Equipment and methods for processing raw materials and carbon produced using said methods

Abstract

The present invention relates to an apparatus (1) for raw material processing. The apparatus (1) comprises 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 to receive raw materials for processing. The heating system (2) can be opened or closed to charge the reaction unit (4). To discharge exhaust gas from the reaction unit (4), exhaust gas channels (11, 11a, 11b) are provided between the reaction unit (4) and the distillation unit (3). The distillation unit (3) has a cooling section (12) including equipment for forced cooling. The cooling section (12) is located inside an air guide housing (12-1) for targeted guidance of ambient air through the cooling section (12) and / or is formed from at least one coaxial tube for passing gas and heat transfer fluid. Temperature sensors (T1, T2, T3) are provided in the area of the heating system (2) and the distillation unit (3). An aspirator (14-1) is provided inside the reaction unit (4) to extract gases from the reaction unit (4) and to create a vacuum. The temperature sensors (T1, T2, T3) and the aspirator (14-1) are connected to a control device (154). The invention also relates to a method for operating the apparatus (1) for raw material processing and to carbon produced using said method.

Description

[Technical Field]

[0001] The present invention relates to an apparatus for processing raw materials. The apparatus comprises a heating system, a distillation unit, and a reaction unit, as well as a control device. The reaction unit can be charged with raw materials for processing. The heating system can be opened or closed to charge the reaction unit.

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

[0003] The prior art provides known devices for the industrial processing of waste rubber products, rubber products, or rubber-like composite products, such as used tires, steel-reinforced rubber belts, rubber-impregnated chain links, conveyor belts, as well as crushed car scrap, organic renewable raw materials, such as wood, contaminated carbon, and contaminated soil. Light oil, gas, metals, especially steel, and carbon are obtained. Conventional plants are based, for example, on rotary kilns, fluidized bed reactors, and drums, and on the use of compressed starting materials processed in an oxygen-free, chemically inert atmosphere.

[0004] German Patent No. 19930071C2 describes a method and apparatus for the recovery of organic substances and substance mixtures. The organic material is brought into contact with the fluidized bed material of a combustion fluidized bed. This method produces a gaseous end product, condensable substances, and a carbon-containing residue.

[0005] German Patent No. 4441423A1 discloses a method and device for obtaining usable gas from waste. The crushed waste is introduced into an airtight sealed drum. In the drum, gas is produced and separated from the simultaneously formed residue. The produced gas is split into cracking gas in a gas converter supplied with air in the presence of a combustion bed of coke. The heat required for this process is transferred by the gas, which is in direct contact with the material to be recycled. A partial flow of the cracking gas leaving the gas converter is used to transfer heat to the gas.

[0006] German Patent No. 4011945C1 discloses a method for degassing organic materials, such as municipal or industrial waste, in a heatable chamber. In this method, the starting material is introduced into the chamber in a compressed state and is distributed over the entire cross-section of the chamber while remaining compressed. Heat is supplied through the chamber wall, which is in pressure contact with the compressed material. The gas products formed are removed by increasing the pressure. The chamber is sealed airtight in the area where the compressed material was introduced. Compressing the solid residue makes it possible to increase the flow resistance in the area where the gas products exit.

[0007] German Patent No. 3932803A1 discloses a method for obtaining carbon and graphite by reacting organic materials with boric acid / boron oxide additives and organic nitrogen compounds in a non-oxidizing atmosphere.

[0008] The operation of conventional plants requires increased expenditures on materials, energy, and logistics. Thus, for example, the creation of a fluidized bed in a fluidized bed reactor requires increased energy expenditures, since on the one hand the fluidized bed must be created and maintained, and on the other hand the materials to be utilized must be mechanically kneaded so that they effectively come into contact with the fluidized bed. Crushing or crushing or compressing the starting materials during preparation and recycling procedures also involves high energy costs.

[0009] WO 2007 / 053088 A1 describes a method and apparatus for processing materials from hydrocarbons. The material is fed into an inner vessel, which in turn can be placed in an outer vessel. Both vessels are each closed with a cover member. The hydrocarbon material is heated by microwave or radio frequency radiation. The resulting exhaust gases are discharged from the vessels through a gas outlet. Two or more containers can be operated in parallel and connected to a gas cleaning system to maintain a nearly continuous gas flow through the gas cleaning system.

[0010] WO 2010 / 012275 A2 discloses an apparatus and process control for processing materials in a cylindrical furnace. The interior surface of the furnace is provided with an insulating layer of inorganic insulating material. Heating elements are positioned against or above the interior surface of the insulating layer. Controlling the process by controlling the temperature of the heating elements helps to achieve high yields of carbon, oil, and fuel gas.

[0011] German Patent Application Publication No. 102012109874A1 discloses an apparatus for processing raw materials, including a heating system, a distillation unit, and a reaction unit into which the raw materials can be charged, as well as a method for operating such an apparatus. The heating system can be opened and closed so that the reaction unit can be filled, and includes an upper member, a jacket member firmly connected to the upper member, and a support member. The upper member is connected to the support member, the length of which can be changed in the vertical direction, and the heating system is opened and closed in the vertical direction by changing the length between the two limit positions of the support member. Summary of the Invention [Problem to be solved by the invention]

[0012] The object of the present invention is to provide an improved apparatus and method for the treatment of various used rubber products, in particular used tires, and rubber composite or rubber-like composite products; renewable raw materials such as wood, shells, or fruit; scrap electronics such as computers and mobile phones; storage media such as automobiles and batteries; and contaminated carbon. The composite products are separated, and valuable components such as carbon, diesel, gas, and, if appropriate, metallic materials are recovered. The contaminated carbon should be separated from the respective impurities. The apparatus should be able to operate in a cost-effective manner with minimal energy input, and the method should be able to be carried out with minimal expenditure, especially in terms of time. The raw materials recovered by this method should be kept as unchanged as possible in their original structure, for example, so that they can be returned to their original use. In addition, the carbon recovered by this method should have advantageous material properties different from those of conventional carbon. [Means for solving the problem]

[0013] The object is achieved by an apparatus for processing raw materials according to the present invention. The apparatus comprises a heating system, a distillation unit, a reaction unit, and a control device. The reaction unit can be filled with raw materials. The heating system can be opened and closed to allow filling with the reaction unit. An exhaust gas flow path for discharging exhaust gas 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 present invention, temperature sensors are formed in the region of the heating system and the distillation unit. Additionally, the cooling section of the distillation unit has another device for forced cooling. The device for forced cooling of the cooling section allows the cooling section to be exposed to a specific flow of a heat carrier fluid, in particular a gas or liquid, for heat removal, or to have a heat flow around it, as opposed to, for example, natural convection. The cooling section is arranged in an air guide housing for targeted guidance of ambient air over the cooling section and / or is formed from at least one coaxial tube for guiding gas inside the inner tube and guiding the heat carrier fluid into the intermediate space between the outside of the inner tube and the inside of the outer tube. The coaxial tube may in particular be double-walled. The heat carrier fluid is preferably a liquid aggregate, in particular water or glycol.

[0015] The apparatus for processing raw materials has an extractor for extracting gas from a reaction unit and creating a negative pressure in the reaction unit, the negative pressure being the pressure around the apparatus. The extractor can be configured as a pump, in particular as a diaphragm pump.

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

[0017] According to a further development of the invention, at least two temperature sensors for determining the temperature in the reaction unit are arranged in an intermediate space formed between the reaction unit and the jacket element of the heating system in the closed state of the heating system.

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

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

[0020] A connection for connecting a gaseous scrubbing medium to a device for introducing the gaseous scrubbing medium, in particular into the reaction unit, can be provided in the exhaust gas flow path between the heating system and the distillation unit. The scrubbing medium, e.g., nitrogen, serves to inert the reaction unit, reducing the risk of explosion, and, as a carrier gas, assists in the separation of the end products formed during operation of the apparatus.

[0021] A fan is advantageously provided inside the wall of the air guide housing for targeted conduction of ambient air over the cooling section, in which the cooling section of the distillation unit can be arranged. 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] The fan is 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 onto the cooling section, and is preferably arranged on the top surface, in particular on the end surface facing vertically upwards, or on the side of the air guide housing.

[0023] An advantage of the present invention is that the extraction device for extracting gas from the reaction unit and creating a negative pressure in the reaction unit is arranged downstream of an oil tank arranged downstream of the distillation unit in the direction of gas flow, so that a negative pressure is also created in the distillation unit.

[0024] According to a further preferred embodiment of the present invention, the heating system comprises an upper member, a jacket member rigidly connected to the upper member, and a support member, the upper member being mounted on the support member whose length can be changed in the vertical direction, and by changing the length of the support member between its two limit positions, the heating system is opened or closed in the vertical direction of movement.

[0025] In this case, the heating system preferably has two support members, which are preferably arranged on either side of the heating system. According to a first alternative, the support members are driven by an electric spindle. According to a second alternative, the support members are formed as hydraulic supports.

[0026] According to a further development of the invention, the jacket member is formed by a hollow cylindrical wall which is open downwards in the longitudinal direction and closed at the top by a circular hood which is connected to the upper member at the hood to form a unit.

[0027] The jacket member advantageously has heating elements uniformly distributed around the circumference of the inner surface of the wall, which is formed of a thermal insulator made of ceramic powder to prevent heat transfer to the outside.

[0028] According to a further development of the invention, the hood can be formed at a central point and has an exhaust gas port for connection with an exhaust gas channel of the heating system, the exhaust gas channel running from the exhaust gas port through the hood to an upper part of the heating system.

[0029] The exhaust channel advantageously has at its distal end a connection to the exhaust port of the hood as a connector with the exhaust channel of the distillation unit.

[0030] The exhaust gas flow path extending from the exhaust gas port through the hood to the upper part of the heating system can be formed in the region of the exhaust gas port to compensate for thermal expansion using automatically variable pipe joints in the longitudinal direction, in particular in the vertical direction.

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

[0032] A high temperature resistant seal is advantageously disposed between the wall and the cover member.

[0033] The cover member of the reaction unit is preferably formed to be circular and has an exhaust gas port at its central point. It is particularly advantageous that the exhaust gas port of the cover member and the exhaust gas port of the jacket member engage with each other when the heating system is in a closed state, forming a tight connection with the exhaust gas flow path.

[0034] The cover member of the reaction unit can be formed with a connection port for connection with a device for introducing a gaseous scrubbing medium, in particular nitrogen, into the reaction unit.

[0035] The reaction unit may have screen elements therein, which are preferably horizontally aligned and spaced apart from one another at different heights, and the screen elements preferably cover the entire cross section of the reaction unit.

[0036] The control device of the raw material processing device is responsible for controlling the operation of the device according to the present concept and the conveying device, such as a temperature sensor and a device for forced cooling, in particular a fan for targeting the ambient temperature to the cooling section, or at least one pump for conveying a liquid heat transfer fluid. The extraction device is advantageously also connected to the drive of the support member, a fill level sensor of the oil tank, a pressure sensor, and a valve of the heating circuit of the heating system. The fill 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, for extracting oil from the oil tank. The oil delivery device starts operating when the oil tank fill level sensor sends a signal to the control device, and oil is delivered from the oil tank.

[0037] The object is also achieved by a method according to the invention for the operation of the apparatus described herein for material processing of raw materials, the method comprising the following steps: - charging the reaction unit with raw materials; - preheating the reaction unit; - opening the heating system and introducing the reaction unit into the heating system, in particular onto the bottom element of the heating system; - closing the heating system so that the reaction unit is located in a closed space; - heating the reaction unit and initiating the carbonization and distillation process, the carbonization and distillation process being carried out by selective heating at a substantially constant reaction temperature in the reaction unit, the temperature being specified; - removing all gases generated from the reaction unit to the distillation unit through an exhaust gas flow path formed between the reaction unit and the distillation unit, and determining the temperature of the gases flowing through the exhaust gas flow path; - cooling and condensing the gas in a distillation unit, the temperature of the gas being controlled by forced cooling of a cooling section of the distillation unit due to the heat power dissipated by the gas; - introducing the distillation product into an oil tank and discharging the oil; - extracting non-condensable gases from the oil tank, wherein a negative pressure relative to the environment is created in the reaction unit, removing oxygen from the reaction unit; - opening the heating system and removing the reaction unit from the heating system; - cooling the reaction unit and removing the final product from the reaction unit and separating the final product; - Removing the final product from the oil tank.

[0038] Targeted heating means that the reaction unit arranged in the heating system is heated during the carbonization and distillation process so that the reaction temperature in the reaction unit, also called the process temperature, is substantially constant and varies only within a predetermined temperature range. In doing so, the reaction temperature is continuously monitored. The temperature value is transmitted to a control device, which controls the opening and closing of the heating circuit valve of the heating system according to the predetermined desired value of the temperature.

[0039] When the heating system is closed, the exhaust gas port of the reaction unit is preferably connected to the exhaust gas port of the exhaust gas flow path of the heating system, and the exhaust gas flow path of the heating system and the exhaust gas flow path of the distillation unit are interconnected on the connecting member, thereby making an airtight connection from the reaction unit to the distillation unit. The heating system is advantageously opened and closed by extending and retracting the support member.

[0040] According to a further development of the invention, by extracting non-condensable gases from the oil tank and thus creating a negative pressure, the absolute value of the pressure in the reaction unit can be set to between 2 mbar and 10 mbar, in particular about 4 mbar.

[0041] To cool and condense the gases in the distillation unit, ambient air can be passed in a targeted manner over the cooling section of the distillation unit, or a gaseous heat transfer fluid, in particular water as a coolant, can flow through the cooling section.

[0042] According to an advantageous embodiment of the invention, during the procedure of cooling and condensing the gases of the distillation unit, the temperature of the gases is adjusted to a value in the range of 95°C to 125°C, in particular through a volumetric flow of ambient air or the power of a fan or the mass of a heat-carrying fluid. The volumetric flow of ambient air or the mass flow of the heat-carrying fluid ensures that heat is dissipated from the cooling section, cooling it. The temperature of the gases is determined in the exhaust flow path formed between the heating system and the distillation unit by at least one temperature sensor, in particular for determining the temperature of the exhaust gases discharged from the heating system.

[0043] The advantage of the present invention is that during the carbonization and distillation process, the exhaust gas flow path formed between the reaction unit and the distillation unit is heated to a temperature in the range of 120°C to 160°C, in particular, thereby avoiding premature condensation of the exhaust gas before it enters the distillation unit and consequent clogging of the exhaust gas flow path.

[0044] The reaction unit is preferably removed from the heating system when the temperature of the gas flowing through the exhaust gas channel is about 60°C.

[0045] According to a further preferred embodiment of the invention, a gaseous scrubbing 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.

[0046] Rinsing is preferably carried out at intervals in each case, thereby removing, in particular, relatively high molecular weight gases from the reaction unit. Washing with an inert gas, such as nitrogen, removes unwanted components, such as the polyaromatic component of polybutadiene or plasticizers, from the reaction unit, especially during the carbonization and distillation processes. The extraction of non-condensable gases, and thus the creation of a negative pressure in the reaction unit, and the introduction of a washing medium into the reaction unit, are advantageously time-shifted with respect to each other. In particular, during the cooling procedure of the reaction unit, the washing medium can be periodically introduced into the reaction unit for a duration ranging from 2 to 3 minutes.

[0047] After the reaction unit has cooled, it is preferably opened to remove the final product 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 procedure of removing the final product from the reaction unit, a gaseous scrubbing medium, in particular nitrogen, is advantageously added to the reaction unit.

[0048] During the procedure of removing the end product from the reaction unit, carbon can be extracted as an end product.

[0049] According to another development of the invention, the extracted non-condensable gases are supplied to a heating system for combustion in the heating system and thus for heating the reaction unit, and / or to a combined heat and power station for generating thermal energy and electrical energy.

[0050] The method is preferably carried out simultaneously in at least four reaction units in a modular manner in the following steps: - charging raw materials into the first reaction unit while the second reaction unit, which already contains the raw materials, is being preheated; - a third step of feeding the preheated reaction unit into a heating system to heat the reaction unit for carrying out the carbonization and distillation process; cooling and emptying the fourth reaction unit after the carbonization and distillation process is completed.

[0051] According to a further development of the invention, the reaction unit is filled with a mass of raw material in the range of 2.5 to 3 tons. The reaction unit advantageously remains in the heating system for a time of about 2.5 to 3.5 hours. The reaction temperature in the reaction unit is preferably 350 to 800°C, in particular 550°C.

[0052] The energy consumption of one process run, especially in the reaction units equipped with used tires, is 60 kWh to 80 kWh. With a number of 12 reaction units and 9 passes per day, the daily energy demand is 6,480 kWh to 8,640 kWh. Assuming an average of 223 production days per year, the annual energy demand is therefore 1.445 MWh to 1.927 MWh. In comparison, the generated energy figures for electricity and heat each are approximately 10.5 MWh per year.

[0053] The method according to the invention is based on a carbonization / distillation process and the device according to the invention is an industrial carbonization / distillation module, also called a VDI module.

[0054] To effectively implement this method, the device is based on a modular design in order to optimize or maximize throughput and make it adjustable to current demands.

[0055] Further advantages of the device according to the invention and of the method according to the invention compared to the prior art can be summarized as follows: No need to separate raw materials in advance Raw materials, especially - waste rubber products, such as used tires, rubber-impregnated chain links, steel-cable reinforced rubber belts, and conveyor belts, which can be processed in their substantially original form, i.e., uncrushed and unshredded, to obtain their structure, and therefore are not crushed or compressed; - organic and renewable raw materials, such as wood in all its forms, especially beech and oak, bamboo, bark, fruit, such as palm and orange peel; - Animal waste, e.g. bones and carcasses, - polluted carbon, - contaminated soil or other materials, for example after an oil spill; - Scrapped vehicles that have not been substantially crushed or dismantled and are therefore intact - Carbon composites, especially those using carbon fibre, especially from the automotive industry Processing of · Ecological, economical, carbon-free technology with extremely low energy consumption and therefore sustainable.

[0056] The various process parameters, such as the temperature and duration of the process and washing with the gaseous washing medium, and the associated performance of the individual components, such as the heating system, the conveying devices of the forced cooling device of the distillation unit, such as fans or at least one pump, the extraction device, depend on the raw materials to be processed in the reaction unit. Therefore, methods or devices with corresponding control programs stored in the control device can be distinguished as follows: a) Apparatus and method for material processing of tires b) Apparatus and method for rubber-impregnated chain links c) Apparatus and method for material handling on conveyor belts d) Equipment and methods for material processing of automobiles or crushed automobiles before dismantling in the automotive industry e) Apparatus and methods for material processing of renewable raw materials such as wood and bamboo, and bio-waste materials such as coconut shells and orange peels f) Apparatus and methods for the treatment of animal waste materials g) Apparatus and method for processing bitumen and asphalt materials h) Apparatus and methods for material processing of energy storage, especially batteries, especially from the automotive industry i) Apparatus and method for material processing of electronic components such as computers, mobile phones, laptops, smartphones, etc. j) Equipment and methods for the physical treatment of contaminated carbon and contaminant-contaminated soils for carbon reactivation.

[0057] Depending on the raw materials to be processed, the raw materials, for example tires and batteries, are advantageously mixed in specific ratios relative to one another in the reaction unit, thereby influencing the process parameters and the final product.

[0058] [Table 1]

[0059] In the above table, the recovered material is given in mg / kg. The third and fourth columns show material from equipment and methods according to h), the fifth column shows material from equipment and methods according to i), the sixth and seventh columns show material from equipment and methods according to d), and the eighth column shows material from equipment and methods according to a).

[0060] In method h), whose raw materials are listed in the fourth column of the table, a 500 kg mass of battery blocks, also known as energy blocks, from the automotive industry and a 500 kg mass of used tires were used as starting materials. Prior to processing, approximately 60 kg of steel sheaths, including screws, were removed from the battery blocks, and the remaining 440 kg of starting material was placed on a separate screen to prevent mixing of the battery blocks and used tires within the reactor. After completion of the process, the residual processed battery blocks, weighing 220.9 kg, were removed from the reactor and chopped into uniform pieces ranging from 0.2 mm to 0.5 mm for further analysis. The analytical data shown in the table indicate that all inorganic and metallic components of the battery blocks were detected with a recovery rate of greater than 98.5%. Metallic and inorganic components, such as cobalt, nickel, magnesium, copper, niobium, and lithium, can be recovered through proven metal refining techniques.

[0061] For method (i), whose raw materials are listed in the fifth column of the table, the starting materials used were 500 kg of waste electronics such as televisions, drills, and cables; 15 kg of scrap electronics such as computers in the form of laptops and mobile phones; and approximately 500 kg of used tires. The computers and mobile phones were placed separately in metal boxes within the reaction unit to prevent mixing with the other starting materials. The processed computer and mobile phone residue removed from the metal boxes after the complete process had a fixed mass of 7.7 kg and was cut into uniform sizes ranging from 0.1 mm for further analysis. Optical emission spectroscopy revealed high recoveries of metals such as cobalt, chromium, lithium, nickel, cadmium, tantalum, gallium, germanium, manganese, rhenium, strontium, and zirconium, which can be recovered by proven metal refining. A recovery or recycling rate of 98% was observed.

[0062] In method (d), whose raw materials are listed in the sixth column of the table, a whole Smart car with a mass of 750 kg was used as the starting material for the process. Prior to the process, only the battery was removed, as well as liquids such as coolant, brake fluid, engine oil, and gasoline. The mass of the solid residue of the processed whole vehicle removed from the reaction unit after the entire process was 450 kg. This mass consisted of 30% carbon and 70% metals, such as steel, spring steel, and precious metals. In addition, approximately 250 kg to 270 kg of diesel was also recovered. The proportion of residual gas was approximately 6% to 8%. This resulted in a recovery or utilization rate of 95%.

[0063] For rapeseed, crushed or not, the carbon content determined by the method according to DIN / EN 12879 was between 98.8% and 99.8%. By the same method, a carbon content ranging from 79.7% to 81.0% was determined for rapeseed pellet samples for carbon black, a carbon content of 99.1% was determined for plastic bottle samples, a carbon content of 98.5% was determined for oak wood samples, a carbon content of 99.4% was determined for industrial waste, and a carbon content of 99.4% was determined for rubber waste. A carbon content of 99.5% was determined for rapeseed pellet samples for oil.

[0064] The carbon / hydrogen and nitrogen content according to ASTM D5291 and the oxygen content according to a method based on ASTM D5622 are each determined using an Elementar VARIO EL Cube, and the fluorine and chlorine contents are determined by pyrolysis ion chromatography using an Analytik Jena combustion module, an absorption module 920, or an ion chromatograph 930 Compact IC Flex.

[0065] The volatile fraction up to 200° C. is identified by headspace GC-MS screening using a Trace GC Ultra with a Thermo Scientific DSQ II mass spectrometer.

[0066] Hydrofluoric and nitric acids are determined by microwave digestion with ICP OES using an Ofen Model StarT from MWS GmbH, and trace elements, especially the inorganic fraction, are determined by ICP OES using an ICP OES Arcos from Spectro.

[0067] Thermogravimetric analysis is performed using a TA Instruments Hi-Res TGA 2950.

[0068] Another important advantage is that steel-rubber composites, which previously could only be separated with high energy expenditure, can now be separated without significant external energy input. The resulting products can be returned to high-quality use within the context of an efficient circular economy, which helps conserve resources. Resulting products include: For example, the density is approximately 927 kg / m at 15°C. 3 , viscosity is 4.74mm 2 / s, diesel with a flash point below 21°C ·gas Metals, mainly steel or iron and titanium, and Amorphous inorganic carbon or carbon aggregates.

[0069] The amorphous inorganic carbon produced by the method according to the invention for operating an apparatus for material processing of carbon-containing raw materials has, depending on the design, a structure of three-dimensional arrays of carbon nanoparticles as aggregates, advantageously with a purity ranging from 95% to 99.9%, depending on the starting raw material. The carbon nanoparticles are cross-linked without long-range order, do not show any large-scale graphitic arrangement, and are not arranged as nanotubes.

[0070] Carbon formed in a structure of spatially ordered nanoparticles can be produced industrially by the device and method according to the invention and therefore has a great economic advantage over laboratory-obtained or produced carbon known in the prior art. The purity of the carbon is greatly influenced, in particular by scrubbing with gaseous scrubbing media during the carbonization and distillation process or cooling of the reaction unit.

[0071] Depending on the starting raw materials, the carbon produced in this process for operating an apparatus for material processing of the raw materials preferably has a BET surface area, determined by the method according to DIN ISO 9277, of 2,500 m 2 / g BET, especially up to 9,500m 2 / g BET, especially 3,500m 2 / g BET or greater than 4,000m 2 / g BET, especially at 4,200m 2 / g BET~4,500m 2 / g BET range and therefore have a high adsorption capacity and do not release substances into the environment, which is therefore not polluted by, for example, leaching.

[0072] The density of the carbon produced by the method according to the invention is preferably about 66 kg / m 3 and, advantageously, can be designed with higher tensile strength than alloy steels.

[0073] The conductivity of the carbon obtained in this way is 4.5·10 7 Ωm~5.8·10 7 The conductivity can be in the Ωm range. The conductivity is determined in accordance with the method according to DIN EN ISO 15091.

[0074] The carbon produced by the method according to the invention for operating an apparatus for raw material processing does not dissolve in concentrated or diluted low-temperature acids, such as sulfuric acid, nitric acid, or hydrochloric acid, and is not attacked by alkaline solutions. Nitric acid spontaneously decomposes into water and nitrogen gas, which may have a catalytic effect. Neither polar nor non-polar organic solvents can dissolve carbon.

[0075] The recovered diesel can be used, for example, in the chemical industry, especially as a raw material for basic chemicals, and in the pharmaceutical industry, for example to generate thermal and electrical energy by CHP, while the gas can be used to generate thermal and electrical energy, for example by gas turbines and generators, or for recycling and use in processes. The recovered metals, such as steel, can be recycled to the steel industry, the physical and chemical properties of the metal being preserved by the very low process temperatures.

[0076] Further details, features and advantages of the invention will become apparent from the following description of exemplary embodiments, which proceeds with reference to the accompanying drawings. [Brief explanation of the drawings]

[0077] [Figure 1] 1 shows an industrial carbonization / distillation module as a device for raw material processing in an open state in a front view. [Figure 2a] 1 shows a side view of an industrial carbonization / distillation module as a device for raw material processing in a closed state. [Figure 2b] 1 shows an industrial carbonization / distillation module as a device for raw material processing in a closed state in a front view. [Figure 3] FIG. 1 is a cross-sectional view of the heating system in an open state. [Figure 4] FIG. 1 is a cross-sectional view of the heating system in a closed state. [Figure 5] 1 shows the bottom part of the heating system. [Figure 6] The distillation unit is shown. [Figure 7] Oil tank shown. [Figure 8a] The reaction unit is shown in a closed state. [Figure 8b] FIG. 2 is a cross-sectional view of the reaction unit in a closed state. [Figure 9a] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9b]1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9c] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9d] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9e] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9f] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9g] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9h] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9i] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9j] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9k] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9l] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9m] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9n] 1 is a microscopic image of carbon produced by an apparatus for raw material processing. [Figure 9p] 1 shows the results of Raman spectroscopy of carbon. [Figure 9q] 1 shows the results of Raman spectroscopy of carbon. DETAILED DESCRIPTION OF THE INVENTION

[0078] In Figures 1, 2a and 2b, an industrial carbonization / distillation module is represented as another apparatus 1 for raw material processing. Figure 1 shows the apparatus 1 in an open state in a front view, Figure 2b shows the apparatus 1 in a closed state in a top view and Figure 2a shows it in a side view.

[0079] The apparatus 1 comprises a heating system 2 and a distillation unit 3. A reaction unit 4 containing raw materials is preheated to a specific temperature in a preheating device (not shown) and then further heated in the heating system 2. A mixture of different raw materials can be introduced into the reaction unit 4, thus eliminating the need for pre-separation of the product. After pre-heating, the reaction unit 4 is placed in the opened heating system 2 and positioned on the bottom member 5 of the heating system 2.

[0080] The upper member 7 of the heating system 2 and the jacket member 8 firmly connected to the upper member 7 are held movably in the movement direction B by support members 6 arranged on both sides of the heating system 2. The support members 6 are arranged at a distance of about 2.9 m from each other. The outer diameter of the jacket member 8 is about 2.5 m.

[0081] In a first limit position according to Fig. 1, the support member 6 is extended. The height of the apparatus 1 is therefore 6.70 m. The upper member 7 and the jacket member 8 provide space for the attachment of the reaction unit 4 to the heating system 2. The heating system 2 is opened. The reaction unit 4 can be introduced into or removed from the heating system 2. The movement of the reaction unit 4 can advantageously be carried out by a rail system (not shown), on which the reaction unit 4 rests. In a second limit position according to Figs. 2a and 2b, the support member 6 is retracted. The height of the apparatus 1 is therefore approximately 3.70 m.

[0082] The jacket member 8 is sealed to the bottom member 5 and the reaction unit is positioned in the closed space. The heating system 2 is closed. The reaction unit 4 is surrounded at the bottom by the bottom member 5 and at the sides and top by the jacket member 8.

[0083] The apparatus 1 has temperature sensors T1, T2, T3 in the region 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 an intermediate space formed between the reaction unit 4 and the jacket member 8 when the heating system 2 is in a closed state. The temperature sensors T2, T3 are positioned, for example, so as to protrude about 1 cm from the inside of the jacket member 8 into the intermediate space, which is about 8 cm wide. The temperature sensors T2, T3 are arranged spaced apart from each other in the vertical direction and determine local or average temperature values in the intermediate space. The temperature in the reaction unit 4 is determined by the temperature values determined via the temperature sensors T2, T3.

[0084] The heating system 2 has an enclosure 9 in its lower region. The enclosure 9 surrounds the sides of the bottom member 5 and the jacket member 8 when the heating system 2 is in a closed state, and can be opened to equip the heating system 2 with the necessary equipment.

[0085] The gases produced during the carbonization process leave the heating system 2 through the provided exhaust gas channel 11 and are cooled in a process-technical sense. The gases are sent to the distillation unit 3 through an exhaust gas port 10a formed at the top of the reaction unit 4 and through the exhaust gas channel 11 arranged in the upper part 7. As a result, the gases flow through the cooling section 12 of the distillation unit 3. According to FIGS. 1, 2a, and 2b, the cooling section 12 is formed by tubes. The tubes, which are inclined with respect to the horizontal, are provided with ribs to increase the heat transfer surface and thus facilitate heat transfer. Heat is transferred from the gases to the ambient air.

[0086] To further increase the heat output transferred from the gas to be cooled to the ambient air, specifically to better control 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. A fan 12-2 is arranged on the upper side, in particular on the end face facing vertically upward, of the air guide housing 12-1, and this fan distributes the ambient air as cooling air evenly throughout the air guide housing 12-1. Alternatively, a fan can also be formed on the side of the air guide housing 12-1. In this case, the ambient air is directed in a targeted manner toward the cooling section 12. Another temperature sensor T1 is arranged in the exhaust gas flow path 11 formed between the heating system 2 and the distillation unit 3 to determine the temperature of the exhaust gas discharged from the heating system 2.

[0087] According to an alternative embodiment, the gas in the cooling section can also be cooled by a heat transfer fluid other than air, for example water. In this case, instead of 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 through the intermediate space between the outside of the inner tube and the inside of the outer tube.

[0088] The cooling section 12 is formed by two tubes aligned parallel to each other. The gas is split into two partial mass flows before entering the cooling section 12 and remixed after flowing through the cooling section 12.

[0089] The distillation product is then introduced into the oil tank 13. In the oil tank 13, the oil obtained from the carbonization process and subsequent distillation settles, which in its viscosity and composition corresponds to diesel or is very similar to an intermediate in crude oil processing. The non-condensable part of the gas is discharged from the oil tank 13. The oil tank 13, with a capacity of about 1,000 liters, also serves as the expansion vessel of the device 1.

[0090] An extraction device 14-1, in particular a pump, in particular a diaphragm pump, for extracting gas through the surface of oil accumulated in the oil tank 13, and an oil delivery device 14-2, in particular a pump, in particular a piston pump, for transporting oil from the oil tank 13 are arranged on the oil tank 13. When gas is extracted, negative pressure is generated in the cooling section 12 of the distillation unit 3, in the exhaust gas flow path 11, and in particular in the reaction unit 4. By the extraction device 14-1, air, and therefore oxygen, which is a component of air, is also intentionally extracted from the reaction unit 4. In this way, a vacuum can be generated in the reaction unit 4.

[0091] The gas extracted above the surface of the oil deposited inside the oil tank 13 can be used directly by a combined heat and power station, called CHP, to generate thermal and electrical energy.

[0092] The apparatus 1 is also configured to have a control device 15 for controlling the operation of the apparatus 1. The control device 15 identifies and displays, for example, the fill level in the oil tank 13, the oil or gas flow, and possible defects in the flow paths of the apparatus 1. The control device 15 is connected to the corresponding sensors. Temperature sensors T1, T2, and T3 are also connected to the control device 15. The values determined by the temperature sensors T1, T2, and T3 serve to control the apparatus 1, in particular the heating system 2, and thus the reaction unit 4, as well as the fan 12-2 and the extraction device 14-1 of the cooling section 12. The control device 15 can be used, among other things, to display the status and process temperature of the different heating circuits of the heating system 2. The configuration of the jacket member 8 of the heating system 2 can also be identified and represented as open, closed, and partially open. Consequently, the control device 15 also serves to extend and retract the support member 6 to open or close the heating system 2.

[0093] Figures 3 and 4 each show a cross-sectional view of the heating system 2. Figure 3 shows the heating system 2 in an open state, and Figure 4 shows the heating system 2 in a closed state.

[0094] 3, the support member 6 is fully extended. The support member 6 and the upper member 7, which is arranged at the upper end of the jacket member 8 firmly connected to the upper member 7, are arranged at a height H above the bottom member 5, and the reaction unit 4 can move freely horizontally between the bottom member 5 and the jacket member 8.

[0095] The casing member 8 is movably supported in its lower region by the support member 6. The lateral support provided by the support member 6 ensures that the casing member 8 can move linearly between its limit positions in the movement direction B. Tipping of the casing member 8 is prevented.

[0096] The jacket member 8 has heating elements 16a uniformly distributed around the circumference of the inner surface of the jacket. The heating elements 16a are arranged substantially vertically and are guided through the wall to the inner surface in the lower region of the jacket member 8. Each heating element 16a is formed by two longitudinally aligned sections interconnected at their upper ends by a bend.

[0097] The jacket element 8 is open vertically downwards and is closed at the top by a hood 17, which is fixed to the upper element 7. The upper element 7 and the jacket element 8 form a tight-fitting unit. The hood 17 is formed with an exhaust gas port 10b at a central point as a connection to the exhaust gas channel 11a. The exhaust gas channel 11a runs from the exhaust gas port 10b through the hood 17 to the upper element 7. The section where the exhaust gas channel 11a passes through the hood 17 is sealed off from the hood 17. In the region of the exhaust gas port 10b, the exhaust gas channel 11a is formed with a pipe fitting 19, which can be, for example, in the form of a telescopic pipe, and whose length can be changed vertically. The pipe fitting 19 is automatically length-adjustable and serves to compensate for the thermal expansion of the reaction unit 4, in particular of the heating system 2, with respect to the jacket element 8 and the hood 17.

[0098] The exhaust gas channel 11a is configured with a heating device 20 as a transition from the reaction unit 4 to the distillation unit 3. The electrically operated heating device 20 surrounding the exhaust gas channel 11a is connected to the control device 15, as is the temperature sensor T1.

[0099] In addition, the exhaust gas flow path 11a has a connection element 11-1 for connecting the exhaust gas flow path 11a to a device for receiving a gaseous scrubbing medium, for example nitrogen. The scrubbing medium can flow into the exhaust gas flow path 11a, in particular into the reaction unit 4, via the connection element 11-1. The connection element 11-1 is arranged between the pipe fitting 19 and the region of the exhaust gas flow path 11a that is surrounded by the heating device 20, in particular at the highest point in the longitudinal direction of the exhaust gas flow paths 11, 11a.

[0100] At its distal end, the exhaust gas channel 11a has a connecting element 18 which starts from the exhaust gas port 10b. The connecting element 18 is advantageously formed as a quick coupling and serves to connect the exhaust gas channel 11a of the heating system 2 to the exhaust gas channel 11b of the distillation unit 3 in the closed state of the heating system 2 according to Fig. 4. By moving the upper element 7 downwards when closing the heating system 2, the exhaust gas channels 11a, 11b and the exhaust gas ports 10a, 10b on the connecting element 18 are interconnected, thereby obtaining an airtight connection from the reaction unit 4 to the distillation unit 3.

[0101] The reaction unit 4, which is arranged on the bottom member 5, is formed to have a wall 21 in the form of a hollow cylindrical container with 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 a cover member 22. A seal is arranged between the wall 21 and the cover member 22 to hermetically seal the reaction unit 4. Screen elements 23 are formed inside the reaction unit 4. The screen elements 23 are aligned horizontally and spaced apart from one another at different heights.

[0102] In the second limiting position shown in Figure 4, the support member 6 is fully retracted. The jacket member 8 rests on the bottom member 5 and completely surrounds the reaction unit 4. The heating system 2 is closed.

[0103] The reaction unit 4, into which the raw materials have been introduced, is advantageously heated uniformly over its bottom and its walls 21. The heating elements 16a are used for heating through the walls 21, while the heating elements 16b arranged on the bottom member 5 supply heat from the bottom to the reaction unit 4. When the heating system 2 is in the closed state, the heating elements 16a, which are formed on the circumference of the jacket member 8, are at equal distances from the walls 21 of the reaction unit 4. The heating elements 16a, 16b are preferably electrically operated.

[0104] 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 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 feedstock and the end product to be produced. This temperature is determined by temperature sensors T2 and T3, which are arranged between the reaction unit 4 and the jacket member 8. This results in an energy consumption of approximately 40 kWh per hour. The reaction unit 4 is fed with raw materials having a mass in the range of 2.5 to 3 t.

[0105] Gases formed during the carbonization process are discharged, in particular extracted, into the exhaust gas channel 11 through an exhaust gas port 10 arranged in the cover member 22. When the heating system 2 is in a closed state, the exhaust gas port 10a of the reaction unit 4 and the exhaust gas port 10b of the hood 17 of the jacket member 8 are gas-tightly connected to each other. This ensures that gas cannot leak into the intermediate space between the reaction unit 4 and the jacket member 8.

[0106] A negative pressure of approximately 2 mbar to 10 mbar, in particular approximately 4 mbar, exists inside the reaction unit 4. This negative pressure is generated by an extractor 14-1 located at the first outlet port of the oil tank 13, which extracts gas through the surface of the oil deposited in the oil tank 13. Due to the targeted extraction of gas from the reaction unit 4, the reaction or process temperature in the reaction unit 4 is reached more quickly. This, in turn, affects the structural composition of the carbonized carbon. Another factor affecting the composition and purity of the carbon is the duration of the carbonization process. The longer the carbonization process is carried out, the purer the carbon will be, and depending on the starting material, it may be used, for example, for medical purposes. Carbon used for medical purposes should be further purified, if necessary. Carbon recovered during a shorter carbonization process is preferably used, for example, as a filter medium or in the construction industry.

[0107] Factors that influence the composition and purity of the carbon also include the scrubbing of the reaction unit 4 with gaseous scrubbing media, in particular nitrogen, on the one hand during the carbonization and distillation processes and, on the other hand, during the process of cooling the reaction unit.

[0108] The heating device 20 surrounding the exhaust gas channel 11a heats the exhaust gas channel 11a, particularly to a temperature in the range of 120°C to 160°C, thereby reducing the temperature difference between the exhaust gas channel 11a and the exhaust gas flowing through it. The temperature of the flowing exhaust gas is determined by a temperature sensor T1. The heating device 20 serves to prevent premature condensation of the exhaust gas before it enters the distillation unit 3, and thus undesirable clogging of the exhaust gas channel 11a. Heating the exhaust gas channel 11a also aids in the outflow of the exhaust gas from the reaction unit 4.

[0109] 5 shows the bottom part 5 of the heating system 2. The bottom part 5 comprises a bottom plate 24 and a centering device 25 for the jacket part 8, the heating element 16b and a support part 28 holding the reaction unit 4. The bottom part 5 is made substantially from ceramic and is reliably thermally insulated towards the outside, particularly towards the bottom. Together with the thermal insulation of the jacket part 8, heat losses in the heating system 2 are thus minimized.

[0110] The reaction unit 4 rests on the support members 28 of the bottom plate 24. The support members 28 are shaped and positioned such that the reaction unit 4 is centrally aligned with the bottom plate 5 when it rests on the support members 28.

[0111] The centering device 25 is formed in the form of a circular disk with a shoulder, so that the disk has two areas of different diameters. The circular surface located between these areas serves as a sealing surface 27.

[0112] The outer periphery of the smaller diameter region of the disk is smaller than the inner periphery of the wall 21 of the reaction unit 4 or jacket member 8. When the heating system 2 is in a closed state, a gap is formed between the jacket surface 26 of the smaller diameter region of the disk and the inner surface of the wall 21. The jacket member 8 rests on the sealing surface 27 of the bottom plate 24, thereby sealing the space enclosed by the jacket member 8 and the bottom plate 24. Seals are disposed on the corresponding surfaces of the bottom plate 24 and the jacket member 8 to seal the enclosed space. Additionally, the jacket member 8 is pressed against and held on the sealing surface 27 of the bottom plate 24 with a pressure in the range of 1 bar to 2 bar.

[0113] The support member 6 is also fixed to the base plate 24 , so that the base plate 24 carries the entire heating system 2 .

[0114] The heating elements 16b are arranged substantially horizontally on the terminal surface 29 of the centering device 25 and guided vertically through the terminal surface 29. The heating elements 16b are bent in a serpentine shape, each resembling a hand with five fingers. The fingers increase in length from the outside to the inside, with the middle finger being the longest. The heating elements 16b are aligned symmetrically with one another, with the tips of the fingers pointing toward the center of the terminal surface 29.

[0115] The support members 28 on which the reaction units 4 rest extend vertically beyond the heating elements 16b, so that the bottoms of the reaction units 4 resting on the support members 28 are positioned above the heating elements 16b. Each of the heating elements 16b is the same distance from the bottoms of the reaction units 4, thereby ensuring uniform heat transfer through the bottoms of the reaction units 4.

[0116] The centering device 25, the support member 28, and the heating element 16b are arranged concentrically around the center point of the bottom plate 24.

[0117] FIG. 6 shows a distillation unit 3, which, in the direction of flow of the final product, has an exhaust gas flow path 11b, a cooling section 12 with an air guide housing 12-1 and a fan 12-2, and an oil tank 13 with an extraction device 14-1 and an oil conveying device 14-2.

[0118] The gases discharged from the heating system 2 pass through the exhaust gas flow path 11b to the cooling section 12, which is also formed from tubes. In the branch 30, the gas mass flow is divided into two partial mass flows by two tubes aligned parallel to one another. The division of the gas mass flow allows for better heat transfer from the gas mass flow to the environment and optimizes the distillation or condensation procedure.

[0119] To further improve heat transfer, the heat transfer surface of the cooling section 12 is increased by forming the tubes with ribs. The heat output, especially the heat of condensation, dissipated from the gas being cooled is further increased and simultaneously controlled by the air guide housing 12-1 and the fan 12-2. Ambient air is uniformly drawn through the air guide housing 12-1 as cooling air and directed onto the cooling section 12 in a targeted manner. The corresponding force 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 is liquefied at a condensation point between 95°C and 125°C. Further inflow into the cooling section 12 cools the cooling section 12 to a temperature below the condensation point of the gas or maintains it at a corresponding temperature level. This control of the heat output increases the production of oil and decreases the production of residual gas. The temperature is determined by a temperature sensor T1 (see Figure 1) located in the exhaust gas flow path 11 formed between the heating system 2 and the distillation unit 3.

[0120] After flowing through the cooling section 12, the partial mass flows that were split before entering the cooling section 12 reunite at an open point 31 and are introduced into the oil tank 13 from above through an inlet port 32.

[0121] The oil, which is denser than the gas, accumulates in the oil tank 13. The non-condensable portion of the distillation product is removed through a first outlet port 33 in the upper region of the oil tank 13. An extraction device 14-1 is arranged at the first outlet port 33 of the oil tank 13 in order to extract the gas through the surface of the oil accumulated in the oil tank 13. Due to the extraction of the gas and the negative pressure thereby created in the device 1, in particular air and therefore oxygen, which is a component of air, is extracted from the reaction unit 4, which affects the carbonization process.

[0122] An oil transfer device 14-2 is disposed at the second outlet port 34 of the oil tank 13 to transfer oil from the oil tank 13.

[0123] FIG. 7 shows the oil tank 13 with the side cut away to reveal the interior.

[0124] The inlet port 32 is located on the top of the oil tank 13, and the distillation product flows into the oil tank 13 from above. The oil settles to the bottom of the oil tank 13, and gas, which is less dense than the oil, collects above the oil surface. The oil level in the oil tank 13 is identified and monitored by a float 35. When a predetermined filling height is reached, the oil is removed from the oil tank 13 for further processing.

[0125] Gas accumulated in the upper region of the oil tank 13 is discharged through the first outlet port 33 and extracted, in particular, by 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 and, in particular, by the oil delivery device 14-2.

[0126] 8a and 8b show the reaction unit 4 in a closed state, with FIG. 8b showing a cross-sectional view of the reaction unit 4. FIG.

[0127] The wall 21 is in the form of a hollow cylindrical container, which has a closed bottom and an open side opposite the bottom that can be closed by a cover member 22. During closing of the reaction unit 4, the cover member 22 is placed vertically on the upwardly facing end face of the wall 21. The cover member 22 is pressed against the end of the wall 21 by its own weight and is releasably carried by the wall 21.

[0128] A high temperature resistant seal is placed between the wall 21 and the cover member 22 to close the reaction unit 4 in an airtight manner. In the closed state, the reaction unit has a height of about 2.4 m.

[0129] The cover element 22 is formed so as to have a connection port 36 next to the exhaust gas port 10a to which a device for introducing a gaseous scrubbing medium, in particular nitrogen, into the reaction unit 4 can be connected.

[0130] At the end of the actual carbonization / distillation process, in which the reaction unit 4 is placed in the heating system 2 and heated or substantially maintained at the desired reaction temperature, the exhaust gas temperature is about 60°C as determined by the temperature sensor T1 placed between the heating system 2 and the distillation unit 3. The reaction unit 4 is removed from the heating system 2, and its temperature is, for example, in the range of 500°C to 600°C.

[0131] After being removed from the heating system 2, the reaction unit 4 is cooled to a temperature determined by the intended use of the product. The mixture in the reaction unit 4 is removed after the reaction unit 4 is opened, i.e., the cover member 22 is removed. The reaction unit 4 is then returned to the process and the material is introduced. The carbon-iron mixture is separated into its components.

[0132] The recovered intrinsic carbon is further formed in the reaction unit 4 during the cooling process at 600°C to 60°C, 20°C, or 30°C in an oxygen-free atmosphere. In this case, a gaseous cleaning medium, in particular nitrogen, is introduced into the reaction unit 4 through the connection port 36, which also influences the cooling process. Alternatively, the gaseous cleaning medium can be introduced through the exhaust port 10a, to which a device for introducing the gaseous cleaning medium can be connected, especially if the connection port 36 is not formed. The introduction of the cleaning medium during the cooling process, i.e., before the reaction unit 4 is emptied, can accelerate the cooling process and, in particular, can serve to clean the final product and thus support the formation of the carbon recovered in the device 1. Cleaning the reaction unit 4 increases the purity of the final product, in particular carbon. Impurities are washed away. The cleaning medium flowing into the reaction unit 4 through the connection port 36 is then discharged again from the reaction unit 4 together with the impurities through the exhaust port 10a formed in the cover member 22. The temperature inside the reaction unit 4 when the reaction unit 4 is opened is in the range of 20°C to 60°C, particularly in the range of 30°C to 60°C.

[0133] During the opening of the reaction unit 4, the cover member 22 is raised vertically and removed from the reaction unit 4, thereby allowing the reaction unit 4 to be emptied and then charged again with material. The reaction unit 4 can also be charged with a washing medium during emptying to achieve the desired purity of the final product, in particular the carbon. The carbon is preferably extracted during the emptying of the reaction unit 4.

[0134] The carbonization / distillation process for raw material processing essentially comprises four reaction units 4 made of high-temperature resistant steel, each with a loading capacity of 2.5 to 3.5 tons (75% mechanical, 25% automatic). While the first reaction unit 4 is being fed with material, the second reaction unit 4, which has already been fed, is preheated. Meanwhile, the third reaction unit 4 has already been fed into the heating system 2 and is heated to carry out the actual carbonization / distillation process. Meanwhile, the fourth reaction unit 4 is cooled and then emptied.

[0135] By using a modular system with, for example, four reaction units 4, the throughput can be increased stepwise and flexibly adapted to the respective demands. The entire process is carried out semi-continuously.

[0136] 9a-9n show microscopic images of carbon produced in the apparatus 1 for raw material processing. The structure of the carbon can be seen in the images produced using a transmission electron microscope, abbreviated as TEM. Transmission electron microscopes are used to detect and characterize the nanometer-level structure and particle size of substances and substance mixtures.

[0137] These images show a very finely divided, three-dimensional, uniform quasi-crystalline structure of primary carbon particles in the sub-nanometer range with very large internal surfaces, which are partially recognizable as larger agglomerates with the same surface structure.

[0138] Figures 9p and 9q show the results of Raman spectroscopy of carbon. -1The absence of a 2D peak at 1000 nm indicates the absence of large-scale graphitic ordering. The carbon produced in Apparatus 1 for Raw Material Processing is amorphous inorganic carbon, in which nanoparticles are cross-linked without long-range order. The carbon is not a nanotube and is not structurally similar to graphene.

[0139] Imaging of the Raman spectrum, as well as determination of the intensity and width of the G-Raman and D-Raman bands, can be performed using a Renishaw confocal Raman microscope, in Via, using 532 nm and 785 nm lasers. [Explanation of symbols]

[0140] 1. Equipment for material processing 2. Heating System 3 Distillation Unit 4 reaction units 5 Bottom member of heating system 2 6 Support member 7 Upper part of heating system 2 8 Jacket member of heating system 2 9. Box 10, 10a, 10b Exhaust gas port 11, 11a, 11b Exhaust gas flow path 11-1 Connection member for exhaust gas flow paths 11 and 11a 12 Cooling section of distillation unit 3 12-1 Air guide housing 12-2 Fan 13 Oil Tank 14-1 Extraction device 14-2 Oil feeding device 15 Control device 16a, 16b heating elements 17 Food 18 Connection member for exhaust gas flow paths 11, 11a 19 Pipe fittings 20 Heating device 21 Wall of Reaction Unit 4 22 Cover member 23 Screen Elements 24 Bottom plate 25 Centering device for jacket member 8 26 Jacket surface of centering device 25 27 Sealing surface of centering device 25 28 Support member for reaction unit 4 29 Terminal surface 30 Branches 31 Opening point 32 Inlet port of oil tank 13 33 First outlet port of oil tank 13 34 Second outlet port of oil tank 13 35 Float 36 Connection port of cover member 22 B. Direction of movement of heating system 2 H Height T1, T2, T3 temperature sensors

Claims

1. An apparatus for raw material processing, comprising a heating system (2), a distillation unit (3), and a reaction unit (4), and a control device (14), - said heating system (2) is configured so that it can be opened and closed to fill said reaction unit (4); - the distillation unit (3) comprises a cooling section (12), - said reaction unit (4) is configured so that it can be filled with said raw materials; An exhaust gas flow path (11, 11a, 11b) for discharging exhaust gas from the reaction unit (4) is formed between the reaction unit (4) and the distillation unit (3), temperature sensors (T1, T2, T3) are formed in the region of said heating system (2) and said distillation unit (3); the cooling section (12) of the distillation unit (3) is formed with a device for forced cooling, the cooling section (12) - placed in an air guide housing (12-1) for a targeted flow of ambient air over said cooling section (12), and / or formed from at least one coaxial tube for guiding a gas inside an inner tube and for guiding a heat carrier fluid in an intermediate space between the outside of said inner tube and the inside of an outer tube; an extractor (14-1) is formed inside the reaction unit (4) to extract gas from the reaction unit (4) and create a negative pressure; The temperature sensors (T1, T2, T3) and the extractor (14-1) are connected to the control device (14).

1. An apparatus (1).

2. 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 jacket member (8) of the heating system (2) in the closed state of the heating system (2).

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

4. 4. The device (1) according to claim 1, wherein at least one temperature sensor (T1) for determining the temperature of the exhaust gases discharged from the heating system (2) is arranged in the exhaust gas flow path (11) between the heating system (2) and the distillation unit (3).

5. 5. The apparatus (1) according to claim 1, wherein the exhaust gas flow path (11) between the heating system (2) and the distillation unit (3) is formed with a connecting element (11-1) for connection to a device for introducing a gaseous scrubbing medium, in particular into the reaction unit (4).

6. 6. The device (1) according to claim 1, characterized in that a fan (12-2) for the targeted guidance of ambient air over the cooling section (12) is formed inside the wall of the air guide housing (12-1) in which the cooling section (12) of the distillation unit (3) is arranged, and that the fan (12-2) is connected to the control device (15).

7. 7. The device (1) according to claim 6, characterized in that the fan (12-2) is arranged on the upper surface of the air guide housing (12-1), in particular on an end face facing vertically upwards, or on a side surface.

8. 8. The apparatus (1) according to claim 1, wherein the extraction unit (14-1) is arranged downstream of an oil tank (13) arranged downstream of the distillation unit (3) in the gas flow direction.

9. 9. The device (1) according to any one of claims 1 to 8, characterized in that the heating system (2) comprises an upper member (7), a jacket member (8) formed to be firmly connected to the upper member (7), and a support member (6) whose length can be changed in the longitudinal direction, the upper member (7) being arranged on the support member (6) so as to be held in such a way that the heating system (2) can be opened or closed in the longitudinal movement direction (B) by changing the length of the support member (6) between two limit positions.

10. 10. The device (1) according to claim 9, characterized in that the heating system (2) has two support members (6), said support members (6) being arranged on each side of the heating system (2).

11. The jacket member (8) is longitudinally - open at the bottom, - closed at the top by a circular hood (17) and connected to the upper part (7) at said hood (17); 11. Device (1) according to claim 9 or 10, characterized in that it has a hollow cylindrical wall formed as follows:

12. 12. The device (1) according to claim 11, characterized in that the hood (17) is formed with an exhaust gas port (10b) at a central point as a connection to an exhaust gas path (11a), the exhaust gas path (11a) extending from the exhaust gas port (10b) through the hood (17) to the upper member (7).

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

14. Apparatus (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 container closed at the bottom, the open side of which can be closed by a cover member (22).

15. 15. The apparatus (1) according to claim 14, characterized in that the cover member (22) of the reaction unit (4) is formed to be circular and has an exhaust gas port (10a) at the central point, and the exhaust gas port (10a) of the cover member (22) and the exhaust gas port (10b) of the jacket member (8) engage with each other in the closed position of the heating system (2) to form a sealed connection with the exhaust gas flow path (11a).

16. 16. The apparatus (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 connection to a device for introducing a gaseous washing medium into the reaction unit (4).

17. A method for operating an apparatus (1) for raw material processing according to any one of claims 1 to 16, comprising: - charging the reaction unit (4) with raw materials; - preheating said reaction unit (4); - opening the heating system (2) and placing said reaction unit (4) in said heating system (2); - closing the heating system (2) so that the reaction unit (4) is placed in a closed space; - heating the heating unit (4) and starting the carbonization and distillation process, the carbonization and distillation process being carried out by selective heating at a substantially constant temperature in the reaction unit (4), the temperature being specified; - discharging the generated gas from the reaction unit (4) to the distillation unit (3) through an exhaust gas flow path (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 flow path (11, 11a); - cooling and condensing the gases in the distillation unit (3), the temperature of which is controlled by forced cooling of the cooling section (12) of the distillation unit (3) by the heat power dissipated by the gases; - introducing said distillation product into an oil tank (13) and draining the oil; - extracting non-condensable gases from the oil tank (13), creating a negative pressure in the reaction unit (4) relative to the environment and removing oxygen from the reaction unit (4); - opening the heating system (2) and removing the reaction unit (4) from the heating system (2); - cooling said reaction unit (4), removing the final product from said reaction unit (4) and separating said final product; - removing said final product from said oil tank (13); A method comprising:

18. 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 to 10 mbar, in particular from about 4 mbar.

19. to cool and condense the gas in the distillation unit (3), ambient air is directed in a targeted manner onto the cooling section (12) of the distillation unit (3), or A liquid heat carrier fluid, in particular water, flows through said cooling section (12) as a coolant.

19. The method according to claim 17 or 18.

20. 20. The method according to any one of claims 17 to 19, characterized in that during the step of cooling and condensing the gas in the distillation unit (3), the temperature of the gas is in the range of 95°C to 125°C.

21. 21. The method according to any one of claims 17 to 20, characterized in that during the carbonization and distillation process, the exhaust gas flow path (11, 11a) formed between the reaction unit (4) and the distillation unit (3) is heated, in particular to a temperature in the range of 120°C to 160°C.

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

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

24. 24. The method according to claim 23, characterized in that the gaseous washing medium is in each case flowed into the reaction unit (4) in time intervals.

25. 25. The method according to claim 24, characterized in that the extraction of non-condensable gases and the introduction of the washing medium into the reaction unit (4) are carried out in a time-shifted manner with respect to each other.

26. 26. The method according to claim 24 or 25, characterized in that the washing medium is flowed cyclically into the reaction unit (4) during the procedure of cooling the reaction unit (4), in each case for a duration ranging from 2 to 3 minutes.

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

28. 28. The method according to any one of claims 17 to 27, characterized in that during the step of removing the final product from the reaction unit (4), the reaction unit (4) is filled with a gaseous scrubbing medium.

29. 29. The method according to any one of claims 17 to 28, characterized in that during the procedure of removing the end product from the reaction unit (4), carbon as end product is extracted.

30. Method according to any one of claims 17 to 29, characterized in that the heating system (2) is opened and closed by extending and retracting a support member (6).

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

32. 32. Carbon produced by the method of any one of claims 17 to 31 for operating an apparatus (1) for material processing of carbon-containing raw materials according to any 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 aggregates, the carbon nanoparticles being cross-linked without long-range order, not having large-scale graphitic ordering and not arranged as nanotubes.

33. The mass-related specific surface area of the carbon is 2,500 m ２ / g Larger than BET, especially up to 9,500m ２ / g BET, especially 3,500m ２ / g BET or greater than 4,000 m ２ / g BET, especially 4,200m ２ / g BET~4,800m ２ / g BET range.

34. The density of the carbon is about 66 kg / m ３ 34. Carbon according to claim 32 or 33, characterized in that:

35. The conductivity of the carbon is 4.5.10 ７ Ωm ~ 5.8 / 10 ７ Carbon according to any one of claims 32 to 34, characterized in that it has a resistance in the range of Ωm.

36. Use of an apparatus (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.

Images