Apparatus and method for treating raw materials, and carbon produced using said method

Abstract

The invention relates to an apparatus (1) for the material treatment of raw materials. The apparatus (1) has a heating system (2), a distillation unit (3), and a reaction unit (4), as well as a control device (15). The reaction unit (4) is designed so that it can be charged with the raw materials for treatment. The heating system (2) can be opened and closed in order to be loaded with the reaction unit (4). An exhaust gas line (11, 11a, 11b) is provided between the reaction unit (4) and the distillation unit (3) in order to discharge the exhaust gases from the reaction unit (4). The distillation unit (3) has a cooling section (12) comprising an apparatus for forced cooling. The cooling section (12) is located inside an air guide housing (12-1) for guiding ambient air via the cooling section (12) in a targeted manner and / or is formed from at least one coaxial tube for the passage of gases and a heat transfer fluid. Temperature sensors (T1, T2, T3) are provided in the region of the heating system (2) and the distillation unit (3). A suction device (14-1) is provided inside the reaction unit (4) in order to extract gases from the reaction unit (4) and generate a vacuum. The temperature sensors (T1, T2, T3) and the suction device (14-1) are connected to the control device (15). The invention also relates to: a method for operating an apparatus (1) for the material treatment of raw materials; and a carbon produced using said method.

Description

[0001] DEVICE AND METHOD FOR TREATING RAW MATERIALS AND CARBON PRODUCED BY THE METHOD

[0002] The invention relates to a device for the material treatment of raw materials. The device comprises a heating system, a distillation unit, a reaction unit, and a control device. The reaction unit can be loaded with the raw materials for treatment. The heating system can be opened and closed for loading the reaction unit.

[0003] Furthermore, the invention relates to a method for operating a device for the material treatment of raw materials and to a carbon produced by the method.

[0004] State-of-the-art devices are intended for the industrial treatment of waste rubber products, rubber goods, or rubber-like composite products, such as old tires, steel-cord-reinforced rubber belts, rubberized chain links, and conveyor belts, as well as shredded end-of-life vehicles, organic renewable raw materials such as wood, contaminated carbon, and contaminated soil. Light oil, gas, metals, especially steel, and carbon are recovered. Conventional plants, for example, are based on the use of rotary kilns, fluidized-bed reactors, and drums, and process compacted feedstock in a chemically inert atmosphere with the exclusion of oxygen.

[0005] DE 199 30 071 C2 describes a process and device for the recycling of organic materials and mixtures of materials. The organic material is brought into contact with fluidized bed material from the combustion fluidized bed. The process produces end products in the form of gases with condensable substances and carbonaceous residues.

[0006] DE 44 41 423 A1 discloses a process and apparatus for extracting usable gas from waste. The shredded waste is placed in a gas-tight drum. Gas is generated in the drum and separated from the simultaneously formed residue. The generated gas is cracked into a cracked gas in a gas converter with the addition of air and in the presence of a glowing coke bed. The heat required in the process is transferred by a gas in direct contact with the material to be recycled. A partial stream of the cracked gas exiting the gas converter is used to transfer the heat to the gas.

[0007] DE 40 11 945 C1 describes a process for degassing organic substances, such as household or industrial waste, in a heatable chamber. In this process, the starting materials are introduced into the chamber under compression and pass through the chamber cross-section while maintaining their compressed state. Heat is supplied via the chamber walls, which are in pressure contact with the compressed material. The resulting gaseous products are discharged at increased pressure. The chamber is sealed gas-tight in its feed area by the compressed material. By further compacting the solid residues, increased flow resistance is achieved in the outflow area of ​​the gaseous products.

[0008] DE 39 32 803 A1 discloses a reaction process for converting organic materials into coal and graphite by adding boric acid / boron oxide and organic nitrogen compounds in a non-oxidizing atmosphere. Operating conventional plants requires increased expenditures for materials, energy, and logistics. For example, generating a fluidized bed in fluidized-bed reactors requires increased energy expenditure. This is because, on the one hand, the fluidized bed must be generated and maintained, and, on the other hand, the materials to be recycled must be mechanically processed so that they effectively contact the fluidized bed. The comminution or compaction of the starting materials during preparation and the recycling process also incurs high energy costs.

[0009] WO 2007 / 053088 A1 describes a method and apparatus for treating hydrocarbon materials. The materials are charged into an inner container, which in turn can be arranged in an outer container. Both containers are each sealed with a lid element. The hydrocarbon material is heated using microwaves or high-frequency radiation. The resulting exhaust gases are removed from the containers through a gas outlet. Two or more containers can be operated in parallel and connected to a gas purification system to maintain a virtually continuous gas flow through the gas purification system.

[0010] WO 2010 / 012275 A2 discloses a device for treating materials with a cylindrical furnace, as well as a process control system. The inner surfaces of the furnace are provided with an insulating layer made of an inorganic thermal insulation material. Heating elements are arranged on or at the inner surfaces of the insulating layers. Controlling the process by regulating the temperature of the heating elements ensures a high yield of carbon, oil, and fuel gas. DE 10 2012 109 874 A1 describes a device for the material treatment of raw materials, comprising a heating system, a distillation unit, and a reaction unit capable of being fed with the raw materials, as well as a method for operating such a device. The heating system, which can be opened and closed for fitting the reaction unit, has a head element and a jacket element firmly connected to the head element, as well as support elements.The head element is connected to the support elements, which are adjustable in length in the vertical direction, in such a way that by changing the length of the support elements between two end positions, the heating system is opened and closed in the vertical direction of movement.

[0011] The object of the present invention is to provide an improved device and a method for treating various waste rubber products, in particular waste tires and rubber composite products or rubber-like composite products, renewable raw materials such as wood, shells or fruit, electronic waste such as computers and mobile phones, motor vehicles and storage media such as batteries, as well as contaminated carbon. The composite products are to be separated, and valuable components such as carbon, light oil, gases, and optionally metallic materials are to be recovered. The contaminated carbon is to be separated from the respective contaminants. The device is to be operated cost-effectively with minimal energy consumption, and the method is to be carried out with minimal effort, particularly time expenditure.The raw materials recovered using the process should retain their original structure as unchanged as possible so that they can be returned to their original use, for example. In addition, the carbon recovered using the process should have advantageous material properties that differ from conventional carbons. This object is achieved by a device according to the invention for the material treatment of raw materials. The device has a heating system, a distillation unit, a reaction unit, and a control device. The reaction unit can be charged with the raw materials. The heating system can be opened and closed for loading with the reaction unit. An exhaust line for discharging the exhaust gases from the reaction unit is formed between the reaction unit and the distillation unit. The distillation unit has a cooling section.

[0012] According to the concept of the invention, temperature sensors are provided in the area of ​​the heating system and the distillation unit. Furthermore, the cooling section of the distillation unit has a device for forced cooling. The device for forced cooling of the cooling section enables a heat transfer fluid—particularly gaseous or liquid—to flow against or around the cooling section in a targeted manner, in comparison to, for example, free convection. The cooling section is arranged within an air guide housing for the targeted conduction of ambient air over the cooling section and / or is formed from at least one coaxial tube for conducting gases inside an inner tube and for conducting a heat transfer fluid in the space between the outside of the inner tube and the inside of the outer tube. The coaxial tube can, in particular, be double-walled.The heat transfer fluid is preferably in the liquid state and can specifically be water or glycol.

[0013] The device for the material treatment of raw materials comprises an extraction device for extracting gases from the reaction unit and generating a negative pressure within the reaction unit. The negative pressure refers to the pressure in the environment surrounding the device. The extraction device can be designed as a pump, in particular as a diaphragm pump. According to the invention, the temperature sensors and the extraction device are connected to the control device.

[0014] According to a further development of the invention, at least two of the temperature sensors for determining the temperature within the reaction unit are arranged in an intermediate space formed between the reaction unit and a jacket element of the heating system when the heating system is closed.

[0015] According to an advantageous embodiment of the invention, the exhaust line between the heating system and the distillation unit has a heating device for heating the exhaust line. The heating device, which preferably completely encloses the exhaust line and is advantageously electrically operated, is connected to the control device.

[0016] At least one temperature sensor for determining the temperature of exhaust gases discharged from the heating system is preferably provided on the exhaust gas line between the heating system and the distillation unit.

[0017] A connecting element for connecting to a device for introducing a gaseous purge medium, particularly into the reaction unit, can be provided on the exhaust line between the heating system and the distillation unit. The purge medium, for example, nitrogen, serves to inertize the reaction unit, reduces the risk of explosion, and, as a carrier gas, supports the separation of end products generated during operation of the device.

[0018] Within a wall of the air guide housing, in which the cooling section of the distillation unit can be arranged, fans are advantageously provided for the targeted guidance of ambient air over the cooling section. The air guide housing, together with the fans, is designed as a device for forced cooling of the cooling section of the distillation unit with ambient air. The fans are connected to the control device.

[0019] The fans formed within the wall of the air guide housing of the cooling section of the distillation unit for the targeted guidance of ambient air over the cooling section are preferably arranged on an upper side, in particular on an end face pointing upwards in a vertical direction, or on a side surface of the air guide housing.

[0020] An advantage of the invention is that the extraction device for extracting gases from the reaction unit and generating a negative pressure within the reaction unit is arranged downstream of an oil tank located downstream of the distillation unit, in the direction of gas flow. Thus, the negative pressure is also generated within the distillation unit.

[0021] According to a further preferred embodiment of the invention, the heating system comprises a head element and a casing element rigidly connected to the head element, as well as support elements. The head element is mounted on support elements whose length can be adjusted vertically. By changing the length of the support elements between two end positions, the heating system is opened and closed in the vertical direction of movement.

[0022] The heating system preferably has two support elements, which are preferably arranged on either side of the heating system. According to a first alternative, the support elements are driven by electric spindles. According to a second alternative, the support elements are designed as hydraulic supports.

[0023] According to a further development of the invention, the casing element is formed with a hollow cylindrical wall. The wall is vertically open downwards and closed at the top with a circular hood. The casing element is connected to the head element at the hood to form a single unit.

[0024] The casing element advantageously has heating elements evenly distributed around the circumference of the inner surface of the wall. The wall is provided with thermal insulation made of ceramic powder to prevent heat transfer to the outside environment.

[0025] According to a further advantageous embodiment of the invention, the hood is provided with an exhaust pipe at its center point, connecting to an exhaust pipe of the heating system. The exhaust pipe extends from the exhaust pipe through the hood into the head element of the heating system.

[0026] The exhaust line advantageously has a connecting element at the distal end to the exhaust nozzle of the hood as a connection to the exhaust line of the distillation unit.

[0027] The exhaust pipe extending from the exhaust nozzle through the hood into the head element of the heating system can be designed in the area of ​​the exhaust nozzle with a pipe connection that is automatically adjustable in length, particularly in the vertical direction, to compensate for thermal expansion.

[0028] A further advantage of the invention is that the reaction unit is designed with a wall in the form of a hollow cylindrical vessel, which is sealed at the bottom. The open side of the wall can be closed by means of a lid element.

[0029] A high-temperature-resistant seal is advantageously arranged between the wall and the cover element.

[0030] The cover element of the reaction unit is preferably circular and has the exhaust outlet at its center. A particular advantage is that the exhaust outlet of the cover element and the exhaust outlet of the casing element interlock when the heating system is closed, forming a tight connection to the exhaust line.

[0031] The cover element of the reaction unit can be designed with a connecting piece for connection to a device for admitting a gaseous flushing medium, in particular nitrogen, into the reaction unit.

[0032] The reaction unit may have sieve elements inside, which are preferably aligned horizontally and spaced apart from one another at different heights. The sieve elements preferably cover the entire cross-section of the reaction unit.

[0033] The control device of the device for the material treatment of raw materials serves to control a method for operating the device according to the design and, in addition to the temperature sensors, the device for forced cooling, in particular the conveying devices, such as the fans for the targeted conduction of ambient air over the cooling section or at least one pump for conveying the liquid heat transfer fluid, and the suction device, is advantageously also connected to a drive of the support elements, a fill level sensor of the oil tank, a pressure sensor, and valves of heating circuits of the heating system. The fill level sensor of the oil tank can be designed as a float. The pressure sensor is advantageously arranged in the region of the oil tank. The control device can also be connected to an oil conveying device for sucking the oil out of the oil tank, in particular a piston pump.In response to a signal sent from the oil tank's fill level sensor to the control device, the oil pumping device is activated and oil is pumped from the oil tank. This object is also achieved by a method according to the invention for operating the device for the material treatment of raw materials. The method comprises the following steps:

[0034] - Feeding a reaction unit with raw materials,

[0035] - Preheating of the reaction unit,

[0036] - opening a heating system and placing the reaction unit into the heating system, in particular onto a floor element of the heating system,

[0037] - Closing the heating system so that the reaction unit is located in a closed room,

[0038] - heating the reaction unit and starting a carbonisation and distillation process, wherein the carbonisation and distillation process is carried out by targeted heating at a substantially constant reaction temperature within the reaction unit, wherein the temperature is determined,

[0039] - discharging gases produced from the reaction unit into a distillation unit through an exhaust gas line formed between the reaction unit and the distillation unit and determining the temperature of the gas flowing through the exhaust gas line,

[0040] - Cooling and condensing the gases in the distillation unit, whereby the temperature of the gases is controlled by forced cooling of a cooling section of the distillation unit via a heat output dissipated by the gases,

[0041] - Introducing the distillation products into an oil tank and separating oil,

[0042] - Extraction of non-condensable gases from the oil tank, whereby a negative pressure is created within the reaction unit to the environment and oxygen is removed from the reaction unit,

[0043] - Opening the heating system and removing the reaction unit from the heating system,

[0044] - Cooling the reaction unit, removing the end products from the reaction unit and separating the end products and

[0045] - Removing the final products from the oil tank. Targeted heating means that the reaction unit located within the heating system is heated during the carbonization and distillation process in such a way that the reaction temperature within the reaction unit, also referred to as the process temperature, remains essentially constant and only varies within a specified temperature range. The reaction temperature is continuously monitored. The temperature value is transmitted to the control device, which controls the opening and closing of the valves of the heating circuits of the heating system, and thus the firing, according to a specified temperature setpoint.

[0046] When closing the heating system, an exhaust port of the reaction unit is preferably coupled to an exhaust port of an exhaust line of the heating system, and the exhaust line of the heating system and an exhaust line of the distillation unit are coupled to one another at a connecting element, thus establishing a gas-tight connection between the reaction unit and the distillation unit. The heating system is advantageously opened and closed by extending and retracting support elements.

[0047] According to a further development of the invention, by sucking out non-condensable gases from the oil tank and thus generating the negative pressure, the absolute value of the pressure within the reaction unit is set in the range from 2 mbar to 10 mbar, in particular of approximately 4 mbar.

[0048] To cool and condense the gases in the distillation unit, ambient air can be specifically directed over the cooling section of the distillation unit, or a liquid heat transfer fluid, in particular water as a coolant, can flow through the cooling section. According to an advantageous embodiment of the invention, during the process of cooling and condensing the gases in the distillation unit, the temperature of the gases is set to a value in a range of 95 °C to 125 °C, in particular via a volume flow of the ambient air or a fan power or a mass flow of a heat transfer fluid. The volume flow of the ambient air or the mass flow of the heat transfer fluid ensures the heat to be dissipated by the cooling section and cools the cooling section.The temperature of the gases is determined in the exhaust gas line formed between the heating system and the distillation unit, in particular the at least one temperature sensor for determining the temperature of exhaust gases discharged from the heating system.

[0049] An advantage of the invention is that during the carbonization and distillation process, an exhaust gas line formed between the reaction unit and the distillation unit is heated, in particular to a temperature in the range of 120 °C to 160 °C, specifically to avoid premature condensation of the exhaust gas before entering the distillation unit and consequently clogging of the exhaust gas line.

[0050] The reaction unit is preferably removed from the heating system at a temperature of the gas flowing through the exhaust line of approximately 60 °C.

[0051] According to a further preferred embodiment of the invention, a gaseous flushing medium, in particular nitrogen, is introduced into the reaction unit during the carbonization and distillation process or during the cooling process of the reaction unit.

[0052] Purging is preferably carried out at time intervals, particularly to remove higher-molecular-weight gases from the reaction unit. Purging with an inert gas, such as nitrogen, removes undesirable components, such as polyaromatic constituents of polybutadiene or plasticizers, from the reaction unit, particularly during the carbonization and distillation processes. The extraction of non-condensable gases and thus the generation of the negative pressure within the reaction unit, as well as the inflow of the purging medium into the reaction unit, are advantageously carried out at staggered times. Especially during the cooling process of the reaction unit, the purging medium can be introduced into the reaction unit periodically for a duration of two to three minutes.

[0053] After cooling the reaction unit, the reaction unit is opened to remove the end products, preferably at a temperature inside the reaction unit in the range of 20 °C to 60 °C, in particular in the range of 30 °C to 60 °C. During the process of removing the end products from the reaction unit, the reaction unit is advantageously pressurized with the gaseous flushing medium, especially nitrogen.

[0054] During the process of removing the end products from the reaction unit, carbon can be extracted as an end product.

[0055] According to a further development of the invention, extracted non-condensable gases are fed to the heating system for combustion within the heating system and thus for heating the reaction unit and / or to a combined heat and power plant for generating thermal energy and electrical energy.

[0056] The process is preferably operated modularly with at least four reaction units simultaneously and the following steps:

[0057] - feeding a first reaction unit while a second reaction unit, which is already fed, is preheated, - feeding a third, fed and preheated reaction unit to the heating system and heating the reaction unit to carry out the carbonisation and distillation process and

[0058] - Cooling and emptying a fourth reaction unit in which the carbonization and distillation process is completed.

[0059] According to a further development of the invention, the reaction unit is charged with raw materials with a mass in the range of 2.5 t to 3 t. The reaction unit advantageously remains in the heating system for a period in the range of approximately 2.5 h to 3.5 h. The reaction temperature within the reaction unit is preferably between 350 °C and 800 °C, in particular 550 °C.

[0060] The energy consumption for one process run with a reaction unit, particularly one equipped with used tires, amounts to 60 kWh to 80 kWh. With twelve reaction units and nine runs per day, this results in a daily energy requirement of 6,480 kWh to 8,640 kWh. With an average of 223 production days per year, the annual energy requirement is therefore between 1,445 MWh and 1,927 MWh. In contrast, the energy generated for electricity and heat amounts to approximately 10.5 MWh per year.

[0061] The method according to the invention is based on a carbonization-distillation process, so that the device according to the invention is a carbonization-distillation industrial module, also referred to as a VDI module.

[0062] To effectively implement the process, the device was designed with modules to optimize or maximize throughput and adapt to current needs. Further advantages of the device and method according to the invention over the prior art can be summarized as follows:

[0063] • no pre-sorting of raw materials,

[0064] • Treatment of starting products, in particular

[0065] - waste rubber products, such as old tires, rubberized chain links, steel-cord reinforced rubber belts and conveyor belts, where the products can be treated in their essentially original form in order to preserve their structure, i.e., for example, they cannot be crushed or shredded, and thus cannot be crushed or compacted,

[0066] - organic and renewable raw materials, for example wood in all forms, especially beech and oak, bamboo as well as shells and fruits, such as coconut shells and orange peels,

[0067] - animal waste, such as bones and carcasses,

[0068] - contaminated carbon,

[0069] - contaminated soil or other materials, for example after oil spills,

[0070] - essentially unshredded or undismantled and thus complete end-of-life vehicles and

[0071] - Carbon composite materials, especially with carbon fibers, especially from the automotive industry,

[0072] • ecological, economical and carbon dioxide-free and therefore sustainable technology with very low energy consumption.

[0073] The various process parameters, such as temperatures and the duration of the process, as well as the flushing with gaseous flushing medium, and the associated performance of individual components, such as the heating system, the conveying devices, the device for forced cooling of the distillation unit, such as the fans or the at least one pump, and the suction device, depend on the raw materials to be treated within the reaction unit. Thus, the processes or devices can be controlled with the corresponding parameters stored in the control device.

[0074] Control programs as follows: a) Device and method for the material treatment of tires, b) Device and method for the material treatment of rubberized chain links, c) Device and method for the material treatment of conveyor belts, d) Device and method for the material treatment of

[0075] Complete vehicles or shredded vehicles from the automotive industry, e) Device and method for the material treatment of renewable raw materials such as wood and bamboo, as well as biowaste such as coconut shells and orange peels, f) Device and method for the material treatment of animal waste, g) Device and method for the material treatment of bitumen or asphalt, h) Device and method for the material treatment of energy storage devices, in particular batteries, specifically from the automotive industry, i) Device and method for the material treatment of electronic components such as computers, mobile phones, laptops and smartphones, and j) Device and method for the material treatment of contaminated carbon and soils contaminated with pollutants to reactivate the carbon.

[0076] Depending on the raw materials to be treated, the raw materials must be mixed advantageously in certain ratios within the reaction unit, for example tires and batteries, in order to influence process parameters or end products.

[0077] 1 Ground to particle size <0.1 mm - results of head space GC-MS screening and thermogravimetry results 2 Thermogravimetry TGA, GC-MS screening results

[0078] Trace elements using ICP OES according to HN03 / HF acid digestion - SOP 671 (679) The recovered raw materials in mg / kg are listed in the table above. The third and fourth columns list the raw materials obtained using a device and process as per h), the fifth column lists the raw materials obtained using a device and process as per i), the sixth and seventh columns list the raw materials obtained using a device and process as per d), and the eighth column lists the raw materials obtained using a device and process as per a).

[0079] In the process according to h), whose raw materials are listed in the fourth column of the table, battery blocks, also known as energy blocks, from the automotive industry with a mass of 500 kg and scrap tires with a mass of approximately 500 kg were used as starting materials. Before the process, the steel casings, including screws, with a mass of approximately 60 kg were removed from the battery blocks, and the remaining 440 kg of starting material was layered on a separate sieve to prevent the battery blocks from mixing with the scrap tires within the reaction unit. The residues of the processed battery blocks removed from the reaction unit at the end of the process had a mass of 220.9 kg and were shredded to a uniform size in the range of 0.2 mm to 0.5 mm for further analysis.The analytical data listed in the table shows that all inorganic or metallic components of the battery blocks are detected with a recovery rate of over 98.5%. The metals and inorganic components, such as cobalt, nickel, magnesium, copper, niobium, and lithium, can be recovered through proven metal refining processes.

[0080] In the process according to i), whose raw materials are listed in the fifth column of the table, the starting materials used were electronic waste, such as televisions, drills, and cables, with a mass of 500 kg, electronic waste, such as computers in the form of laptops and mobile phones, with a mass of 15 kg, and scrap tires with a mass of approximately 500 kg. The computers and mobile phones were placed separately in a metal box in the reaction unit to avoid mixing with the other starting materials. The residues of the processed computers and mobile phones, removed from the metal box at the end of the process, had a fixed mass of 7.7 kg and were shredded to a uniform size in the range of 0.1 mm for further analysis.Optical emission analysis revealed a high recovery rate for metals such as cobalt, chromium, lithium, nickel, cadmium, tantalum, gallium, germanium, manganese, rhenium, strontium, and zirconium, which can be recovered through proven metal refining processes. A recovery rate or utilization rate of 98% was observed.

[0081] In the process according to d), whose raw materials are listed in the sixth column of the table, a complete Smart vehicle with a mass of 750 kg was used as the starting material for the process. Before the process, only the liquids, such as the coolant and brake fluid, the engine oil and gasoline, as well as the battery, were removed. The solid residues of the processed complete vehicle, removed from the reaction unit after the end of the process, had a mass of 450 kg. This mass was composed of 30% carbon and 70% metals, such as steel, spring steel, and precious metals. In addition, approximately 250 kg to 270 kg of light oil were recovered. The proportion of residual gas was approximately 6% to 8%. This results in a recovery rate or utilization rate of 95%.

[0082] For samples of rapeseed - unmilled or milled - carbon contents between 98.8% and 99.8% are determined using the method according to DIN / EN 12879, while for samples of rapeseed pellets turned into soot, carbon contents in the range of 79.7% to 81.0% are determined using the same method, for samples of plastic bottles a carbon content of 99.1%, for samples of oak wood a carbon content of 98.5%, for samples from industrial waste a carbon content of 99.4% and for samples from rubber waste a carbon content of 99.4%. For samples of rapeseed pellets turned into oil, a carbon content of 99.5% is determined.

[0083] The carbon, hydrogen, and nitrogen content is determined according to ASTM D5291, and the oxygen content is determined using a method based on ASTM D5622, each using the VARIO EL Cube from Elementar. The fluorine and chlorine content are determined using pyrolysis ion chromatography with the Analytik Jena combustion module, the 920 absorption module, and the 930 Compact IC Flex ion chromatograph, respectively.

[0084] Evaporable components up to 200 °C are determined by head space GC-MS screening with Trace GC Ultra in conjunction with a DSQ II mass spectrometer from Thermo Scientific.

[0085] Hydrofluoric acid and nitric acid are determined by microwave digestion for ICP OES with oven model StarT from MWS Gmbh, while trace elements, especially inorganic components, are determined by ICP OES with ICP OES Arcos from Spectro.

[0086] Thermogravimetric analyses are performed using Hi-Res TGA 2950 from TA Instruments.

[0087] Further key advantages include the fact that steel-rubber composites, which previously required high energy expenditure to separate, can now be separated without significant external energy consumption. The resulting products can be recycled for high-quality use in the spirit of an efficient circular economy, which contributes to conserving resources. The resulting products include:

[0088] • light oil, for example with a density of about 927 kg / m 3 at 15 °C, a viscosity of 4.74 mm 2 / s and a flash point below 21 °C,

[0089] • Gas, • Metals, mainly steel or iron and titanium, as well as

[0090] • Amorphous, inorganic carbon or carbon agglomerates.

[0091] The amorphous, inorganic carbon produced by the method according to the invention for operating a device for the material treatment of carbon-containing raw materials has, according to the concept, a structure of a three-dimensional arrangement of carbon nanoparticles as agglomerates and, depending on the starting raw materials, advantageously has a purity in the range of 95% to 99.9%. The carbon nanoparticles are cross-linked without long-range order, do not exhibit a large-scale graphitic arrangement, and are not arranged as nanotubes.

[0092] The carbon formed with the structure of three-dimensionally arranged nanoparticles is produced industrially using the device and method according to the invention and thus offers a significant economic advantage over prior art carbons obtained or produced in the laboratory. The purity of the carbon is significantly influenced by purging with a gaseous purge medium, particularly during the carbonization and distillation processes, or during the cooling of the reaction unit.

[0093] Depending on the raw materials, the carbon produced during the process for operating the device for the material treatment of raw materials preferably has a BET surface area determined using the method according to DIN ISO 9277 of greater than 2,500 m 2 / g BET, especially up to 9,500 m 2 / g BET, especially larger than 3,500 m 2 / g BET or greater than 4,000 m 2 / g BET, especially in the range of 4,200 m 2 / g BET up to 4,500 m 2 / g BET, and thus a very high adsorption capacity without releasing substances into the environment. This means that the environment is not polluted, for example, by leaching. The carbon produced by the process according to the invention preferably has a density of approximately 66 kg / m 3 and can advantageously be designed with a greater tensile strength than alloyed steel.

[0094] The carbon obtained in this way can have an electrical conductivity in the range of 4.5-10 7 sqm up to 5.8- 10 7 Qm. Electrical conductivity is determined using the method according to DIN EN ISO 15091.

[0095] The carbon produced in the process according to the invention for operating the device for the material treatment of raw materials is insoluble in concentrated or dilute cold acids, such as sulfuric acid, nitric acid, and hydrochloric acid, and is not attacked by alkalis. Nitric acid spontaneously decomposes into water and nitrous gases, which may indicate a catalytic effect. Neither polar organic solvents nor nonpolar solvents can dissolve the carbon.

[0096] The recovered light oil is used, for example, in the chemical industry, particularly as a raw material for basic chemicals, and in the pharmaceutical industry to generate thermal and electrical energy, for example, using a combined heat and power plant. The gas can be used to generate thermal and electrical energy, for example, using a gas turbine and generator, or for recycling and use in the process. The recovered metals, such as steel, can be returned to the steel industry – very low process temperatures allow metals to retain their physical and chemical properties.

[0097] Further details, features, and advantages of the invention will become apparent from the following description of exemplary embodiments with reference to the accompanying drawings. Figure 1: Carbonization-distillation industrial module as a device for the material treatment of raw materials in the opened state, in a front view.

[0098] Figure 2a: Carbonization-distillation industrial module as a device for the material treatment of raw materials in a closed state in side view and

[0099] Figure 2b: front view,

[0100] Figure 3: Sectional view of the heating system in open state,

[0101] Figure 4: Sectional view of the heating system in closed state,

[0102] Figure 5: Base element of the heating system,

[0103] Figure 6: Distillation unit,

[0104] Figure 7: Oil tank and

[0105] Figure 8a: Reaction unit in closed state and

[0106] Figure 8b: Sectional view of the reaction unit in closed state,

[0107] Figures 9a to 9n: microscopic images of carbon produced by the device for the material treatment of raw materials and

[0108] Figures 9p and 9q: Results of Raman spectroscopy of carbon.

[0109] Figures 1, 2a, and 2b depict a carbonization-distillation industrial module as a device 1 for the material treatment of raw materials. Figure 1 shows the device 1 in the open state in a front view, while Figure 2b shows the device 1 in the closed state in a front view, and Figure 2a shows it in a side view.

[0110] The device 1 comprises a heating system 2 and a distillation unit 3. The reaction unit 4, which is charged with raw materials, is preheated to a specific temperature in a preheating device (not shown) and then further heated in the heating system 2. The reaction unit 4 can be charged with a mixture of different raw materials, so pre-sorting of the products is not necessary. After preheating, the reaction unit 4 is transferred into the open heating system 2 and positioned on the base element 5 of the heating system 2.

[0111] The head element 7 and the casing element 8 of the heating system 2, which is firmly connected to the head element 7, are movably mounted in the direction of movement B by means of support elements 6 arranged on both sides of the heating system 2. The support elements 6 are spaced approximately 2.9 m apart. The casing element 8 has an outer diameter of approximately 2.5 m.

[0112] In the first end position according to Figure 1, the support elements 6 are extended. The device 1 has a height of approximately 6.70 m. The head element 7 and the casing element 8 provide space for equipping the heating system 2 with the reaction unit 4. The heating system 2 is open. The reaction unit 4 can be inserted into the heating system 2 or removed from the heating system 2. The movement of the reaction unit 4 can advantageously take place by means of a rail system (not shown) on which the reaction unit 4 rests. In the second end position according to Figures 2a, 2b, the support elements 6 are retracted. The device 1 has a height of approximately 3.70 m.

[0113] The casing element 8 sits on the base element 5 such that the reaction unit 4 is positioned in an enclosed space. The heating system 2 is closed. The reaction unit 4 is surrounded at the bottom by the base element 5 and at the sides and top by the casing element 8.

[0114] The device 1 has temperature sensors T1, T2, T3 in the area of ​​the heating system 2 and the distillation unit 3 for determining specific process temperatures. At least two temperature sensors T2, T3 are arranged in a gap formed between the reaction unit 4 and the casing element 8 when the heating system 2 is closed. The temperature sensors T2, T3 are positioned, for example, projecting approximately 1 cm from the inside of the casing element 8 into the approximately 8 cm wide gap. The temperature sensors T2, T3 are arranged spaced apart from one another in the vertical direction in order to determine local temperature values ​​or an average temperature within the gap. The temperature values ​​determined by the temperature sensors T2, T3 are used to determine the temperature within the reaction unit 4.

[0115] The heating system 2 has a housing 9 in the lower area. The housing 9, which encloses the base element 5 and the side surfaces of the casing element 8 when the heating system 2 is closed, is opened to equip the heating system 2.

[0116] The gases produced during the carbonization process are removed from the heating system 2 through the provided exhaust line 11 and cooled by the process. The gases are conducted to the distillation unit 3 through the exhaust nozzle 10a formed at the uppermost point of the reaction unit 4 and the exhaust line 11 arranged in the head element 7. The gases then flow through the cooling section 12 of the distillation unit 3. The cooling section 12 is formed from tubes as shown in Figures 1, 2a, and 2b. The tubes, which are inclined to the horizontal, are provided with fins to increase the heat transfer surface and thus improve heat transfer. The heat is transferred from the gases to the ambient air.

[0117] To further increase the heat transfer from the gases to be cooled to the ambient air, and specifically to improve temperature control of the gases flowing through the cooling section 12 of the distillation unit 3, the cooling section 12 is surrounded by an air guide housing 12-1. Fans 12-2 are arranged on the upper side, in particular on the vertically upward-facing end face of the air guide housing 12-1, which fans draw the ambient air evenly through the air guide housing 12-1 as cooling air. Alternatively, the fans can also be arranged on a side surface of the air guide housing 12-1. In this case, the ambient air is directed in a targeted manner over the cooling section 12. A further temperature sensor T1 is arranged on the exhaust gas line 11 formed between the heating system 2 and the distillation unit 3 in order to determine the temperature of the exhaust gases discharged from the heating system 2.

[0118] According to an alternative embodiment, the gases within the cooling section can also be cooled with a heat transfer fluid other than air, for example, water. Instead of tubes with fins formed on the outer surface, the cooling section is constructed of coaxial tubes. The gases flow inside the inner tube, while the preferably liquid heat transfer fluid is passed through the space between the outside of the inner tube and the inside of the outer tube.

[0119] The cooling section 12 is designed with two parallel pipes. The gases are divided into two partial mass flows before entering the cooling section 12 and are mixed again after flowing through the cooling section 12.

[0120] The distillation products are then fed into an oil tank 13. The oil obtained from the carbonization process and the subsequent distillation, which corresponds to a light oil in its consistency and composition and is very similar to the intermediate products of crude oil processing, settles in the oil tank 13. The non-condensable portion of the gas is discharged from the oil tank 13. With a capacity of approximately 1,000 liters, the oil tank 13 also serves as an expansion vessel for the device 1.

[0121] Arranged on the oil tank 13 are a suction device 14-1, in particular a pump, specifically a diaphragm pump, for sucking the gases over the surface of the oil accumulating within the oil tank 13, and an oil conveying device 14-2, in particular a pump, specifically a piston pump, for conveying the oil out of the oil tank 13. By sucking out the gases, a negative pressure is generated within the cooling section 12 of the distillation unit 3, the exhaust line 11, and specifically within the reaction unit 4. The suction device 14-1 also specifically sucks out the air, and thus the oxygen as a component of the air, from the reaction unit 4. A vacuum can thus be generated within the reaction unit 4.

[0122] The gases extracted from the surface of the oil accumulating within the oil tank 13 can be used to generate thermal energy and electrical energy directly in a combined heat and power plant, referred to as CHP for short.

[0123] The device 1 is also designed with a control device 15 for controlling the method for operating the device 1. The control device 15 determines and displays, for example, the fill level within the oil tank 13, the flow of oil or gas, and a possible defect in a line of the device 1. The control device 15 is connected to corresponding sensors. The temperature sensors T1, T2, T3 are also coupled to the control device 15. The values ​​determined by the temperature sensors T1, T2, T3 are used to control the device 1, in particular the heating system 2 and thus the heating of the reaction unit 4 as well as the fans 12-2 of the cooling section 12 and the extraction device 14-1. The control device 15 can be used to display, among other things, the status of various heating circuits of the heating system 2 as well as process temperatures.Likewise, the arrangement of the casing element 8 of the heating system 2 can be determined and displayed in the open, closed, and partially open states. The control device 15 thus also serves to extend and retract the support elements 6 to open and close the heating system 2.

[0124] Figures 3 and 4 each show a sectional view of the heating system 2. In Figure 3, the heating system 2 is shown in the open state and in Figure 4 in the closed state.

[0125] According to Figure 3, the support elements 6 are fully extended. The head element 7 arranged at the upper ends of the support elements 6 and the casing element 8 firmly connected to the head element 7 are arranged at a height H above the base element 5 such that the reaction unit 4 is freely movable in the horizontal direction between the base element 5 and the casing element 8.

[0126] The casing element 8 is movably supported in the lower area against the support elements 6. The lateral support against the support elements 6 ensures a straight movement of the casing element 8 in the direction of movement B between the end positions. Tilting of the casing element 8 is avoided.

[0127] The casing element 8 has heating elements 16a evenly distributed around the circumference of the inner surface of the casing. The heating elements 16a are arranged essentially vertically and are guided through the wall to the inner surface in the lower region of the casing element 8. The heating elements 16a are each formed from two vertically aligned sections, which are connected to each other at the upper end by a deflection element.

[0128] The casing element 8, which opens vertically downwards, is closed at the top with a hood 17 and fastened to the head element 7. The head element 7 and the casing element 8 form a coherent unit. The hood 17 is formed at its center with an exhaust nozzle 10b as a connection to the exhaust line 11a. The exhaust line 11a extends from the exhaust nozzle 10b through the hood 17 into the head element 7. The passage of the exhaust line 11a through the hood 17 is sealed to the hood 17. In the region of the exhaust nozzle 10b, the exhaust line 11a is formed with a pipe connection 19 that is adjustable in length in the vertical direction, for example in the form of a telescopic pipe. The pipe connection 19, which is automatically adjustable in length, serves to compensate for thermal expansion of the reaction unit 4, in particular with respect to the casing element 8 and the hood 17 of the heating system 2.

[0129] The exhaust line 11a is designed as a transition from the reaction unit 4 to the distillation unit 3 with a heating device 20. The electrically operated heating device 20, which surrounds the exhaust line 11a, is connected to the control device 15, as is the temperature sensor T1.

[0130] In addition, the exhaust line 11a has a connecting element 11-1 for connecting the exhaust line 11a to a device for admitting a gaseous purging medium, for example, nitrogen. The purging medium can flow into the exhaust line 11a and in particular into the reaction unit 4 via the connecting element 11-1. The connecting element 11-1 is arranged between the pipe connection 19 and the region of the exhaust line 11a enclosed by the heating device 20, specifically at the vertically highest point of the exhaust line 11, 11a.

[0131] The exhaust line 11a has a connecting element 18 at the distal end, starting from the exhaust nozzle 10b. The connecting element 18, which is advantageously designed as a quick-action coupling, serves to connect the exhaust line 11a of the heating system 2 to the exhaust line 11b of the distillation unit 3 when the heating system 2 is closed, as shown in Figure 4. Due to the downward movement of the head element 7 when the heating system 2 is closed, the exhaust lines 11a, 11b are coupled to the connecting element 18, as well as the exhaust nozzles 10a, 10b, so that a gas-tight connection from the reaction unit 4 to the distillation unit 3 is established.

[0132] The reaction unit 4 arranged on the base element 5 is formed with a wall 21 in the form of a hollow cylindrical vessel with an outer diameter of approximately 1.8 m, which is closed at the base. The open side of the wall 21 can be closed by means of a cover element 22. A seal is arranged between the wall 21 and the cover element 22, so that the reaction unit 4 is tightly sealed. Sieve elements 23 are formed inside the reaction unit 4. The sieve elements 23 are aligned horizontally and arranged at different heights, spaced from one another.

[0133] In the second end position shown in Figure 4, the support elements 6 are fully retracted. The casing element 8 sits on the base element 5 and completely encloses the reaction unit 4. The heating system 2 is closed.

[0134] The reaction unit 4, which is charged with raw materials, is advantageously heated evenly via the base and the wall 21. The heating elements 16a serve to heat the reaction unit 4 via the wall 21, while heating elements 16b arranged on the base element 5 supply heat to the reaction unit 4 through the base. When the heating system 2 is closed, the heating elements 16a formed on the circumference of the jacket element 8 are equally spaced from the wall 21 of the reaction unit 4. The heating elements 16a, 16b are preferably electrically operated.

[0135] The reaction unit 4 remains in the heating system 2 for a period of approximately 2.5 to 3.5 hours, during which the main reaction and conversion of the raw materials takes place within the reaction unit 4. Depending on the feed and the end products to be produced, the reaction temperature within the reaction unit 4 is between 350°C and 800°C, in particular between 400°C and 600°C, specifically approximately 550°C. This temperature is determined by means of the temperature sensors T2, T3 arranged in the space formed between the reaction unit 4 and the jacket element 8. This consumes energy in the range of 40 kWh per hour. The reaction unit 4 is fed with raw materials weighing between 2.5 t and 3 t.

[0136] The gases generated during the carbonization process are discharged, specifically extracted, into the exhaust line 11 through the exhaust outlet 10 located on the cover element 22. When the heating system 2 is closed, the exhaust outlet 10a of the reaction unit 4 and the exhaust outlet 10b of the hood 17 of the casing element 8 are connected to each other in a gas-tight manner. This ensures that no gases can escape into the space between the reaction unit 4 and the casing element 8.

[0137] Within the reaction unit 4, a negative pressure prevails with an absolute value in the range of 2 mbar to 10 mbar, specifically of approximately 4 mbar, which is generated by the extraction device 14-1 arranged at a first outlet nozzle of the oil tank 13 for extracting the gases via the surface of the oil accumulating within the oil tank 13. By specifically extracting the oxygen from the reaction unit 4, the reaction temperature or the process temperature within the reaction unit 4 is reached in a shorter time. Furthermore, the structure formation of the carbon as the end product is influenced. A further factor influencing the formation and purity of the carbon is the duration of the carbonization process. The longer the carbonization process, the purer the carbon and, depending on the starting materials, the carbon can be used, for example, for medical purposes.Carbon used for medical purposes may need to be further purified. Carbon recovered during a relatively shorter carbonization process is preferably used as filter material or in the construction industry, for example.

[0138] The factors influencing the formation and purity of the carbon also include the flushing of the reaction unit 4 with the gaseous flushing medium, in particular nitrogen, on the one hand during the carbonization and distillation process and on the other hand during the cooling process of the reaction unit 4.

[0139] The heating device 20 surrounding the exhaust line 11a heats the exhaust line 11a, in particular to a temperature in the range of 120°C to 160°C, in order to reduce the temperature difference between the exhaust line 11a and the exhaust gas flowing through the exhaust line 11a. The temperature of the flowing exhaust gas is determined by the temperature sensor T1. The heating device 20 serves to prevent premature condensation of the exhaust gas before entering the distillation unit 3 and thus also to prevent undesirable clogging of the exhaust line 11a. Heating the exhaust line 11a supports the outflow of the exhaust gas from the reaction unit 4.

[0140] Figure 5 shows the base element 5 of the heating system 2. The base element 5 comprises a base plate 24 and a centering device 25 for the casing element 8, heating elements 16b, and support elements 28 for holding the reaction unit 4. The base element 5 is essentially made of ceramic to ensure thermal insulation from the outside, particularly from below. In combination with the thermal insulation of the casing element 8, this minimizes heat loss from the heating system 2.

[0141] The reaction unit 4 rests on the support elements 28 of the base plate 24. The support elements 28 are designed and arranged such that the reaction unit 4, when resting on the support elements 28, is aligned centrally with the base element 5.

[0142] The centering device 25 is designed in the form of a circular disc with a shoulder. The disc thus has two areas with different diameters. The circular area arranged between the areas serves as the sealing surface 27.

[0143] The outer circumference of the area of ​​the disc with the smaller diameter is smaller than the inner circumference of the wall 21 of the reaction unit 4 or of the casing element 8. When the heating system 2 is closed, a gap is formed between a casing surface 26 of the area of ​​the disc with the smaller diameter and the inner side of the wall 21. The casing element 8 rests on the sealing surface 27 of the base plate 24, so that the space enclosed by the casing element 8 and the base plate 24 is tightly closed. To seal the enclosed space, seals are arranged on the corresponding surfaces of the base plate 24 and the casing element 8. In addition, the casing element 8 is pressed and held against the sealing surface 27 of the base plate 24 with a pressure in the range of 1 bar to 2 bar.

[0144] Since the support elements 6 are also attached to the base plate 24, the base plate 24 supports the entire heating system 2.

[0145] The heating elements 16b are arranged essentially horizontally on an end surface 29 of the centering device 25 and guided vertically through the end surface 29. The meandering, curved heating elements 16b each have the shape of a hand with five fingers. The length of the fingers increases from the outside to the inside, so that the middle finger has the greatest length. The heating elements 16b are aligned symmetrically to one another, with the tips of the fingers pointing towards the center of the end surface 29. The support elements 28, on which the reaction unit 4 rests, protrude vertically beyond the heating elements 16b, so that the base of the reaction unit 4 resting on the support elements 28 is arranged above the heating elements 16b. The heating elements 16b are each at the same distance from the base of the reaction unit 4 to ensure uniform heat input through the base of the reaction unit 4.

[0146] The centering device 25, the support elements 28 and the heating elements 16b are arranged concentrically around the center of the base plate 24.

[0147] Figure 6 shows the distillation unit 3, comprising the exhaust gas line 11 b, the cooling section 12 with the air guide housing 12-1 and the fans 12-2 as well as the oil tank 13 with the suction device 14-1 and the oil conveying device 14-2 in the order of the flow direction of the end products.

[0148] The gases discharged from the heating system 2 are conducted through the exhaust line 11b to the cooling sections 12, which are also made of pipes. The gas mass flow is split at a branch 30 into two partial mass flows by two parallel pipes. Splitting the gas mass flow improves heat transfer from the gas mass flow to the environment, thus optimizing the distillation or condensation process.

[0149] To further improve heat transfer, the tubes are designed with fins to increase the heat transfer surfaces of the cooling sections 12. The air guide housing 12-1 and the fans 12-2 further increase and simultaneously control the heat output to be dissipated by the gases to be cooled, in particular the amount of condensation heat. The ambient air is drawn evenly through the air guide housing 12-1 as cooling air and directed in a targeted manner over the cooling sections 12. The appropriate power or air volume flow of the fans 12-2 ensures that the exhaust gases flowing through the cooling section 12 of the distillation unit 3 can be liquefied at a condensation temperature in the range of 95°C to 125°C.With the additional flow to the cooling sections 12, the cooling sections 12 are cooled to a temperature below the condensation temperature of the gases or maintained at the corresponding temperature level. With the heat output controlled in this way, a higher oil yield is achieved with a lower residual gas yield. The temperature is determined using the temperature sensor T1 arranged, as shown in Figure 1, on the exhaust line 11 formed between the heating system 2 and the distillation unit 3.

[0150] After flowing through the cooling sections 12, the partial mass flows divided before entering the cooling sections 12 are reunited at an outlet point 31 and introduced into the oil tank 13 from above through an inlet nozzle 32.

[0151] The oil, which has a greater density than the gas, settles in the oil tank 13. The non-condensable portion of the distillation products is discharged from the upper region of the oil tank 13 through a first outlet nozzle 33. To extract the gases via the surface of the oil accumulating within the oil tank 13, the extraction device 14-1 is arranged at the first outlet nozzle 33 of the oil tank 13. By extracting the gases and the resulting negative pressure within the device 1, in particular the air, and thus the oxygen as a component of the air, is extracted from the reaction unit 4, thus influencing the carbonization process.

[0152] To pump the oil out of the oil tank 13, the oil pumping device 14-2 is arranged at a second outlet nozzle 34 of the oil tank 13.

[0153] Figure 7 shows an oil tank 13 with a cut-open side surface to provide a view of the interior.

[0154] The inlet nozzle 32 is located on top of the oil tank 13, so that the distillation products flow into the oil tank 13 from above. The oil settles at the bottom of the oil tank 13, while the gases, which have a lower density than the oil, concentrate above the oil level. The oil level in the oil tank 13 is determined and monitored using a float 35. When a predetermined fill level is reached, the oil is removed from the oil tank 13 for further processing.

[0155] The gases accumulating in the upper region of the oil tank 13 are discharged through the first outlet nozzle 33, in particular by means of the suction device 14-1, while the oil accumulating in the lower region of the oil tank 13 is suctioned through the second outlet nozzle 34, in particular by means of the oil conveying device 14-2.

[0156] In Figures 8a and 8b, the reaction unit 4 is shown in the closed state, with Figure 8b showing a sectional view of the reaction unit 4.

[0157] The wall 21, which is designed in the form of a hollow cylindrical vessel with a closed bottom, can be closed on the open side opposite the bottom by means of a lid element 22. During the process of closing the reaction unit 4, the lid element 22 is placed vertically onto the upwardly facing end face of the wall 21. The lid element 22 is pressed against the end face of the wall 21 due to its own weight and rests releasably against the wall 21.

[0158] A high-temperature-resistant seal is arranged between the wall 21 and the cover element 22 to tightly seal the reaction unit 4. When closed, the reaction unit 4 has a height of approximately 2.4 m.

[0159] The cover element 22 is formed with a connecting piece 36 next to the exhaust gas nozzle 10a. A device for admitting a gaseous purging medium, in particular nitrogen, into the reaction unit 4 can be connected to the connecting piece 36. The actual carbonization-distillation process, in which the reaction unit 4 is arranged within the heating system 2 and is heated or essentially maintained at the desired reaction temperature, is terminated at an exhaust gas temperature of approximately 60°C, determined by the temperature sensor T1 arranged in the exhaust line 11 formed between the heating system 2 and the distillation unit 3. The reaction unit 4 is removed from the heating system 2 and has a temperature, for example, in the range of 500°C to 600°C.

[0160] After removal from the heating system 2, the reaction unit 4 is cooled to a temperature defined depending on the product's use. The mixture located inside the reaction unit 4 is removed after opening the reaction unit 4, i.e., after removing the cover element 22. The reaction unit 4 is then returned to the process and recharged. The carbon-iron mixture is separated into its components.

[0161] The recovered unique carbon is further formed during the cooling process between 600°C and 60°C, or 20°C or 30°C, within the reaction unit 4 in the oxygen-free atmosphere. The gaseous purging medium, in particular nitrogen, flows into the reaction unit 4 through the connection piece 36, which also influences the cooling process. Alternatively, the gaseous purging medium can be introduced through the exhaust port 10a, to which the device for admitting the gaseous purging medium can be connected, particularly if the connection piece 36 is not provided. The inflow of the purging medium during the cooling process and thus before the reaction unit 4 is emptied can accelerate the cooling process, but primarily serves to purify the end products and could thus also support the formation of the carbon recovered with the device 1.Flushing the reaction unit 4 increases the purity of the end products, particularly the carbon. Impurities are flushed out. The flushing medium flowing into the reaction unit 4 through the connection piece 36 is discharged from the reaction unit 4 together with the impurities through the exhaust outlet 10a formed in the cover element 22. The reaction unit 4 is opened at a temperature inside the reaction unit 4 in the range of 20°C to 60°C, in particular in the range of 30°C to 60°C.

[0162] During the process of opening the reaction unit 4, the cover element 22 is lifted vertically and removed from the reaction unit 4 so that the reaction unit 4 can be emptied and subsequently refilled. Even during the emptying process, the reaction unit 4 can be exposed to the flushing medium to achieve the desired purity of the end products, especially the carbon. The carbon is preferably removed by suction during the emptying of the reaction unit 4.

[0163] Four reaction units 4 made of high-temperature-resistant steel, each with a capacity ranging from 2.5 t to 3.5 t (75% mechanical, 25% automated), are simultaneously involved in the carbonization-distillation process for the material treatment of the raw materials. While the first reaction unit 4 is being charged, the second reaction unit 4, which is already charged, is preheated. Meanwhile, the third reaction unit 4 is already fed into the heating system 2 and is heated, so that the actual carbonization-distillation process takes place. Meanwhile, the fourth reaction unit 4 is cooled and then emptied.

[0164] By using the modular system, for example, with four reaction units, throughput can be gradually increased and flexibly adapted to current needs. The entire process runs quasi-continuously.

[0165] Figures 9a to 9n show microscopic images of carbon produced using device 1 for the material treatment of raw materials. The images, taken with a transmission electron microscope (TEM), reveal the structure of the carbon. Transmission electron microscopy is used to identify and characterize the structure and particle size of substances and mixtures of substances in the nanometer range.

[0166] The images show a very fine, three-dimensional, homogeneous, and pseudocrystalline structure of the primary carbon particles in the subnanometer range with a very large internal surface area. The carbon particles are partially visible as larger agglomerates with the same surface structure.

[0167] Figures 9p and 9q show the results of Raman spectroscopy of the carbon. The missing 2D maximum at 2,700 cm' 1shows the absence of a large-scale graphitic arrangement. The carbon produced by device 1 for the material treatment of raw materials is amorphous, inorganic carbon in which the nanoparticles are cross-linked without long-range order. The carbon exhibits neither nanotubes nor any structural similarity to graphene.

[0168] Raman spectrum recordings and determining the intensity and width of G-Raman and D-Raman bands can be performed using the Renishaw inVia Confocal Raman Microscope with 532 nm and 785 nm lasers. LIST OF REFERENCE SYMBOLS

[0169] 1 device for material treatment

[0170] 2 Heating system

[0171] 3 Distillation unit

[0172] 4 reaction unit

[0173] 5 Floor element of the heating system 2

[0174] 6 Support element

[0175] 7 Head element of the heating system 2

[0176] 8 Jacket element of the heating system 2

[0177] 9 Enclosure

[0178] 10, 10a, 10b exhaust nozzle

[0179] 11 , 11a, 11 b exhaust pipe

[0180] 11-1 Connection element of the exhaust pipe 11 , 11a

[0181] 12 Cooling section of the distillation unit 3

[0182] 12-1 Air guide housing

[0183] 12-2 fans

[0184] 13 Oil tank

[0185] 14-1 Suction device

[0186] 14-2 Oil extraction device

[0187] 15 Control device

[0188] 16a, 16b Heating element

[0189] 17 hood

[0190] 18 Connecting element of the exhaust pipe 11 , 11a

[0191] 19 Pipe connection

[0192] 20 Heating device

[0193] 21 Wall of reaction unit 4

[0194] 22 Cover element

[0195] 23 Sieve element

[0196] 24 Base plate 25 Centering device for casing element 8

[0197] 26 Surface of the centering device 25

[0198] 27 Sealing surface of the centering device 25

[0199] 28 Support element for reaction unit 4

[0200] 29 End surface

[0201] 30 branch

[0202] 31 Mouth

[0203] 32 Oil tank inlet nozzle 13

[0204] 33 first outlet nozzle of the oil tank 13

[0205] 34 second outlet nozzle of the oil tank 13

[0206] 35 swimmers

[0207] 36 Connection piece of the cover element 22

[0208] B Direction of movement of the heating system 2

[0209] H Height

[0210] T1, T2, T3 temperature sensor

Claims

PATENT CLAIMS 1. Device (1) for the material treatment of raw materials, comprising a heating system (2), a distillation unit (3) and a reaction unit (4) as well as a control device (15), wherein - the heating system (2) is designed to be openable and closable for fitting the reaction unit (4), - the distillation unit (3) has a cooling section (12) and - the reaction unit (4) is designed to be feedable with the raw materials, wherein an exhaust gas line (11, 11a, 11b) is formed between the reaction unit (4) and the distillation unit (3) for discharging the exhaust gases from the reaction unit (4), characterized in that - temperature sensors (T1, T2, T3) are formed in the area of ​​the heating system (2) and the distillation unit (3), - the cooling section (12) of the distillation unit (3) is designed with a device for forced cooling, wherein the cooling section (12) - is arranged within an air guide housing (12-1) for the targeted guidance of ambient air over the cooling section (12) and / or - is formed from at least one coaxial tube for passing gases inside an inner tube and for passing a heat transfer fluid in the space between the outside of the inner tube and the inside of the outer tube, and - a suction device (14-1) is designed to suck gases out of the reaction unit (4) and to generate a negative pressure within the reaction unit (4), wherein the temperature sensors (T1, T2, T3) and the Suction device (14-1) is connected to the control device (15). Device (1) according to claim 1, characterized in that at least two of the temperature sensors (T2, T3) for determining the temperature within the reaction unit (4) are arranged in an intermediate space formed, when the heating system (2) is closed, between the reaction unit (4) and a casing element (8) of the heating system (2). Device (1) according to claim 1 or 2, characterized in that the exhaust gas line (11) between the heating system (2) and the distillation unit (3) is formed with a heating device (20) for heating the exhaust gas line (11), wherein the heating device (20) is connected to the control device (15). Device (1) according to one of claims 1 to 3, characterized in that at least one temperature sensor (T1) for determining the temperature of exhaust gases discharged from the heating system (2) is arranged on the exhaust gas line (11) between the heating system (2) and the distillation unit (3).Device (1) according to one of claims 1 to 4, characterized in that the exhaust gas line (11) between the heating system (2) and the distillation unit (3) is designed with a connecting element (11-1) for connection to a device for admitting a gaseous flushing medium, in particular into the reaction unit (4). Device (1) according to one of claims 1 to 5, characterized in that fans (12-2) for specifically directing ambient air over the cooling section (12) are designed within a wall of the air guide housing (12-1), in which the cooling section (12) of the distillation unit (3) is arranged, wherein the fans (12-2) are connected to the control device (15). Device (1) according to claim 6, characterized in that the fans (12-2) are arranged on an upper side, in particular on a front surface facing upwards in the vertical direction, or on a side surface of the air guide housing (12-1). Device (1) according to one of claims 1 to 7, characterized in that the suction device (14-1) is arranged downstream of an oil tank (13) arranged downstream of the distillation unit (3) in the flow direction of the gases.Device (1) according to one of claims 1 to 8, characterized in that the heating system (2) has a head element (7) and a casing element (8) which is firmly connected to the head element (7), as well as support elements (6) which are adjustable in length in the vertical direction, wherein the head element (7) is held on the support elements (6) in such a way that the heating system (2) is opened and closed in the vertical direction of movement (B) by changing the length of the support elements (6) between two end positions. Device (1) according to claim 9, characterized in that the heating system (2) has two support elements (6), wherein the support elements (6) are arranged on both sides of the heating system (2). Device (1) according to claim 9 or 10, characterized in that the casing element (8) has a hollow-cylindrical wall which is adjustable in the vertical direction. - opened downwards and - is closed at the top with a circular hood (17) and is connected to the head element (7) at the hood (17). Device (1) according to claim 11, characterized in that the hood (17) is designed at the center point with an exhaust gas nozzle (10b) as a connection to an exhaust gas line (11a), wherein the exhaust gas line (11a) extends from the exhaust gas nozzle (10b) through the hood (17) into the head element (7). Device (1) according to claim 12, characterized in that the exhaust gas line (11a) is designed with an automatically length-adjustable pipe connection (19) in the region of the exhaust gas nozzle (10b) to compensate for thermal expansion. Device (1) according to one of claims 1 to 13, characterized in that the reaction unit (4) is designed with a wall (21) in the form of a hollow cylindrical vessel which is closed at the bottom, and the open side of the wall (21) can be closed by means of a cover element (22).Device (1) according to claim 14, characterized in that the cover element (22) of the reaction unit (4) is circular and has an exhaust nozzle (10a) at the center point, wherein the exhaust nozzle (10a) of the cover element (22) and the exhaust nozzle (10b) of the casing element (8) engage with each other when the heating system (2) is closed and form a tight connection to the exhaust line (11a). Device (1) according to claim 14 or 15, characterized in that the cover element (22) of the reaction unit (4) is designed with a connecting nozzle (36) for connecting to a device for admitting a gaseous flushing medium into the reaction unit (4). Method for operating a device (1) for the material treatment of raw materials according to one of claims 1 to 16, comprising the following steps:. - feeding a reaction unit (4) with raw materials, - Preheating of the reaction unit (4), - opening a heating system (2) and placing the reaction unit (4) into the heating system (2), - closing the heating system (2) so that the reaction unit (4) is arranged in a closed space, - heating the reaction unit (4) and starting a carbonisation and distillation process, wherein the carbonisation and distillation process is carried out by targeted heating at a substantially constant temperature within the reaction unit (4), wherein the temperature is determined, - discharging gases produced from the reaction unit (4) into a distillation unit (3) through an exhaust gas line (11, 11a) formed between the reaction unit (4) and the distillation unit (3) and determining the temperature of the gas flowing through the exhaust gas line (11, 11a), - cooling and condensing the gases in the distillation unit (3), whereby the temperature of the gases is controlled by forced cooling of a cooling section (12) of the distillation unit (3) via a heat output dissipated by the gases, - introducing the distillation products into an oil tank (13) and separating oil, - Extracting non-condensable gases from the oil tank (13), whereby a negative pressure is generated within the reaction unit (4) relative to the environment and oxygen is removed from the reaction unit (4), - Opening the heating system (2) and removing the reaction unit (4) from the heating system (2), - cooling the reaction unit (4), removing the end products from the reaction unit (4) and separating the end products and - Removing the final products from the oil tank (13). A method according to claim 17, characterized in that the pressure within the reaction unit (4) is set to an absolute value in the range from 2 mbar to 10 mbar, in particular of approximately 4 mbar. A method according to claim 17 or 18, characterized in that for cooling and condensing the gases in the distillation unit (3) - targeted ambient air via the cooling section (12) of the distillation unit (3) or - a liquid heat transfer fluid, in particular water as a coolant, flows through the cooling section (12). Method according to one of claims 17 to 19, characterized in that during the process of cooling and condensing the gases in the distillation unit (3), the temperature of the gases is in a range from 95°C to 125°C. Method according to one of claims 17 to 20, characterized in that during the carbonization and distillation process, an exhaust gas line (11, 11a) formed between the reaction unit (4) and the distillation unit (3) is heated, in particular to a temperature in the range from 120°C to 160°C. Method according to one of claims 17 to 21, characterized in that the reaction unit (4) is removed from the heating system (2) at a temperature of the gas flowing through the exhaust gas line (11, 11a) of approximately 60°C.Method according to one of claims 17 to 22, characterized in that during the carbonization and distillation process and / or during the process of cooling the reaction unit (4), a gaseous flushing medium is flowed into the reaction unit (4). Method according to claim 23, characterized in that the gaseous purging medium is flowed into the reaction unit (4) at time intervals. Method according to claim 24, characterized in that the suction of non-condensable gases and the flow of the purging medium into the reaction unit (4) take place at staggered times. Method according to claim 24 or 25, characterized in that the purging medium is periodically flowed into the reaction unit (4) during the cooling process of the reaction unit (4) for a duration in the range of two to three minutes. Method according to one of claims 17 to 26, characterized in that the reaction unit (4) is opened for removal of the end products at a temperature inside the reaction unit (4) in the range of 20°C to 60°C, in particular in the range of 30°C to 60°C.Method according to one of claims 17 to 27, characterized in that during the process of removing the end products from the reaction unit (4), the reaction unit (4) is exposed to a gaseous flushing medium. Method according to one of claims 17 to 28, characterized in that during the process of removing the end products from the reaction unit (4), carbon is extracted as the end product. Method according to one of claims 17 to 29, characterized in that the heating system (2) is opened and closed by extending and retracting support elements (6). Method according to one of claims 17 to 30, characterized in that extracted, non-condensable gases are fed to the heating system (2) for combustion within the heating system (2) and for heating the reaction unit (4). Carbon produced by the method according to one of claims 17 to 31 for operating a device (1) for the material treatment of carbon-containing raw materials according to one of claims 1 to 16, characterized in that the carbon is amorphous and has a structure of a three-dimensional arrangement of carbon nanoparticles as agglomerates, wherein the carbon nanoparticles are cross-linked without long-range order, do not have a large-scale graphitic arrangement and are not arranged as nanotubes. Carbon according to claim 32, characterized in that the carbon has a mass-related specific surface area greater than 2,500 m 2 / g BET, especially up to 9,500 m 2 / g BET, especially greater than 3,500 m 2 / g BET or greater than 4,000 m 2 / g BET, especially in the range of 4,200 m 2 / g BET up to 4,800 m 2 / g BET. Carbon according to claim 32 or 33, characterized in that the carbon has a density of about 66 kg / m 3 Carbon according to one of claims 32 to 34, characterized in that the carbon has an electrical conductivity in the range of 4.5-10 7 sqm up to 5.8- 10 7 Qm. Use of the device (1) for the material treatment of raw materials according to one of claims 1 to 16 for producing carbon according to one of claims 32 to 35.

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