JP2004521184A - Liquefaction of residue at normal pressure - Google Patents

Abstract

The present invention relates to a method and an apparatus for liquefying hydrocarbon-containing residues at normal pressure, which describes an oil-forming step in a temperature range from 300 to 430 ° C. using similar catalysts, wherein the additives Guarantees separation, detoxification and stabilization of the resulting oil. The product quality obtained from plastics, waste oils, animal products and other substances with fats and hydrocarbons is similar to the quality of fuels, where the products obtained are extremely pure and contain toxic substances. Not included.

Description

[0001]
The present invention relates to a method and a device for compressing or liquefying biological or inorganic residues having a high hydrocarbon content at normal pressure. The product consists almost exclusively of hydrocarbons, which are suitable in this form for use in energy and drive technology. The remaining solids, which cannot be converted to the liquid phase, are processed into valuables by mechanical, electrical and thermal drying and separation.
[0002]
Methods for burning, vaporizing, compressing into combustion bricks and pyrolyzing the residue are known. The disadvantage of this method is the low yield of electrical energy in small devices. High electrical efficiency is only possible by the almost complete conversion of the hydrocarbon portion into diesel engine fuel by the generator. Just a small device prevents the debris from scattering, which in the case of problematic substances like meat flour not only consumes more fuel for transport, but also creates a healthy way.
[0003]
Thus, starting from pyrolysis, methods were sought to convert the residual hydrocarbons almost completely to hydrocarbon concentrates and to separate these hydrocarbons almost completely from the residual residues. This was already achieved tens of thousands of years ago by the Oil Formation Act. This method is typically based on the formation of an oxygen atmosphere above ground.
[0004]
At that time, the dead organic matter is transported from the sea to the air again, where it is not only lost, but also settles and mixes with the natural clay material on the ground. Here, the sediment forming one type of oil shale changed at an average temperature of about 120 ° C. over tens of thousands of years, forming liquid petroleum. Due to the liquid state of the oil, and thus the mobile state, it transforms from the sediment into a layer of sand with sufficient void volume to extrude and supply the oil, from which it is now conveyed.
[0005]
It is therefore an object of the present invention to reform and modify the process so that it can be used for the conversion of plastics and chlorine-containing oils and wood components, as well as residues that are later regenerated, such as oils and fats. is there. It is therefore an object of the present invention to find a way to use additives which are originally similar to marine clay substances, to detoxify them, separate them into thin liquid hydrocarbons and to convert the products formed during the separation. Find a way to stabilize. Stabilization is used here to prevent subsequent concentration of the oil formed.
[0006]
The object of the present invention is furthermore to make the process in a short time of seconds instead of a long historical time and in a manner which guarantees a high product quality of the residue despite all contaminants and additives such as foam formers. It is to be implemented in.
[0007]
The process is therefore suitable for mineral hydrocarbon products such as waste oils having a phosphate component as foam formers, for plastics with chlorine and fluorine containing substances such as PVC and Teflon and for composites such as waste fats and distillation residues. Should be suitable for hydrocarbons.
[0008]
Accordingly, it is a primary object of the present invention to provide a method for converting a residue into a usable form without burning and vaporizing.
[0009]
According to the present invention, in order to solve the above-mentioned problems, it is provided that these substances are introduced together with a surface-active additive into a hot oil circulation at 300 to 450 ° C and converted into oil in a boiling range of 100 to 350 ° C. Is done. Advantageous configurations of the method are described in the dependent claims.
[0010]
Surprisingly, a complete solution of the above problem has been found by increasing the petroleum formation temperature of 120 ° C. to 390 ° C. on average, which reduces the processing to a time of seconds. A class of clay materials which makes it possible to economically regenerate all three functions, detoxification, separation and stabilization, is a calcium-aluminum-silicate in the form of A504 from Tricat.
[0011]
The concept for the solution is that the circulation is parallel to the rotary evaporator, with a safety container in the circulation, and a rotary evaporator connected downstream at the flue gas side, a distillation apparatus with a return pipe And having an extruder screw, a residual oil evaporator for the residue discharged on the residue side, and having electrolysis for the phosphate-containing inorganic residue.
[0012]
The implementation of the complete method is described directly on the basis of FIGS.
[0013]
FIG. 1 illustrates the method of the present invention. In the rotary evaporator 1, the original decomposition and stabilization of the produced hydrocarbon concentrate are performed. A distillation evaporator 2 connected downstream of the flue gas distills the oil thus produced again into high-value oil. In order to achieve a reaction temperature of 390 ° C., a starting oil burner in the form of an oil burner 3 is used, in which the produced oil is burned for the starting step. This takes place in the combustion chamber 4, which is heated in operation by gas from the vacuum pump 10. In the operating state, the operation from the burner 3 is not performed, and the burner supplies only the combustion air during the operation.
[0014]
The rotary evaporator 1 has a honeycomb ceramic layer 5 on both sides, which takes into account that the combustion chamber burns stably and that the heating of the evaporator tubes works optimally with the increased radiant part of the heating medium. The hydrocarbons which evaporate under the combined action of the calcium-aluminum-silicate separation added here are collected in the safety steam container 6. This container is large, if possible, because the foam generated by the foam-forming agent does not reach the product. The portion that does not evaporate is collected at the bottom of the safety container, from where it returns to the rotary evaporator, whereby a circulation is formed.
[0015]
The two evaporators, the rotary evaporator 1 and the distillation evaporator 2, are connected to an outlet 7, which removes solids precipitated from the two evaporators 1 and 2. On the product side, evaporated material condensed in the distillation column is discharged via two product containers 8 and 9. In this case, the container 8 is an intermediate product tank for temporarily storing oil to maintain the liquid level in the rotary evaporator, and the container 9 is a product tank for storing the final product.
[0016]
In the case of an introduced substance containing water, the intermediate product tank 8 is the original product tank and the product tank 9 is used for obtaining the water portion. The gaseous products from the product tank 9 and the safety container 6 are sucked into the combustion chamber via the vacuum pump 10.
[0017]
The vacuum pump on the right is only connected if the temperature in the safety container drops at the suction position due to the formation of water vapor. This separates the water vapor portion from the atmosphere in the safety container. The discharge of the solid is performed by a screw press 11 having a press cylinder 12. The conical press cylinder 12 increases the solids concentration by squeezing out the oil.
[0018]
Safety techniques for handling these devices with combustible oil are ensured via regulating techniques and, in the event of an accident, via a pressurized water cooling vessel 13 having a volume of cooling water 14 and compressed air 15 present thereon. Is done. In the event of an accident, cooling by the pressurized water 14 collects cooling water below the device, thus avoiding contamination of groundwater by the cooling water storage tank 16.
[0019]
A stirring device 17 is used to complete the movement of the solids introduced and formed. At that time, care should be taken that the amount of solids in the reactor does not become too large to prevent circulation. In a special embodiment, the solids are conveyed via a discharge screw to a suction pipe, which is connected to an inlet to a safety container above the level of the circulating liquid. There is a separation sieve below this inlet, on which solids drip and which are discharged periodically from the sieve through openings and scrapers.
[0020]
The advantage of this additional solids separation is that the tubular conduit is completely open and the drainage proceeds, the conduit forming an additional separating circuit to the safety container. This circulation allows for a constant separation of the solids formed and does not impose a liquid circulation on these substances. Separation via the bottom outlet, on the other hand, only takes place periodically after the device has been discharged, since a precise supply is necessary to prevent the lower vessel from overflowing with the contents of the reactor.
[0021]
Another innovative separation of solids that cannot be evaporated by the catalyst is that in the circulation between the tubular evaporator and the safety vessel, a mixture of the product vapor from the tubular evaporator and the non-evaporating liquid is tangentially below the safety vessel. Side is connected to flow into the hydrocyclone 48, the hydrocyclone communicates upwards to the safety container and downwards to the liquid container 49, the liquid container being in the upper part with the lower part of the rotary evaporator. Coupled, thereby ensuring circulation.
[0022]
The solid matter discharged from the screw press 11 is conveyed to the discharge screw 18 by the extrusion screw 12, where it is further dried by indirect heating. The expelled oil vapor reaches the safety container from here. Similarly, an introduction screw 19 is present in the flue gas stream, and the substance introduced in the introduction screw is dried by indirect heating with the flue gas from the inlet 20 and is immediately introduced into the circulating liquid by means of a subsequent introduction tubular conduit. . The introduction into the liquid avoids the contamination of the vapor with a finely divided introduction, such as meat powder contaminated with prions, and allows for a 100% conversion of the problem substances introduced.
[0023]
The thus cooled flue gas reaches the outside via the flue gas pipe 21. At this time, condensed liquid condensed in the flue gas pipe 21 in a heated state is formed, and is discharged outside by a condensed liquid discharging means having a neutralizing device 22.
[0024]
The flue gas achieved in this case is cooled to 450 ° C. in a rotary evaporator, to 350 ° C. in a distillation evaporator, to 250 ° C. in a post-dryer and to 150 ° C. in a feed dryer. For the start-up phase, the dryer is additionally equipped with a burner, which guarantees the required minimum temperature.
[0025]
The production of the product in the distillation evaporator 2 is protected by a foam suppressor 23, which ensures that only the vapor reaches the distillation column 24 without the liquid part of the foam, and that the product is thus formed particularly clean. consider.
[0026]
In the distillation column 24 low boilers form at the upper end of the column and are removed in a conduit 25. The product is formed in the underlying reservoir and is withdrawn in conduit 26. The distillation column is preferably a bell tray column.
[0027]
The properties of the product are determined by the boiling point of the respective column section and the receiver, taking into account the control of the product. This is performed by a condenser 27 and a solenoid valve 29. Activate backwash 30 to reduce the product evaporation temperature. At the end of the condenser 27 is attached a vacuum conduit 28, which leads to the product container 9. The values adjusted for the average boiling point of the product emissions are 270 ° C. for diesel oil, 280 ° C. for fuel oil, 250 ° C. for kerosene and 160 ° C. for gasoline at high aromatics.
[0028]
The condenser obtains cooling water by a cooling water circulation 31. The cooling water passes counter-currently through the condenser before reaching the cooling water circulation 32. If the pressure of the device rises above the adjusted value despite the cooling and vacuum pumps, excess gas reaches the torch via the overpressure valve 33. Similarly, the pressurized water opening and the cooling water compression nozzle 34 are used to control critical operating conditions. Here, a cooling water stream is used to cool the temperature of the very hot zone of the device at 390 ° C. to a non-critical lower ignition temperature of less than 320 ° C. in case of accident or critical operating conditions.
[0029]
The introduced substances introduced into the apparatus by the supply means at the inlet 20 are residues 35, catalyst 36 and lime 37. The catalyst is introduced in the form of a fine powder, since it is present in a homogeneous suspension in the rotary evaporator. Sodium-aluminum-silicate is used instead of calcium-magnesium-silicate. In this case, the lime converts this sodium-aluminum-silicate to calcium-magnesium-silicate by ion exchange. In addition, calcium-magnesium silicate is an effective substance for the introduction of sodium-magnesium silicate.
[0030]
This conversion is always introduced, especially when using plastic waste, as the PVC contained in the plastic waste is removed by salt formation from the sodium portion of the catalyst by ion exchange or exchanges with hydrogen. Due to the subsequent reaction of the catalyst with lime or calcium hydroxide, the catalyst always takes the form of calcium-magnesium silicate and acts as active substance. The lime is fed by means of a vacuum pump, via a pH measurement in the gas, by a long running feed until pH 7 is again achieved in case of a drop in the pH value. Soda or caustic soda can be introduced instead of lime.
[0031]
In order to regenerate and purify the product gas introduced into the burner in front of the vacuum pump, the still liquid components are separated in a high-speed cyclone 38.
[0032]
This cyclone consists of a cyclone whose inlet nozzle extends in the form of a Bentley nozzle. The nozzle has, as an extension, a taper at the inlet, where the speed increases to a value of about 100 m / s, and a parallel section having at least 5 times the diameter and a 6 ° expansion of 3 to 6 times the diameter. An extension having a portion. The stabilized stream then separates the liquid better. The oil portion pushed out at the discharge port is returned to the safety container 6 by the heavy oil pump 39.
[0033]
The oil conveyed from the heavy oil pump 39 is used for maintaining the liquid level in the rotary evaporator 1 like the oil from the intermediate product container 9, and the liquid circulation and the reliable operation thereof are performed by the rotary evaporator. It depends on the oil circulation between the oil and the safety container being maintained at a sufficient level.
[0034]
At that time, heavy oil is important in the circulation because the reaction with the substance to be introduced is performed and the reaction with the circulating liquid is not performed. This should be maintained well to obtain liquid circulation. The device is therefore initially started with a kind of thermo-oil, such as is used for heat medium with thermo-oil, which is a water-poor oil that is difficult to evaporate. This oil is currently replenished where it is difficult to separate introduced substances such as asphalt in residual oils, but at elevated catalyst temperatures where it separates.
[0035]
Discharge of solids precipitated in the evaporator at the lower end of the evaporator is performed by a valve or a supply screw and a solenoid valve 40. A signal is then provided by the thermocouple 43, which, when deposited on the lower end, causes a temperature drop to the evaporator contents as a signal of the effluent. If solids settle, this is due to the temperature drop in the thermocouple to the circulating liquid. If this temperature drop exceeds a certain value, the exhaust is activated longer until it falls below this value again. This automates the periodic continuous discharge.
[0036]
The intermediate product container 9, additional residue oil containers for the waste oil to be treated and the residual oil and the supply of heavy oil from the heavy oil pump 39 are provided by a float switch 41 in a safety container. If the required level drops below a certain value, supply oil until this level is reached again. The signal for the supply of lime 36 is generated by a pH measuring sensor 42 in a vacuum conduit. A signal for temperature control is generated by the temperature sensor and the measurement sensor 43. In this case, not only is the valve controlled at the outlet, but also a temperature sensor is used as a sensor for measuring the heat-generating components of the device and the amount of catalyst added.
[0037]
The temperature sensor in the rotary evaporator above the tube bundle increases the amount of catalyst with increasing temperature, because in this case the reaction increases and the temperature decreases. If the temperature drops, start the addition burner. The starting burner is interrupted after the reaction temperature has been reached and the speed of the vacuum pump has reached a sufficient level, that is to say the minimum speed of the vacuum pump required for gas supply has been reached. If the temperature subsequently decreases, the vacuum increases and the burner is ignited again only after the temperature has further decreased.
[0038]
As the temperature further increases, the amount of feed to cool the device increases. The temperature is controlled by the amount of the substance introduced. As it rises further, the amount of gas to the burner is reduced by providing a gas flow opening to the torch. The energy supply can be formed by suction of the water vapor formed in the safety container.
[0039]
In the case of wet introduction, the water vapor and low-boiling parts formed at low temperatures are discharged at the upper end of the safety vessel by means of a water separator 44, the liquid part is dried via the high-speed cyclone 38 and passed to the combustion chamber Introduce.
[0040]
In this case, the vacuum pump connected to the circulation is separated by a solenoid valve in a non-operational stage so as not to lose the vacuum. The two gas streams from the condenser and from the water separator reach the combustion chamber 4 via the gas line 45, allowing for thermally stable operation without supplying different energies. In this case, the amount of gas relative to the total amount of products is about 3 to 7% in the energy part. On average about 4.5% of the gas is formed relative to the input material or product.
[0041]
In doing so, consideration must be given to adjusting the amount of gas constantly to the energy demands of the device. The safety conduit 46 to the torch is therefore opened only in case of sudden overproduction. For improved utilization of this gas energy, the evaporator tubes are provided with ribs in the rear part and are coated with a metal sponge or modified with a flame deflector 47 to flow. This baffle increases the flue gas path and allows for improved heat transfer in the evaporator.
[0042]
FIG. 2 shows the device of the present invention. The rotary evaporator 51 comprises a cylinder container having a tube bundle. The tube is not ribbed when viewed in the direction of the flame. The tube lying behind it in the shadow of the tube's rays has an enlarged surface structure such as a rib, metal sponge casting or baffle. The rotary evaporator 51 has a collection chamber on the lower and upper side of the tube, which is connected to a safety vapor container 56 having a tube next to it, thereby forming a circulation.
[0043]
A hydrocyclone 98 is arranged below the safety vapor container 56, which forms a circulation with the underlying liquid container 99 and the connecting tubular conduit between the rotary evaporator and the liquid container 99. A pump for discharging solids is arranged in a lower portion of the liquid container 99.
[0044]
On the right side of the rotary evaporator 51, there is a distillation evaporator 52 connected rearward on the flue gas side, and a distillation column is arranged on the distillation evaporator. To the left is a starting burner in the form of an oil burner 53, which is attached to a ceramic-coated combustion chamber 54. A gas conduit communicates with the combustion chamber, and the gas conduit is connected to a vacuum pump 60. The burner 53 has a separate circuit for air and oil supply, oil supply is temporarily interrupted during operation, but combustion air is always connected during operation.
[0045]
The rotary evaporator 51 has a honeycomb ceramic layer on both sides, and the layer is formed of a honeycomb ceramic block having a thickness of 50 to 100 mm. This material is preferably magnesium-aluminum-silicate (cordierite). A safety steam container 56 is arranged above the oil burner 53.
[0046]
It is large in size and has components to block bubbles. The safety container has a connection conduit to the rotary evaporator 51 and forms a liquid circulation with the rotary evaporator.
[0047]
The two evaporators, the rotary evaporator 51 and the distillation evaporator 52, are connected by an outlet 57 arranged below. The outlet is connected to two evaporators 51 and 52. A distillation column is arranged on the upper side, which column advantageously comprises a bell tray column. The column has an outlet in the receiver, the outlet being associated with the tubular conduit and the outlet vessel. The outflow vessels are two product vessels 58 and 59.
[0048]
In this case, the container 58 is an intermediate product tank, preferably a cylindrical atmospheric container, which is capable of storing oil. The vessel is connected to the safety vapor vessel by a conduit and a transport pump, the pump being connected via a level switch. Vessel 59 is a product tank for storing the final product, i.e., the product container is connected to various conduits. The intermediate product container 58 is connected to the safety container via a pump. Product container 58 is associated with a consumer or tank.
[0049]
In the case of a water-containing introduction substance, the intermediate product tank 58 is the original product tank, and the product tank 59 is used for obtaining a water portion. The gaseous products from the product tank 59 and the safety container 56 are sucked into the combustion chamber via the vacuum pump 60. The vacuum pump on the right-hand side is then only connected if the temperature in the safety container drops due to the formation of water vapor at the suction position. This separates the water vapor portion from the atmosphere in the safety container.
[0050]
The discharge of the solid is performed by a screw press 61 having a press cylinder 62. The conical press cylinder 62 increases the solids concentration by extruding the oil. Safety techniques for handling these devices with combustible oil are ensured by regulating techniques and in the event of an accident by a volume of cooling water 64 and a pressurized water cooling vessel 63 with compressed air 65 present thereon. In the case of an accident, the groundwater is prevented from being contaminated by the cooling water storage tank 66 by cooling with the pressurized water 64.
[0051]
A stirring device 67 is used to complete the movement of the solids introduced and formed. It is mounted on a rotary evaporator such that a stirrer projects through one of the tubes to the underside of the tube and the liquid reaches the underside of the tube. The solid discharged subsequently is conveyed by the extrusion screw 62 to the discharge screw 68, where it is further dried by indirect heating. The discharged oil vapor reaches the safety container from here.
[0052]
An introduction screw 69 is also present in the chimney or exhaust gas tube, which is arranged at the end. The introduction screw has double walls. Flue gas is supplied to the intermediate wall separately from the screw contents. The screw has a coupling conduit to inlet 70. The flue gas conduit transitions to a flue gas pipe 71. At the lower end of the flue gas pipe 71 there is a condensate discharge means having a neutralizer 72, the condensate discharge pipe facing out.
[0053]
A foam suppressing device 73 is arranged in the distillation evaporator 52. It consists of sieve or metal sponge castings arranged one on top of the other and is located below the distillation column 74. The low-boiling fraction is removed in distillation column 74 via conduit 75. The product is formed in an underlying receiver and is withdrawn in conduit 76 where a tubular conduit attached to the receiver is associated with the product container.
[0054]
A temperature sensor is located above the receptacle of the distillation column, and the temperature sensor is electrically connected by a liquid bleed solenoid valve. Within a determined temperature at which product quality is imparted, the circuit opens the solenoid valve. The properties of the product are determined by the boiling temperature of the respective column section and the receiver, taking into account the control of the product. This is performed by a condenser 77 and a solenoid valve 79. Backwash 80 and solenoid discharge valve are electrically activated with an electrical connection conduit to the product temperature indicator. At the end of the condenser 77 is attached a vacuum conduit 78, which leads to a product container 59.
[0055]
The condenser obtains cooling water by a cooling water circulation 81. The cooling water passes counter-currently through the condenser and then reaches the cooling water outlet 82. If the pressure of the device rises above the regulated value despite the cooling and vacuum pumps, excess gas reaches the torch via the overpressure valve 83.
[0056]
Similarly, a cooling water pressurizing nozzle 84 is coupled to a solenoid valve, which is electrically connected to a flame detector and a flue gas detector, from which its opening impulse is obtained. The cooling water stream is thus used to cool the temperature of the very hot zone of the device at 390 ° C. to a non-critical low ignition temperature of less than 320 ° C. in the event of an accident or in critical operating conditions.
[0057]
The inlet substance inlet 70 is connected to the inlet for the residue 85, the catalyst 86 and the lime 87 via a supply means. The residue contains hydrocarbons and has the form of meat flour, fat, waste oil, vacuum residue, plastic, wood flour or rubber. The catalyst is introduced in the form of a fine powder and has a chemical structure of powdered calcium-magnesium-silicate or sodium-aluminum-silicate. The sodium-aluminum silicate is subsequently converted into calcium-magnesium silicate by ion exchange. Thus, calcium-magnesium-silicate is an effective substance when introducing sodium-magnesium-silicate.
[0058]
This change is always introduced, in particular when using plastic waste, because the PVC contained in the plastic waste removes sodium by salt formation from the catalyst by ion exchange or exchanges with hydrogen. In this case, due to the reaction of the catalyst with lime or calcium hydroxide, the catalyst always takes the form of calcium-magnesium silicate and acts as active substance. The lime is supplied by means of a vacuum pump via pH measurement in the gas by continuing to supply for a long time until the pH 7 is again reached if the pH value drops. Soda or caustic soda can be introduced instead of lime.
[0059]
The burner gas conduit is connected to the high speed cyclone 88. It consists of a cyclone whose introduction nozzle extends in the form of a Venturi nozzle. The nozzle has a taper at the inlet as an extension, at which the speed increases to a value of about 100 m / s, and a parallel part with a diameter of at least 5 times and a 6 ° enlargement and 3-6 times Having an enlarged portion having a diameter of The stabilized stream then separates the liquid better.
[0060]
A heavy oil pump 89 is disposed in the outlet 57, and the heavy oil pump is connected to the safety container 56. Similarly, a connecting conduit is arranged between the intermediate product container 59 and the rotary evaporator 51. The rotary evaporator 51 contains a kind of thermo oil which is hardly evaporated and has a low water content, and is used as a heating medium having thermo oil.
[0061]
Solids precipitated in the evaporator at the lower end of the evaporator are discharged via a valve or feed screw, solenoid valve 90. It is electrically connected to a thermocouple 93 via a regulator and a frequency-varying motor in the electronics.
[0062]
The intermediate product container 59, the residual oil container and the heavy oil connection conduit from the heavy oil pump 89 are controlled by a float switch 91 in the safety container. The signal of the supply of lime 87 is generated by a pH measuring sensor in a vacuum conduit. The temperature adjustment signal is generated by the temperature sensor and the measurement sensor 93. This controls not only the outlet valve, but also the heat generating components of the device and the amount of catalyst supplied.
[0063]
The temperature sensor in the rotary evaporator on the upper side of the tube bundle is electrically connected to the supply device for the amount of catalyst. As the temperature rises, the feeder is adjusted to a higher feed rate.
[0064]
If the temperature drops, start the addition burner. When the reaction temperature has been reached and the vacuum pump has achieved the minimum number of revolutions required for gas supply, the addition burner is interrupted. If the temperature continues to drop, the vacuum is increased and the burner is ignited again only when the temperature drops further.
[0065]
If the temperature rises further, the amount of feed to cool the device is increased. The temperature is controlled by the amount of feed. When further raised, the gas flow to the torch reduces the amount of gas to the burner by providing an opening for the gas flow. The energy supply is generated by suction of the water vapor formed in the safety container. In the case of wet introduction, the water vapor and low boiler fractions formed at low temperatures are discharged at the upper end of the safety vessel by means of a water separator 94 and the liquid fraction is dried via a high-speed cyclone 88 to form a combustion chamber. To be introduced.
[0066]
In this case, the vacuum pump connected to the circulation is disconnected via a solenoid valve in a non-operational stage in order to maintain the vacuum. The two gas streams from the condenser and from the water separator reach the combustion chamber 54 via the gas conduit 95, allowing for thermally stable operation without dissimilar energy supply. In this case, the gas amount in the energy part is about 3 to 7% based on the total product amount. On average 4.5% of gas is produced relative to the input material or product.
[0067]
At that time, consideration should be given to adjusting the amount of gas to always match the energy demand of the device. The safety conduit 96 to the torch is therefore opened only in case of sudden overproduction. To make good use of this gas energy, the evaporator tubes are provided with ribs in the rear part and are coated with a metal sponge or modified with a flame deflector 97 to flow. The safety conduit 96 is provided with an overpressure valve for 0.2-0.5 bar overpressure.
[0068]
The safety conduit is connected to the overpressure vessel outside the vessel, the overpressure vessel being formed as a cyclone. At the lower end of this vessel is a liquid separator and a condensation vessel. The gas conduit of the overpressure vessel is optionally formed as a torch. For this purpose, an ignition device is provided depending on the flow observer.
[0069]
The method of the present invention will be described in detail with reference to examples.
[0070]
The rotary evaporator 1 has a volume of 500 liters and the neighboring distillation evaporator 2 has a volume of 500 liters as well. Disposed in the evaporator are one hundred two inch diameter tubes and two cm thick ribs. The first three tubes, viewed in the direction of the burner, have no ribs.
[0071]
To achieve a reaction temperature of 390 ° C., a starting burner in the form of an oil burner 3 having a power of 200 kW is used, in which the oil produced for the starting process burns. This takes place in a combustion chamber 4 having a volume of 100 liters, the combustion chamber operating at a maximum of 16 m. ³ / H under a reduced pressure of 0.2 bar using gas from a vacuum pump 10 having an efficiency of / h. The operation from the burner 3 is not performed in the operation state, and the burner is 200 m during the operation. ³ / H of combustion air only.
[0072]
The rotary evaporator 1 has, on both sides, a honeycomb ceramic layer 5 composed of 4 × 4 honeycombs having a thickness of 100 mm and an area of 150 × 150 mm. To function optimally due to the increased radiation part. The hydrocarbons which evaporate in conjunction with the separating action of the calcium-aluminum-silicate added here have a volume of 5 m. ³ Is collected in the safety steam container 6.
[0073]
This container is large, if possible, because the foam generated by the foam-forming agent does not reach the product. The non-evaporable part is collected at the bottom of the safety container and separates in the hydrocyclone on the underside of the lower side of the safety container, from there via a 500 liter liquid and slurry separation container via the connecting tubular conduit of the DN200. Again to the rotary evaporator, whereby a circulation is formed.
[0074]
Two evaporators, rotary evaporator 1 and distillation evaporator 2, have a volume of 0.5 m ³ And the outlet removes the precipitated solids from the two evaporators 1 and 2. On the product side, the evaporated material condensing in a distillation column 0.4 mm in diameter and 6 m in height has a volume of 1 m each. ³ Is discharged onto the product containers 8 and 9. In this case, the container 8 is an intermediate product tank for temporarily storing oil in order to maintain the liquid level in the rotary evaporator, and the container 9 is a product tank for storing the final product.
[0075]
In the case of an introduced substance containing water, the intermediate product tank 8 is the original product tank and the product tank 9 is used for obtaining the water portion. The gaseous products from the product tank 9 and the safety container 6 are sucked into the combustion chamber via the vacuum pump 10. In this case, the vacuum pump on the right is connected only when the temperature in the safety container has dropped due to the formation of water vapor at the suction position. This separates the water vapor portion from the atmosphere in the safety container.
[0076]
The discharge of the solid is performed by a screw press 11 having a press cylinder 12. It has a diameter of 250 mm and has a screw height tapering from 80 mm to 50 mm. The conical tapered press cylinder 12 increases the solids concentration by extruding the oil. There is a perforated filtration cylinder with a 1 mm diameter hole around the screw press. The emissions are 6% for plastics with 3% PVC consisting of 3% calcium chloride, 1% catalyst in the form of calcium-aluminum-silicate and 2% residual oil. The product amount is 500 kg / h of oil in the boiling range of the heating oil when 550 kg / h of plastic is introduced.
[0077]
The safety technology dealing with these devices using combustible oils is regulation technology and, in the event of an accident, a total volume of 10 m with the contents of the cooling water 14 and the compressed air 15 present thereon. ³ Is ensured by the pressurized water cooling vessel 13 having In the case of an accident, the cooling water is collected at the lower side of the device by cooling with the cooling water 14, whereby ³ To prevent groundwater contamination by the cooling water holding tank 16 having the total volume of
[0078]
A stirring device 17 is used to complete the movement of the solids introduced and formed. The solids subsequently discharged are conveyed to the discharge screw 18 by the extrusion screw 12, where they are further dried by indirect heating. The discharge screw also has a diameter of 250 mm and a length of 1 m. It is a double wall with a 40 mm flue gas hollow. The expelled oil vapor reaches the safety container from here.
[0079]
Similarly, in the flue gas stream there is an inlet screw 19, also having a diameter of 250 mm, a length of 1 m and a flue gas hollow of 40 mm, in which the substance introduced from the inlet 20 is indirectly heated by the flue gas. It is dried and introduced directly into the circulating fluid by means of a subsequent inlet tubular conduit. The introduction into the liquid avoids the contamination of the vapor with finely divided inputs such as meat powder contaminated with prions and allows for a 100% conversion of the problem substances introduced.
[0080]
The flue gas thus cooled reaches the outside via a flue gas pipe 21 having a diameter of 250 mm. At that time, the condensed liquid condensed in the flue gas pipe 21 in the heated state is formed and discharged to the outside by the condensed liquid discharge pipe having the neutralizer 22. The cooling of the flue gas achieved is 450 ° C. in the rotary evaporator stage, 350 ° C. in the distillation evaporator, 250 ° C. in the post-dryer and 150 ° C. in the inlet dryer. At the start, the dryer has an additional burner to ensure the required minimum temperature.
[0081]
Product formation in the distillation evaporator 2 is protected by foam suppression means 23, which takes into account that only the vapor reaches the distillation column 24 without the liquid part of the foam, and that the product is particularly cleanly formed. . The foam suppressing means has a sponge casting structure made of aluminum and has a thickness of 4 mm. A low boiler is formed at the upper end of the column in a distillation column 24 having 20 receivers of 5 units each having 4 receivers and a receiver spacing of 30 mm and is removed in a conduit 25. The product is formed in the underlying receiver and is discharged in conduit 26. The distillation column is a bell tray column.
[0082]
The properties of the product are determined by the boiling temperature of the respective column section and the receiver, taking into account the control of the product. This is performed by a condenser 27 and a solenoid valve 29. Activate backwash 30 to reduce product evaporation temperature.
[0083]
At the end of the condenser 27 a vacuum conduit 28 is attached, which pours into the product container 9. The value adjusted as the average boiling temperature at the product outlet is 270 ° C. for diesel oil, since the input material is mostly plastics with PE and PP.
[0084]
The condenser has a cooling efficiency of water up to 200 kW. Cooling water is obtained by a cooling water supply pipe 31 having a diameter of 1.5 inches. The cooling water passes counter-currently through the condenser and then reaches the cooling water discharge pipe 32. If the pressure of the device rises above the regulated value despite the cooling and vacuum pumps, the overpressure valve 33 will cause excess gas to reach the torch.
[0085]
In order to prevent critical operating conditions, pressurized water openings are likewise used for 100 l / min water discharge by cooling water pressurizing nozzles 34 at 1 and 2 minute intervals. Here, in the event of an accident or in critical operating conditions, a cooling water stream is used to cool the temperature of the hottest zone of the device at 390 ° C. to a non-critical lower ignition temperature of less than 320 ° C.
[0086]
The substances introduced into the apparatus via the supply means at the inlet 20 are residues 35, catalyst 36 and lime 37. The catalyst is introduced in the form of a fine powder, since it is present in a homogeneous suspension in the rotary evaporator. 6 kg / h of calcium-aluminum-silicate are used. Every hour, 15 kg of lime are added, adjusted via a pH probe. Thus, calcium-magnesium-silicate is an effective substance when introducing sodium-magnesium-silicate.
[0087]
The still gaseous components are discharged in a high-speed cyclone 38 in order to sort and purify the product gas introduced into the burner in front of a vacuum pump. Fast cyclones consist of cyclones in which the inlet nozzle extends in the form of a Venturi nozzle. The nozzle has, as an extension, a taper at the inlet, a speed in the section increasing to a value of about 100 m / s, and a parallel section having at least 5 times the diameter and a 6 ° expansion and 3 to 6 times the diameter Having an enlarged portion having The stabilized stream then separates the liquid better. The cyclone has the narrowest diameter at the venturi inlet section of 300 mm diameter and 15 × 25 mm.
[0088]
The oil portion extruded at the outlet is returned to the safety container 6 by the heavy oil pump 39 having a pump efficiency of 50 l / h. It is used here to maintain the liquid level in the rotary evaporator 1 as well as the oil from the intermediate product container 9 and the liquid circulation of the rotary evaporator and thus the reliable operating mode is It relies on maintaining a sufficient level of oil circulation between the safety containers.
[0089]
At that time, heavy oil is important in the circulation, since the reaction with the substance to be introduced takes place and the reaction with the circulating liquid does not take place. This is maintained sufficiently to obtain liquid circulation. Therefore, the apparatus is first started with a low-oil-evaporating oil, a kind of thermo-oil such as that used for heat transfer media with thermo-oil. This oil is currently replenished by parts which are difficult to separate, e.g. asphalt in residual oil, but which separate at high catalyst temperatures.
[0090]
The discharge of solids settled in the evaporator at the lower end of the evaporator is performed by a valve or a supply screw having a diameter of 25 mm, a solenoid valve 40. A signal is then generated by the thermocouple 43, which, when settling at the lower end, produces a drop in the temperature of the evaporator contents as a signal at the outlet.
[0091]
This allows for a drop in temperature at the thermocouple to the circulating liquid if solids settle. If this temperature drop exceeds a certain value, the discharge is activated until it falls below this value again. As a result, periodic continuous ejection is automated.
[0092]
The supply of heavy oil from the intermediate product container 9, additional waste oil containers for the waste oil to be treated and the residual oil and the heavy oil pump 39 is effected by a float switch 41 in the safety container. If the required level drops below a certain value, supply oil until the level is reached again. The signal for supplying lime 36 is generated by a pH measuring sensor 42 in a vacuum conduit. A signal for temperature control is generated by the temperature sensor and the measurement sensor 43. In this case, not only is the outlet valve controlled, but also the temperature sensor is used as a sensor for measuring the heat-generating components of the device and the amount of catalyst added.
[0093]
The temperature sensor in the rotary evaporator above the tube bundle increases the amount of catalyst with increasing temperature, because in this case the reaction increases and the temperature decreases. Start the addition burner when the temperature drops. After the reaction temperature has been reached and the full speed of the vacuum pump has been reached, ie the minimum speed of the vacuum pump required for the gas supply, the starting burner is interrupted. If the temperature continues to drop, the vacuum is increased and the burner is ignited again only when the temperature drops further. The limit temperature at which the reaction with the gas takes place naturally is 410 ° C. for this introduced substance.
[0094]
If the temperature rises further, the amount of feed to cool the device is increased, with the safety vessel being adjusted to a temperature about 100 ° C. lower than the rotary evaporator. The temperature is adjusted according to the amount of feed. If it rises further, the amount of gas to the burner is reduced by releasing and supplying the gas flow to the torch. The energy supply is generated by suction of the water vapor formed in the safety container. The water vapor and low boiling parts formed at low temperature in the case of wet introduction are discharged at the upper end of the safety vessel at the water separator 44 and the liquid part is dried via the high speed cyclone 38 and introduced into the combustion chamber. I do.
[0095]
In this case, the vacuum pump connected to this circuit is separated by a solenoid valve in the non-operational stage so as not to lose the vacuum. The two gas streams from the condenser and the water separator reach the combustion chamber 4 via the gas conduit 45, allowing for thermally stable operation without dissimilar energy being supplied. The amount of gas generated relative to the total product is 4.5% gas in the energy part with respect to the introduced substance or product.
[0096]
In doing so, care must be taken to adjust the gas volume to always meet the energy demands of the device. The safety conduit 46 to the torch is therefore opened only in case of sudden overproduction. In order to make good use of this gas energy, the evaporator tubes are covered with metal sponge on the rear part and are improved with a flame deflector 47 to flow. This baffle increases the flue gas path and allows for improved heat transfer in the evaporator.
[0097]
According to another embodiment, the device of the present invention will be described in detail. The rotary evaporator 51 consists of a cylindrical vessel having a tube bundle of 100 tubes having a diameter of 2 inches and a height of 1200 mm. The collecting chambers at the lower and upper ends have a height of 300 mm. The tube has no ribs when viewed in the direction of the flame. The tube lying behind the shadow of the tube's rays has a surface-enhancing structure such as a rib, foam metal casting or deflector. The rotary evaporator 51 has a collecting chamber on the lower and upper side of the tube, which is connected by a tube with the safety vapor container 56 located next to it, so that a circulation is formed.
[0098]
Below the safety vapor container there is a hydrocyclone with a tangential inflow tubular opening DN150, and at the lower end of the safety vapor container there is a liquid container 600 mm in diameter and 1 m high. It has a connecting conduit DN250 to the rotary evaporator in the upper part.
[0099]
On the right side of the rotary evaporator, there is a distillation evaporator 52 connected downstream on the flue gas side, on which the distillation column is arranged. To the left is a starting burner in the form of a Hermann oil burner 53 with a power of 200 kW, mounted on a ceramic-coated combustion chamber 54 having a diameter of 500 mm and a length of 800 mm. Gas suction efficiency 16m at 2.5 inch diameter and 0.2 bar reduced pressure in the combustion chamber ³ / H, a gas conduit with a vacuum pump 60 of / h.
[0100]
Burner 53 is 200m in air ³ / H and a separate circuit for 20 l / h of oil supply, the oil supply is temporarily interrupted during operation, but the combustion air bubbles are always connected during operation.
[0101]
The rotary evaporator 51 has a honeycomb ceramic layer on both sides, and the ceramic layer is formed of a honeycomb ceramic block having a thickness of 50 to 100 mm. The honeycomb is a 4 × 4 honeycomb having a cross-sectional area of 150 × 150 mm. This material is preferably magnesium-aluminum-silicate (cordierite). Above the burner 53, a safety steam container 56 having a diameter of 2 mm and a height of 3 m is arranged. It is large and has foam suppression components. The container has a connection conduit to the rotary evaporator 51, with which a liquid circulation is formed.
[0102]
The two evaporators, the rotary evaporator 51 and the distillation evaporator 52, are both identically formed and are connected to an outlet 57 arranged below. The outlet is connected to two evaporators 51 and 52. The distillation column is arranged on the upper side and consists of a bell tray column with a diameter of 400 mm, a receiver spacing of 300 mm and 6 × 5 units, ie each unit is processed into 6 receivers. The column has an outlet in the receiver, the outlet being associated with the tubular conduit and the outlet vessel. This is two product containers 58 and 59, each having a diameter of 1500 mm and a height of 2 m.
[0103]
In this case, the container 58 is an intermediate product tank, preferably a cylindrical atmospheric container, which is capable of storing oil. The vessel is connected to the safety steam vessel by a conduit and a transport pump having an efficiency of 1000 l / h, the transport pump being opened and closed by a level switch. Vessel 59 is a product tank for storing the final product, i.e., the product container is connected to various conduits. The intermediate product container 58 is connected to the safety container via a 500 l / h pump. Product container 58 is associated with a user or tank.
[0104]
In the case of an introduced substance having water, the intermediate product tank 58 is the original product tank and the product tank 59 is used for obtaining the water portion. The gaseous products from the product tank 59 and the safety container 56 are sucked into the combustion chamber via the vacuum pump 60.
[0105]
The vacuum pump on the right then opens only if the temperature in the safety container drops due to the formation of water vapor at the suction position. This separates the water vapor portion from the atmosphere in the safety container.
[0106]
The discharge of the solid is performed by a press cylinder 62 and a screw press 61 having a diameter of 250 mm. The conical tapered press cylinder 62 increases the solids concentration by extruding the oil. The safety technology for handling this device with combustible oil is regulation technology and 10m in case of accident ³ Of cooling water 64 and a pressurized water cooling container 63 having compressed air 65 present thereon. In the case of an accident, 20m by cooling with cooling water 64 ³ To prevent groundwater from being contaminated by the cooling water storage tank 66.
[0107]
A stirrer 67 is used to complete the transfer of the solids introduced and formed. The stirrer is mounted on the rotary evaporator such that the stirrer projects through one of the tubes to the underside of the tube and the liquid reaches the underside of the tube. The solid discharged subsequently is conveyed by the extrusion screw 62 to the discharge screw 68, where it is further dried by indirect heating. From here the discharged oil vapor reaches the safety container.
[0108]
Also located at the end is an inlet screw 69 having a diameter of 250 mm in a chimney or exhaust gas pipe of diameter 250 mm. The introduction screw has a double wall with a hollow of 50 mm. Flue gas is introduced separately from the screw contents in the intermediate wall. The screw has a coupling conduit to inlet 70. The flue gas conduit transitions to a flue gas pipe 71. At the lower end of the flue gas pipe 71 a condensate discharge is present towards the outside with a neutralizer 72 having a condensate discharge pipe.
[0109]
A bubble suppressor 73 is disposed in the distillation evaporator 52. The foam suppressor consists of six superimposed sieves and is located below the distillation column 74. The low boiling point portion is removed into distillation column 74 via a 1 inch diameter conduit 75. The product is formed in an underlying receptacle, removed in conduit 76, and a tubular conduit attached to the receptacle is associated with the product container.
[0110]
A temperature sensor is located above the receiver of the distillation column and is electrically connected to a 1 inch diameter liquid discharge solenoid valve. A switch opens the solenoid valve within a predetermined temperature at which product quality is determined. The properties of the product are determined by the boiling temperature of the respective column section and the receiver, taking into account the regulation of the product.
[0111]
This is done by a condenser 77 and a solenoid valve 79 in a 1.5 inch conduit having a 1.5 inch solenoid valve. The backwash 80 and solenoid valve are electrically activated with an electrical connection conduit to the product temperature indicator. At the end of the condenser 77 is attached a vacuum conduit 78, which leads to a product container 59.
[0112]
20 cooling pipes having a diameter of 1 inch and a condenser having a cooling efficiency of 200 kW obtain cooling water through a cooling water supply pipe 81. The cooling water passes counter-currently through the condenser and then reaches the cooling water discharge pipe 82. If the pressure of the device exceeds the regulated value despite the cooling and vacuum pumps, excess gas will reach the torch via the overpressure valve 83. Similarly, a cooling water pressurizing nozzle 84 is coupled to the solenoid valve, which is electrically connected to the flame and flue gas detector, from which its open impulse is obtained.
[0113]
In the event of an accident or in critical operating conditions, cooling water cools the temperature of the hottest zone of the device at 390 ° C to a non-critical lower ignition temperature of less than 320 ° C.
[0114]
An introduction substance introducer 70 having an efficiency of 600 kg / h of plastic is connected via a feed device with a residue introduction 85, a 6 kg / h catalyst 86 and a 15 kg / h lime 87. The residue contains hydrocarbons and has the form of a plastic. The catalyst is introduced in the form of a fine powder and has a chemical structure of powdered calcium-magnesium-silicate.
[0115]
This conversion is always carried out, especially when using plastic waste, since the PVC contained in the plastic waste removes sodium from the catalyst by salt exchange or exchanges with hydrogen for ion exchange. Due to the reaction of the catalyst with lime or calcium hydroxide, the catalyst always takes the form of calcium-magnesium silicate and acts as active substance. Lime is supplied by a vacuum pump by supplying pH until pH 7 is again achieved if the pH value is reduced by adjusting the pH in the gas. Soda or caustic soda can be introduced instead of lime.
[0116]
The burner gas conduit is connected to the high speed cyclone 88. The fast cyclone consists of a cyclone having a diameter of 300 mm, the introduction nozzle of the cyclone extending in the form of a Venturi nozzle. The nozzle has, as an extension, a tapered portion at the inlet at the height of 15 × 25 mm, a parallel portion with a length of 75 mm and an enlarged portion with a 6 ° enlarged portion with a length of 60 mm. The stabilized stream then separates the liquid better.
[0117]
A heavy oil pump 89 having a transfer capacity of 100 l / h is arranged in the discharge port 57 and is connected to the safety container 56. Similarly, a connecting conduit is arranged between the intermediate product container 59 and the rotary evaporator 51.
[0118]
The rotary evaporator 51 includes a kind of thermo-oil, such as oil used in water with low water evaporation and thermo-oil containing thermo-oil.
[0119]
The discharge of the solids precipitated in the evaporator at the lower end of the evaporator is effected by means of a valve or a supply screw having a diameter of 250 mm, a solenoid valve 90. The solenoid valve is connected to the thermocouple 93 via a regulator in the electronics and a frequency varying motor of the valve.
[0120]
The intermediate product container 58, the residue container and the heavy oil coupling conduit from the heavy oil pump 89 are provided by a float switch 91 in the safety container. The signal supplying lime 87 is generated by a pH measuring sensor 92 in a vacuum conduit.
[0121]
A signal for temperature control is generated by a temperature and measurement sensor 93. In this case, not only the exhaust valve is adjusted by the sensor, but also the heat generating components of the apparatus and the amount of catalyst added.
[0122]
A temperature sensor in the rotary evaporator above the tube bundle is in electrical communication with the catalyst supply. As the temperature increases, the feeder is adjusted to more additions. Start the addition burner when the temperature drops. This is interrupted when the reaction temperature has been reached and the vacuum pump has reached the minimum speed required for gas supply. If the temperature continues to drop, the vacuum is increased and the burner is ignited only when the temperature drops further.
[0123]
If the temperature rises further, the amount of feed to cool the device is increased. The temperature is adjusted according to the amount of gas introduced. As it rises further, the amount of gas to the burner is reduced by opening the gas flow supply to the torch. The energy supply can then be generated by suction of the water vapor formed in the safety container. In the case of wet introduction, the water vapor and low boiler fractions which form at lower temperatures are discharged at the upper end of the safety vessel by means of a water separator 94 and the liquid fraction is dried via a high speed cyclone 88 and introduced into the combustion chamber. .
[0124]
In this case, the vacuum pump connected to the circulation is disconnected via a solenoid valve in a non-operation state so as not to impair the vacuum. The two gas streams from the condenser and the water separator reach the combustion chamber 54 via a gas conduit 95, allowing for a thermally stable operation without supplying dissimilar energy. In this case, the amount of gas relative to the total amount of products is about 3 to 7% in the energy part. On average 4.5% of gas is produced relative to the input material or product.
[0125]
In doing so, care must be taken to ensure that the gas volume is always adapted to the energy demands of the device. Thus, in the event of a sudden overproduction, the safety conduit 96 to the torch is opened. To make good use of this gas energy, the evaporator tubes are provided with ribs in the rear part and are covered with a metal sponge or flow better through the flame deflector 97. The safety conduit 96 has a 0.2-0.5 bar overpressure overpressure valve.
[Brief description of the drawings]
FIG.
It is a 1st work process figure which implements liquefaction processing of the present invention.
FIG. 2
It is a 2nd work process figure which performs liquefaction processing of the present invention.
[Explanation of symbols]
1 Rotary evaporator
2 Distillation evaporator
3 Oil burner
4 Combustion chamber
5 Catalyst
6 Safety steam container
7 outlet
8 Product container / intermediate product tank
9 Product container / product tank
10 Vacuum pump
11 Screw press
12 Press cylinder / Extrusion screw
13 Overpressure water cooling vessel
14 Cooling water
15 Compressed air
16 Cooling water storage tank
17 stirrer
18 Discharge screw
19 Introduction screw
20 Inlet
21 Exhaust gas pipe / flue gas pipe
22 Condensate discharger with neutralizer
23 foam suppressor
24 distillation column
25 conduit
26 conduit
27 Condenser
28 Vacuum conduit
29 solenoid valve
30 Backwash
31 Cooling water supply pipe
32 Cooling water discharge pipe / cooling water reverse flow pipe
33 Safety valve / overpressure valve
34 Cooling water overpressure nozzle
35 residue
36 catalyst
37 lime
38 High speed cyclone
39 Fuel Oil Pump
40 solenoid valve
41 Floating switch
42 pH measurement sensor
43 Temperature and measurement sensors / thermocouples
44 Water separator
45 gas conduit
46 Safety conduit
47 Flame deflector
48 cyclone device
49 Settling vessel
50 oil pump
51 Rotary evaporator
54 Combustion Chamber
55 catalyst
56 Safety steam container
57 outlet
58 Product container / intermediate product tank
59 Product container / product tank
60 vacuum pump
61 Screw Press
62 Press Cylinder / Extrusion Screw
63 Overpressure water cooling container
64 cooling water
65 compressed air
66 Cooling water storage tank
67 Stirrer
68 Discharge screw
69 Introduction screw
70 Inlet
71 Exhaust gas pipe / flue gas pipe
72 Condensate discharger with neutralizer
73 foam suppressor
74 distillation column
75 conduit
76 conduit
77 condenser
78 Vacuum conduit
79 Solenoid valve
80 Backwash
81 Cooling water supply pipe
82 Cooling water discharge pipe / Cooling water reverse flow pipe
83 Safety valve / Overpressure valve
84 Cooling water pressurizing nozzle
85 residue
86 catalyst
87 lime
88 High speed cyclone
89 Fuel Oil Pump
90 solenoid valve
91 Floating switch
92 pH measurement sensor
93 Temperature and measurement sensors / thermocouples
94 Water separator
95 gas conduit
96 Safety conduit
97 Flame deflector
98 cyclone equipment / hydrocyclone
99 sedimentation container / liquid container
100 pumps

Claims (15)

In a process for liquefying residues having a high hydrocarbon content at normal pressure, this substance is introduced together with surface-active additives into a hot oil circulation at 300-450 ° C. and converted to oil in the boiling range of 100-350 ° C. A method of liquefying a residue under normal pressure. 2. The process according to claim 1, wherein the surface-active additive is a soil mineral in the calcium-aluminum-silicate active substance or is converted to this substance by adding lime to the circulating oil. 3. The process as claimed in claim 1, wherein the introduction material comprises a ternary hydrocarbon-containing residue, a clay mineral in the form of calcium-aluminum-silicate or sodium-aluminum-silicate and lime convertible into this form. 4. The method according to claim 3, wherein the circulating liquid or oil is fed directly via a pipe, the feed pipe ending on or in the liquid. The method of claim 1 wherein the apparatus is maintained under slight vacuum by a vacuum pump and the pressure at the inlet is near atmospheric. 6. The process as claimed in claim 1, wherein the temperature of the circulation is increased by an additional burner, the vacuum is increased and the supply is reduced and the excess gas is released by the resulting separation gas. 7. The method according to claim 1, wherein a hydrocyclone and a separation vessel are mounted below the safety vessel, which close off the circulation to the rotary evaporator and continuously separate the solids. 7. The process as claimed in claim 1, wherein the formation of harmful products of chlorine and fluorine is prevented by ion exchange of additives and other regenerated substances such as lime or soda. The separation reaction and the stabilization reaction are carried out in one oil circulation, the catalyst is suspended in the circulation, and the circulation is carried out by heating from the separation gas and cooling by the introduced substance. The described method. A device for carrying out a method for liquefying hydrocarbon-containing residues at normal pressure, comprising a circulating vessel for separating, detoxifying and stabilizing oil in a tube bundle evaporator and a regulating vessel and a safety vessel for returning liquid components, Apparatus for carrying out a method for liquefying hydrocarbon-containing residues at normal pressure, characterized in that the system is combined with a combustion chamber for burning the separation gas. 11. The apparatus according to claim 10, wherein a flue gas-heated distillation apparatus is present on the side remote from the burner alongside the separation parts of the apparatus, the distillation apparatus being connected on the product side to the evaporation space of the separation apparatus. 12. The apparatus according to claim 10, wherein a flue gas pipe having a heating device for the residue and the introduced substance is connected to the rear of the distillation apparatus. An electrolysis is connected behind the solids outlet after drying and heating, the electrolysis converting the insoluble calcium phosphate residue from the treatment of animal residues to soluble monocalcium phosphate or phosphoric acid. 13. The device according to any one of the preceding items, up to 12. The solids are discharged from the lower part of the evaporator to a suction pipe via a transfer mechanism, for example a transfer screw, which is led to one of the parts above the liquid level of the device, where this part is introduced. 11. The device according to claim 10, comprising a separating sieve below the opening. 15. Apparatus according to claim 10, wherein a hydrocyclone and a liquid container are arranged below the safety container, which are connected to the rotary evaporator 51 via a tubular conduit.