Apparatus and method for material treatment of raw materials and carbon produced by method

Abstract

The invention relates to a device (1) for material treatment of raw materials. The device (1) has a heating system (2), a distillation unit (3), a reaction unit (4) and a control device (15). The reaction unit (4) is formed such that the reaction unit can be filled with a raw material for processing. The heating system (2) can be opened and closed to fill the reaction unit (4). An exhaust line (11, 11a, 11b) for discharging exhaust gas from the reaction unit (4) is arranged between the reaction unit (4) and the distillation unit (3). The distillation unit (3) has a cooling section (12) with means for forced cooling. According to the invention, the cooling section (12) is arranged in an air-conducting housing (12-1) for the targeted conduction of ambient air through the cooling section (12), and / or the cooling section is formed from at least one coaxial tube for the passage of a gas 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). An extraction device (14-1) for extracting gas from the reaction unit (4) and generating a negative pressure is formed in the reaction unit (4). The temperature sensors (T1, T2, T3) and the extraction device (14-1) are connected to a control device (15). The invention further relates to a method for operating a device (1) for the material treatment of raw materials, and to carbon produced by said method.

Description

[0001] The invention relates to a device for material processing of raw materials. The device has a heating system, a distillation unit and a reaction unit and a control device. The reaction unit can be filled with raw materials for processing. The heating system can be turned on and off to fill the reaction unit.

[0002] The invention further relates to a method for operating an apparatus for material processing of raw materials, and to the carbon produced by said method.

[0003] The invention provides a device known from the prior art for industrial processing, in particular for processing waste rubber products, rubber products or rubber-like composite products (such as used tires, steel-reinforced rubber belts, rubberized chain links and conveyor belts) and crushed scrapped vehicles, organic renewable raw materials (such as wood), contaminated carbon and contaminated soil. Light oils, gases, metals (especially steel) and carbon are obtained. Conventional devices are based on, for example, using rotary kilns, fluidized bed reactors and drums and processed compressed starting materials in a chemically inert atmosphere with the exclusion of oxygen.

[0004] DE 199 30 071 C2 describes a method and an apparatus for recovering organic substances and substance mixtures. The organic material is brought into contact with the fluidized bed material of a combustion fluidized bed. The method produces an end product in the form of a gas with condensable substances and carbonaceous residues.

[0005] DE 44 41 423 A1 discloses a method and a device for obtaining usable gas from waste. Crushed waste is introduced into a gas-tight sealed drum. Gas is generated in the drum and separated from the residue formed at the same time. The generated gas is decomposed into cracked gas in a gas converter with air supply and in the presence of a hot coke bed. The heat required in the process is transferred by the gas in direct contact with the material to be recycled. A partial flow of the cracked gas from the gas converter is used to transfer heat to the gas.

[0006] DE 40 11 945 C1 discloses a method for degassing organic matter (such as domestic waste and industrial waste, etc.) in a heatable chamber. In this method, the starting material is introduced into the chamber by compression and passes through the chamber cross section while maintaining the compressed state. Heat is supplied via the chamber wall that is in pressure contact with the compressed material. The formed gaseous products are removed under increased pressure. The chamber is sealed in an airtight manner by the compressed material in its filling area. By recompressing the solid residue, an increased flow resistance is achieved in the outflow area of ​​the gaseous product.

[0007] DE 39 32 803 A1 discloses a process for the reaction of organic materials, in which boric acid / boron oxide and an organic nitrogen compound are added to carbon and graphite in a non-oxidizing atmosphere.

[0008] The operation of conventional plants requires increased expenditures in terms of materials, energy and logistics. Thus, for example, the production of a fluidized bed in a fluidized bed reactor requires increased energy consumption, since on the one hand the fluidized bed must be produced and maintained, and on the other hand the materials to be utilized must be mechanically handled so that they effectively contact the fluidized bed. The crushing or compacting of the starting materials in the preparation and during the recycling process also results in high energy costs.

[0009] WO 2007 / 053088 A1 describes a method and a device for treating materials from hydrocarbons. These materials are fed into an inner container, which in turn can be arranged in an outer container. The two containers are each closed with a cover element. The hydrocarbon material is heated by means of microwaves or high-frequency radiation. The exhaust gas generated is discharged from the containers through a gas outlet. Two or more containers can be operated in parallel and connected to a gas cleaning system to maintain an almost continuous gas flow through the gas cleaning system.

[0010] WO 2010 / 012275 A2 discloses a device for treating materials with a cylindrical furnace and control of the process. The inner surface of the furnace is provided with an insulating layer of inorganic thermal insulation material. Heating elements are arranged at or on the inner surface of the insulating layer. Control of the process achieves a high yield of carbon, oil and fuel gas by controlling the temperature of the heating elements.

[0011] DE 10 2012 109 874 A1 discloses a device for material processing of raw materials, the device having a heating system, a distillation unit and a reaction unit that can be filled with raw materials, and a method for operating such a device. The heating system (which can be opened and closed to fill the reaction unit) has a head element and a sheath element firmly connected to the head element and a support element. The head element is connected to the support elements, which can be changed in length in the vertical direction, so that the heating system is opened and closed in the vertical movement direction by changing the length between the two end positions of the support element.

[0012] The object of the present invention is to provide an improved device and method for treating different used rubber products (especially used tires) and rubber composite products or rubber-like composite products, renewable raw materials (such as wood, shells or fruits), electronic waste (such as computers and mobile phones), motor vehicles and storage media (such as batteries) and polluted carbon. These composite products have to be separated and valuable components, such as carbon, light oil, gas and (if appropriate) metallic materials, will be recovered. Polluted carbon should be separated from the corresponding impurities. The device should be able to operate effectively with minimum energy input costs, and the method should be able to be implemented with minimum expenditure, especially time expenditure. The raw materials recovered by the method should remain unchanged as much as possible in terms of the starting structure, so that, for example, it can be returned to its original purpose. In addition, the carbon recovered by the method should have favorable material properties different from conventional carbon.

[0013] This object is achieved by a device for material processing of raw materials according to the present invention. The device has a heating system, a distillation unit and a reaction unit and a control device. The reaction unit can be filled with raw materials. The heating system can be turned on and off to fill the reaction unit. An exhaust line for exhausting waste gases from the reaction unit is formed between the reaction unit and the distillation unit. The distillation unit has a cooling section.

[0014] According to the concept of the invention, temperature sensors are formed in the region of the heating system and the distillation unit. In addition, the cooling section of the distillation unit has a device for forced cooling. The device for forced cooling of the cooling section makes it possible (for example, compared to free convection) for the cooling section to be subjected to a specific flow of a heat-carrying fluid (in particular gaseous or liquid) in order to remove heat, or for a heat flow to flow around it. The cooling section is arranged in an air-guiding housing, which is used to conduct ambient air through the cooling section in a targeted manner, and / or the cooling section is formed by at least one coaxial tube, which is used to conduct gas in the inner tube and to conduct the heat-carrying fluid in the intermediate space between the outer tube and the outer tube. The coaxial tube can be in particular double-walled. The heat-carrying fluid is preferably in a concentrated liquid state and can be specifically water or ethylene glycol.

[0015] The device for material processing of raw materials has an extraction device for extracting gas from the reaction unit and generating negative pressure in the reaction unit. Negative pressure refers to the pressure of the environment surrounding the device. The extraction device can be formed as a pump, in particular as a diaphragm pump.

[0016] According to the invention, the temperature sensor and the extraction device are connected to the control device.

[0017] 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 in the switched-off state.

[0018] According to an advantageous embodiment of the invention, the exhaust gas line between the heating system and the distillation unit has a heating device for heating the exhaust gas line. The heating device is connected to the control device, the heating device preferably completely surrounds the exhaust gas line and is advantageously electrically operated.

[0019] At least one temperature sensor for determining the temperature of the exhaust gases discharged from the heating system is preferably arranged in the exhaust line between the heating system and the distillation unit.

[0020] A connecting element can be provided on the exhaust gas line between the heating system and the distillation unit, which is used to connect to a device for introducing a gaseous flushing medium, in particular into the reaction unit. The flushing medium (for example nitrogen) serves to make the interior of the reaction unit inert, reduce the risk of explosion, and acts as a carrier gas to support the separation of the end product produced during operation of the device.

[0021] The fan is advantageously arranged in the wall of an air guide housing in which the cooling section of the distillation unit can be arranged, for conducting ambient air in a targeted manner through the cooling section. The air guide housing with the fan is formed as a device for forced cooling of the cooling section of the distillation unit with ambient air. The fan is connected to a control device.

[0022] A fan formed in the wall of the air guide housing of the cooling section of the distillation unit for conducting ambient air in a targeted manner through the cooling section is preferably arranged on the top side, in particular on the end face pointing upward in the vertical direction, or on the side of the air guide housing.

[0023] The advantage of the present invention is that the extraction device for extracting gas from the reaction unit and generating negative pressure in the reaction unit is arranged downstream of the oil tank, which is arranged downstream of the distillation unit in the flow direction of the gas. Therefore, negative pressure is also generated in the distillation unit.

[0024] According to another preferred embodiment of the invention, the heating system has a head element and a sheath element firmly connected to the head element and a support element. The head element is mounted on the support elements, which can change length in the vertical direction. By changing the length between the two end positions of the support element, the heating system is turned on and off in the vertical movement direction.

[0025] In this case, the heating system preferably has two support elements, which are preferably arranged on both sides of the heating system.According to a first alternative, the support element is driven by an electric spindle.According to a second alternative, the support element is formed as a hydraulic support.

[0026] According to a further development of the invention, the sheath element is formed with a hollow cylindrical wall. The wall is open in the vertical direction downwards and is closed at the top with a circular cover. The sheath element is connected to the head element at the cover to form a unit.

[0027] The sheath element advantageously has heating elements evenly distributed around the circumference of the inner surface of the wall.To prevent heat transfer to the outside, the wall is formed with a thermal insulation made of ceramic powder.

[0028] According to a further advantageous embodiment of the invention, the hood is formed with an exhaust port at a central point, which exhaust port serves as a connection to an exhaust line of the heating system.The exhaust line extends from the exhaust port through the hood into the head element of the heating system.

[0029] The exhaust gas line advantageously has a connecting element at the distal end facing away from the exhaust gas port of the hood, which connecting element serves as a connection to the exhaust gas line of the distillation unit.

[0030] The exhaust line extending from the exhaust port through the hood into the head element of the heating system can be formed in the region of the exhaust port for compensating thermal expansion with a pipe connection which is automatically variable in length, in particular in the vertical direction.

[0031] Another advantage of the invention is that the reaction unit is formed with a wall in the form of a hollow cylindrical vessel, which is closed at the bottom. The open side of the wall can be closed by means of a cover element.

[0032] A high temperature-resistant seal is advantageously arranged between the wall and the cover element.

[0033] The cover element of the reaction unit is preferably formed circularly and has an exhaust port at the center point. It is particularly advantageous if the exhaust port of the cover element and the exhaust port of the jacket element engage with each other in the closed state of the heating system and form a tight connection to the exhaust line.

[0034] The cover element of the reaction cell can be formed with a connection port for connecting to a device for introducing a gaseous flushing medium, in particular nitrogen, into the reaction cell.

[0035] The reaction unit may have mesh elements inside, which are preferably aligned horizontally and arranged at different heights, at a distance from each other. The mesh elements preferably cover the entire cross section of the reaction unit.

[0036] The control device of the device for material processing of raw materials is used to control the method for operating the device according to the present concept and, in addition to the temperature sensor, controls the device for forced cooling, in particular a conveying device, such as a fan for guiding ambient air through the cooling section in a targeted manner or at least one pump for conveying a liquid heat transfer fluid, and the extraction device is advantageously also connected to the drive of the support element, the filling level sensor of the oil tank, the pressure sensor and the valve of the heating circuit of the heating system. The filling level sensor of the oil tank can be formed as a float. The pressure sensor is advantageously arranged in the area of ​​the oil tank. The control device can also be connected to an oil delivery device, in particular a piston pump, which is used to extract oil from the oil tank. The oil delivery device acts on the signal sent by the filling level sensor of the oil tank to the control device and delivers the oil out of the oil tank.

[0037] This object is also achieved by a method according to the invention for operating a device for material processing of raw materials. The method comprises the following steps:

[0038] - filling the reaction unit with raw materials,

[0039] - Preheating the reaction unit,

[0040] - opening the heating system and introducing the reaction unit into the heating system, in particular onto the bottom element of the heating system,

[0041] - Turn off the heating system so that the reaction unit is arranged in a closed space,

[0042] - heating the reaction unit and starting a carbonization and distillation process, wherein the carbonization and distillation process is carried out by selective heating at a substantially constant reaction temperature in the reaction unit, wherein the temperature is determined,

[0043] - removing any produced gases from the reaction unit to the distillation unit by means of a gas exhaust line formed between the reaction unit and the distillation unit and determining the temperature of the gases flowing through the gas exhaust line,

[0044] - cooling and condensing the gases in the distillation unit, wherein the temperature of the gases is controlled by forced cooling of the cooling section of the distillation unit by means of the heat output dissipated by the gases,

[0045] - introducing these distillation products into oil tanks and discharging the oil,

[0046] - extracting non-condensable gases from the tank, wherein a negative pressure to the environment is generated in the reaction unit and oxygen is removed from the reaction unit,

[0047] - opening the heating system and removing the reaction unit from the heating system,

[0048] - cooling the reaction unit, removing the end product from the reaction unit and isolating the end product, and

[0049] -Removal of final product from tank.

[0050] Targeted heating is understood to mean that the reaction unit arranged in the heating system is heated during the carbonization and distillation process so that the reaction temperature (also called process temperature) in the reaction unit is essentially constant and varies only within a predetermined temperature band. In doing so, the reaction temperature is permanently monitored. The temperature value is transmitted to a control device, which controls the opening and closing of the valves of the heating circuit of the heating system and thus ignites according to a predetermined desired temperature value.

[0051] When the heating system is switched off, the exhaust port of the reaction unit is preferably coupled to the exhaust port of the exhaust line of the heating system, and the exhaust line of the heating system and the exhaust line of the distillation unit are coupled to each other on the connecting element, so that a gas-tight connection from the reaction unit to the distillation unit is produced. The heating system is advantageously opened and closed by extending and retracting the support element.

[0052] According to a further development of the invention, by extracting non-condensable gases from the tank and thereby generating a negative pressure, the absolute value of the pressure in the reaction unit can be set in the range from 2 mbar, in particular from about 4 mbar to 10 mbar.

[0053] In order to cool and condense the gases in the distillation unit, ambient air can be passed through a cooling section of the distillation unit in a targeted manner, or a liquid heat transfer fluid, in particular water as coolant, can flow through the cooling section.

[0054] According to an advantageous embodiment of the invention, during the procedure of cooling and condensing the gases in the distillation unit, the temperature of the gases is regulated to a value in the range from 95° C. to 125° C., in particular via the volume flow of ambient air or the output of a fan or the mass flow of a heat transfer fluid. The volume flow of ambient air or the mass flow of a heat transfer fluid ensures that heat will be dissipated from the cooling section and cools the cooling section. In the exhaust line formed between the heating system and the distillation unit, in particular at least one temperature sensor for determining the temperature of the exhaust gases discharged from the heating system determines the temperature of the gases.

[0055] An advantage of the invention is that during the carbonization and distillation process, the exhaust line formed between the reaction unit and the distillation unit is heated, in particular to a temperature in the range from 120° C. to 160° C., in particular in order to avoid premature condensation of the exhaust gas before entering the distillation unit and thus clogging the exhaust line.

[0056] The reaction unit is preferably removed from the heating system when the temperature of the gas flowing through the exhaust line is approximately 60°C.

[0057] 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 procedure for cooling the reaction unit.

[0058] Flushing preferably occurs at time intervals in each case, in particular in order to remove relatively high molecular weight gases from the reaction unit. Flushing with the aid of an inert gas (such as nitrogen) removes undesirable components, such as polyaromatic components of polybutadiene or plasticizers, from the reaction unit, particularly during the carbonization and distillation processes. Extraction of non-condensable gases and therefore generation of negative pressure in the reaction unit and inflow of flushing medium into the reaction unit advantageously occur in a time-shifted manner relative to each other. Specifically, during the procedure of cooling the reaction unit, the flushing medium can be periodically introduced into the reaction unit for a duration in the range of two to three minutes.

[0059] After the reaction unit has been cooled, the reaction unit is preferably opened for removing the end product when the temperature within the reaction unit is in the range from 20° C. to 60° C., in particular in the range from 30° C. to 60° C. During the procedure for removing the end product from the reaction unit, a gaseous flushing medium, in particular nitrogen, is advantageously applied to the reaction unit.

[0060] During the process of removing the end product from the reaction unit, carbon may be extracted as the end product.

[0061] According to a further development of the invention, the extracted noncondensable gases are fed to a heating system to be combusted within the heating system and thus used to heat the reaction unit and / or to a combined thermal power station for generating thermal and electrical energy.

[0062] The method preferably utilizes at least four reaction units simultaneously and operates in a modular manner, having the following steps:

[0063] - filling the first reaction unit and preheating the already filled second reaction unit,

[0064] - introducing the filled and preheated third reaction unit into the heating system and heating the reaction unit to perform the carbonization and distillation process; and

[0065] - Cooling and draining the fourth reaction unit, in which the carbonization and distillation processes are completed.

[0066] According to a further development of the invention, the reaction unit is filled with a mass of raw materials in the range from 2.5 t to 3 t. The reaction unit is advantageously kept in the heating system for a period of about 2.5 h to 3.5 h. The reaction temperature in the reaction unit is preferably between 350° C. and 800° C., in particular 550° C.

[0067] The energy consumption of the process operated with a reaction unit, in particular equipped with used tires, is 60 kWh to 80 kWh. The operation of twelve reaction units with nine passes per day results in a daily energy demand of 6,480 kWh to 8,640 kWh. With an average of 223 production days per year, the annual energy demand is therefore 1.445 MWh to 1.927 MWh. In contrast, the energy value of the generated electricity and heat is each about 10.5 MWh per year.

[0068] The method according to the invention is based on a carbonization / distillation process, so that the device according to the invention is an industrial carbonization / distillation module, also called a VDI module.

[0069] In order to implement the method efficiently, the plant is based on a design that utilizes modules, so as to thereby optimize or maximize the production volume and be able to adapt it to current needs.

[0070] Further advantages of the device according to the invention and the method according to the invention compared to the prior art can be summarized as follows:

[0071] No pre-sorting of raw materials,

[0072] · Handling of raw materials, especially

[0073] - waste rubber products, such as used tires, rubberized chain links, steel cord-reinforced rubber belts and conveyor belts, wherein, in order to obtain their structure, these products can be processed in their substantially original form, i.e., for example, neither crushed nor shredded and thus not compressed or compacted,

[0074] - organic and renewable raw materials, such as all forms of wood, especially beech and oak, bamboo and fruit peels and rinds, such as coconut and orange peels,

[0075] -Animal waste, such as bones and animal carcasses,

[0076] - polluted carbon,

[0077] - contaminated soil or other materials, for example after an oil spill,

[0078] - a scrap vehicle which has not been substantially crushed or disassembled and is therefore a complete vehicle; and

[0079] - carbon composite materials, in particular with carbon fibers, especially from the automotive industry,

[0080] Ecological, economical and CO2-free and therefore sustainable technology with very low energy consumption.

[0081] Various process parameters, such as the temperature and duration of the process and the flushing with a gaseous flushing medium, and the performance of the individual components associated therewith, such as the heating system, the conveying device for the device for forced cooling of the distillation unit, such as a fan or at least one pump, and the extraction device, depend on the raw materials to be treated in the reaction unit. Thus, methods or devices with corresponding control programs stored in the control device can be distinguished as follows:

[0082] a) an apparatus and a method for material processing of tires,

[0083] b) an apparatus and a method for material treatment of rubberized chain links,

[0084] c) an apparatus and method for material handling on a conveyor belt,

[0085] d) Devices and methods for material handling of complete or crushed vehicles for the automotive industry,

[0086] e) Apparatus and methods for material processing of renewable raw materials such as wood and bamboo and biogenic waste such as coconut shells and orange peels,

[0087] f) apparatus and methods for material processing of animal waste,

[0088] g) Apparatus and methods for material processing of bitumen or asphalt,

[0089] h) an apparatus and a method for material processing of energy stores, in particular batteries, in particular from the automotive industry,

[0090] i) apparatus and methods for material processing of electronic components such as computers, mobile phones, laptops and smartphones, and

[0091] j) Apparatus and methods for the physical treatment of contaminated carbon and soil contaminated by pollutants to reactivate the carbon.

[0092] Depending on the raw materials to be processed, these are advantageously mixed in a certain ratio relative to one another within the reaction unit (eg tire and battery) in order to influence the process parameters or the end product.

[0093]

[0094]

[0095]

[0096] 1 Grinding to particle size <0.1mm - Results Headspace GC-MS screening and thermogravimetric analysis results

[0097] 2 Thermogravimetric analysis TGA, results GC-MS screening

[0098] 3 Trace Elements Using ICP OES Based on HNO3 / HF Acid Digestion - SOP 671(679)

[0099] In the above table, the recovered raw materials are expressed in mg / kg. The third and fourth columns list the raw materials according to the apparatus and method according to h), and the fifth column lists the raw materials according to the apparatus and method according to i), while the sixth and seventh columns list the raw materials according to the apparatus and method according to d), and the eighth column lists the raw materials according to the apparatus and method according to a).

[0100] In the method according to h), the raw materials of which are listed in the fourth column of the table, a battery block (also called energy block) with a mass of 500 kg from the automotive industry and a used tire with a mass of about 500 kg are used as starting materials. Before the process, a steel jacket with a mass of about 60 kg including the screw is removed from the battery block and the remaining 440 kg of starting material is stacked on a separate screen in order to avoid mixing of the battery block with the used tire in the reaction unit. The residue of the processed battery block removed from the reaction unit after the complete process has a mass of 220.9 kg and is chopped into a uniform size in the range of 0.2 mm to 0.5 mm for further analysis. As can be seen from the analytical data presented in the table, all inorganic or metallic components of the battery block are detected with a recovery rate of more than 98.5%. Metallic and inorganic components, such as cobalt, nickel, magnesium, copper, niobium and lithium can be recovered by sophisticated metal refining.

[0101] In the case of the method according to (i), the raw materials of which are listed in the fifth column of the table, the starting materials used are 500 kg of electronic waste (such as televisions, drilling rigs and cables), 15 kg of electronic waste (such as computers and mobile phones in the form of laptops) and a mass of about 500 kg of used tires. The computers and mobile phones are placed separately in a metal box in the reaction unit to avoid mixing with other starting materials. The residues of the processed computers and mobile phones removed from the metal box after the complete process have a fixed mass of 7.7 kg and are chopped into uniform sizes ranging from 0.1 mm for further analysis. Optical emission analysis reveals high recovery rates of metals (such as cobalt, chromium, lithium, nickel, cadmium, tantalum, gallium, germanium, manganese, rhenium, strontium and zirconium) that will be recovered by mature metal refining. A recovery or recycling rate of 98% was observed.

[0102] In the method according to (d), the raw materials are listed in the sixth column of the table, and a complete intelligent vehicle with a mass of 750 kg is used as the starting material of the method. Before the process, only liquids such as cooling fluids and brake fluids, engine oils and gasoline and batteries are removed. The solid residue of the processed complete vehicle removed from the reaction unit after the complete process has a mass of 450 kg. This substance consists of 30% carbon and 70% metals (such as steel, spring steel and precious metals). In addition, about 250 kg to 270 kg of light oil are recovered. The proportion of residual gas is about 6% to 8%. This leads to a recovery rate or utilization rate of 95%.

[0103] In the case of unground or ground rapeseed samples, the carbon content was determined according to the method of DIN / EN 12879 to be between 98.8% and 99.8%, while in the case of rapeseed grain samples for carbon black, the carbon content was determined to be in the range of 79.7% to 81.0%, in the case of plastic bottle samples, the carbon content was determined to be 99.1%, in the case of oak wood, the carbon content was determined to be 98.5%, in the case of industrial waste samples, the carbon content was determined to be 99.4%, and in the case of rubber waste, the carbon content was determined to be 99.4%. For rapeseed grain samples for oil, the carbon content was determined to be 99.5%.

[0104] The carbon / hydrogen and nitrogen contents according to ASTM D5291 and the oxygen content according to a method based on ASTM D5622 were determined in each case using a VARIO EL Cube from Elementar, and the fluorine and chlorine contents were determined by means of pyrolysis ion chromatography using an Analytik Jena combustion module, absorption module 920 or ion chromatograph 930 Compact IC Flex.

[0105] The vaporizable fraction up to 200° C. was determined by headspace GC-MS screening using a Trace GC Ultra coupled to a Thermo Scientific DSQ II mass spectrometer.

[0106] Hydrofluoric acid and nitric acid were determined by microwave digestion using an Ofen Model Star T from MWS GmbH, while trace elements, in particular the inorganic fraction, were determined by means of ICP OES using an ICP OES Arcos from Spectro.

[0107] Thermogravimetric analysis was performed using a Hi-Res TGA 2950 from TA Instruments.

[0108] Another significant advantage is that steel-rubber composites, which until now could only be separated with high energy expenditure, can be separated without using a large amount of external energy. The products produced can be put back into high-quality use in the spirit of an effective circular economy, which helps to save resources. The products produced include:

[0109] Light oil, for example, has a heat release rate of about 927 kg / m at 15°C. 3 Density, 4,74mm 2 / s viscosity and a flash point below 21°C,

[0110] ·gas,

[0111] Metals, primarily steel or iron and titanium, and

[0112] Amorphous inorganic carbon or carbon agglomerates.

[0113] According to the design, the amorphous inorganic carbon produced by the method for operating a device for material processing of carbon-containing raw materials according to the invention has a structure of three-dimensionally arranged carbon nanoparticles as agglomerates and, depending on the starting raw materials, advantageously has a purity ranging from 95% to 99.9%. These carbon nanoparticles are not long-range orderly cross-linked, do not exhibit any large-scale graphitized arrangement and are not arranged as nanotubes.

[0114] Carbon formed with a structure of three-dimensionally arranged nanoparticles is produced industrially by means of the device and method according to the invention and therefore has significant economic advantages over carbon obtained or produced in the laboratory known from the prior art. The purity of the carbon is significantly influenced by flushing with a gaseous flushing medium, in particular during the carbonization and distillation process or during the cooling of the reaction unit.

[0115] Depending on the starting raw materials, the carbon produced in the method for operating a plant for material processing of raw materials preferably has a carbon content of more than 2,500 m / s as determined by the method according to DIN ISO 9277. 2 / g BET, especially up to 9,500m 2 / g BET, specifically greater than 3,500m 2 / g BET or greater than 4,000m 2 / g BET, especially from 4,200m 2 / g BET to 4.500m 2 / g BET range and therefore have a very high adsorption capacity without any release of substances into the environment. The environment is therefore not contaminated, for example, by leaching.

[0116] The carbon produced by the method according to the invention preferably has a carbon content of about 66 kg / m3 density and can be advantageously designed to have greater tensile strength than alloy steel.

[0117] The carbon obtained in this way can have a 7 Ωm to 5.8·10 7 Electrical conductivity in the Ωm range. The electrical conductivity is determined by the method according to DIN EN ISO 15091.

[0118] The carbon produced in the method for operating a device for material processing of raw materials according to the invention is insoluble in concentrated or dilute cold acids, such as sulfuric acid, nitric acid, hydrochloric acid, and is not attacked by alkaline solutions. Nitric acid spontaneously decomposes into water and nitrous gas, which may indicate a catalytic effect. Neither polar organic solvents nor non-polar solvents can dissolve the carbon.

[0119] The recovered light oil is used, for example, in the chemical industry, in particular as a raw material for basic chemicals, and in the pharmaceutical industry, for example by means of CHP for the generation of heat and electricity, while the gas can be used for the generation of heat and electricity, for example by means of gas turbines and generators, or for recycling and use in the process. The recovered metals (such as steel) can be recycled into the steel industry, where the physical and chemical properties of the metal can be maintained by very low process temperatures.

[0120] Further details, features and advantages of the present invention will become clear from the following description of exemplary embodiments with reference to the accompanying drawings, in which:

[0121] Figure 1 : Industrial carbonization / distillation module as a device for material processing of raw materials, front view in the open state,

[0122] Figure 2a : An industrial carbonization / distillation module as a device for material processing of raw materials, side view in a closed state, and

[0123] Figure 2b : front view,

[0124] Figure 3 : Cross-section of the heating system in the open state,

[0125] Figure 4 : Cross-section of the heating system in the off state,

[0126] Figure 5 : bottom element of the heating system,

[0127] Figure 6 : Distillation unit,

[0128] Figure 7 : Oil tank, and

[0129] Figure 8a : the reaction unit is in the closed state, and

[0130] Figure 8b : Cross-sectional view of the reaction unit in the closed state,

[0131] Figures 9a to 9n : Microscopic image of carbon produced by the device for material processing of raw materials, and

[0132] Figure 9p and Figure 9q : Results of Raman spectroscopy of carbon.

[0133] exist Figure 1 , Figure 2a and Figure 2b In FIG. 1 , an industrial carbonization / distillation module is represented as an apparatus 1 for material processing of raw materials. Figure 1 The device 1 is shown in an open state in a front view, while Figure 2b Previous view and Figure 2a The device 1 is shown in a side view in the closed state.

[0134] The device 1 has a heating system 2 and a distillation unit 3. The reaction unit 4 filled with raw materials is preheated to a certain temperature in a preheating device (not shown) and then further heated in the heating system 2. The reaction unit 4 can be filled with a mixture of different raw materials, so that no pre-sorting of the product is required. After preheating, the reaction unit 4 is brought into the opened heating system 2 and positioned on the bottom element 5 of the heating system 2.

[0135] The head element 7 and the jacket element 8 (firmly connected to the head element 7) of the heating system 2 are movably held in the movement direction B by means of support elements 6 arranged on both sides of the heating system 2. The support elements 6 are arranged at a distance of about 2.9 m from each other. The jacket element 8 has an outer diameter of about 2.5 m.

[0136] In accordance with Figure 1 In the first end position, the support element 6 is extended. Thus, the device 1 has a height of about 6.70 m. The head element 7 and the jacket element 8 open up space for equipping the heating system 2 with the reaction unit 4. The heating system 2 is opened. The reaction unit 4 can be introduced into the heating system 2 or removed from the heating system 2. The movement of the reaction unit 4 can advantageously be carried out by means of a rail system (not shown) on which the reaction unit 4 stands. Figure 2a , Figure 2b In the second end position, the support element 6 is retracted. The device 1 thus has a height of approximately 3.70 m.

[0137] The jacket element 8 is placed on the bottom element 5 so that the reaction unit 4 is positioned in a closed space. The heating system 2 is closed. The reaction unit 4 is surrounded by the bottom element 5 at the bottom and by the jacket element 8 at the side surface and the top.

[0138] The device 1 has temperature sensors T1, T2, T3 in the region of the heating system 2 and the distillation unit 3 for determining certain process temperatures. When the heating system 2 is in the switched-off state, at least two temperature sensors T2, T3 are arranged in the intermediate space formed between the reaction unit 4 and the jacket element 8. The temperature sensors T2, T3 are positioned so as to protrude, for example, by about 1 cm from the interior of the jacket element 8 into the approximately 8 cm wide intermediate space. The temperature sensors T2, T3 are arranged at a vertical distance from one another in order to determine local temperature values ​​or average temperatures in the intermediate space. The temperature values ​​determined via the temperature sensors T2, T3 are used to determine the temperature in the reaction unit 4.

[0139] The heating system 2 has in the lower region a housing 9. The housing 9 closing the side surfaces of the bottom element 5 and the jacket element 8 is opened in order to equip the heating system 2 when the heating system 2 is in the closed state.

[0140] The gas produced during the carbonization process is discharged from the heating system 2 through the exhaust line 11 provided and is cooled down according to the process technology. The gas is passed to the distillation unit 3 through the exhaust port 10a formed at the uppermost point of the reaction unit 4 and through the exhaust line 11 arranged in the head element 7. Subsequently, the gas flows through the cooling section 12 of the distillation unit 3. The cooling section 12 is composed of a cooling section 12 according to Figure 1 , Figure 2a , Figure 2b These tubes, which are inclined relative to the horizontal, are provided with ribs in order to increase the heat transfer surface and thus improve the heat transfer from the gas to the ambient air.

[0141] In order to further increase the heat output to be transferred from the gas to be cooled to the ambient air, and in particular, to improve the control of the temperature of the gas 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 end face of the air guide housing 12-1 pointing upward in the vertical direction, which fans draw the ambient air as cooling air uniformly through the air guide housing 12-1. Alternatively, these fans can also be formed on the side surface of the air guide housing 12-1. In this case, the ambient air is guided through the cooling section 12 in a targeted manner. A further temperature sensor T1 is arranged on the exhaust line 11 formed between the heating system 2 and the distillation unit 3 in order to determine the temperature of the exhaust gas discharged from the heating system 2.

[0142] According to an alternative embodiment, the gas in the cooling section can also be cooled with a heat transfer fluid other than air, for example water. In this case, instead of the tubes, the cooling section is formed with ribs of coaxial tubes formed on the surface of the outer jacket. The gas flows inside the inner tube, while a preferably liquid heat transfer fluid passes in the intermediate space between the outside of the inner tube and the inside of the outer tube.

[0143] The cooling section 12 is formed with two tubes aligned parallel to each other. The gas is divided into two partial mass flows before entering the cooling section 12 and is mixed again after flowing through the cooling section 12.

[0144] Subsequently, the distillation product is introduced into the oil tank 13. In the oil tank 13, the oil obtained from the carbonization process and the subsequent distillation, whose consistency and composition correspond to light oil or an intermediate very similar to crude oil processing, settles. The non-condensable part of the gas is discharged from the oil tank 13. The oil tank 13, which has a capacity of about 1,000 liters, also serves as an expansion vessel for the device 1.

[0145] An extraction device 14-1, in particular a pump, in particular a diaphragm pump, for extracting gas via the surface of the oil accumulated in the oil tank 13, and an oil delivery device 14-2, in particular a pump, in particular a piston pump, for delivering oil from the oil tank 13 are arranged on the oil tank 13. When these gases are extracted, a negative pressure is generated in the cooling section 12 of the distillation unit 3, in the exhaust line 11 and in particular in the reaction unit 4. Air and therefore oxygen as a component of air are also purposefully extracted from the reaction unit 4 by the extraction device 14-1. A vacuum can thus be generated in the reaction unit 4.

[0146] The gas extracted above the surface of the oil accumulated in the tank 13 can be used directly with a combined heat and power plant called CHP for generating heat and electricity.

[0147] The device 1 is also formed with a control device 15 for controlling the method for operating the device 1. The control device 15 determines and indicates, for example, the filling level in the oil tank 13, the flow of oil or gas, and possible defects in the pipeline of the device 1. The control device 15 is connected to corresponding sensors. Temperature sensors T1, T2, T3 are also connected to the control device 15. The values ​​determined by the temperature sensors T1, T2, T3 are used for controlling the device 1, in particular the heating system 2, and therefore for heating the fan 12-2 of the reaction unit 4 and the cooling section 12 and the extraction device 14-1. The control device 15 can be used in particular for indicating the state and process temperature of the different heating circuits of the heating system 2. The arrangement of the sheath element 8 of the heating system 2 can also be determined and shown as being in an open, closed and partially open state. Therefore, the control device 15 is also used for extending and retracting the support element 6 to open and close the heating system 2.

[0148] Figure 3 and Figure 4 Each shows a cross-sectional view of a heating system 2 . Figure 3 represents the heating system 2 being on, and Figure 4 Indicates a heating system that is switched off.

[0149] according to Figure 3 , the support element 6 is fully extended. The head element 7 arranged at the upper end of the support element 6 and the sheath element 8 firmly connected to the head element 7 are arranged at a height H above the bottom element 5, so that the reaction unit 4 can move freely in the horizontal direction between the bottom element 5 and the sheath element 8.

[0150] The housing element 8 is movably supported in the lower region on the support element 6. By means of the lateral support on the support element 6, a linear movement of the housing element 8 between the end positions in the movement direction B is ensured. Tilting of the housing element 8 is avoided.

[0151] The jacket element 8 has heating elements 16a uniformly distributed on the circumference of the inner surface of the jacket. The heating elements 16a are arranged essentially in the vertical direction and are guided through the wall to the inner surface in the lower region of the jacket element 8. The heating elements 16a are each formed by two vertically aligned sections, which are connected to each other at the upper end by means of deflection.

[0152] The jacket element 8, which is open downward in the vertical direction, is closed at the top by a cover 17 and is fastened to the head element 7. The head element 7 and the jacket element 8 form a connected unit. The cover 17 is formed with an exhaust port 10b at a central point, which serves as a connection to the exhaust line 11a. The exhaust line 11a extends from the exhaust port 10b through the cover 17 into the head element 7. The passage of the exhaust line 11a through the cover 17 is sealed relative to the cover 17. The exhaust line 11a is formed with a pipe connection 19 in the region of the exhaust port 10b, which can change the length in the vertical direction, for example in the form of a telescopic pipe. The pipe connection 19, which can be automatically adjusted in length, is used to compensate for the thermal expansion of the reaction unit 4, in particular the thermal expansion of the jacket element 8 with the cover 17 relative to the heating system 2.

[0153] The exhaust gas line 11a forms the transition from the reaction unit 4 to the distillation unit 3 via a heating device 20. The electrically operated heating device 20 surrounding the exhaust gas line 11a is connected to the control device 15, as is the temperature sensor T1.

[0154] In addition, the exhaust line 11a has a connecting element 11-1 for connecting the exhaust line 11a to a device for receiving a gaseous flushing medium (e.g., nitrogen). The flushing 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 surrounded by the heating device 20, in particular at the highest point of the exhaust lines 11, 11a in the vertical direction.

[0155] The exhaust line 11a has a connection element 18 at the distal end starting from the exhaust port 10b. Figure 4 When the heating system 2 is in the switched-off state, the connecting element 18, advantageously formed as a quick-connect coupling, serves to connect the exhaust line 11a of the heating system 2 to the exhaust line 11b of the distillation unit 3. Due to the downward movement of the head element 7 when the heating system 2 is switched off, the exhaust lines 11a, 11b on the connecting element 18 and the exhaust ports 10a, 10b are coupled to one another, so that a gas-tight connection from the reaction unit 4 to the distillation unit 3 is produced.

[0156] The reaction unit 4 arranged on the bottom element 5 is formed with a wall 21 in the form of a hollow cylindrical vessel, the wall having an outer diameter of about 1.8 m, which is closed at the bottom. 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 closed. A screen element 23 is formed inside the reaction unit 4. The screen elements 23 are aligned in the horizontal direction and are spaced apart from each other and arranged at different heights.

[0157] exist Figure 4 In the second end position shown, the support element 6 is completely retracted. The jacket element 8 rests on the bottom element 5 and completely closes the reaction cell 4. The heating system 2 is switched off.

[0158] The reaction cell 4 filled with raw materials is advantageously heated uniformly on the bottom and the wall 21. The heating element 16a is used for heating via the wall 21, while the heating element 16b arranged on the bottom element 5 supplies heat to the reaction cell 4 through the bottom. When the heating system 2 is in the closed state, the heating elements 16a formed on the circumference of the jacket element 8 are at an equal distance from the wall 21 of the reaction cell 4. The heating elements 16a, 16b are preferably electrically operated.

[0159] The reaction unit 4 is kept in the heating system 2 for a period of about 2.5h to 3.5h, wherein the main reaction and conversion of the raw materials occur in the reaction unit 4. The reaction temperature in the reaction unit 4 is between 350°C and 800°C, in particular between 400°C and 600°C, in particular about 550°C, depending on the feed and on the final product to be produced. This temperature is determined by means of temperature sensors T2, T3 arranged between the reaction unit 4 and the jacket element 8. This consumes energy in the range of 40kWh per hour. The reaction unit 4 is filled with raw materials with a mass in the range of from 2.5t to 3t.

[0160] The gases formed during the carbonization process are discharged through the exhaust port 10 arranged on the cover element 22, in particular extracted into the exhaust line 11. When the heating system 2 is in the closed state, the exhaust port 10a of the reaction unit 4 and the exhaust port 10b of the cover 17 of the jacket element 8 are connected to each other in a gas-tight manner. This ensures that no gas can escape into the intermediate space between the reaction unit 4 and the jacket element 8.

[0161] Inside the reaction unit 4, there is a negative pressure with an absolute value in the range of from 2 mbar to 10 mbar, specifically about 4 mbar, which is generated by an extraction device 14-1 arranged at the first outlet port of the oil tank 13, which is used to extract gas via the surface of the oil accumulated in the oil tank 13. With the targeted extraction of oxygen from the reaction unit 4, on the one hand, the reaction temperature or the process temperature in the reaction unit 4 is reached in a shorter time. On the other hand, this affects the structural formation of carbon as the final product. Another factor that affects the formation and purity of carbon is the duration of the carbonization process. The longer the carbonization process takes place, the cleaner the carbon is, and depending on the starting material, the carbon can also be used for medical purposes, for example. If necessary, the carbon used for medical purposes should be purified in addition. The carbon recovered during the relatively short carbonization process is preferably used as, for example, a filter material or in the construction industry.

[0162] Factors influencing the formation and purity of the carbon also include flushing the reaction unit 4 with a gaseous flushing medium, in particular nitrogen, during the carbonization and distillation process on the one hand and during the cooling process of the reaction unit 4 on the other hand.

[0163] By means of a heating device 20 surrounding the exhaust line 11a, the exhaust line 11a is heated, in particular to a temperature in the range from 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 exhaust gas flowing through is determined by means of a 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 prevents undesired blockage of the exhaust line 11a. The heating of the exhaust line 11a supports the outflow of the exhaust gas from the reaction unit 4.

[0164] exist Figure 5 , a bottom element 5 of the heating system 2 is shown. The bottom element 5 has a base plate 24 and a centering device 25 for the jacket element 8, a heating element 16b and a support element 28 for holding the reaction unit 4. The bottom element 5 is essentially formed of ceramic in order to ensure thermal insulation towards the outside, in particular towards the bottom. In combination with the thermal insulation of the jacket element 8, the heat losses of the heating system 2 are therefore minimized.

[0165] The reaction unit 4 stands on a support element 28 of the base plate 24. The support element 28 is formed and arranged such that the reaction unit 4 is aligned centrally with the bottom element 5 when it rests on the support element 28.

[0166] The centering device 25 is formed in the form of a circular disk with a shoulder. The disk thus has two regions with different diameters. The circular surface arranged between these regions serves as a sealing surface 27.

[0167] The outer circumference of the region with smaller diameter of dish is less than the inner circumference of the wall 21 of reaction unit 4 or sheath element 8.When heating system 2 is in closed state, a gap is formed between the sheath surface 26 in the region with smaller diameter of dish and the inboard of wall 21.Sheath element 8 stands on the sealing surface 27 of base plate 24 so that the space enclosed by sheath element 8 and base plate 24 is tightly enclosed.Seal is arranged on the corresponding surface of base plate 24 and sheath element 8, so that the sealed enclosed space.In addition, sheath element 8 is pressed and remains on the sealing surface 27 of base plate 24, and pressure is in the range of from 1 bar to 2 bar.

[0168] Since the supporting element 6 is also fastened to the base plate 24 , the base plate 24 carries the entire heating system 2 .

[0169] The heating elements 16 b are arranged substantially horizontally on the end surface 29 of the centering device 25 and are guided vertically through the end surface 29. The heating elements 16 b bent in a meandering manner each have the form 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 16 b are aligned symmetrically with each other, wherein the tips of the fingers point to the center point of the end surface 29.

[0170] The support element 28 on which the reaction unit 4 stands protrudes in the vertical direction beyond the heating element 16b, so that the bottom of the reaction unit 4 standing on the support element 28 is arranged above the heating element 16b. The heating elements 16b are each at the same distance from the bottom of the reaction unit 4 to ensure that heat is introduced uniformly through the bottom of the reaction unit 4.

[0171] The centering device 25 , the supporting element 28 and the heating element 16 b are arranged concentrically around the center point of the base plate 24 .

[0172] Figure 6 A distillation unit 3 is shown which has, in order of flow direction of the end product, an exhaust line 11 b , a cooling section 12 with an air guiding housing 12 - 1 and a fan 12 - 2 , and an oil tank 13 with an extraction device 14 - 1 and an oil delivery device 14 - 2 .

[0173] The gases discharged from the heating system 2 pass through the exhaust line 11 b to the cooling section 12, which is also formed by pipes. The gas mass flow at the branch 30 is divided into two partial mass flows by two pipes aligned parallel to each other. The division of the gas mass flow allows a better heat transfer from the gas mass flow to the environment in order to optimize the distillation or condensation process.

[0174] In order to further improve the heat transfer, the tubes are formed with ribs in order to increase the heat transfer surface of the cooling section 12. The heat output to be dissipated from the gas to be cooled, in particular the heat of condensation, is further increased and is controlled simultaneously by the air guide housing 12-1 and the fan 12-2. Ambient air is uniformly sucked in as cooling air through the air guide housing 12-1 and is guided in a targeted manner through the cooling section 12. The corresponding power or air volume flow of the fan 12-2 ensures that the exhaust gas 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 inflow into the cooling section 12, the cooling section 12 is cooled to a temperature below the gas condensation temperature or is kept at a corresponding temperature level. By controlling the heat output in this way, a higher oil yield is achieved with a lower residual gas yield. According to Figure 1 The temperature is determined by means of a temperature sensor T1 which is arranged on the exhaust gas line 11 formed between the heating system 2 and the distillation unit 3 .

[0175] After flowing through the cooling section 12 , the partial mass flows which were divided before entering the cooling section 12 are recombined at the opening point 31 and introduced into the oil tank 13 from above through the inlet port 32 .

[0176] Oil having a greater density than the gas is deposited in the oil tank 13. The non-condensable part of the distillation product is removed in the upper region of the oil tank 13 through the first outlet port 33. In order to extract the gas via the surface of the oil accumulated in the oil tank 13, the extraction device 14-1 is arranged at the first outlet port 33 of the oil tank 13. With the extraction of the gas and the negative pressure thus generated in the device 1, in particular air and therefore oxygen as an air component are extracted from the reaction unit 4, and the carbonization process is affected.

[0177] In order to deliver oil from the oil tank 13 , the oil delivery device 14 - 2 is arranged on the second outlet port 34 of the oil tank 13 .

[0178] exist Figure 7 , the oil tank 13 is shown with a cut-away side surface to observe the interior.

[0179] The inlet port 32 is arranged on the upper side of the oil tank 13 so that the distillation product flows into the oil tank 13 from above. The oil settles at the bottom of the oil tank 13, while the gas, which is less dense than the oil, collects above the oil level. The oil level in the oil tank 13 is determined and observed using a float 35. When a predetermined filling height is reached, the oil is removed from the oil tank 13 for further processing.

[0180] Gas accumulated in the upper region of the oil tank 13 is discharged through the first outlet port 33, in particular extracted by means of the extraction device 14-1, while oil accumulated in the lower region of the oil tank 13 is extracted through the second outlet port 34, in particular by means of the oil delivery device 14-2.

[0181] exist Figure 8a and Figure 8b , the reaction unit 4 is shown in a closed state, wherein Figure 8b A cross-sectional view of a reaction unit 4 is shown.

[0182] The wall 21 in the form of a hollow cylindrical vessel with a closed bottom can be closed at the open side opposite the bottom by means of a cover element 22. During the procedure of closing the reaction unit 4, the cover element 22 is placed in the vertical direction on the upwardly pointing end face of the wall 21. Due to its own weight, the cover element 22 presses against the end face of the wall 21 and is releasably supported on the wall 21.

[0183] A high temperature resistant seal is arranged between the wall 21 and the cover element 22 for closing the reaction unit 4 in a tight manner. In the closed state, the reaction unit 4 has a height of approximately 2.4 m.

[0184] The cover element 22 is formed next to the exhaust port 10a with a connection port 36. A device for introducing a gaseous flushing medium, in particular nitrogen, into the reaction unit 4 can be connected to the connection port 36.

[0185] The actual carbonization / distillation process, in which the reaction unit 4 is arranged in the heating system 2 and is heated or substantially maintained at the desired reaction temperature, ends at an exhaust gas temperature of about 60° C. determined by a temperature sensor T1 arranged 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 in the range of, for example, from 500° C. to 600° C.

[0186] After being removed from the heating system 2, the reaction unit 4 is cooled to a temperature defined according to the use of the product. After the reaction unit 4 has been opened, i.e. after the cover element 22 has been removed, the mixture located inside the reaction unit 4 is removed. The reaction unit 4 is then fed back into the process and filled. The carbon-iron mixture is separated into its components.

[0187] The recovered unique carbon is further formed in an oxygen-free atmosphere without oxygen during the cooling process between 600°C and 60°C or 20°C or 30°C in the reaction unit 4. In this case, a gaseous flushing medium, in particular nitrogen, flows into the reaction unit 4 through the connection port 36, which also affects the cooling process. Alternatively, the gaseous flushing medium can be introduced through the exhaust port 10a, to which a device for introducing a gaseous flushing medium can be connected, in particular when the connection port 36 is not formed. During the cooling process and therefore before emptying the reaction unit 4, the inflow of the flushing medium can accelerate the cooling process, but most importantly, it is used to clean the final product, and therefore can also support the formation of carbon recovered by the device 1. Flushing the reaction unit 4 improves the purity of the final product, in particular the purity of the carbon. Impurities are flushed away. The flushing medium that flows into the reaction unit 4 through the connection port 36 is discharged from the reaction unit 4 again together with the impurities through the exhaust port 10a formed in the cover element 22. The reaction unit 4 is opened when the temperature within the reaction unit 4 is in the range from 20°C to 60°C, in particular in the range from 30°C to 60°C.

[0188] During the procedure of opening the reaction unit 4, the cover element 22 is raised in the vertical direction and removed from the reaction unit 4, so that the reaction unit 4 can be emptied and then filled again. The reaction unit 4 can also be filled with a flushing medium during the emptying procedure in order to obtain a desired purity of the final product, in particular carbon. The carbon is preferably extracted during the emptying of the reaction unit 4.

[0189] The carbonization / distillation process for the material treatment of the raw materials simultaneously involves four reaction units 4 made of high temperature resistant steel, each with a filling amount ranging from 2.5 t to 3.5 t (75% mechanical, 25% automatic). When the first reaction unit 4 is filled, the already filled second reaction unit 4 is preheated. At the same time, the third reaction unit 4 has been fed into the heating system 2 and heated, so that the actual carbonization / distillation process takes place. At the same time, the fourth reaction unit 4 is cooled and then emptied.

[0190] By using a modular system, for example with four reaction units 4, the production capacity can be increased stepwise and flexibly adapted to the respective requirements. The entire process is carried out quasi-continuously.

[0191] exist Figures 9a to 9n, a microscopic image of carbon produced using a device 1 for material processing of raw materials is shown. The structure of the carbon can be seen from the image produced using a transmission electron microscope (TEM for short). Transmission electron microscopes are used to detect and characterize the structure and particle size of substances and substance mixtures in the nanometer range.

[0192] These images show a very finely divided, three-dimensional, homogeneous pseudomorphic structure of primary carbon particles in the subnanometer range with a very large inner surface. These carbon particles are partially recognizable as larger agglomerates with the same surface structure.

[0193] Figure 9p and Figure 9q The Raman spectrum of carbon is shown in Figure 2. -1 The lack of a 2D maximum at indicates the absence of large-scale graphitized arrangement. The carbon produced using the apparatus 1 for material processing of raw materials is an amorphous inorganic carbon in which the nanoparticles are not cross-linked in a long-range orderly manner. The carbon is neither a nanotube nor structurally similar to graphene.

[0194] The imaging of Raman spectra and the determination of the intensity and width of the G-Raman and D-Raman bands can be accomplished using a Renishaw inVia confocal Raman microscope using 532 nm and 785 nm lasers.

[0195] List of Reference Numerals

[0196] 1 Devices for material handling

[0197] 2 Heating system

[0198] 3 Distillation unit

[0199] 4 Reaction unit

[0200] 5 Bottom element of heating system 2

[0201] 6 Support elements

[0202] 7 Head element of heating system 2

[0203] 8 Sheath element of heating system 2

[0204] 9. Housing

[0205] 10, 10a, 10b Exhaust port

[0206] 11, 11a, 11b Exhaust lines

[0207] 11-1 Connection elements of exhaust lines 11, 11a

[0208] 12 Cooling section of distillation unit 3

[0209] 12-1 Air guide housing

[0210] 12-2 Fan

[0211] 13 Oil Tank

[0212] 14-1 Extraction device

[0213] 14-2 Oil transfer device

[0214] 15 Control Device

[0215] 16a, 16b Heating element

[0216] 17 Hood

[0217] 18 Connecting element of exhaust line 11, 11a

[0218] 19 Pipe connector

[0219] 20 Heating device

[0220] 21 Wall of reaction unit 4

[0221] 22 Cover element

[0222] 23 Screen element

[0223] 24 Base Plate

[0224] 25 Centering device for sheath element 8

[0225] 26. Surface of the jacket of the centering device 25

[0226] 27 Sealing surface of centering device 25

[0227] 28 Support element for reaction unit 4

[0228] 29 End surface

[0229] 30 branches

[0230] 31 Opening point

[0231] 32 Inlet port of oil tank 13

[0232] 33 First outlet port of oil tank 13

[0233] 34 Second outlet port of oil tank 13

[0234] 35 Float

[0235] 36 Connection port of cover element 22

[0236] B Moving direction of heating system 2

[0237] H Height

[0238] T1, T2, T3 temperature sensors

Claims

1. A device (1) for material processing of raw materials, comprising a heating system (2), a distillation unit (3) and a reaction unit (4) and a control device (15), wherein: the heating system (2) is formed such that it can be switched on and off in order to fill the reaction unit (4), - the distillation unit (3) has a cooling section (12), and - the reaction unit (4) is formed so that it can be filled with the raw materials, Wherein, an exhaust line (11, 11a, 11b) for discharging waste gas from the reaction unit (4) is formed between the reaction unit (4) and the distillation unit (3), characterized in that: - temperature sensors (T1, T2, T3) are formed in the region of the heating system (2) and the distillation unit (3), - the cooling section (12) of the distillation unit (3) is formed with a device for forced cooling, wherein the cooling section (12) - is arranged in an air guide housing (12-1) which serves to route ambient air in a targeted manner through the cooling section (12), and / or - is formed by at least one coaxial tube for conducting a gas inside an inner tube and for conducting a heat transfer fluid in an intermediate space between the outside of the inner tube and the inside of the outer tube, and - an extraction device (14-1) for extracting gas from the reaction unit (4) and generating negative pressure is formed in the reaction unit (4), The temperature sensors (T1, T2, T3) and the extraction device (14-1) are connected to the control device (15).

2. The device (1) according to claim 1, characterized in that At least two of the temperature sensors (T2, T3) for determining the temperature in the reaction unit (4) are arranged in an intermediate space formed between the reaction unit (4) and a sheath element (8) of the heating system (2) when the heating system (2) is in the off state.

3. The device (1) according to claim 1 or 2, characterized in that The exhaust gas pipeline (11) between the heating system (2) and the distillation unit (3) is formed with a heating device (20) for heating the exhaust gas pipeline (11), wherein the heating device (20) is connected to the control device (15).

4. The device (1) according to any one of claims 1 to 3, characterized in that At least one temperature sensor (T1) for determining the temperature of the exhaust gases emitted from the heating system (2) is arranged on the exhaust line (11) between the heating system (2) and the distillation unit (3).

5. The device (1) according to any 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 formed with a connecting element (11-1) for connecting to a device for introducing a gaseous flushing medium, in particular into the reaction unit (4).

6. The device (1) according to any one of claims 1 to 5, characterized in that Fans (12-2) for conducting ambient air in a targeted manner through the cooling section (12) are formed in the 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).

7. The device (1) according to claim 6, characterized in that The fans (12-2) are arranged on the upper side, in particular on the end face pointing upward in the vertical direction, or on the side surface of the air guiding housing (12-1).

8. The device (1) according to any one of claims 1 to 7, characterized in that The extraction device (14-1) is arranged downstream of the oil tank (13), which is arranged downstream of the distillation unit (3) in the flow direction of the gases.

9. The device (1) according to any one of claims 1 to 8, characterized in that The heating system (2) comprises a head element (7) and a sheath element (8) and support elements (6), the sheath element being formed to be firmly connected to the head element (7), the support elements being able to vary in length in the vertical direction, wherein the head element (7) is arranged to be held on the support elements (6) so that the heating system (2) is opened and closed in the vertical movement direction (B) by varying the length between two end positions of the support elements (6).

10. The 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).

11. The device (1) according to claim 9 or 10, characterized in that The sheath element (8) has a hollow cylindrical wall which is formed so that it is - Open at the bottom and - It is closed at the top by a circular cover (17) and is connected to the head element (7) at the cover (17).

12. The device (1) according to claim 11, characterized in that The cover (17) is formed with an exhaust port (10b) at a central point, which serves as a connection to an exhaust line (11a), wherein the exhaust line (11a) extends from the exhaust port (10b) through the cover (17) into the head element (7).

13. The device (1) according to claim 12, characterized in that The exhaust line (11a) is formed with an automatically longitudinally variable pipe connection (19) for compensating for thermal expansion in the region of the exhaust port (10b).

14. The device (1) according to any one of claims 1 to 13, characterized in that The reaction unit (4) is formed with a wall (21) in the form of a hollow cylindrical vessel, which is closed at the bottom and the open side of which can be closed by means of a cover element (22).

15. The device (1) according to claim 14, characterized in that The cover element (22) of the reaction unit (4) is formed circularly and has an exhaust port (10a) at the center point, wherein the exhaust port (10a) of the cover element (22) and the exhaust port (10b) of the sheath element (8) engage with each other and form a sealed connection to the exhaust line (11a) when the heating system (2) is in a closed state.

16. The device (1) according to claim 14 or 15, characterized in that The cover element (22) of the reaction unit (4) is formed with a connection port (36) for connecting to a device for allowing a gaseous flushing medium to enter the reaction unit (4).

17. A method for operating a device (1) for material processing of raw materials according to any one of claims 1 to 16, the method comprising the following steps: - filling the reaction unit (4) with raw materials, - preheating the reaction unit (4), - opening the heating system (2) and bringing the reaction unit (4) into the heating system (2), - shutting down the heating system (2) so that the reaction unit (4) is arranged in a closed space, - heating the reaction unit (4) and starting the carbonization and distillation process, wherein The carbonization and distillation process is carried out by selective heating at a substantially constant temperature in the reaction unit (4), wherein the temperature is determined, - discharging the produced gas from the reaction unit (4) into the distillation unit (3) through a gas exhaust line (11, 11a) formed between the reaction unit (4) and the distillation unit (3) and determining the temperature of the gas flowing through the gas exhaust line (11, 11a), - cooling and condensing the gases in the distillation unit (3), wherein the temperature of the gases is controlled by forced cooling of the cooling section (12) of the distillation unit (3) by means of the heat output dissipated by the gases, - introducing the distillation product into the oil tank (13) and discharging the oil, - extracting non-condensable gases from the tank (13), wherein a negative pressure relative to the environment is generated in the reaction unit (4) 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).

18. The method according to claim 17, characterized in that The pressure in the reaction unit ( 4 ) is adjusted to an absolute value in the range from 2 mbar, in particular from about 4 mbar to 10 mbar.

19. The method according to claim 17 or 18, characterized in that In order to cool and condense the gases in the distillation unit (3), - the ambient air is guided in a targeted manner through the cooling section (12) of the distillation unit (3); or A liquid heat transfer fluid, in particular water, flows through the cooling section (12) as a coolant.

20. The method according to any 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 ranges from 95°C to 125°C.

21. The method according to any one of claims 17 to 20, characterized in that During the carbonization and distillation process, the exhaust 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.

22. The method according to any one of claims 17 to 21, characterized in that The reaction unit (4) is removed from the heating system (2) when the temperature of the gas flowing through the exhaust line (11, 11a) is about 60°C.

23. The method according to any one of claims 17 to 22, characterized in that During the carbonization and distillation process and / or during the procedure of cooling the reaction unit (4), a gaseous flushing medium is introduced into the reaction unit (4).

24. The method according to claim 23, characterized in that The gaseous flushing medium flows into the reaction unit (4) at respective time intervals.

25. The method according to claim 24, characterized in that The extraction of non-condensable gases and the flow of the flushing medium into the reaction unit (4) take place offset in time relative to one another.

26. The method according to claim 24 or 25, characterized in that During the procedure of cooling the reaction unit ( 4 ), the flushing medium flows periodically into the reaction unit ( 4 ), in each case for a duration ranging from two minutes to three minutes.

27. The method according to any one of claims 17 to 26, characterized in that The reaction unit (4) is opened when the temperature within the reaction unit (4) is in the range from 20°C to 60°C, in particular in the range from 30°C to 60°C, in order to remove the end products.

28. The method according to any 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 filled with a gaseous flushing medium.

29. The method according to any 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.

30. The method according to any one of claims 17 to 29, characterized in that The heating system (2) is switched on and off by extending and retracting the support element (6).

31. The method according to any one of claims 17 to 30, characterized in that The extracted non-condensable gases are used for combustion within the heating system (2) and for heating the reaction unit (4) of the heating system (2).

32. Carbon produced by the method according to any one of claims 17 to 31 for operating an apparatus (1) for material processing of carbonaceous raw materials according to any one of claims 1 to 16, characterized in that The carbon is amorphous and has a structure of three-dimensionally arranged carbon nanoparticles as agglomerates, wherein the carbon nanoparticles are not crosslinked in a long-range orderly manner, do not have a large-scale graphitized arrangement, and are not arranged into nanotubes.

33. The carbon according to claim 32, characterized in that The carbon has a mass greater than 2,500 m 2 / g BET, especially up to 9,500m 2 / g BET, specifically greater than 3,500m 2 / g BET or greater than 4,000m 2 / g BET, especially from 4,200m 2 / gBET to 4,800m 2 / g mass-dependent specific surface area in the BET range.

34. Carbon according to claim 32 or 33, characterized in that The carbon has a mass of about 66 kg / m 3 density.

35. Carbon according to any one of claims 32 to 34, characterized in that The carbon has a 7 Ωm to 5.8·10 7 Conductivity in the Ωm range.

36. Use of the device (1) for material processing of raw materials according to any one of claims 1 to 16 for producing carbon according to any one of claims 32 to 35.

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