especially in satellites, in nuclear reactors and for permafrost stabilization.

[0042] Another special application is so-called embedded heat pipes in metalworking machines and drilling machines for cooling cutting tools and drills [see also: - TC Jen et al., Investigation of heat pipe cooling in drilling applications, Part I: preliminary numerical analysis and verification, International Journal of Machine Tools & Manufacture 42 (2002) 643-652; - Shailesh Kumar Sharma et al., Embedded Heat Pipe-Assisted Cooling in Machining Process: A Comprehensive Review, Proceedings of International Conference on Thermofluids, Lecture Notes in Mechanical Engineering, https: / / doi.org / 10.1007 / 978-981-15-7831-1_62; or - US 2011 / 0308709 A1, Mandrel with integrated heat pipe;

[0043] The development of ceramic heat pipes has also opened up new areas of application in the high-temperature range [see also: - WO 2020 / 039358, Ceramic heat pipe with porous ceramic wick; or - J. Pause, M. Beckmann, Institute for Energy Technology, TU Dresden NEW APPLICATION AREAS FOR HEAT PIPES, International ECEMP Colloquium, 2010].

[0044] On the other hand, high temperatures can be set and maintained with a deviation of only 0.1°C using heat pipe technology in Isotherm furnace linings [see also: - Datasheet, Isothermal Furnace Liner, Boyd Corporation; or - Datasheet, Isothermal Furnace Liner, ACT, Advanced Cooling Technologies]. The application of heat pipe technology for a heat management system for mechanochemical mills is not known. Objective of the present invention

[0045] The present invention was based on the objective of proposing a single- or multi-stage mechanochemical reactor, selected from the group consisting of ball mills, attritor ball mills, vibrating ball mills, resonant acoustic mixers, hammer mills, impact mills, pin mills, cutting mills, jet mills and twin-shaft extruders, which no longer exhibits the disadvantages of the prior art, but is equipped with a cooling or heating system so that it can be scaled up from laboratory scale to industrial scale without losing temperature control.

[0046] The cooling or heating system should allow the temperature in the mechanochemical reactor to be kept constant within a temperature range of -195°C to 1000°C. The cooling or heating system should be self-regulating and react quickly to undesirable temperature spikes or drops. This should prevent, on the one hand, desired chemical reactions in the milled material from becoming frozen, and on the other hand, prevent the milled material from overheating or the chemical reactions from getting out of control. The solution according to the invention

[0047] Accordingly, the single- or multi-stage mechanochemical reactor with a self-regulating thermal management system according to independent claim 1 was found, which is hereinafter referred to as the reactor according to the invention. Advantageous embodiments of the reactor according to the invention are the subject of dependent patents 2 to 19.

[0048] Furthermore, the mechanochemical process according to dependent claim 20 was discovered, which is hereinafter referred to as the process according to the invention. An advantageous embodiment of the process according to the invention is the subject of dependent claim 21.

[0049] Furthermore, the use of the reactor and the process according to the invention has been found in the fields of chemistry, biochemistry, nanotechnology, pharmaceuticals, biology and microbiology, and environmental engineering according to dependent claim 22, which is hereinafter referred to as the use according to the invention. Advantageous embodiments of the use according to the invention are the subject of dependent claims 23 and 24. Advantages of the invention

[0050] In view of the prior art, it was surprising and unforeseeable for the person skilled in the art that the problem underlying the present invention would be solved by means of the reactor, the method and the use according to the invention.

[0051] The reactor according to the invention can be implemented in numerous embodiments. It can advantageously be selected from the group consisting of ball mills, attritor ball mills, vibrating ball mills, resonant acoustic mixers, hammer mills, impact mills, pin mills, cutting mills, jet mills, and twin-shaft extruders. It no longer exhibits the disadvantages of the prior art; rather, its self-regulating thermal management system based on heat pipes, which is to be used according to the invention, allows it to be scaled up from laboratory to industrial scale without compromising temperature control.

[0052] The self-regulating thermal management system based on heat pipes, as used according to the invention, allows the temperature in the reactor according to the invention to be kept constant within a temperature range of -195°C to 1000°C. It reacts quickly to undesired temperature spikes or drops. This prevents, on the one hand, desired chemical reactions in the milled material from becoming frozen in the reactor according to the invention, and on the other hand, prevents the milled material from overheating or the chemical reactions from getting out of control or proceeding faster and more intensely than expected. In industrial processes, it can be dangerous if the heat generated can no longer be controlled.

[0053] The method according to the invention can be carried out in an exceptionally wide temperature range, since suitable heat tubes and flat heat pipes are available for an operating temperature range of -195°C to 1000°C. This makes the method according to the invention very versatile and extremely broadly applicable.

[0054] According to the use according to the invention, the reactor and the process according to the invention can be used for grinding sensitive materials, for the production of suspensions or slurries, and for carrying out chemical reactions and syntheses in the fields of chemistry, biochemistry, nanotechnology, pharmaceuticals, biology and microbiology, and environmental technology, in particular for the elimination of perpetual chemicals, the recycling of plastics, and the sequestration of carbon dioxide by mineralization.

[0055] Further significant advantages of the self-regulating thermal management system to be used according to the invention are its maintenance-free operation, low susceptibility to malfunctions, and high operational reliability.

[0056] The reactor according to the invention also allows the production of particularly finely divided suspensions under controlled thermal conditions.

[0057] Further advantages will become apparent from the following description. Detailed description of the invention

[0058] The reactor according to the invention is a single- or multi-stage mechanochemical reactor. "Single-stage" means that the reactor according to the invention has only one grinding chamber. "Multi-stage" means that the reactor according to the invention has at least two grinding chambers arranged one after the other, viewed in the direction of flow of the material being ground from coarse to fine, or that at least two reactors according to the invention are connected one after the other, viewed in the direction of flow of the material being ground from coarse to fine.

[0059] The reactor according to the invention is selected from the group consisting of ball mills, attritor ball mills, vibrating ball mills, resonant acoustic mixers, hammer mills, impact mills, pin mills, cutting mills, jet mills and twin-shaft extruders. These form the basis of the reactor according to the invention.

[0060] Preferably, ball mills, attritor ball mills, resonant acoustic mixers or pin mills are used.

[0061] The designs and functions of these mechanochemical mills are generally known. They are used, for example, by the companies... - Netzsch, https: / / www.netzsch.com / de / , - Retsch GmbH, RETSCH - laboratory mills, jaw crushers, sieving machines, - Hosokawa Alpine, https: / / www.hosokawa-alpine.de / mechanischeerfahrenstechnik / technologien / mahlen / , - UNION PROCESS, chrome-extension: / / efaidnbmnnnibpcaijpcaleclefindmkaj / https: / / unionprocess.com / wpcontent / uploads / 2020 / 12 / up-dry-grinding-attritors.pdf, - Bühler, https: / / www.buhlergroup.com / global / de / product-families / bead-mills.html, or - Resodyn, https: / / resodynmixers.com / manufactured and distributed.

[0062] The selection of materials for components such as walls, drive shafts, inlets and outlets for materials to be ground, and agitation elements such as attritors, pins, hammers, cutting tools, etc., as well as for the grinding media or grinding balls of the reactor according to the invention, depends firstly on the temperature range in which the reactor according to the invention is to be operated, and secondly on the hardness and thermal conductivity of the materials and their corrosion resistance to the material being ground. According to the invention, this selection requires great care.

[0063] If the reactor according to the invention is to be operated at temperatures above 300°C, the components, preferably the static components, are preferably made of metals or metal alloys with a melting point T > 1000°C and a mean coefficient of thermal expansion α < 20·10 -61 / K at temperatures from 25°C to 900°C and a thermal conductivity λ >10 W / mK at 300°C. Examples of suitable metals and metal alloys are titanium, chromium, iron, manganese, tantalum, nickel, cobalt, and copper and their alloys, such as stainless steel or copper-aluminum alloys, or the alloys marketed under the trademarks Monel® (nickel-copper alloys), Inconel® (nickel-chromium alloys), Haynes® (cobalt-nickel-chromium-tungsten alloys), Invar® (iron-nickel alloys), and Hastelloy® (nickel-molybdenum alloys). If the reactor according to the invention is also to be operated at temperatures below 300°C, copper and aluminum are particularly suitable.

[0064] The static components, especially those that come into contact with the ground material, can be coated with thermally conductive ceramics with a thermal conductivity λ >10 W / mK, preferably >60 W / mK, and particularly >100 W / mK. Examples of suitable thermally conductive ceramics are silicon carbide, aluminum nitride, and boron nitride ceramics.

[0065] Preferably, however, the naturally non-static agitation devices such as attritors, agitators, pin plates, hammers, cutting tools and extruder screws are made of metals and / or metal alloys with a thermal conductivity λ <10 W / mK in order to minimize heat exchange with the environment.

[0066] To protect against corrosion and abrasion and to minimize heat exchange, the agitating agents can be coated with hard ceramics with low thermal conductivity λ <5 W / mK, in particular <3 W / mK, such as glass ceramics (Macor®) or zirconia.

[0067] The grinding media or grinding balls consist of a high- and low-temperature resistant, impact-resistant, and abrasion-resistant material with high hardness and a very high melting point. Materials with high thermal conductivity (λ) are preferred.

[0068] Suitable materials for the grinding media or grinding balls are the aforementioned metals or metal alloys.

[0069] Other suitable materials for grinding media or grinding balls are aluminium oxide, steatite, porcelain, zirconium oxide, glass, flint, steels, chromium steels, tungsten carbide, silicon carbide, silicon nitride, cubic boron nitride or boron carbide, as well as highly thermally conductive boron nitride, silicon carbide and aluminium nitride ceramics.

[0070] The grinding media can have any desired diameter, depending in particular on the size and design of the mill, the type of acceleration (e.g., by rotation of the mill wall, by rotating or vibrating the container surrounding the grinding chamber, by centrifugal forces, by compressed air, by impacts, or by electrostatic and / or magnetic attraction), and on the materials to be ground. The diameters can therefore be advantageously adapted to the specific task. Preferably, the diameters range from 0.5 cm to 10 cm.

[0071] The grinding media can be spheres or ellipsoids, or have irregular shapes, resulting in various contact possibilities per collision. Furthermore, the grinding media can have smooth or roughened surfaces, or cup-shaped depressions like a golf ball, in which material can accumulate. The surface of the grinding media can have a layer of the material being ground or be doped with it.

[0072] Grinding balls are preferably used as grinding media.

[0073] Since the reactor according to the invention is intended not only for grinding solid material into powders, but also for chemical reactions and syntheses such as the reactions and syntheses listed above, in a preferred embodiment the surfaces of the grinding media, the reactor inner walls or the walls of the grinding chambers, the drive shafts and / or the agitation means are doped and / or coated with piezoelectric materials.

[0074] The piezoelectric materials selected are preferably those from the group consisting of carbon, quartz, glass, barium titanate (BTO), lead zirconium titanate (PZT), lead magnesium niobate (PMN), gallium orthophosphate, berlinite, tourmalines, Rochelle salt, piezoelectric thin films made of zinc oxide, aluminum nitride, silicon nitride, silicon carbide, aluminum oxide, zirconium oxide and titanium nitride, polyvinylidene fluoride (PVDF), and ferroelectric polycrystalline ceramics. Carbon, quartz, and glass are used in particular.

[0075] In a further preferred embodiment, the surfaces of the grinding media, the reactor inner walls or the walls of the grinding chambers, the drive shafts and / or the agitation means are provided with catalytically effective coatings and / or dopings.

[0076] Preferably, the catalytically active coatings and dopings from the group consisting of metals, metal alloys, metal compounds and microporous and nanoporous materials are used.

[0077] Metals can Actinium, symbol: Ac, atomic number: 89 Aluminium, symbol: Al, atomic number: 13 Americium, symbol: Am, atomic number: 95 Antimony, symbol: Sb, atomic number: 51 Arsenic, symbol: As, atomic number: 33 Astatine, symbol: At, atomic number: 85 Barium, symbol: Ba, atomic number: 56 Berkelium, symbol: Bk, atomic number: 97 Beryllium, symbol: Be, atomic number: 4 Bismuth, symbol: Bi, atomic number: 83 Lead, symbol: Pb, atomic number: 82 Bohrium, symbol: Bh, atomic number: 107 Boron, symbol: B, atomic number: 5 Cadmium, symbol: Cd, atomic number: 48 Cesium, symbol: Cs, atomic number: 55 Calcium, symbol: Ca, atomic number: 20 Californium, symbol: Cf, atomic number: 98 Cerium, symbol: Ce, atomic number: 58 Chromium, symbol: Cr, atomic number: 24 Cobalt, symbol: Co, atomic number: 27 Copernicium, symbol: Cn, atomic number: 112 Curium, symbol: Cm, atomic number: 96 Darmstadtium, symbol: Ds, atomic number: 110 Dubnium, symbol: Db, atomic number: 105 Dysprosium, symbol: Dy, atomic number: 66 Einsteinium, symbol: Es, atomic number: 99 Iron, symbol: Fe, atomic number: 26 Erbium, symbol: Er, atomic number: 68 Europium, symbol: Eu, atomic number: 63 Fermium, symbol: Fm, atomic number: 100 Flerovium, symbol: Fl, atomic number: 114 Francium, symbol: Fr, atomic number: 87 Gadolinium, symbol: Gd, atomic number: 64 Gallium, symbol: Ga, atomic number: 31 Germanium, symbol: Ge, atomic number: 32 Gold, symbol: Au, atomic number: 79 Hafnium, symbol: Hf, atomic number: 72 Hassium, symbol: Hs, atomic number: 108 Holmium, symbol: Ho, atomic number: 67 Indium, symbol: In, atomic number: 49 LOD, Symbol: I, Atomic number: 53 Iridium, symbol: Ir, atomic number: 77 Potassium, symbol: K, atomic number: 19 Carbon, symbol: C, atomic number: 6 Copper, symbol: Cu, atomic number: 29 Lanthanum, symbol: La, atomic number: 57 Lawrencium, symbol: Lr, atomic number: 103 Lithium, symbol: Li, atomic number: 3 Livermorium, symbol: Lv, atomic number: 116 Lutetium, symbol: Lu, atomic number: 71 Magnesium, symbol: Mg, atomic number: 12 Manganese, symbol: Mn, atomic number: 25 Meitnerium, symbol: Mt, atomic number: 109 Mendelevium, symbol: Md, atomic number: 101 Molybdenum, symbol: Mo, atomic number: 42 Moscovium, symbol: Mc, atomic number: 115 Sodium, symbol: Na, atomic number: 11 Neodymium, symbol: Nd, atomic number: 60 Neptunium, symbol: Np, atomic number: 93 Nickel, symbol: Ni, atomic number: 28 Nihonium, symbol: Nh, atomic number: 113 Niobium, symbol: Nb, atomic number: 41 Nobelium, symbol: No, atomic number: 102 Oganesson, symbol: Og, atomic number: 118 Osmium, symbol: Os, atomic number: 76 Palladium, symbol: Pd, atomic number: 46 Phosphorus, symbol: P, atomic number: 15 Platinum, symbol: Pt, atomic number: 78 Plutonium, symbol: Pu, atomic number: 94 Polonium, symbol: Po, atomic number: 84 Praseodymium, symbol: Pr, atomic number: 59 Promethium, symbol: Pm, atomic number: 61 Protactinium, symbol: Pa, atomic number: 91 Mercury, symbol: Hg, atomic number: 80 Radium, symbol: Ra, atomic number: 88 Rhenium, symbol: Re, atomic number: 75 Rhodium, symbol: Rh, atomic number: 45 Roentgenium, symbol: Rg, atomic number: 111 Rubidium, symbol: Rb, atomic number: 37 Ruthenium, symbol: Ru, atomic number: 44 Rutherfordium, symbol: Rf, atomic number: 104 Samarium, symbol: Sm, atomic number: 62 Scandium, symbol: Sc, atomic number: 21 Seaborgium, symbol: Sg, atomic number: 106 Selenium, symbol: Se, atomic number: 34 Silver, symbol: Ag, atomic number: 47 Silicon, symbol: Si, atomic number: 14 Strontium, symbol: Sr, atomic number: 38, Tantalum, symbol: Ta, atomic number: 73 Technetium, symbol: Tc, atomic number: 43 Tellurium, symbol: Te, atomic number: 52 Tennessee, symbol: Ts, atomic number: 117 Terbium, symbol: Tb, atomic number: 65 Thallium, symbol: TI, atomic number: 81 Thorium, symbol: Th, atomic number: 90 Thulium, symbol: Tm, atomic number: 69 Titanium, symbol: Ti, atomic number: 22 Uranium, symbol: U, atomic number: 92 Vanadium, symbol: V, atomic number: 23 Hydrogen, symbol: H, atomic number: 1 Wolfram, symbol: W, atomic number: 74 Ytterbium, symbol: Yb, atomic number: 70 Yttrium, symbol: Y, atomic number: 39 Zinc, symbol: Zn, atomic number: 30 Tin, symbol: Sn, atomic number: 50 Zirconium, symbol: Zr, atomic number: 40, may be used. When using reactive metals such as alkali and alkaline earth metals and radioactive metals, the appropriate standard and known precautions must be taken. The following metal alloys can be used: Aluminum alloys: - Alloys with copper, magnesium, silicon or manganese as the main alloying element - Duralumin is a wrought alloy made of aluminum, copper, magnesium, manganese and silicon. - Partinium - Aluminum-manganese alloy - Aluminum-magnesium alloy - Hydronalium: Trade name for an aluminum casting alloy containing 3-12% magnesium - Aluminum-silicon alloy, primarily as a casting alloy - Silumin: Brand name for a range of hypoeutectic to eutectic aluminium-silicon casting alloys. - Aluminum-lithium alloy (These are particularly lightweight.) - Aluminum-zinc-magnesium alloy - Titanal Lead alloys: - Hard lead consists of lead and antimony - Shot refers to an alloy of lead, arsenic and antimony. Solder is a lead-tin alloy. More recently, tin alloys containing copper or silver have also been used. Sodium-lead alloys are used as drying agents and in the production of tetraethyl lead. Bismuth alloys: Rose's metal consists of bismuth, lead, and tin. Wood's metal consists of bismuth, lead, tin, and cadmium - Lipowitz metal, Orion metal - Rapid soldering, - Darcot metal - Cobalt alloys Stellites are hard alloys consisting of 20-68% cobalt. Other significant components in varying amounts include chromium, tungsten, nickel, molybdenum, and occasionally up to 2.5% carbon. - Vitallium is a metal alloy made of cobalt, chromium and molybdenum (see chromium-cobalt-molybdenum alloy) Iron alloys: - Steel is a collective term for plastically deformable iron-carbon alloys with a maximum of 2.06 percent carbon. - Cast iron is a collective term for non-plastically deformable iron-carbon alloys and at least 2.06% C (usually around 4% carbon). - Iron-nickel alloy - Invar consists (mainly) of iron and nickel. Kovar consists (mainly) of iron, nickel and cobalt. - Ferroalloy Aluminum alloy: - Devarda's alloy Gallium alloy: Galinstan is a eutectic alloy of gallium, indium and tin. Gold alloys: - Titanium gold: Alloy: 99% gold, 1% titanium, primarily used in the production of wedding rings and in medical technology. Its color is comparable to 18k yellow gold, but slightly grayer. - Coloured gold (generally) is an alloy of gold, silver (to lighten the yellow and to improve mechanical workability) and copper (for the “noble” intense gold colour or for the red tint). - Yellow gold: the proportion of silver corresponds to that of copper. - Rose gold: the proportion of silver is significantly lower than that of copper (also known regionally as Turkish gold). - Russian gold: a slightly lighter red gold with the unusual gold content of 583. - Pale gold: the proportion of silver is significantly higher than that of copper. - Green gold is gold with predominantly or exclusively silver. Small amounts of cadmium are often added to intensify the green color, but this has been banned throughout the EU since 2011. White gold and gray gold are alloys of gold with platinum, palladium, or silver. However, there are also white gold alloys containing cobalt, chromium, manganese-germanium, and other metals. Nickel was also used in the past. Electrum is an alloy of gold and silver known since antiquity. The name is also used for amber. Since 1920, Elektron has been the protected name for a magnesium alloy produced by the former IG Farbenindustrie, Griesheim plant. - Normmetall or Norm-Metall (in Switzerland also: Garantiemetall) is a gold-containing alloy with less than 333 ‰ gold content. - Hard gold: Gold produced using electroplating techniques with small amounts (a few atomic %) of cobalt, nickel or iron. Copper alloys: - Bronzes or brasses, with tin determining the bronzes and zinc the brasses. - Bronze (true bronze) is an alloy consisting only of copper and tin. - Aluminium bronze is an alloy that can consist of copper and aluminium as well as proportions of nickel and iron. Brass is an alloy of copper and zinc, commonly used as a rolled and wrought material with an addition of lead, and sometimes aluminum. - Tombac refers to copper-rich brass. - Lead bronze is an alloy of copper, tin and lead. Isabellin is an alloy of copper, nickel and manganese, primarily used for thermally resistant wires (heating conductor alloy) - Constantan is a comparable alloy of copper, nickel and manganese. - Nickelin is a comparable alloy of copper, nickel and manganese. - Nickel silver (Alpaca, Pakfong) is an alloy of copper, nickel and zinc. - Red brass is an alloy of copper, tin, zinc and lead used, among other things, for fittings. Beryllium copper, made from copper and beryllium, was particularly used for spark-free tools in mining. - White copper is a light-colored copper-arsenic alloy. Magnesium alloys: - Elektron is a name for a magnesium alloy that was protected in the 1920s. Nickel-based alloys: - Plessite consists of intergrown kamacite (beam iron) and taenite (band iron) and occurs in nickel-iron meteorites. - Chronin refers to alloys of nickel and chromium. Monel is an alloy of nickel, copper, iron and manganese. - Inconel and Incoloy are heat-resistant alloys made of nickel, chromium and up to 5% iron, with temperatures up to 800 °C. Supermalloy is an alloy of nickel, iron and molybdenum. Mercury alloys: - Silver amalgam - Gold amalgam, a compound of mercury and gold, is not a purpose-built alloy, but merely an environmentally harmful intermediate stage in gold extraction. Silver alloys: - Sterling silver: An alloy of 925 / 1000 silver, which is alloyed with copper or other materials. This alloy is mostly used for the production of coins, jewelry, and cutlery. - Vermeil: Silver that has been fire-gilded. - Niello (Tula silver): (used primarily in the Middle Ages for works of art and tableware) is made with silver, copper, lead, sulfur, and ammonium chloride. - Tibetan silver: Alloy with a very low silver content of 250 / 1000. Tungsten alloys or composite materials: - Tungsten is one of the refractory metals, which, due to their high melting point (SM Tungsten = 3422 °C), are difficult to alloy with other metals and are therefore mostly sintered into composite materials such as hard metals for machining materials. - Widia, the protected name for a hard metal consisting of tungsten, cobalt, carbon and titanium. - A tungsten-silver composite material is also misleadingly referred to as a sweat cooling alloy. - True alloys, on the other hand, include tungsten-molybdenum alloys, high-density tungsten alloys with alloying elements such as nickel, copper, iron, and molybdenum in varying compositions. - As an alloying element with a proportion of a few percent by weight, tungsten is usually a component of both high-quality steels (see also list of alloying elements) and wire alloys used for lighting purposes (e.g. the brand Osram® as a contraction of osmium and tungsten). Zinc alloy: - Zamak alloy - Fine zinc casting alloys are predominantly used for die-cast parts, including those produced using investment casting. - Titanium zinc is a zinc alloy with a very low copper and titanium content, which is preferred for galvanizing. - Alzen (ZnAl35), also Alzeen, are brand names of zinc-aluminum alloys. Tin alloys: Britannia metal is an alloy of 90-95% tin with up to 9% antimony and 1% copper. According to the "Foundry Lexicon" (formerly), it was used for household goods and decorative objects ("false bronzes"). - Pewter is an alloy of tin, copper and / or lead. Solder is a lead-tin alloy. More recently, tin alloys containing copper or silver have also been used. - "Potin gris" is a historical French bronze (copper alloy with tin content). Intermetallic compounds: - Zintl phases. - Laves phases. - Hume-Rothery phases. Magnetic and magnetizable alloys:

[0078] Alloys of iron with at least one metal selected from the group consisting of ruthenium, osmium, cobalt, rhodium, iridium, nickel, palladium, platinum, copper, silver, gold, zinc, cadmium, scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium oxide, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten, manganese, rhenium, aluminum, gallium, indium, thallium, germanium, tin, lead, antimony, and bismuth; examples of suitable metal alloys are soft magnetic metal alloys such as Permalloy® based on nickel and iron, nickel-iron-zinc alloys, or Sendust based on aluminum, silicon, and iron; RE 1-y Fe 100-v-w-x-z Co w M z B x, where RE represents a rare earth metal from the group Cerium, Praseodymium, Neodymium, Samarium, Europium, Gadolinium, Terbium oxide, Terbium oxide, Dysprosium, Holmium, Erbium, Thulium, Ytterbium and Lutetium and M represents a metal from the group Titanium, Zirconium, Hafnium, Vanadium, Niobium, Tantalum, Chromium, Molybdenum and Tungsten and v = 5-15, w ≥ 5, x = 9-30, y = 0.05-0.5 and z = 0.1-5; The aforementioned metals and metal alloys may contain at least one further metal and / or nonmetal selected from the group consisting of lithium, sodium, potassium, rubidium, cesium, beryllium, magnesium, calcium, strontium, barium, boron, carbon, silicon, nitrogen, phosphorus, arsenic, oxygen, sulfur, selenium, tellurium, fluorine, chlorine, bromine, and iodine, in non-stoichiometric amounts. NdFeB is a particularly suitable material of this type.

[0079] Examples of suitable catalytically active metal compounds are borides, oxides, sulfides, selenides, tellurides, carbides, silicides, germanides, nitrides, phosphides, arsenides, antimonides, fluorides, chlorides, bromides and iodides, coordination compounds with organic and / or inorganic ligands, isopoly acids and heteropoly acids (polyoxometalates; POM), as well as covalent organometallic compounds, sandwich compounds and carbenes.

[0080] In particular, hematite, non-stoichiometric hematites, ferrites, nickel ferrites, nickel salts and polyoxometalates (POM) are used.

[0081] Examples of suitable POMs are known from the international patent application WO 2016 / 116259 A1, page 14, line 32, to page 23, line 17, and in particular from Table 1, “Summative formulas of suitable POMs”.

[0082] Examples of suitable microporous materials include zeolites and metal-organic frameworks (MOFs). Zinc-modified zeolites are used in particular.

[0083] The grinding of the catalytically active coatings generates nanoparticles and microparticles, and / or the surfaces of the drive shafts, walls, grinding media, and / or agitators are repeatedly reactivated, thereby increasing the catalytic effects. Furthermore, the metals and metal alloys can be repeatedly regenerated through reduction using any carbon-containing materials that may be present. This can also lead to the formation of new active centers on the catalysts through torsion and lattice defects, and these centers can be supplied with electrons for redox reactions via piezoelectric properties.

[0084] The reactor according to the invention is equipped with a self-regulating thermal management system for a temperature range of -195°C to 1000°C, preferably from -150°C to 800°C, preferably from -80°C to 500°C, particularly preferably from -80°C to 300°C and especially from -80°C to 200°C.

[0085] The self-regulating thermal management system comprises at least one heat pipe and / or at least one flat heat pipe (vapor chamber or heat spreader) and at least one heat source and at least one heat sink, which are in thermally conductive contact with each other. The at least one heat pipe and / or the at least one flat heat pipe are arranged in thermally conductive contact with the material being ground and the grinding media in the at least one grinding chamber of the at least one reactor, and the at least one static component serves as either a heat source or a heat sink for the at least one heat pipe and / or the at least one flat heat pipe, depending on the configuration.

[0086] The heat pipes must be temperature-optimized. This means that the materials used to construct the heat pipes must be gas-tight within the temperature range defined by the thermal energy source, as well as chemically stable, mechanically and thermally stable, and resistant to deformation with respect to both the heat transfer medium and the cooling medium. Furthermore, the materials should preferably have high thermal conductivity, at least in the areas where thermal energy is absorbed or released, to ensure that the thermal energy from the source can be effectively absorbed and released in a heat sink. The other areas of the heat pipes do not necessarily need to be thermally conductive; they can be thermally insulating.

[0087] Examples of suitable materials for the heat pipes are thermally conductive ceramics such as silicon carbide, boron nitride and aluminum nitride ceramics and metals or metal alloys with a melting point T >1000°C, a mean coefficient of thermal expansion α <20·10 -6 1 / K at 25°C to 900°C and a thermal conductivity λ >10 W(m·K). Examples of suitable metals and metal alloys are titanium, chromium, iron, manganese, tantalum, nickel, cobalt and copper and their alloys, such as stainless steel or copper-aluminum alloys, or the alloys sold under the brands Monel® (nickel-copper alloys), Inconel® (nickel-chromium alloys), Haynes® (cobalt-nickel-chromium-tungsten alloys), Invar® (iron-nickel alloys) and Hastelloy® (nickel-molybdenum alloys).

[0088] It is advantageous if the coefficients of thermal expansion α of the heat pipe materials and the components to which they are thermally connected are not too different; ideally, they are the same.

[0089] The heat tubes and flat heat pipes can have a wide variety of dimensions, which depend in particular on their intended use and the dimensions of the cooling device according to the invention. Thus, the lengths can range from a few millimeters to several meters.

[0090] The heat pipes can have different cross-sections, such as squares, rectangles, and triangles (which may have rounded corners and / or sides), as well as ellipses, ovals, or circles. The size of the cross-sections can also vary widely and depends on the intended use of the heat pipes and the dimensions of the reactors according to the invention. Accordingly, the cross-sections of the heat pipes can have diameters ranging from a few millimeters to several centimeters.

[0091] Similarly, the wall thickness of the heat pipes can vary widely. It depends primarily on the required dimensional stability of the heat pipes and is preferably in the range of 0.5 mm to 5 mm.

[0092] Furthermore, heat pipes can have different shapes when viewed longitudinally. They can be straight, simply or multiple times curved in the plane, simply or multiple times curved in space, meandering or spiral [see also: COMANESCU, D.; COMANESCU, A.; FILIPOIU, ID & ALIONTE, CG, A NEW HEAT PIPE COOLING DEVICE, 2 DAAAM INTERNATIONAL SCIENTIFIC BOOK 2010, pp. 593-606 CHAPTER 52].

[0093] The heat pipes can be coated with a highly thermally conductive material, particularly in the areas of heat absorption and heat emission. This highly thermally conductive material must be thermally and chemically stable within the respective temperature range of the hot gases. Graphite, hexagonal or cubic boron nitride, aluminum nitride, copper, or silver are preferably used. Cubic boron nitride has an ultra-high thermal conductivity comparable to that of diamond.

[0094] The lining, wick, or capillary structure with wicking action on the inside of the heat pipe walls can also be made of a wide variety of materials. Essential for their selection are the temperature range specified by the thermal energy source and their stability against the working fluid or heat transfer medium. Furthermore, corrosion must not occur due to contact between the capillary structure and the walls under the influence of the heat transfer medium. A person skilled in the art can select the materials based on their known property profiles.

[0095] The insert, wick, or capillary structure can be composed of nanoparticles, fibrous materials, or nano- or microporous materials with appropriately sized pore dimensions. Furthermore, the wicking effect can be created by wire meshes, such as copper wire meshes or electrically non-conductive wire meshes, and fiber bundles made of ceramic, glass, or high-temperature-resistant plastics inside the heat pipes. Additionally, the wicking effect can also be generated by surface structures consisting of protrusions and depressions, such as grooves, columns, spheres, or cups, on the inner walls of the heat pipes.

[0096] The capillary structure with wicking effect can also be introduced subsequently. Examples of suitable methods include the crystallization or precipitation of mesoporous materials such as zeolites.

[0097] The above applies analogously to the selection of materials for the flat heat pipes or vapor chamber. Here, too, the dimensions can vary considerably and, in particular, can be ideally adapted to the dimensions of the reactor according to the invention.

[0098] The working fluids or heat transfer fluids are also adapted to the respective specified temperature range. Thus, in order of increasing boiling points, nitrogen, methane, propane and ammonia are preferably used in the low temperature range, methanol, water, aqueous salt solutions and water-toluene mixtures in the medium temperature range, and mercury, lithium, sodium, potassium, tin and lead-bismuth eutectic in the high temperature range.

[0099] According to the invention, at least one heat pipe and / or at least one flat heat pipe or vapor chamber is / are thermally connected to at least one static component of the reactor according to the invention. In particular, the at least one static component is a - a reactor wall enclosing the grinding chamber and having at least one bore for the preferably precisely fitting reception of at least one heat pipe and / or at least one recess for the preferably precisely fitting reception of at least one flat heat pipe or vapor chamber, - at least one thermally, mechanically and chemically stable, heat-conducting round rod arranged in the grinding chamber with at least one bore for preferably precisely fitting the reception of at least one heat pipe or - a static pin plate with at least one bore for preferably precisely fitting the mounting of at least one heat pipe.

[0100] The thermally conductive connection between the at least one heat pipe in the at least one bore, between the at least one flat heat pipe and the recess, and between the at least one flat heat pipe and at least one heat pipe can be made by non-destructive mechanical pressing, welding, soldering with metal solders, in particular copper solders, brass solders and hard solders for aluminum, bonding with thermally conductive adhesives containing highly thermally conductive particles of silver, copper, graphite, aluminum nitride or boron nitride, clamps, and, in the case of heat pipes, also by screwing.

[0101] Depending on the circumstances, the reactor according to the invention can serve as a heat source or as a heat sink.

[0102] If it serves as a heat source, the heat generated in the grinding chamber by grinding the material or by chemical reactions under mechanochemical conditions is transferred through the heat tubes and / or the flat heat pipes to at least one heat sink. The heat tubes and / or the flat heat pipes strive to homogenize or equalize the temperature of the heat source or heat sink. This means that the circulation of the working fluid or heat transfer medium stops as soon as the heat source reaches the temperature of the heat sink. When the heat source then heats up again, the circulation restarts.

[0103] Heat sinks are - Metal blocks made of aluminum or copper with cooling fins that release heat into the ambient air (temperature 20°C to 30°C), - Ice (0°C), - Dry ice (-78.4°C), - Bath cryostats, which store objects in a liquid-filled chamber, - Evaporator cryostats that generate precisely adjustable cooling temperatures, - Refrigerator cryostats or cryocoolers that operate using technical cooling processes and do not require cooling liquids, - the cold sides of Peltier elements; the heat is then dissipated via the hot side of the Peltier element; in particular, a cascade-type Peltier element with at least two stages is used. Cascade-type Peltier elements are known from German patent DE 4231702 C2, American patent US 5,936,192 A, or international patent application WO 96 / 15412 A2 and can be obtained, for example, from Uwe electronic GmbH, Unterhaching, Germany. - Cold baths according to Table 1, Table 1: Cold baths Refrigerant Organic solvent Temperature (°C) dry ice p-Xylene +13 [1] dry ice 1,4-Dioxane +12 dry ice Cyclohexane +6 Liquid nitrogen Ethylene glycol -10 dry ice Ethylene glycol -15 dry ice o-Xylene -29 dry ice 3-Heptanone -38 dry ice Acetonitril -41 dry ice Cyclohexanone -46 dry ice m-Xylene -47 dry ice Diethylene glycol diethyl ether -52 dry ice n-octane -56 dry ice Diisopropyl ether -60 dry ice chloroform -63 dry ice Ethanol -72 dry ice 2-Propanol -77 dry ice acetone -78 Liquid nitrogen Ethyl acetate -84 Liquid nitrogen 1-Butanol -89 Liquid nitrogen Hexane -94 Liquid nitrogen acetone -94 Liquid nitrogen toluene -95 Liquid nitrogen Methanol -98 Liquid nitrogen Cyclohexane -104 Liquid nitrogen carbon disulfide -110 Liquid nitrogen Ethanol -116 Liquid nitrogen 1-Propanol -127 Liquid nitrogen Pentane -131 Liquid nitrogen 1.5-hexadia -141 Liquid nitrogen Isopentane -160 Liquid nitrogen (per se) -196 - Freezing mixtures according to Table 2 Table 2: Freezing mixtures coolant Salt T(°C) note Ice (Water) 0 Ice Ammonium chloride -5 Salt / ice mixing ratio: 0.3:1 Ice Sodium thiosulfate pentahydrate -8 Salt / ice mixing ratio: 1.1:1 Ice Calcium chloride hexahydrate -10 Salt / ice mixing ratio: 1:2.5 Ice acetone -10 Ice Sodium chloride -20 Salt / ice mixing ratio: 1:3 Ice Calcium chloride hexahydrate -40 1:0,8

[0104] The reactor according to the invention can also be used as a heat sink. For this purpose, the heat tubes and / or the flat heat pipes are thermally connected to at least one heat source. Suitable heat sources include all controllable heat sources that can be thermally connected to the heat tubes and / or the flat heat pipes and that allow for a constant temperature setting.

[0105] Examples of suitable heat sources are - boiling water baths (100°C at normal pressure), - Hot air (hair dryer, blower), - electrically heated hot plates, - Thermostatic ovens, - Heat pumps, - Ovens with PID controllers: ID controllers (Proportional-Integral-Derivative) offer precise temperature control by constantly adjusting the heating power based on the current temperature, - Circulating thermostats and - the hot side of Peltier elements.

[0106] In this embodiment of the reactor according to the invention, the circulation of the working fluid or heat transfer medium also stops when a temperature equilibrium is reached between the heat source and the heat sink. This is also referred to in the literature as heat homogenization.

[0107] The reactor according to the invention further comprises a periphery for electronic, optical, optoelectronic, hydraulic, pneumatic and mechanical control and regulation as well as for measuring and displaying the physical and chemical parameters.It includes standard and well-known electronic data processing systems, electrically, electronically, optically, optoelectronically, mechanically, hydraulically, and pneumatically activated actuators, electric and pneumatic drive motors or gas motors with speed controllers for the agitators, pressure, temperature, and flow measuring devices, pressure relief valves, vacuum pumps, sensors for chemical compounds, sampling devices, devices for measuring the particle size of the ground materials and the raw and finished products, powder conveyors, powder sieves, powder dosing units, powder inlets and outlets, inlets and outlets for gases and liquids, storage containers for ground materials, raw materials, and finished products, extraction systems, scales, spectrometers, suitable mounting devices with and without vibration dampers, and safety devices such as protective shields and thermal insulation. This list is not exhaustive but exemplary.

[0108] The dual function of the reactor according to the invention, as described above, greatly expands the application possibilities of mechanochemistry.

[0109] Another significant advantage is that in the reactor according to the invention, the heat source and the heat sink can be spatially separated from each other and the heat transfer takes place using solid, mechanically, chemically and thermally stable as well as dimensionally stable heat conductors, which is an important safety aspect.

[0110] Last but not least, the design of the reactor according to the invention enables upscaling from laboratory scale to industrial scale.

[0111] The reactor according to the invention is ideally suited for carrying out the process according to the invention. This can be carried out continuously or discontinuously, whereby the solid material to be ground or the starting materials can be circulated through the grinding chamber.

[0112] In the first embodiment of the process according to the invention, coarse, particulate material is preferably introduced batchwise or continuously into the grinding chamber of the reactor according to the invention using conventional and known powder feeders and metering devices and ground therein under controlled thermal conditions, after which the finely ground material is discharged batchwise or continuously. Within the scope of the present invention, "coarse" means a mean particle size d 50 in the range ≥1000 µm and “finely detailed” a mean particle size d 50 This refers to the particle size range of 1 nm to <1000 µm. In batch or discontinuous operation, the material being ground is repeatedly circulated through the grinding chamber to produce particularly fine particles.

[0113] In the second embodiment of the process according to the invention, the starting materials for chemical syntheses, such as coarse or fine-particle starting materials, in particular fine-particle starting materials, and / or gaseous starting materials such as hydrogen, nitrogen, oxygen, halogens or carbon dioxide, and / or organic and / or inorganic liquids, are fed into the grinding chamber containing the grinding media and reacted therein mechanochemically under controlled thermal conditions. The reaction products are then discharged from the grinding chamber. This second embodiment is also carried out continuously or discontinuously, in particular discontinuously, or in a closed loop.

[0114] In the third embodiment of the process according to the invention, coarse or fine-particle starting materials and organic and / or inorganic liquids are fed into the grinding chamber, whereby a suspension or slurry, particularly of high concentration, is produced mechanochemically under controlled thermal conditions. The resulting suspension is then discharged from the grinding chamber. This third embodiment is also carried out continuously or discontinuously, particularly discontinuously, or in a closed loop [see also: ▪ EP 0 130 788 A1, Process for producing a coal-water slurry; or - EP 3 102 185 B1, Nanosuspension of natural materials and preparation method thereof].

[0115] As shown above, the reactor and the process according to the invention can be used to great effect for the grinding of sensitive materials, for the production of suspensions or slurries, and for carrying out chemical reactions and syntheses in the fields of chemistry, biochemistry, nanotechnology, pharmaceuticals, biology and microbiology, and environmental technology, in particular for the elimination of permanent chemicals, for the recycling of plastics, for the depolymerization of plastics such as PET and recovery of the monomers, and for the direct capture of carbon dioxide from gases, especially from the air, by mechanochemical mineralization (Direct Gas Capture by Mechanochemical Mineralization; DGCMM).

[0116] In the direct capture of carbon dioxide from the air by mineralization using the process according to the invention in the reactor according to the invention, at least one synthetic, natural and / or modified natural basic mineral is used, which forms sparingly soluble carbonates with carbon dioxide and / or adsorbs the carbon dioxide. The exothermic reaction with carbon dioxide is thermally controlled by means of the thermal management system to be used according to the invention.

[0117] Examples of suitable basic minerals are - Sodium oxide (NaO) - Sodium hydroxide (NaOH), - Potassium oxide (KO), - Potassium hydroxide (KOH), - Magnesium oxide (MgO), - Magnesium hydroxide (Mg(OH)2) - Calcium oxide (CaO), - Calcium hydroxide (Ca(OH2), - Strontium oxide (SrO), - Strontium hydroxide (Sr(OH)2), - barium oxide (BaO), - Barium hydroxide (Ba(OH)2) - Geopolymers (Polysialate (Si-O-Al), networks from tetrahedral [SiO4] 4- - and [AlO4] 5- -Earthquake), - Burnt and Felled Calcium Aluminate, - Amesit Mg2Al(AlSiO5)(OH)4 - Anorthit (Ca(Al2Si2O8) (90-100 % Anorthit)), - Bytownit ((Ca,Na)[(Si,Al)4O8] (70-90 % Anorthite)), - Labradorite ((Ca,Na)[(Si,Al)4O3] (50-70 % Anorthite)), - Andesin ((Na,Ca)[(Si,Al)4O8] (30-50 % Anorthit)), - Oligoklas ((Na,Ca)(Si,Al)4O8 (10-30 % Anorthit)), - Gehlenit (Ca2,Al2SiO7), - Hydrotalkit (Mg6Al2[(OH) 16 ]CO3] 4H2O), - Mordenit (Na2,Ca,K2)4(Al8Si 40 )O 96 ·28H2O, - Palygorskit (Attapulgit, (Mg,Al)4[OH|(Si,Al)4O 10 ]2 (4+4)H2O), - Vermiculite ((Mg 0,5 ,Ca 0,5 ,Na,K) 0,7 (Mg,Fe,Al)3[(OH)2|(Al,Si)2Si2O 10 ]·4H2O), - Chabasit-Ca (Ca2[Al4Si8O 24 ]·13H2O), - Chabasit-Mg ((Mg 0.7 K 0.5 Ca 0.5 Na 0.1 )[Al3Si9O 24 ]·10H2O) - Chabasit-Sr ((Sr,Ca)2[Al4Si8O 24 ]·11H2O), - Akermanit (Ca2MgSi2O7), - Antigorit (Blätterserpentin; Mg3Si2O5(OH)4), - Brucit (Mg(OH)2), - Bredigit (Ca y Mg(SiO4)4, - Calciumbentonit (Agrarbentonit), - Calciumpyroxenen, - Chrysotil (Faserserpentin; Mg3Si2O5(OH)4), - Cuspidin (Ca4Si2O7F2), - beta-Dicalciumsilikat (CaSiO4), - gamma-Dicalciumsilikat (CaSiO4), - Enstatit (Mg2Si2O6), - Fosterit (Mg2[SiO4]), - Klinochrysotil - Lizardit (Mg3Si2O5(OH)4), - Merwinit (Ca3Mg(SiO4)2), - Olivin (Mg2SiO4), (Ca2SiO4), - Orthochrysotil, - Parachrysotil, - Periklas (MgO), - Plagioklasen, - Sepiolite (Meerschaum, Mgs[(OH)2|Si e O 15 ]2·(4+8)H2O), - Smectites, calcium and magnesium smectites, - Steel slag - Talk (Mg3[(OH)2|Si4O 10 ]), - Toberomite (Ca4Si6O 17 (H2O)2·(Ca·3H2O)), - alumina cement, - Wollastonite (Ca3[Si3O9]), - Berthierin (Fe 2+ ,Fe 3+ ,Al)3(Si,Al)2O5(OH)4, - Cronstedtite (Fe 2+ ,Fe 3+ )3(Si,Fe 3+ )2O5(OH)4, - Fayalite (Fe2SiO4) - Greenalith (Fe 2+ , Fe 3+ ) 2-3 Si2O5(OH)4, - Siderite (FeCO3) forming hematite-iron-carbon mixtures and - Siderite-forming ferrite-iron-carbon mixtures.

[0118] If calcium hydroxide is used that has been produced from quicklime, during whose production the carbon dioxide is captured (CCS, Carbon Capture and Storage) or used directly as in sugar factories, the climate-protecting effect of DCGMM is increased even further [see also: - Greco-Coppi, M., Hofmann, C., Walter, D. et al., Negative CO emissions in the lime production using an indirectly heated carbonate looping process. Mitig. Adapt. Strategist. GlobChange 28, 30 (2023). https: / / doi.org / 10.1007 / s11027-023-10064-7; - Agustin Laveglia et al., From quarry to carbon sink: process-based LCA modeling of lime-based construction materials for net-zero and carbon-negative transformation, Green Chemistry 11, 2024; - Lhoist, Press release, Wülfrath, July 28, 2023, “CalCC” for CO capture, Europe promote innovative technologies; - CemNet.com » Cement News » VTT electric kiln targets carbon neutral cement production, 09 December 2022, Published under Cement News Tagged Under: VTT Finland Western Europe Finnsementti Nordkalk].

[0119] The basic minerals are used as milled materials in the form of fine- or coarse-grained bulk materials with a preferred particle size of 0.1 mm to 10 mm. The particles can have any shape, such as spheres, hollow spheres, shards, granules, ground chunks, pellets, rings, spheres with core-shell structures, ellipsoids, cubes, cuboids, pyramids, cones, cylinders, rhombuses, dodecahedra, truncated dodecahedra, icosahedra, truncated icosahedra, dumbbells, tori, plates, or needles with circular, oval, elliptical, square, triangular, quadrilateral, pentagonal, hexagonal, heptagonal, octagonal, or star-shaped cross-sections. They can also have the form of shards, rings, dumbbells, tori, needles, and plates bent in at least one direction in space.

[0120] For the implementation of DCGM, preferably at least one ball mill, attritor ball mill, or vibrating ball mill according to the invention, or at least one resonance acoustic mixer according to the invention, is used. Preferably, at least one ball mill, attritor ball mill, or vibrating ball mill according to the invention, and in particular an attritor ball mill, is used.

[0121] The base plate of the attritor ball mill according to the invention is equipped with a gas inlet device. The gas inlet device can cover the entire surface of the base plate or only a portion thereof. It comprises a nozzle plate with openings that have a smaller diameter than the material being ground. On the inlet side, it is connected to a gas supply line through which the gas, e.g., combustion gases or air, is pumped into the grinding chamber by means of a pump or compressor. The supply line can be equipped with a flow meter. The quantity of gas supplied depends primarily on the pressure drop in the grinding chamber due to the mineralization of the carbon dioxide. The carbon dioxide concentration in the supplied gas is monitored by means of a carbon dioxide sensor.

[0122] The cover plate of the attritor ball mill according to the invention is equipped with a pressure gauge and a gas outlet device. The gas outlet device comprises a sieve to capture material carried along by the flow and a pressure-maintaining valve to maintain overpressure in the reactor. It is connected to a gas outlet equipped with a carbon dioxide sensor.

[0123] Preferably, the attritor ball mill according to the invention is filled for grinding up to one third of its free internal volume with the grinding media and up to another third with the carbonate-forming minerals.

[0124] When hot combustion gases are directed into the attritor ball mill according to the invention, the mill serves as a heat source from which the heat is transferred to a heat sink via temperature-optimized heat pipes. This prevents overheating of the attritor ball mill due to the exothermic reaction of the carbon dioxide with the carbonate-forming minerals.

[0125] If, on the other hand, cold and moist air is introduced into the attritor ball mill according to the invention, it serves as a heat sink, which is heated by means of a heat source via the heat pipes in order to avoid the condensation of water in the grinding chamber.

[0126] Once the carbon dioxide sensor in the gas outlet indicates an increase in the carbon dioxide concentration in the escaping gas, a so-called carbon dioxide breakthrough, the grinding process is stopped and the carbonates are removed separately from the grinding balls. The carbonates can then be easily disposed of or used for other purposes.

[0127] The great advantage of DGCMM is that the grinding process repeatedly creates reactive surfaces on the carbonate-forming minerals, allowing them to be rapidly and quantitatively converted to carbonates with carbon dioxide.

[0128] The present invention will now be described with reference to the Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Fig. 9, Fig. 10, Fig. 11, Fig. 12 to Fig. 13 explained in more detail. Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Fig. 9, Fig. 10, Fig. 11, Fig. 12 to Fig. Figure 13 serves to illustrate the essential features of the mechanochemical reactors according to the invention. Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Fig. 9, Fig. 10, Fig. 11, Fig. 12 to Fig. Figure 13 are therefore not drawn to scale, but highlight their essential features. They are also exemplary and do not limit the invention. It shows Fig.1 the top view of the longitudinal section along the longitudinal axis L through an attritor ball mill 1 with flat heat pipes 3 or vapor chambers 3, which are fitted into the recesses 1.1.1 of the static wall 1.1 surrounding the grinding chamber 1.3 and are thermally connected to a heat source 4 or a heat sink 5 via heat pipes 2; Fig. 2 the top view of the cross-section through the attritor ball mill 1 of the Fig. 1 along the cross-sectional area AA; Fig. 3 the side view of the attritor ball mill 2 the Fig. 1; Fig. 4 the top view of the longitudinal section along the longitudinal axis L through a horizontal ball mill 1, which rotates around a static round bar 1.1;1.8 arranged along the longitudinal axis L in the grinding chamber 1.3 with bores 1.1.8 for receiving the heat tubes 2 and a stabilizing static rod 1.1.2 arranged centrally along the longitudinal axis L; Fig.5 the top view of the longitudinal section along the longitudinal axis L through the enlarged section of the starting area E1 of the horizontal ball mill 1 of the Fig. 4 with the through-opening 7.1.2 for the slidingly mounted round rod end 1.1.5 in the vertical reactor wall 7.1 and the through-opening 7.2.2 in the first vertical inner protective shield 7.2; Fig. 6 the top view of the longitudinal section along the longitudinal axis L through the enlarged section of the end region E2 of the horizontal ball mill 1 of the Fig. 4 with the through opening 7.2.2 in the second vertical inner protective cover 7.2 for the round bar end 1.1.5 which is slidably mounted in the circumferential holder 7.1.1; Fig. 7 the top view of the cross-section through the horizontal ball mill 1 of the Fig. 4 with the conveying webs 7.4 running parallel to the longitudinal axis L for the material to be ground 1.2 and the grinding media 1.4 and with the rotating bearing or drive rollers 8: Fig. 8 the top view of the longitudinal section along the longitudinal axis L through a further embodiment of an attritor ball mill 1 with bores 1.1.8 running parallel to the longitudinal axis L in the reactor wall 1.1 for receiving heat tubes 2, which are inserted to different lengths; Fig. 9 the top view of the cross-section perpendicular to the longitudinal axis L through the attritor ball mill 1 of the Fig. 8 with bores 1.1.8 for the heat pipes 2 and a bore 1.1.9 for a temperature measuring device; Fig. 10 the top view of the longitudinal section along the longitudinal axis L through the acoustically driven vibratory mill 1 with the heat-conducting round rod 1.8 arranged centrally along the longitudinal axis L in the grinding chamber 1.3; 1.1 with the bore 1.1.8 for receiving the heat tube 2 and with the acoustomechanical sound wave generator or resonance system 9 for generating sound waves 9.1 as an agitation means 1.6; Fig.11 the top view of the longitudinal section along the longitudinal axis L through the vertical pin mill 1 with the static pin plate 1.1 with the grinding pins 1.9 arranged on imaginary circumferential concentric circles at a distance from each other and perpendicular to the pin plate 1.1, which project into the grinding chamber 1.3, as well as with the bores 1.1.8 for the heat pipes 2 and with the rotating pin plate 1.6 whose grinding pins 1.9.1 arranged perpendicular to the pin plate 1.6 engage in the gaps between the grinding pins 1.9 of the stationary pin plate 1.1, wherein the material to be ground 1.2 or the starting products 1.2 are fed in via the material inlet 1.10 and the ground material 1.2.1 or the reaction products 1.2.1 are discharged continuously or discontinuously via the outlet 1.11; Fig. 12 the top view of the side of the stationary pin plate 1.1 of the pin mill 1 of the Fig. 11 with the heat pipes 2 and the heat source 4 or the heat sink 5 and Fig. 13 the schematic representation of a reactor plant R for the continuous or discontinuous grinding of material 1.2 or the continuous or discontinuous execution of chemical reactions with the storage vessels V1 to V4 for material 1.2 or starting materials 1.2, the mixing and conveying device 12, the powder conveyors 1.10.5, 1.12.1 and 1.13.2 and the pin mill 1 of the Fig. 11 and Fig. 12.

[0129] In the Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Fig. 9, Fig. 10, Fig. 11, Fig. 12 to Fig. The reference symbols in section 13 have the following meaning. 1 Mechanochemical reactor with a self-regulating thermal management system based on heat tubes 2 and / or flat heat pipes 3; ball mill; attritor ball mill; impact mill; pin mill; vibratory mill; acoustically driven vibratory mill with a self-regulating thermal management system 1.1 Static component; reactor wall; round bar; pin plate 1.1;1.8 Heat-conducting round bar 1.1 with bores arranged in the grinding chamber 1.3 1.1.1 Recess for receiving the flat heat pipe 3 Horizontal static rod 1.1.3 Vertical inner protective shield; protective screen 1.1.4 Sliding surface 1.1.2 1.1.5 Slidingly mounted round bar end 1.1.6 Circumferential sliding surface 1.1.7 Circumferential gap 1.1.8 Borehole for receiving the heat pipe 2 1.1.9 Hole for a temperature measuring device 1.1.10 Passage for the heat pipe 2 through the vertical inner protective cover 1.1.3 1.2 Ground material; starting material; ground material mixture; starting material mixture; mixture 1.2.1 Ground material; reaction products; suspensions or slurries, carbonate minerals 1.3 Grinding room 1.4 Grinding media; grinding ball 1.5 Cover plate 1.5.1 Rotary bearings; Shaft bearings 1.5.2 Circumferential releasable fastening; flange; circumferential stop surface 1.5.3 Connection direction 1.1 + 1.5 1.5.4 Acceptance direction 1.1 - 1.5 1.6 Stirrer; agitation medium rotating pin plate 1.6.1 Shaft; Drive shaft 1.6.2 Striking bar; striking disc; striking club; striking fan 1.6.3 Direction of rotation 1.6.4 End plate near wall 1.7 Base plate 1.8.1 Disc arranged vertically to the round bar 1.1; 1.8 1.9 Grinding pin arranged in an imaginary circumferential circle on the static pin plate 1,1 1.9.1 Grinding pin arranged in an imaginary circumferential circle on the rotating pin plate 1.6 1.10 Grinding material inlet; Raw material inlet 1.10.1 First shut-off valve in the inlet 1.10 1.10.2 Second shut-off valve in the inlet 1.10 1.10.3 Third shut-off valve in the inlet 1.10 1.10.4 Third shut-off valve in the inlet 1.10 Discharge for ground material or reaction products 1.11.1 First shut-off valve in the discharge 1.11 1.11.2 Second shut-off valve in the discharge 1.11 1.11 1.11.3 T-junction 1.12 Powder conveyor in discharge 1.11 1.12.1 Third shut-off valve in discharge 1.11 1.13 Return; Bypass 1.13.1 First shut-off valve in the return line 13 1.13.2 Powder feeder in return 13 1.13.3 Second shut-off valve in the return line 13 1.13.4 T-junction 2. Heat pipe; Heatpipe 2.1 Pipe wall of heat pipe 2 2.2 Insert, wick or capillary structure of the heat pipe 2 2.3 Steam chamber with working medium of the heat pipe 2 or the heat pipe 2 3 flat heat pipes; vapor chamber, heat spreader 3.1 Chamber wall of the flat heat pipe 3, the vapor chamber 3 or the heat spreader 3 3.2 Insert, wick or capillary structure of the flat heatpipe 3, the vapor chamber 3 or the heat spreader 3 3.3 Vapor chamber with working fluid or heat transfer medium of the flat heat pipe 3, the vapor chamber 3 or the heat spreader 3 3.4 Support structure of the flat heat pipe 3, the vapor chamber 3 or the heat spreader 3 4 Heat source 5 heat sinks 7 Rotatable, horizontal, tubular reactor wall of ball mill 1 7.1 Rotating, vertical reactor wall of ball mill 1 7.1.1 Circumferential support for the slidingly mounted round bar end 1.1.5 7.1.2 Through-opening for the sliding round rod end 1.1.5 through the vertical reactor wall 7.1 7.2 Vertical inner protective cover; protective screen 7.2.1 The edge of the through-opening 7.2.2 of the protective cover 7.2 circumferential sliding ring 7.2.2 Passage opening for the sliding pipe end 1.1.5 through the vertical inner protective plate 7.2 7.2.3a Circumferential gap between the vertical inner protective cover 7.2 and the edge of the circumferential support 7.1.1 in the end area E2 7.2.3b Circumferential gap between the circumferential sliding ring 7.2.1 and the circumferential sliding surface 1.1.4 of the vertical inner protective cover 1.1.3 in the end region E2 7.3 Drive shaft 7.4 Carrying ribs running parallel to the longitudinal axis L 7.5 Circumferential gap between the vertical inner protective shield 7.2 and the rotatable, vertical reactor wall 7.1 in the starting area E1 and the end area E2 8 Bearing roller; drive roller 9 Device for generating acoustic and / or mechanical oscillations and / or vibrations; sound wave generator; resonance system 9.1 Sound wave front 10 Pre-product discontinuation 11 Rotary valve; metering pump 12 Mixing and conveying device ▲▼ Conveyor directions ► ◄ Conveyor directions AA Cross-sectional area B1 Area of ​​the first bend of the heat pipe 2 B2 Area of ​​the second bend of the heat pipe 2 E1 starting area, enlarged section, see Fig. 5 E2 end area, enlarged section, see Fig. 6 L Longitudinal axis M Motor Q transverse axis R reactor plant V1, V2 Storage container for milled material or semi-finished product V3, V4 Storage container for milled material or semi-finished product Detailed description of the figures Figures 1 to 3 Vertical attritor ball mill 1 with a heat management system based on heat tubes 2 and flat heat pipes 3 as well as upscaling example 1

[0130] The vertical attritor ball mill 1 is rotationally symmetrical (see the longitudinal axis L).

[0131] The cylindrical grinding chamber 1.3 of the attritor ball mill 1 is 50 cm high and has a diameter of 20 cm. Accordingly, the free volume without agitator 1.6 is 15,707.96 cm³. 3 .

[0132] The vertical reactor wall 1.1 (= static component 1.1) consists of a copper-aluminum alloy with a melting point of 1070°C and a thermal conductivity λ of 70 W / mK at 20°C. The thermal conductivity increases with increasing temperature. In a first embodiment, the vertical reactor wall 1.1, which surrounds the central grinding chamber 1.3, is polished on the inside; in a second embodiment, it is coated with a highly thermally conductive sintered silicon carbide ceramic with a thermal conductivity λ of 100 W / mK to 120 W / mK. The reactor wall 1.1 has the external shape of a 50 cm high block with a square cross-section Q perpendicular to the longitudinal axis L, with an edge length of 22 cm. The cross-sectional area is therefore 484 cm². 2The four rectangular outer walls of reactor wall 1.1 each have a width of 22 cm and a height of 50 cm. A rectangular recess 1.1.1, 0.6 cm deep, 48 cm high, and 20 cm wide, is recessed into each outer wall and surrounded by a 1 cm wide rim. Flat heat pipes 3 are precisely fitted into the four recesses 1.1.1, so that they are thermally connected to reactor wall 1.1.

[0133] The flat heatpipes 3, vapor chamber 3 or heat spreader 3 comprise the chamber wall 3.1, the wick 3.2, the vapor chamber 3.3 with the working medium or heat transfer medium and the support structure 3.4 made of copper, titanium or aluminium.

[0134] Depending on the temperature range to be set, the following flat heat pipes 3 are used in the various designs: - 10°C to 60°C: Titanium or aluminum flat heat pipes, working fluid: water; - 0°C to 100°C: Copper flat heat pipes, working fluid: water; - 0°C to 150°C: Copper flat heat pipes, working fluid: water-toluene mixture; -48°C to 80°C: Aluminum flat heat pipes, working fluid: acetone, -60°C to 80°C: Copper flat heat pipes, working fluid: methanol; -80°C to 150°C: Copper flat heat pipes, working fluid: methane.

[0135] Three vertical copper heat pipes 2 with a flat cross-sectional profile are soldered to each side of the outer surfaces of the flat heat pipes 3. The same working fluid is used in the heat pipes 2 as in the flat heat pipes 3.

[0136] The twelve heat pipes 2 run vertically downwards and are bent twice in sections B1 and B2, so that they enter the heat sink 5 or the heat source 4 in a bundled configuration. If the heat sink 5 is used, the reactor 1 serves as the heat source 4. Conversely, if the heat sink 5 is not used, the reactor 1 serves as the heat sink 5.

[0137] The distance between reactor 1 and heat sink 5 or heat source 4 is not critical, as the heat pipes 2 can transfer the heat largely without loss and almost isothermally over long distances.

[0138] When a temperature of 80°C is set in reactor 1, the hot ends of the copper-water heat pipes 2 are located in a correspondingly heated thermostatic oven 4.

[0139] When the reactor is set to -15°C, the cold ends of the copper-methanol heat pipes are in contact with a correspondingly cooled cryocooler.

[0140] The grinding chamber is sealed at the top by a square, 1 cm thick, removable cover plate 1.5, creating a pressure-tight seal. Standard and well-known sealing and fastening devices are used for this purpose (not shown). The cover plate 1.5 consists primarily of austenitic stainless steel with a thermal conductivity λ <10 W / mK. This minimizes heat loss or heat input through the cover plate 1.5.

[0141] The cover plate 1.5 contains a centrally located rotary or shaft bearing 1.1.5 for the passage of the shaft 1.6.1 of the agitator 1.6, which runs along the longitudinal axis L, into the grinding chamber 1.3. The shaft 1.6.1 has a diameter of 1.4 cm and is 49.8 cm long inside the grinding chamber. Horizontal and obliquely inclined beaters 1.6.2 are attached to the shaft 1.6.1. These beaters radiate radially from the shaft 1.6 and are weight-balanced to prevent imbalance during rapid rotation in the direction 1.6.3 during grinding. The beaters 1.6.2 are of different lengths: 9 cm and 4.5 cm. This configuration achieves maximum turbulence of the material to be ground 1.3 and the grinding media 1.4. At the lower end of shaft 1.6, the end plate closest to the wall is attached, which prevents the material to be ground 1.2 and the grinding media 1.4 from becoming stuck in dead corners in the area of ​​the base plate 1.7. The agitator 1.6 also consists essentially of austenitic stainless steel with a thermal conductivity λ of 10 W / mK. This minimizes heat loss or heat input via shaft 1.6.1.

[0142] In other embodiments, striking discs, striking clubs and / or striking fans 1.6.2 will be used instead of the striking bars 1.6.2.

[0143] The agitator 1.6 is driven by a conventional and well-known, variable-speed electric motor (not shown). The speed is preferably between 100 and 1000 revolutions per minute.

[0144] The cover plate 1.5 may also include closable inlets for gaseous, liquid, and especially solid materials to be ground 1.3, connections for pressure and temperature sensors, a pressure relief valve for releasing gases that may be produced during chemical reactions, or a viewing window for optical and spectroscopic observation of the grinding process. These are not shown for clarity.

[0145] The grinding chamber 1.3 is sealed at the bottom by a square, 1 cm thick, removable base plate 1.7 made of austenitic stainless steel, creating a pressure-tight seal. This plate may include a closable outlet for the discharge of ground material or reaction products, with the grinding media 1.4 being retained by sieves. This arrangement is not shown for clarity.

[0146] Grinding media 1.4 consists of grinding balls 1.4 with a diameter of 1 cm, made of highly thermally conductive sintered silicon carbide ceramic with a thermal conductivity λ of 100 W / mK to 120 W / mK. This ensures particularly good heat exchange.

[0147] For example, the grinding chamber 1.3 can be filled to one-third of its free volume with the grinding balls 1.4 and to one-quarter with the material to be ground 1.2 or the starting materials 1.2 for synthesis. The grinding time can range from, for example, 30 minutes to several days.

[0148] The thermal effects can be observed using thermographic cameras.

[0149] Reactor 1 is ideally suited for carrying out chemical syntheses under thermally controlled mechanochemical conditions. Upscaling example 1: Upscaling a frieze rearrangement by a factor of 200

[0150] In DE 10 2022 115 870 A1, embodiment 3, pages 18 to 19, paragraph

[0102] describes the Fries rearrangement of 1.07 g of phenyl acetate in a 50 mL grinding jar containing 25 zirconium dioxide grinding balls with a diameter of 1 cm to 2- and 4-hydroxyacetophenone. The grinding jar is operated in a vibrating mill (MM500 nano, Retsch) for 8 hours at 30 Hz. During this time, the temperature rises to 60°C due to friction.

[0151] The vertical attritor ball mill 1 of the Fig. 1, Fig. 2 to Fig.As described above, chamber 3 is equipped with copper flat heat pipes 3 containing water as the working medium and copper heat tubes 2 also containing water as the working medium. The inner surface of the walls of the grinding chamber 1, 3 is coated with a highly thermally conductive boron nitride ceramic with a thermal conductivity λ of 120 W / mK. The cold ends of the copper heat tubes 2 are located in a thermostat set to 25°C, acting as a heat sink 5. The attritor ball mill 1 constitutes the heat source 4.

[0152] The attritor ball mill 1 is filled to half its grinding chamber 1.3 with grinding balls 1.4 with a diameter of 1 cm made of a highly thermally conductive sintered silicon carbide ceramic with a thermal conductivity λ of 100 W / mK to 120 W / mK. 214 g of liquid phenyl acetate, 500 g of sodium chloride, and 1152 g of aluminum chloride are added. The attritor ball mill 1 is then closed, after which the material 1.2 is ground for 96 hours at a constant speed of 800 revolutions per minute of the agitator 1.6. The heat generated during grinding is dissipated via the reactor wall 1.1 and the copper flat heat pipes 3 and copper heat tubes 2 into the heat sink 5. This ensures that a temperature of 25°C is maintained during grinding. After grinding is complete, 0.4 L of water is added and the mixture is ground for another 15 minutes. Then, 2000 g of sand is added to the reaction mixture and ground for another 15 minutes. The resulting powder is extracted with dichloromethane.The collected extracts are evaporated under vacuum. The reaction product 2-hydroxyacetophenone is separated by vacuum distillation. The remaining reaction product 4-hydroxyacetophenone is purified by recrystallization from an ethanol-water mixture. The rearrangement of the phenyl acetate proceeds almost quantitatively. Figures 4 to 7 Horizontal ball mill 1 with a central static round bar 1.1;1.8 for holding heat pipes 2

[0153] The horizontal, tubular reactor wall 7, rotatable in the direction of rotation 1.6.3, and the two vertical reactor walls 7.1 of the ball mill 1 consist essentially of austenitic stainless steel with a thermal conductivity λ <10 W / mK. This minimizes heat loss or heat input through the horizontal reactor wall 7 and the two vertical reactor walls 7.1.

[0154] The thickness of the reactor walls 7; 7.1 can vary widely and depends primarily on the stability requirements determined by the dimensions of the ball mill 1.

[0155] In a second embodiment, the inner surfaces of the reactor walls 7; 7.1 and the inner vertical protective shields 7.2 are coated with a hard, non-thermally conductive ceramic such as an aluminum oxide or silicon oxide ceramic in order to further minimize heat exchange between the grinding chamber 1.3 and the environment and, if necessary, to prevent corrosion by the grinding material 1.2.

[0156] On the inside of the reactor wall 7, conveying ribs 7.4 made of austenitic stainless steel run parallel to the longitudinal axis L. In the second embodiment, they are also coated with silicon carbide ceramic. They act as scoops, transporting the material to be ground 1.2 and the grinding media 1.4 made of silicon carbide ceramic upwards in the direction of rotation 1.6.3 until they detach from the reactor wall 7. Fig. Figure 7 shows four drive bridges 7.4, which are arranged in a cross shape relative to each other.

[0157] In the initial section E1 of the ball mill 1, the horizontal reactor wall 7 is connected to the vertical reactor wall 7.1. The reactor wall 7.1 has a centrally arranged circumferential support 7.1.1 with the through-opening 7.1.2 for the slidingly mounted, horizontal round bar end 1.1.5 made of austenitic stainless steel. The round bar end 1.1.5 is an externally open tube section through which four heat pipes are guided. The round bar end 1.1.5 and the edge of the through-opening are equipped with circumferential sliding surfaces 1.1.6 made of high-temperature-resistant polyetheretherketone. The round bar end 1.1.5 is connected to the vertical inner protective plate 1.1.3 or protective disc 1.1.3 made of stainless steel. The protective cover 1.1.3 also serves as a vertical support for the highly thermally conductive, hard material made of highly thermally conductive sintered silicon carbide ceramic with a thermal conductivity λ of 100 W / mK to 120 W / mK of the horizontal static round bar 1.1;1.8. The protective cover 1.1.3 is surrounded by the circumferential edge 7.2.1 of the through-opening 7.2.2 in the inner vertical protective shield 7.2 for the round rod end 1.1.5. The vertical inner protective shield 7.2 is firmly connected all around to the inside of the horizontal reactor wall 7. The edge 7.2.1 and the edge of the protective shield 1.1.3 are also equipped all around with sliding surfaces 1.1.6 made of high-temperature-resistant polyetheretherketone. The protective shield 1.1.3 also contains the penetrations 1.1.10 for the heat pipes 2.

[0158] In the end region E2 of the ball mill 1, the horizontal reactor wall 7 is also rigidly connected to the horizontal reactor wall 7. Between them is another circumferential gap 7.5. On the inside of the vertical reactor wall 7.1, the holder 7.1.1 for the slidingly mounted round bar end 1.1.5 is arranged. The inside of the holder 7.1.1 and the outside of the round bar end 1.1.5 are equipped with circumferential sliding surfaces 1.1.6 made of high-temperature-resistant polyetheretherketone. Between the circumferential edge of the holder 7.1.1 coated with polyetheretherketone and the circumferential edge 7.2.1 of the passage opening 7.2.2 through the vertical inner protective plate 7.2 is the narrow circumferential gap 7.2.3a, which facilitates the rotation of the reactor walls 7; 7.1 about the longitudinal axis L. Another gap 7.2.3b is located between edge 7.2.1 and the surrounding edge coated with polyetheretherketone as a sliding surface 1.1.4 of the vertical inner protective shield 1.1.3.

[0159] The configurations described above prevent the ingress of ground material 1.2 into the circumferential gaps 7.5 between the two vertical inner protective baffles 7.2 and the two vertical reactor walls 7.1. Furthermore, the gaps have a thermally insulating and mechanically stabilizing effect.

[0160] The two vertical inner protective panels 1.1.3 are connected centrally by a horizontal static rod 1.1.2 with a round cross-section made of austenitic stainless steel. This rod serves to stabilize the round bar 1.1; 1.8.

[0161] The four heat tubes 2 consist of the copper tube wall 2.1, the coil 2.2, and the steam chamber 2.3 containing the working fluid or heat transfer medium, which is selected according to the temperature range to be set. They are thermally supported in the bores 1.1.8 and arranged crosswise around the rod 1.1.2. Their free ends are connected to either a heat sink 5 or a heat source 4, depending on the application.

[0162] The entire arrangement ; 7.1; 1.1;1.8; 1.1.2; 1.1.3; 1.1.4; 1.1.5; 1.1.7 and the heat pipes 2 can be pulled out of the ball mill 1 for maintenance.

[0163] The ball mill 1, or rather its reactor wall 7, is mounted on rotatable bearing rollers 8. In another embodiment, these can also serve as drive rollers 8.

[0164] The vertical reactor wall 7.1 in the end region E2 is connected centrally to the drive shaft of a speed-controlled motor M. Preferably, the speed of the ball mill 1 is between 60 and 100 revolutions per minute.

[0165] The material to be ground 1.2 or the reaction products 1.2 and the grinding media 1.4 are fed into the grinding chamber 1.3 through an upper, closable inlet device (not shown) when the ball mill 1 is at rest. After grinding, the ground material 1.2 or the reaction products are discharged from the grinding chamber 1.3 through a lower outlet device (not shown) while the ball mill 1 is at rest, either together with or after sieving, or separately from the grinding media 1.4. The material is then blown out with gas or rinsed with liquid.

[0166] The ball mill 1 is ideally suited for the thermally gentle grinding of substances from the pharmaceutical sector (e.g., additives and excipients), the food sector (e.g., preservatives, spices, minerals, salts, and dried fruits), the feed sector (e.g., amino acids, feed additives, salts, and vitamins), the cosmetics sector (e.g., color pigments and plant-based substances), and the chemical industry (e.g., waxes, specialty chemicals, plastics, construction chemicals, catalysts, and dyes) where there is a risk of thermal damage, without the use of liquid nitrogen. For this purpose, the grinding chamber 1.3 can be cooled to -40°C using the horizontal static round bar 1.1;1.8 and copper heat pipes 2 with methanol as the working fluid and a bath cryostat or an ice-calcium chloride hexahydrate cold mixture as a heat sink 5. Figures 8 and 9: Vertical attritor ball mill 1 with a heat management system based on heat pipes 2

[0167] The vertical attritor ball mill 1 (reactor 1) of the Fig. 8 consists of the ones at the Fig. 1, Fig. 2 to Fig. The materials described in section 3 are also used. It is rotationally symmetrical (see the longitudinal axis L) and its cylindrical grinding chamber 1.3 is also 50 cm high and has a diameter of 20 cm. Accordingly, the free volume without agitator 1.6 is also 15,707.96 cm³. 3 .

[0168] The main differences to the attritor ball mill 1 of the Fig. 1, Fig. 2 to Fig.The three components are characterized by a circular cross-section Q, a thickness of 2 cm of the vertical reactor wall 1.1, and twelve bores 1.1.8, 49 cm deep and 0.8 cm wide, arranged symmetrically around the longitudinal axis L from bottom to top. Heat pipes 2, with pipe walls 2.1, wicks 2.2 or capillary structure 2.2, and steam chamber 2.3, are inserted into the bores 1.1.8 to varying heights in a heat-conducting manner. For example, a heat pipe 2 is inserted alternately to the end of a bore 1.1.8 and another heat pipe to half its height, leaving the remaining space of the bore 1.1.8 empty. In another embodiment, bores 1.1.8 with a depth of 49 cm alternate with bores 25 cm deep. The bores 1.1.8 are equipped with heat pipes 2 of corresponding lengths. This ensures that the heat resulting from grinding is dissipated evenly and effectively, or that the grinding chamber is heated evenly. Upscaling example 2: Upscaling an arylation reaction by a factor of 200

[0169] In Supplementary Materials for the publication "Redox reactions of small organic molecules using ball milling and piezoelectric materials" by Koji Kubota, Yadong Pang, Akira Miura, Hajime Ito, Corresponding authors Emails: hajito@eng.hokudai.ac.jp (HI); kbt@eng.hokudai.ac.jp (KK), Published 20 December 2019, Science 366, 1500 (2019), DOI: 10.1126 / science.aay8224, the mechanochemical arylation of thiophene-2-carboxylic acid methyl ester-3-diazonium tetrafluoroborate with furan to thiophene-2-carboxylic acid methyl ester-3-(furan-2'-yl) in the presence of barium titanate on a gram scale in 71% yield is described.

[0170] To scale up this synthesis by a factor of 200, the cover plate 1.5 of reactor 1 is equipped with a pressure relief valve to release the nitrogen produced during the reaction. Twelve copper heat pipes 2, containing a water-toluene mixture as the working fluid, are used to cool reactor 1 in the arrangement described above. A thermostat set to 20°C serves as the heat sink 5.

[0171] Reactor 1 is half-filled with 1 cm diameter grinding spheres 1.4 made of the silicon carbide ceramic described above, 409.6 g of thiophene-2-carboxylic acid methyl ester-3-diazonium tetrafluoroborate, 1866 g of barium titanate, and 1.746 L of furan as the grinding material 1.3. The grinding material 1.3 is ground for 30 hours at a stirring speed of 1000 revolutions per minute. After grinding, the resulting thiophene-2-carboxylic acid methyl ester-3-(furan-2'-yl) is extracted from the grinding material 2 and isolated and purified by column chromatography in a conventional and known manner. 180 g of purified reaction product are obtained. Upscaling Example 3: Direct gas capture by mechanochemical mineralization (DGCMM)

[0172] For the DGCMM, 3 is the base plate 1.7 of the reactor 1 according to the invention. Fig. 8 and Fig.9 is connected to a gas introduction device (not shown) by means of which air at a temperature of 23°C is introduced into the grinding chamber 1.3. The gas introduction device comprises a nozzle plate with fine openings in the base plate 1.7 with a sieve to retain grinding media 1.3 and minerals 1.2.1 in the grinding chamber 1.3, a shut-off valve, a connector for attaching an air line, an air flow meter and a carbon dioxide sensor in the air line, and a pump for conveying the air with an air filter on the intake side.

[0173] The cover plate 1.5 of the reactor 1 according to the invention is equipped with a pressure gauge and a gas outlet device (not shown). The gas outlet device comprises a sieve to capture regrind carried along by the flow and a pressure-maintaining valve to maintain an overpressure of 1 bar in the reactor. The gas outlet device is connected to a gas outlet equipped with a carbon dioxide sensor.

[0174] Twelve copper heat pipes 2, containing water as the working fluid, are used as heat pipes 2. Since the reactor 1 according to the invention serves as a heat sink 5, the heat pipes 2 are thermally connected to a thermostatic furnace 4 set to 100°C as the heat source 4. When the reactor 1 according to the invention reaches this temperature, the isothermal circulation of the working fluid in the heat pipes 2 ceases due to self-regulation. The circulation restarts when the reactor temperature drops below 100°C. In this way, both the condensation of water in the grinding chamber 1.3 and the overheating of the reactor 1 according to the invention are prevented.

[0175] For grinding, the reactor 1 according to the invention is filled to one third of its free internal volume (approx. 5 L) with the grinding media 1.4 and with 8 kg calcium hydroxide pellets.

[0176] Then the agitator 1.6; 1.61; 1.6.2 is started and run at 400 revolutions per minute.

[0177] The 8 kg or approximately 108 mol calcium hydroxide pellets react over time with the carbon dioxide in the passed air to form approximately 10.8 kg of calcium carbonate. Since the grinding process continuously creates fresh reactive sites on the ground material 1.2, the yield is quantitative. In total, approximately 4.75 kg or about 2421 liters of carbon dioxide are mineralized from the air over time. The corresponding volume of air passed through, with an initial carbon dioxide content of 0.044%, is approximately 5500 m³. 3 Air.

[0178] Once the carbon dioxide sensor in the gas outlet indicates an increase in the carbon dioxide concentration in the exiting air, a so-called carbon dioxide breakthrough, the grinding process is stopped. The calcium carbonate 1.2.1 and the grinding balls 1.4 are removed from reactor 1 and separated. The calcium carbonate 1.2.1 is pure and can be safely disposed of or used for other purposes. Figure 10

[0179] The vertical reactor 1 comprises a cylindrical grinding chamber 1.3 with a diameter of 16 cm and a height of 40 cm and a volume of approximately 8 L, containing the material to be ground 1.2 and the grinding media 1.4. It is surrounded by a 0.8 cm thick stainless steel reactor wall 1.1 and has a stainless steel base plate 1.7 of the same thickness, which is rigidly connected to the reactor wall. The grinding media 1.4, with a diameter of 0.5 cm, are made of the silicon carbide ceramic described above. The base plate 1.7 has an outlet (not shown) with a sieve for separating the liquid or solid ground material 1.2.1 or the reaction products 1.2.1. The grinding chamber 1.3 is closed at the top by a removable stainless steel cover plate 1.5, 0.8 cm thick. The base plate 1.7 is coupled to a device 9 for generating acoustic and / or mechanical oscillations and / or vibrations or sound wavefronts 9.1 of preferably 60 Hz. Such devices 9 and arrangements are used, for example, in - US 7 188 993 B1, Apparatus and method for resonant vibratory mixing, Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Fig. 9, Fig. 10, Fig. 11, Fig. 12, Fig. 13, Fig. 14, Fig. 15, Fig. 16, Fig. 17, Fig. 18 to Fig. 19 in conjunction with the description in column 10, line 13 to column 21, line 40, - US 10 835 880 B2, Continuous acoustic mixers, Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Fig. 9, Fig. 10 to Fig. 11 in conjunction with the description in column 2, line 7, to column 9, line 51, They are also available in different sizes from Resodyn Acoustic Mixers, website: Industrial Mixers, Laboratory Mixing - Resodyn Acoustic Mixers. For the arrangement of the Fig. For example, the OMNIram® acoustic mixer from Resodyn Acoustic Mixers can be used, which can process up to 5 kg of ground material 1.2 and allows temperature control from -9°C to 90°C. However, with the thermal management system according to the invention, it is possible to set higher and lower temperatures.

[0180] For this purpose, a static, vertical round bar 1.1;1.8 with a diameter of 2.5 cm and a height of 43 cm, made of the silicon carbide ceramic described above, is attached centrally along the longitudinal axis L in the grinding chamber of reactor 1 as a static component 1.1. The upper end of the round bar protrudes from the removable cover plate 1.5, which also contains closable connections (not shown) for adding the material to be ground 1.2 to the grinding chamber 1.3. The round bar 1.1;1.8 has a bore 42 cm long and 1 cm wide, into which a 0.9 cm diameter copper-methanol heat pipe 2; 2.1; 2.2; 2.3, with a working range of -60°C to 200°C, is precisely inserted in thermally conductive contact. The heat pipe 2; 2.1; 2.2; 2.3 has a total length of 120 cm and features a bend in the horizontal direction and another bend in the vertical direction. In a second embodiment, the heat pipe 2; 2.1; 2.2; 2.3 forms a rounded arc.In both embodiments, its vertical end is thermally connected to a heat source 4 or a heat sink 5, with which a temperature above 90°C or below -9°C can be set in the grinding chamber 1.2.

[0181] In one embodiment, grinding balls 1.4 with a diameter of 0.5 cm are made of sintered silicon carbide or boron nitride ceramic.

[0182] Reactor 1 is ideally suited for the production of particularly fine-particle solid suspensions with medium particle sizes d 50 <1 µm at low temperatures, such as suspensions of temperature-sensitive pharmaceutical or biocidal agents, vaccines, biological and biochemical preparations, pigments, reactive metals and catalysts in organic solvents. Figures 11 and 12

[0183] The vertically arranged pin mill 1 (reactor 1) comprises a static pin plate 1.1 on which static grinding pins 1.4.1, projecting horizontally into the grinding chamber 1.3, are arranged as grinding elements 1.4 on imaginary concentric circles around the transverse axis Q. The grinding pins 1.4.1 are connected to the pin plate 1.1 by a material bond or force bond.

[0184] The entire grinding chamber 1.3 is surrounded by a reactor wall in the form of a closed, round container. The reactor wall is formed by the vertical static pin plate 1.1 and a circumferential, horizontally oriented reactor wall section that extends to the circumferential stop surface of a flange 1.5.2 (releasable fastening device 1.5.2) and is bonded to the static pin plate 1.1. A vertical, tubular connection (not shown) for the tubular feed 1.10 or feed 1.10 is bonded to the top of the grinding chamber 1.3. A tubular connection (not shown) for the vertical, tubular discharge 1.11 for the ground material 1.2.1 or the ground reaction products 1.2.1 is also bonded to the bottom.

[0185] The tubular connector for the tubular feed 1.10 or feed 1.10, or the tubular connector for the vertical tubular discharge 1.11 for the ground material 1.2.1 or the ground reaction products 1.2.1, can, or both connectors can, be arranged tangentially to the grinding chamber 1.3 in a second and third embodiment. In all three embodiments, the ground material 1.2.1 or the ground reaction products 1.2.1 are ejected by the rotary motion of the rotating pin plate 1.6.

[0186] In the three embodiments, a sieve (not shown) can be arranged before the discharge 1.11 to classify the ground material 1.2.1 or the ground reaction products 1.2.1 in order to retain any remaining coarse ground material 1.2 for fine grinding in the grinding chamber 1.3.

[0187] The static components described above are made of a Monel® alloy with a thermal conductivity λ of 26 W / mK to ensure good heat flow from the grinding chamber 1.3 – depending on whether it serves as a heat source 4 or a heat sink 5 – to the hot or cold ends of the heat pipes 2. The ends of the four heat pipes 2 are thermally conductive and precisely fitted into four bores 1.1.8 in the outer surface of the static pin plate 1.1. The four bores 1.1.8 are arranged on an imaginary vertical line that runs parallel to the longitudinal axis L of the rector 1. To the left and right of these bores 1.1.8, at the level of the cross-sectional area, there is another bore 1.1.8 each for receiving two further heat pipes 2 (see Fig. 12, side view).

[0188] All six heat pipes are thermally connected to a heat source 4 to maintain a high temperature in the grinding chamber 1.3. In this embodiment, heat pipes 2 made of Monel® are preferably used to avoid stresses in the static pin plate 1.1 and the heat pipes 2 caused by differing coefficients of thermal expansion. If the six heat pipes are thermally connected to a heat sink 5 to maintain low temperatures in the grinding chamber 1.3, copper heat pipes are preferably used.

[0189] The grinding chamber 1.3 is closed by the vertical cover plate 1.5, which essentially acts as the lid of the round container. The cover plate 1.5 is detachably connected to the circumferential stop surface of the flange 1.5.2. To open the grinding chamber 1.3, after releasing the circumferential detachable fastening device 1.5.2, it is moved in the removal direction 1.5.4 on the drive shaft 1.6.1; to close the grinding chamber 1.3, it is moved in the connection direction 1.5.3. The drive motor is not shown.

[0190] The cover plate 1.5 contains a centrally located rotary bearing 1.5.1 or a shaft bearing 1.5.1 for the passage of the drive shaft 1.6.1, which rotates in the direction of rotation 1.6.3, for the rotating, vertical pin plate 1.6. Grinding pins 1.9.1, projecting horizontally into the grinding chamber 1.3, are attached to or on the rotating pin plate 1.6 by frictional or material bonding on imaginary, concentric circles around the transverse axis Q such that they engage in the spaces between the grinding pins 1.9 of the static pin plate 1.1. By moving the drive shaft 1.6.1 in the directions 1.5.3 or 1.5.4, the grinding chamber 1.3 is reduced or enlarged. This allows the fineness of the grinding to be controlled.

[0191] The components described above are made of austenitic stainless steel with a thermal conductivity λ <10 W / mK. This minimizes excessive heat loss or gain through the components. Additional insulating measures, such as embedding the reactor in insulating materials, can also be implemented.

[0192] The reactor 1 is ideally suited for the continuous and discontinuous grinding of grinding material 1.2 of all kinds or for the continuous and discontinuous carrying out of chemical reactions between solid starting materials 1.2 under controlled thermal conditions. Figure 13

[0193] Reactor 1 according to the Fig. 11 and Fig. 12 (see there) is the essential component of the reaction plant R according to the Fig.13. The reactor system R is used for the continuous or discontinuous grinding of regrind 1.2 or for the continuous or discontinuous execution of chemical reactions. It comprises at least four storage vessels V1 to V4 for solid regrind 1.2 or liquid and solid feedstocks 1.2. The solid regrind 1.2 or feedstocks 1.2 are discharged via feedstock outlets 10 and conveyed by rotary valves 11, or, in the case of liquid feedstocks, by metering pumps 11, into a mixing and conveying device 12. Conventional and well-known mixing and conveying devices 12, such as extruders, are used.

[0194] The resulting powdery or slurry-like regrind mixture 1.2 or the powdery or slurry-like feedstock mixture 1.2 (collectively referred to as "mixture 1.2") leaves the mixing and conveying devices 12 and enters the regrind inlet 1.10 or feedstock inlet 1.10 and is conveyed through the open first gate valve 1.10.1 into the powder conveyor 1.10.5. The conveying directions are indicated by the black arrows. Depending on whether powder or slurry is being conveyed, screw conveyors with or without shafts are used; they are collectively referred to here as "powder conveyors". The powder conveyor 1.10.5 conveys the mixture 1.2 through the open second, third, and fourth gate valves 1.10.2; 1.10.3; 1.10.4 through the inlet 1.10 into the reactor 1 with the heat pipes 2 and the heat source 4 or the heat sink 5. The ground materials 1.2.1 or the ground reaction products 1.2.The powder leaves the reactor through discharge 1.11 and the open first and second shut-off valves 1.11.1 and 1.11.2 and is conveyed by the powder conveyor 1.12 through the open third shut-off valve 1.12.1 into storage vessels (not shown). The first and second shut-off valves 1.13.1 and 1.13.3, viewed in the conveying direction, are closed upstream and downstream of the powder conveyor 1.13.2 in the return line 1.13 or bypass 1.13, which branches off at the T-junction 1.11.2. Continuous grinding or conversion is thus possible.

[0195] The reactor system R also enables batch grinding or conversion, in which the mixture 1.2, together with the increasingly concentrated ground materials 1.2.1 or reaction products 1.2.1, is circulated through reactor 1. Initially, with the second shut-off valve 1.11.2 closed and shut-off valves 1.10.1, 1.10.2, 1.10.4, 1.11.1, 1.13.1, and 1.13.3 open, the feed line 1.10, reactor 1, outlet 1.11, T-junction 1.11.3, return 1.13, and powder feeder 1.13.2 are completely filled with the mixture 1.2 up to T-junction 1.13.4. The atmosphere displaced by mixture 1.2 inside reactor R is released through pressure relief valves. The addition of mixture 1.2 is then stopped, and the third shut-off valve 1.10.3 in the inlet 1.10 is closed. The temperature in reactor 1 is then adjusted as described above.At the same time, the grinding process is started by rotating the drive shaft 1.6.1, and the powder conveyor 1.13.2 is started.

[0196] Through this closed-loop operation, the ground materials 1.2.1 or the reaction products 1.2.1 become increasingly concentrated in the mixture 1.2. Samples are taken and measured to monitor the progress of the grinding or reaction. After grinding is complete, the circuit is emptied via the open shut-off valves 1.11.2 and 1.12.1 and the powder conveyor 12. If necessary, the ground materials 1.2.1 or the reaction products 1.2.1 are blown out with an inert gas or air, or rinsed with an inert solvent or dispersant. For this purpose, the suitable devices described above are provided in the periphery of the reactor system R. A new cycle is then started.

[0197] The great advantage of the reactor system R is that it enables the implementation of an extraordinarily large number and variety of mechanochemical processes under thermally controlled conditions. The low-temperature insulation of the reactors according to the invention shown in Figures 1 to 13 by means of ice layers

[0198] If the reactors 1 according to the invention are set to temperatures below 0°C using the thermal management system to be applied according to the invention, ice layers are allowed to form on the reactors, particularly in a humid atmosphere. This effect is advantageous because ice has very low thermal conductivity and therefore contributes to maintaining the set temperature.

Claims

[1] A single- or multi-stage mechanochemical reactor (1) selected from the group consisting of ball mills, attritor ball mills, vibrating ball mills, resonant acoustic mixers, hammer mills, impact mills, pin mills, cutting mills, jet mills and twin-shaft extruders, equipped with a self-regulating thermal management system for a temperature range of -195°C to 1000°C, wherein - the self-regulating thermal management system comprises at least one heat pipe (2), at least one flat heat pipe (3) or at least one heat pipe (2) and at least one flat heat pipe (3) and at least one heat source (4) and at least one heat sink (5) which are in thermally conductive contact with each other, - that at least one heat pipe (2) and / or at least one flat heat pipe (3) is or are attached in and / or to at least one static component (1.1) of the reactor (1) and is or are in thermally conductive contact with the material to be ground (1.2) or the material to be ground (1.2) and the grinding media or grinding balls (1.4) in at least one grinding chamber (1.3) of the at least one reactor (1) and - that at least one static component (1.1) serves as a heat source (4) or as a heat sink (5) for the at least one heat pipe (2) and / or the at least one flat heat pipe (3). [2] Single- or multi-stage mechanochemical reactor (1) according to claim 1, characterized by , that at least one static component (1.1) - a reactor wall (1.1) that encloses the grinding chamber (1.3) and has at least one bore (1.1.8) for receiving at least one heat pipe (2) and / or at least one recess (1.1.1) for receiving at least one flat heat pipe or vapor chamber (3), - at least one thermally, mechanically and chemically stable, heat-conducting round rod (1.1;1.8) arranged in the grinding chamber (1.3) with at least one bore (1.1.8) for receiving at least one heat tube (2) or - a static pin plate (1.1) with at least one bore (1.1.8) for receiving at least one heat pipe (2). [3] Single- or multi-stage mechanochemical reactor (1) according to claim 1 or 2, characterized by , that the at least one static component (1.1) is made of metals and / or metal alloys with a melting point T >1000°C, a mean coefficient of thermal expansion α <20·10 -61 / K is manufactured at temperatures from 25°C to 900°C and a thermal conductivity λ >10 W / mK and / or is coated with a ceramic of a thermal conductivity λ >10 W / mK or, in the case of a round bar, is manufactured (1.1;1.8). [4] Single- or multi-stage mechanochemical reactor (1) according to claim 3, characterized by , that the metals and / or metal alloys are selected from the group consisting of titanium, chromium, iron, manganese, tantalum, nickel, cobalt, copper, aluminum, stainless steel, copper-aluminium alloys, nickel-copper alloys, nickel-chromium alloys, cobalt-nickel-chromium-tungsten alloys, iron-nickel alloys and nickel-molybdenum alloys, and the ceramics are selected from the group consisting of sintered boron nitride, aluminum nitride and silicon carbide ceramics. [5] Single- or multi-stage mechanochemical reactor (1) according to any one of claims 1 to 4, characterized by, that the at least one static component (1.1) that comes into contact with the ground material (1.2) is coated with thermally conductive ceramics with a thermal conductivity λ >10 W / mK. [6] Single- or multi-stage mechanochemical reactor (1) according to claim 5, characterized by that the thermally conductive ceramics are selected from the group consisting of silicon carbide, aluminum nitride and boron nitride ceramics. [7] Single- or multi-stage mechanochemical reactor (1) according to any one of claims 1 to 6, characterized by , that the reactor (1) comprises at least one agitation device (1.6) selected from the group consisting of agitators, rotating pin plates, hammers, cutting tools and extruder screws made of metals and / or metal alloys with a thermal conductivity λ <10 W / mK. [8] Single- or multi-stage mechanochemical reactor (1) according to claim 7, characterized by, that the metal alloy with a thermal conductivity λ <10 W / mK is an austenitic stainless steel. [9] Single- or multi-stage mechanochemical reactor (1) according to claim 7 or 8, characterized by , that the at least one agitation agent (1.6) is coated with at least one hard ceramic having a thermal conductivity λ <5 W / mK. [10] Single- or multi-stage mechanochemical reactor (1) according to claim 9, characterized by that at least one hard ceramic is a glass ceramic and / or zirconia. [11] Single- or multi-stage mechanochemical reactor (1) according to any one of claims 1 to 10, characterized by , that the grinding media or grinding balls (1.4) consist of a high- and low-temperature resistant, impact-resistant, abrasion-resistant material of high hardness and a very high melting point. [12] Single- or multi-stage mechanochemical reactor (1) according to claim 11, characterized by, that the grinding media or grinding balls (1.4) are made of materials which also have a high thermal conductivity λ. [13] Single- or multi-stage mechanochemical reactor (1) according to claim 11 or 12, characterized by , that the grinding media or grinding balls (1.4) consist of aluminium oxide, steatite, porcelain, zirconium oxide, glass, flint, steels, chromium steels, tungsten carbide, silicon carbide, silicon nitride, cubic boron nitride or boron carbide as well as highly thermally conductive boron nitride, silicon carbide or aluminium nitride ceramics. [14] Single- or multi-stage mechanochemical reactor (1) according to any one of claims 1 to 13, characterized by, that the surfaces of the grinding media or grinding balls (1.4), and / or the reactor inner walls or the walls of the grinding chambers (1.3), the drive shafts (1.6.1) and / or the agitation means (1.6; 1.6.2; 1.6.3; 1.6.4) of the reactor (1) are doped or coated with piezoelectric materials and / or with catalytically active materials selected from the group consisting of metals, metal alloys, metal compounds and microporous and nanoporous materials. [15] Single- or multi-stage mechanochemical reactor (1) according to any one of claims 1 to 14, characterized by, that the at least one heat pipe (2) has a pipe wall (2.1), a liner or wick (2.2) or a capillary structure (2.2) and a vapor chamber (2.3) with the working medium or heat transfer medium and that the at least one flat heat pipe (3) has a chamber wall (3.1), a liner or wick (2.2) or a capillary structure (2.2), a vapor chamber (3.3) with the working medium or heat transfer medium and a support structure (3.4). [16] Single- or multi-stage mechanochemical reactor (1) according to claim 15, characterized by , that the at least one heat pipe (2) and the at least one flat heat pipe (3) are made of at least one material selected from the group consisting of thermally conductive ceramics, silicon carbide, boron nitride and aluminum nitride ceramics and metals or metal alloys with a melting point T >1000°C, a mean coefficient of linear thermal expansion α <20·10 -61 / K at 25°C to 900°C and a thermal conductivity λ >10 W(m·K). [17] Single- or multi-stage mechanochemical reactor (1) according to claim 15 or 16, characterized by that the metals or metal alloys are selected from the group consisting of titanium, chromium, iron, manganese, tantalum, nickel, cobalt, copper, aluminum, stainless steel, copper-aluminium alloys, nickel-copper alloys, nickel-chromium alloys, cobalt-nickel-chromium-tungsten alloys, iron-nickel alloys and nickel-molybdenum alloys. [18] Single- or multi-stage mechanochemical reactor (1) according to any one of claims 15 to 17, characterized by, that the insert, wick or capillary structure (2.2; 3.2) consists of materials and structures selected from the group consisting of nanoparticles, fibrous materials, nano-, meso- or microporous materials, electrically conductive and electrically non-conductive wire meshes, fiber bundles of ceramic, glass and high-temperature resistant plastics and surface structures of protrusions and depressions. [19] Single- or multi-stage mechanochemical reactor (1) according to any one of claims 15 to 18, characterized by , that the working fluid or heat transfer medium for the low temperature range is selected from the group consisting of nitrogen, methane, propane and ammonia, for the medium temperature range from the group consisting of methanol, water, aqueous salt solutions and water-toluene mixtures and for the high temperature range from the group consisting of mercury, lithium, sodium, potassium, tin and lead-bismuth eutectic. [20] Mechanochemical process for grinding materials (1.2), for the production of suspensions or slurries and for carrying out chemical reactions and syntheses under thermally controlled mechanochemical conditions, characterized by , that the milled material (1.2) or the starting materials (1.2) for the chemical reactions and syntheses or for the suspensions or slurries are filled into the milling chamber (1.3) of at least one single- or multi-stage mechanochemical reactor (1) according to one of claims 1 to 19 and milled and / or reacted therein, and the resulting milled material (1.2.1), the resulting reaction products (1.2.1), the resulting suspensions or slurries (1.2.1) or the carbonate minerals (1.2.1) formed with carbon dioxide are discharged from the milling chamber (1.3). [21] Mechanochemical process according to claim 20, characterized bythat the process is carried out continuously, discontinuously, or discontinuously in a cyclical manner. [22] Use of the single- or multi-stage mechanochemical reactor (1) according to any one of claims 1 to 19 and the mechanochemical process according to claim 20 or 21 in the fields of chemistry, biochemistry, nanotechnology, pharmaceuticals, medicine, biology and microbiology and environmental engineering. [23] Use of the mechanochemical process according to claim 20 for the grinding of materials (1.2), for the production of suspensions or slurries, for carrying out chemical reactions and syntheses and for the direct capture of carbon dioxide from gases by mineralization (Direct Gas Capture by Mechanochemical Mineralization; DGCMM) under thermally controlled mechanochemical conditions. [24] Use of the mechanochemical process according to claim 20 or 21 for the elimination of perpetual chemicals, the recycling of plastics, the depolymerization of plastics and the recovery of monomers under thermally controlled mechanochemical conditions.

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