US20130240411A1 - Device and method for separating mixtures which contain oil or bitumen and additives - Google Patents
Device and method for separating mixtures which contain oil or bitumen and additives Download PDFInfo
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- US20130240411A1 US20130240411A1 US13/813,251 US201113813251A US2013240411A1 US 20130240411 A1 US20130240411 A1 US 20130240411A1 US 201113813251 A US201113813251 A US 201113813251A US 2013240411 A1 US2013240411 A1 US 2013240411A1
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- Prior art keywords
- solvent
- bitumen
- oil
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
- C10G1/045—Separation of insoluble materials
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/28—Recovery of used solvent
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- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
- E01C19/00—Machines, tools or auxiliary devices for preparing or distributing paving materials, for working the placed materials, or for forming, consolidating, or finishing the paving
- E01C19/02—Machines, tools or auxiliary devices for preparing or distributing paving materials, for working the placed materials, or for forming, consolidating, or finishing the paving for preparing the materials
- E01C19/10—Apparatus or plants for premixing or precoating aggregate or fillers with non-hydraulic binders, e.g. with bitumen, with resins, i.e. producing mixtures or coating aggregates otherwise than by penetrating or surface dressing; Apparatus for premixing non-hydraulic mixtures prior to placing or for reconditioning salvaged non-hydraulic compositions
- E01C19/1004—Reconditioning or reprocessing bituminous mixtures, e.g. salvaged paving, fresh patching mixtures grown unserviceable; Recycling salvaged bituminous mixtures; Apparatus for the in-plant recycling thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/02—Settling tanks with single outlets for the separated liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2221/00—Applications of separation devices
- B01D2221/04—Separation devices for treating liquids from earth drilling, mining
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4006—Temperature
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/44—Solvents
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/80—Additives
Definitions
- the present invention relates to a device and to a method for separating mixtures which contain oil or bitumen and additives.
- the device and the method are particularly applicable to separating stone chippings and bitumen in evacuated asphalt road surfaces.
- the mineral phase can be separated from the oil phase also with oil sands and oil shale, and a separation of bitumen and carrier felt can be induced with the recycling of bitumen felt, oil binder and oil.
- a method is disclosed in DE 600 10 533 T2,with which the aggregate is separated from the bitumen share, by way of a thermal decomposition of the bitumen encasing. Bitumen is thereby used as a fuel and is activated by introducing hot gases into a drum which contains the excavated material.
- the method however has the disadvantage that it is coupled to the manufacture of new asphalt and may only be carried out at a high energy expense.
- a device for separating mixtures, which contain oil or bitumen and additives, includes a reaction vessel, into which the mixture and a solvent can be brought through a feed opening and/or a filling conduit, into a reaction space, further including a supply container with a vapor space, at least one capture container with a withdrawal conduit and with a riser conduit, and a condensation vessel.
- the mixture is filled in through the feed opening while the solvent is introduced through the filling conduit, but also only one opening can be provided for this purpose for space-saving reasons.
- the opening in any case is closed via a valve.
- the solvent dissolves the oil-containing or bitumen-containing material from the additives, in the reaction space in an initial method step.
- the solvent dissolves the oil-containing or bitumen-containing material from the additives, in the reaction space in an initial method step.
- the solvent laden with oil or bitumen in a further method step, is removed from the reaction space, while the additives remain in this. Thereafter, the material remaining in the reaction space is removed from this by way of a lock.
- a transport belt below the lock said transport belt immediately transporting away the additives.
- the material can be removed again through the feed opening, also by way of tilting the reaction vessel.
- the oil-laden or bitumen-laden solvent from the reaction space collects in the supply container as a sediment on a base, while the solvent in the upper part of the supply container, the vapor space, is located in the gas phase.
- At least one conduit, the withdrawal conduit departs from the base of the supply container, to capture containers. If the withdrawal conduit is opened, for example by way of opening a valve contained therein, then the oil-laden or bitumen-laden solvent flows into the capture container.
- the capture container is heated in a further method step, in order to separate the solvent from the oil or bitumen.
- the evaporated solvent is transported away via the riser conduit which leads from the capture container into the vapor space of the supply vessel, while the oil or bitumen stays back in the capture container.
- a filled capture container can be removed after closure of the valves, and be replaced by an empty one.
- the solvent is constantly kept in the vapor phase in the vapor space by way of a suitable temperature. Solvent can be supplied to the supply container through the riser conduit in a simple manner, without requiring separate pumps or other energy-consuming apparatus.
- the vapor space is connected to the reaction space which in turn is in connection with the condensation vessel.
- the solvent in one method step gets into the condensation vessel and is liquefied there.
- the liquefied solvent from here can either be filled into a reaction vessel again, in order to start a renewed washing procedure.
- the device according to the invention thus has the advantage of a significantly simpler construction compared to devices for separating stone chippings and bitumen, which are known from the state of the art.
- a device according to the invention requires no wash drum and achieves a reliable separation of oil or bitumen and additives, even without the support of ultrasound.
- the energy consumption for carrying out the method is significantly reduced compared to methods and devices known from the state of the art.
- the reaction space at the discharge conduit includes a particle filter which prevents fine particles being sucked as well.
- Mixing devices such as stirrers or ultrasound cleaning devices for the improved through-mixing of the solvent can also be contained in the reaction space, for supporting the washing procedure.
- a device may advantageously include several reaction spaces which are connected parallel to one another. A washing procedure then takes place in each reaction space, wherein the individual washing procedures particularly advantageously take place in staggered manner with regard to time, in order to ensure a uniform accumulation of the separated materials.
- Several capture containers can just as well be provided, in order to continuously capture oil or bitumen.
- reaction space including a discharge conduit which is connected to the supply container.
- discharge conduit can be connected to the vapor space.
- a direct connection between the reaction space and the supply container is given by the discharge conduit, and this connection permits substances to be transported in a defined direction between the connected spaces.
- the discharge conduit out of the reaction space into the supply container is advantageously designed according to the principle of a siphon. Thus a discharge is effected alone on account of the rising solvent level.
- the vapor space can be connected via a conduit to the condensation vessel.
- the solvent can be led directly out of the vapor space into the condensation vessel, condense more rapidly by way of this and also be brought more rapidly to the mixture for cleaning.
- condensation vessel being in connection with the reaction space via a further conduit.
- This has the advantage of a direct introduction of the condensed solvent into the reaction space, by which means the solvent can be brought onto the mixture to be cleaned or purified, in a more rapid manner.
- the device according to the invention by way of a pump, can be maintained at a slight vacuum, thus e.g. between 5 mbar and 10 mbar below the atmospheric pressure.
- a slight vacuum thus e.g. between 5 mbar and 10 mbar below the atmospheric pressure.
- the pump or the blower which is used for this can be provided with an additional condenser which is cooled by a cooling device at a few degrees above 0° C. and condenses solvent vapors out of the discharge air, so that the solvent can be constantly reused and no exit of the solvent into the environment takes place.
- the vapor space by way of a heater can be kept at a temperature of 60° C. to 65° C., in order to maintain the solvent in the vapor space in the vapor phase, since a boiling delay occurs at greater temperatures.
- the capture container is advantageously held at a temperature of between 75° C. and 95° C. by way of a heating element for heating, but this range can be varied depending on the boiling point of the used solvent.
- the condensation vessel can be held at lower temperatures, such as between 10° C. and 15° C., for condensing the solvent and this can be effected by way of a cooling element. With the application of greater temperatures, a larger condensation vessel is required, whereas lower temperatures lead to an increasing condensation of water which again must be removed through a filter.
- a further embodiment can envisage the reaction space including a conveying device, on which the mixture containing oil and bitumen and additives, and the solvent are conveyed.
- the mixture for this is led in a counter-flow to the solvent, by which means a particularly efficient washing by the solvent takes place.
- the solvent is dichloromethane.
- chloroform, diesel, naphtha, acetone, methanol, tetrahydrofurane, butyl methyl ether, carbon tetrachloride, propane gas, benzene or toluene can be applied for this purpose.
- the separation of the oil-laden or bitumen-laden solvent from the additives in the reaction space can be controlled or regulated with regard to time, in order to increase the efficiency of the method.
- a clouding of the solvent determined by a measurement apparatus which carries out a turbidity measurement, can be used as a control variable or controlled variable.
- One advantageous further development can envisage a heating of the reaction space being carried out for drying the additives of the mixture and for removing the remaining solvent.
- the method becomes more efficient on account of this, since the additives can be removed in a completely dried manner, and the removed solvent can be used for the renewed washing
- reaction space for heating being heated about 10 minutes at a temperature of 60° C.
- the reaction space can be heated for a shorter time at a temperature of over 100° C. in dependence on the applied material and the boiling point of the solvent, in order to shorten the drying times.
- the air can be sucked through the reaction space, which is particularly advantageous if the device is maintained at a vacuum.
- the device and the method are applied with the treatment of asphalt containing bitumen.
- the end product of the method consists of bitumen or oil and additives, preferably mineral aggregates, and which were separated from one another by the method.
- Embodiment examples of the method are represented in sketched manner in FIGS. 1 to 6 and are explained by way of these figures.
- FIG. 1 is a schematic view of a first embodiment example of a device according to the invention, with several reaction vessels, wherein different steps of the method are represented in the individual reaction vessels,
- FIG. 2 is an enlarged schematic view of one of the reaction vessels with a solvent feed conduit which is designed differently compared to the embodiment represented in FIG. 1 ,
- FIG. 3 is a schematic view of a second embodiment example of a device according to the invention, with a single reaction vessel, in which a conveyor belt runs,
- FIG. 4 is a representation corresponding to FIG. 3 with an embodiment example of an alternative solvent feed onto the conveyor belt,
- FIG. 5 is a representation according to FIG. 3 , with a worm instead of the conveyor belt and
- FIG. 6 is a representation of the device, according to FIG. 5 , with the worm and the solvent feed through the worm.
- FIG. 1 shows a schematic view of a device according to the invention, with several reaction vessels, wherein different steps of the method are represented in the individual reaction vessels.
- reaction vessels 1 - 8 are each constructed identically, even if for reasons of an improved overview, not all components are represented on each reaction vessel 1 - 8 .
- Each reaction vessel 1 - 8 includes a reaction space 11 which via a feed opening 12 and a valve contained therein, can be filled with the material 14 to be purified.
- the material 14 to be purified in the present case is asphalt which contains bitumen or mineral additives.
- liquid solvent 210 in the present case dichloromethane, can be filled into the reaction space 11 via a filling conduit 19 by opening the valve 18 contained therein.
- the solvent 210 dissolves the oil-containing or bitumen-containing constituents of the material 14 to be purified, from the additives, which is hereinafter indicated as the “washing procedure”. Finally, the oil-laden or bitumen-laden solvent 210 , by way of the rising liquid level of the solvent 210 , is removed via a discharge conduit 16 in a bend 20 , out of the reaction space 11 and led into a supply container 100 .
- This discharge conduit 16 in the present embodiment example is a siphon and can be closed via a valve 17 .
- This washing procedure can be repeated until the desired degree of purity of the material 14 to be cleaned has been achieved. Also a simultaneous separation of several products can be effected by way of the provision of several supply containers.
- a mixing device 300 which includes a stirrer or an ultrasound cleaning device is attached for improving the mixing.
- a measurement apparatus 310 which measures the clouding of the oil-laden or bitumen-laden solvent 210 and which controls or regulates the washing procedure in dependence on the measured clouding, is contained in the discharge conduit 16 . Thus additional solvent 210 is filled when the ascertained clouding is too high.
- the measurement apparatus 310 for this purpose contains a light source, for example an LED, and a detector, e.g. a bolometer and measures the absorption of the light emitted by the light source, in the laden solvent 210 . Alternatively, another radiation source with a detector which matches this is also possible.
- a particle filter 320 is contained in the reaction space 11 , below the bend 20 on the discharge conduit 16 , and this filter prevents fine particles being sucked as well.
- This particle filter 320 is attached on a funnel-like widening which acts as a suction opening.
- the reaction vessel is heated for about 10 minutes long to 60° C. or is heated for a shorter time to above 100° C., in order to dry the material 21 which has now been purified and to finally remove the remaining solvent residues. Air can also be sucked through the reaction space 11 for supporting the drying.
- the material 21 which is now dried and purified is removed from the reaction space 11 via a lock 13 by way of opening a valve contained therein and can be transported further via a transport belt 15 .
- the reaction vessels 1 - 8 represented in FIG. 1 are connected in parallel and permit a continuous purification of the material 14 to be purified.
- the material 14 to be purified is filled into the reaction vessel 1 , whereas the material 14 has already been filled in the reaction vessel 2 and solvent 210 is now added.
- the oil or bitumen is dissolved in the solvent 210 and flows via the discharge conduit 16 into the supply container 100 , and the same procedure is represented in the reaction vessel 4 , but here the clouding of the solvent 210 is already significantly reduced, since a large part of the oil or bitumen has already been washed out.
- reaction vessel 5 a more extensive washing out of the solvent 210 is shown in the reaction vessel 5 , and this is represented by way of a constantly reducing clouding of the laden solvent 210 .
- the solvent is removed from the reaction space 11 in the reaction vessel 6 and only the purified material 21 remains therein.
- This vessel is therefore heated for drying the purified material 21 and for removing remaining solvent residues.
- a heater is applied on the outer walls of the reaction vessel for heating, for this.
- the lock 13 is opened by way of opening the valve and the purified material 21 falls onto a transport belt 15 running below the exit of the lock 13 .
- new material 14 to be purified is filled into the reaction vessel 8 .
- the washing procedure in the reaction vessels 1 - 8 is carried out at room temperature.
- the solvent laden with oil or bitumen in the supply vessel 100 forms a sediment 110 which collects on the base of the supply vessel 100 . From there, this solvent sediment 110 via the opening of a valve 102 of a withdrawal conduit 101 gets into a capture container 103 , for example a barrel.
- the capture container 103 is heated to a temperature of 75° C. to 95° C., so that the solvent 210 evaporates and the bitumen or the oil remains in the capture container 103 .
- the vaporization can be accelerated by way of sucking or blowing air through the capture container.
- the selected temperature range is designed for the use of dichloromethane as a solvent 210 and can slightly change with the application of different materials.
- the vaporized solvent 210 escapes via a riser conduit 104 on opening the valve 105 contained in the riser conduit 104 , into a vapor space 120 .
- This vapor space 120 in the supply container 100 is located above the sediment 110 and can be separated from this by way of separation elements.
- a temperature of 60° C. to 65° C. and which is produced by a heater prevails in the vapor space 120 .
- This temperature region maintains the solvent 210 in the gas phase while a boiling delay occurring at even higher temperatures is prevented.
- the capture container 103 can be removed after heating and cooling the bitumen or oil and be replaced with a new one, wherein a continuous separation of bitumen or oil and a continuous exchange of the capture container 103 are made possible by way of the provision of several capture containers 103 .
- the supply vessel 100 more specifically the vapor space 120 is connected to a condensation vessel 200 via a conduit 130 .
- the gaseous solvent 210 via this conduit 130 gets into a condenser or a condensation vessel 200 which is maintained at a temperature of 10° C. to 15° C. by way of a cooling device. An increasing condensation of water occurs below these temperatures, and this water must be removed through a filter which is not represented.
- the solvent 210 is liquefied in the condensation vessel 200 by way of condensation and can be fed again to the respective reaction vessels 1 - 8 via a filling conduit 19 .
- the device is maintained at a slight vacuum, approx. 5 mbar to 10 mbar below atmospheric pressure, by way of a blower 190 or a pump. Due to this, it is impossible for solvent to exit into the surroundings on account of possibly present or occurring leakages.
- the through-blowing of the capture container 103 and of the reaction spaces 11 is made possible by way of the blower 190 and the vacuum which is created by way of this.
- This blower 190 is connected to an additional condensation vessel or condenser 180 which condenses solvent vapors out of the discharge air, so that the solvent is available for further washing procedure without an losses. For this, the condenser 180 is cooled down to a few degrees above 0° C.
- reaction vessel 1 by way of example the reaction vessel 1 , is represented in an enlarged manner in FIG. 2 .
- identical elements are provided with identical reference numerals.
- the reaction vessel 1 now has no introduction of the solvent 210 effected from above into the reaction space 11 , but the solvent 210 coming from the condensation vessel 200 lying above the reaction vessel 1 is led through the filling conduit 19 firstly past the reaction vessel 1 .
- the filling conduit 19 at its end includes a bend and runs out in a lower part of the reaction vessel 1 .
- the filling conduit 19 includes a pump 23 for supporting a feed of solvent.
- the solvent 210 however can also get into the reaction space 1 also without the application of the pump 23 due to the position of the reaction space 1 below the condensation vessel 200 .
- An upwardly directed distributor head 22 which is formed in a hemispherical manner and includes openings on its surface, is attached at the end of the filling conduit 19 in the reaction vessel 1 , so that the solvent 210 can exit as uniformly as possible through the distributor head 22 and thus encompasses the material 14 to be purified.
- FIG. 3 in a schematic representation shows a further embodiment example of a device for carrying out the method according to the invention.
- the material 14 to be purified in the represented embodiment example oil sand which contains bitumen and mineral additives, is introduced into a reaction space 11 via a feed opening 12 .
- the material 14 to be cleaned is introduced into a first receiver container 260 and from there is led via a valve into a second receiver container 270 which is opened or closed by way of the feed opening 12 .
- the reaction space 11 includes a conveyor belt 220 as a conveying device, onto which, when the feed opening 12 is opened, the material 14 to be purified falls and is transported by the conveyor belt 220 in the direction of the condensation vessel 200 .
- the conveyor belt 220 includes a multitude of capture grids 240 at uniform distances, on which the material 14 to be purified clings and is caught, for simplified transport.
- the solvent 210 in the present case acetone, as a condensate, is deposited through a discharge conduit out of the condensation vessel 200 onto the conveyor belt 200 , at an end of the conveyor belt 220 which is opposite to the feed opening.
- This discharge conduit for example can include a pipe conduit or a funnel system.
- the conveyor belt 220 starting from the end, at which the material 14 to be purified is deposited, runs in a rising manner up to the end, at which the solvent 210 is deposited, so that the solvent 210 flows counter to the transport direction of the conveyor belt 220 .
- the solvent 210 rinses through the material 14 to be purified in the counter-flow direction and dissolves the oil-containing or bitumen-containing constituents of the material 14 to be purified, from the additives, within the framework of the washing procedure.
- the capture grids 240 can be simply passed by the liquid solvent 210 , while the solid constituents of the material 14 to be purified remain in the capture grids 240 and are transported.
- the reaction space 11 hereby is maintained at a temperature in the range of 15° C. to 25° C.
- the reaction space 11 is maintained at a temperature in the range of 17° C. to 23° C. In some embodiments, the reaction space 11 is maintained at a temperature of 20° C., thus room temperature. This can be effected by way of heating elements or cooling elements which are not shown in FIG. 3 for reasons of a better overview.
- the sold constituents of the material 14 to be purified are thus purified or cleaned to an increasing extent and fall at the end of the conveyor belt 220 located below a condensation vessel 200 , from which the solvent 210 is brought onto the conveying belt 220 , into a capture device 280 provided with a heater 230 .
- the capture device 280 is heated, for example about 10 minutes to a temperature of 60° C., in order to remove solvent residues remaining on the solid constituents.
- the purified material 21 is removed out of the device through a lock 13 and can be used again, or should the purification not have been effected to a satisfactory extent, is deposited onto the conveyor belt 220 again and the washing procedure is carried out once again.
- the solvent 210 which is conveyed into the gaseous condition by way of the heating of the heater 230 is fed via a further riser conduit 290 to the condensation vessel 200 where it condenses and is deposited afresh onto the conveyor belt 220 .
- the further riser conduit 290 for this can be opened and closed via a valve 390 .
- Conduits are pipe conduits in the embodiment examples represented in the figures.
- the supply container 100 is located directly below the feed opening 12 and is in connection with the reaction space 11 .
- the reaction space 11 includes a particle filter 320 below the end of the conveyor belt 220 which is situated below the feed opening 12 , in order to ensure that no solid constituents of the material 14 to be purified get into the supply container 100 .
- the solvent 210 forms a solvent sediment 110 at the base of the supply container 100 .
- a vapor space 120 is located above the sediment 110 .
- the solvent 210 in the vapor space 120 is kept in the gaseous state by way of a heater 250 running around the supply container 100 , at a temperature of 60° C. to 65° C.
- the base of the supply container 100 is closed by a valve 102 of a withdrawal conduit 101 .
- the withdrawal conduit 101 connects the supply container 100 to a capture container 103 .
- the valve 102 When the valve 102 is open, the solvent 210 can get through the withdrawal conduit 101 into the capture container 103 .
- This capture container 103 is connected via a further valve to a barrel, but in an embodiment which is not represented, the capture container 103 may directly be a barrel and thus be separated from the device according to the invention and transported away, in a particularly simple manner.
- the capture container 103 is heated by the heater 250 to 60° C. so that solvent 210 thus acetone evaporates and the bitumen or the oil remains in the capture container 103 . Air can be blown through the capture container 103 by way of a blower which is not shown, for accelerating the vaporization.
- Vaporized solvent 210 escapes via a riser conduit 104 on opening the valve 105 contained in the riser conduit 104 , into the vapor space 120 . Since the reaction space 11 and the vapor space 120 are connected to one another, the vaporous solvent 210 can also get into the reaction space 11 , condense there and settle again on the conveyor belt 220 . The solvent vapor condenses at the latest on reaching the condensation vessel 200 , and the solvent 210 settles on the conveyor belt 220 in the liquid state.
- the connection between the vapor space 120 and condensation vessel 200 in the represented embodiment example is effected via the reaction space 11 through the space above and below the conveyor belt 220 , but can also be designed as a separate conduit.
- the condensation vessel 200 is kept at a temperature of 10° C. to 15° C. by way of a cooling device.
- a blower 190 attached on the condensation vessel 200 maintains the device at a slight vacuum, thus roughly 5 mbar to 10 mbar below the atmospheric pressure. By way of this, an exit of solvent by way of leaks is avoided.
- the blower 190 is connected to an additional condenser 180 and this condenser condenses the solvent vapors out of the discharge air, for which it is cooled to a few degrees above 0° C., and 3° C. in the represented embodiment example.
- a condensation vessel 200 can be all devices together.
- FIG. 4 in a schematic view corresponding to FIG. 3 represents a further embodiment example of the device for separating mixtures with a conveyor belt 220 .
- the solvent 210 coming from the condensation vessel 200 in the embodiment example shown in FIG. 4 is collected in a capture space 330 at the lower end of the condensation vessel 200 and in contrast to the embodiment example shown in FIG. 3 can no longer get into the reaction space 11 in an uninhibited manner.
- the capture space 330 includes a run-over protection 340 so that given a filled level of the solvent 210 in the capture space 330 , said level rising above the run-over protection 340 , the solvent 210 can run off into the reaction space 11 onto the conveyor belt 220 without intervention of a user.
- the solvent 210 collected in the capture space 330 is pumped via a pump 23 into the reaction space 11 .
- an end-pipe 340 with openings in the reaction space 11 is attached between a lower end and an upper end of the conveyor belt 220 .
- the openings are located on the upper side of the end-pipe 340 , i.e. on a side which faces the material 14 to be purified.
- the solvent enters into the reaction space 11 through the openings of the end-pipe 340 .
- the solvent 230 in the end-pipe 340 is under pressure due to the pump 23 , so that the solvent 210 can be injected or sprayed out of the openings onto the conveyor belt 220 .
- FIG. 5 A view of a device for separating mixtures with a worm 350 running in the reaction space instead of the conveyor belt 220 is shown in FIG. 5 , in a manner corresponding to FIG. 3 .
- the worm 350 is driven by a drive unit 360 and rotates about a longitudinal axis.
- the worm 350 functions similarly to an Archimedean screw, i.e. the material 14 to be purified is deposited onto the worm 350 via the feed opening 12 and is transported further in the direction of the capture device 280 by a worm thread 400 .
- the solvent 210 flows through the material 14 to be purified, in a counter-flow and can be deposited directly from the condensation vessel 200 onto the worm 350 .
- the condensation vessel 200 moreover yet includes a conduit 370 which departing from the condensation vessel 200 ends with the end-pipe 340 at the worm 350 .
- the end-pipe 340 includes openings, through which the solvent 210 is sprayed onto the worm 350 .
- the pump 23 is attached on the conduit 370 and sucks the solvent 210 out of the condensation vessel 200 and pumps it through the conduit 370 up to the end-pipe 340 .
- FIG. 6 in a view corresponding to FIG. 5 represents a further embodiment example of the device for separating mixtures.
- the conveying device is the worm 350 which is set into rotation about its longitudinal axis by the drive unit 360 and thus transports the material to be purified on the worm gear 400 .
- the conduit 370 from the condensation vessel 200 into the reaction space 11 is however led through the drive unit 360 into an interior of the worm shaft 380 .
- the worm shaft 380 includes openings extending in the direction of the rotation axis.
- the solvent 210 exits through these openings into the reaction space 11 , wherein it is accelerated by the centrifugal force acting by way of the rotation of the worm 350 , through the openings of the worm shaft 380 and flows in a counter-flow through the material 14 to be purified.
- One aspect of the invention includes a device for separating mixtures 14 which contain oil or bitumen and additives, wherein the device includes at least one reaction vessel 1 having a reaction space 11 , a feed opening 12 and a discharge conduit 16 , further including a supply container 100 having a vapor space 120 , further including at least one capture container 103 having a withdrawal conduit 101 and a riser conduit 104 , and further including a condensation vessel 200 , wherein the discharge conduit 16 is in connection with the supply container 100 , the supply container 100 via the withdrawal conduit 101 with the capture container 103 , the capture container 103 via the riser conduit 104 with the vapor space 120 , the vapor space 120 via a conduit 130 with the condensation vessel 200 , and the condensation vessel 200 via a further conduit 19 with the reaction space 11 .
- a further aspect relates to a device according to the preceding aspect, wherein the reaction space 11 contains a particle filter 320 .
- a further aspect relates to a device according to one of the preceding aspects, wherein stirrers or ultrasound cleaning devices 300 for improved mixing of a solvent 210 are contained in the reaction space 11 .
- a further aspect relates to a device according to one of the preceding aspects, wherein several reaction vessels 1 , 2 , 3 , 4 , 5 , 6 , 7 , 8 , are arranged in parallel.
- a further aspect relates to a device according to one of the preceding aspects, wherein the discharge conduit 16 includes a siphon.
- a further aspect relates to a device according to one of the preceding aspects, wherein the device has a slight vacuum of 5 to 10 mbar below atmospheric pressure.
- a further aspect relates to a device according to one of the preceding aspects, wherein the vapor space 120 has a temperature of 60° C. to maximal 65° C.
- a further aspect relates to a device according to one of the preceding aspects, wherein the capture container 103 has a temperature of 75° C. to 95° C.
- a further aspect relates to a device according to one of the preceding aspects, wherein the condenser 200 has a temperature of 10° C. to 15° C.
- One aspect of the invention relates to a method for separating mixtures 14 which contain oil or bitumen and additives, having the following steps:
- a further aspect of the invention relates to a method according to the preceding aspect, wherein the solvent 210 includes dichloromethane, chloroform, diesel, naphtha, acetone, methanol, tetrahydrofurane, butyl methyl ether, carbon tetrachloride, propane gas, benzene or toluene.
- the solvent 210 includes dichloromethane, chloroform, diesel, naphtha, acetone, methanol, tetrahydrofurane, butyl methyl ether, carbon tetrachloride, propane gas, benzene or toluene.
- a further aspect relates to a method according to one of the preceding aspects, wherein the separation of the oil-laden or bitumen-laden solvent 210 is controlled or regulated in a temporal manner, preferably via a turbidity measurement of the solvent 210 .
- a further aspect relates to a method according to one of the preceding claims, wherein the reaction space 11 is heated for 10 minutes to 60° C. for heating.
- a further aspect relates to a method according to one of the preceding aspects, wherein air is sucked or blown through the capture container 103 , for the accelerated vaporization of the solvent 210 .
- a further aspect relates to a method according to one of the preceding aspects, wherein bitumen-containing asphalt is used as a mixture 14 .
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Abstract
A device and a method for separating mixtures that contain oil or bitumen and additives. The device and the method are applicable in particular to separating stone chippings and bitumen in excavated asphalt road surfaces. In the case of oil sands and oil shale, a mineral phase can be separated from an oil phase and separation of bitumen and carrier felt can be induced in recycling of bitumen felt, oil binder and oil. The individual components of the mixture are separated from one another using a solvent, wherein the solvent takes up the oil or bitumen. The oil and bitumen are subsequently separated from the solvent so that the solvent can be reused.
Description
- The present application is a national phase application of PCT application PCT/EP2011/003866, filed pursuant to 35 U.S.C.§371, which claims priority to European Application EP 10 07 5333.4, filed Jul. 30, 2010. Both applications are incorporated herein by reference in their entirety.
- The present invention relates to a device and to a method for separating mixtures which contain oil or bitumen and additives. The device and the method are particularly applicable to separating stone chippings and bitumen in evacuated asphalt road surfaces. Moreover, with it, the mineral phase can be separated from the oil phase also with oil sands and oil shale, and a separation of bitumen and carrier felt can be induced with the recycling of bitumen felt, oil binder and oil.
- Mixtures of oil or bitumen and additives are applied widely in many fields of technology. In road construction for example, asphalt, a mixture of bitumen as a binder and ground mineral additives of certain rock types and of a certain size spectrum, is used as a surface. For recycling old road surfacing, this is milled away from the subsurface, reduced in size, deposited and later or however directly added again to new asphalt surfacing as an aggregate, wherein the mineral phase is still encased by bitumen. The size spectrum of the mineral part can therefore not be varied as extensively as with new aggregate which has not yet been used. For this reason, it is desirable to separate the bitumen share from the mineral additive and to feed both to the recycling in a separate and metered manner. The same also applies to oil sands or oil binders with which one would like to reliably separate oil and additives for a successful recycling.
- Methods and devices for achieving this aim are already known from the state of the art. The document DE 10 2006 038 614 A1 describes a method, with which the quality loss with the recycling of broken, excavated asphalt is reduced by way of the addition of chemical additives such as softeners and hardeners at temperatures of about 140° C. The disadvantage of this method is the fact that a comparatively high temperature and numerous chemicals need to be used.
- A method is disclosed in DE 600 10 533 T2,with which the aggregate is separated from the bitumen share, by way of a thermal decomposition of the bitumen encasing. Bitumen is thereby used as a fuel and is activated by introducing hot gases into a drum which contains the excavated material. The method however has the disadvantage that it is coupled to the manufacture of new asphalt and may only be carried out at a high energy expense.
- It is therefore the object of the present invention, to develop a method and a device, with which a reliable separation of a mixture of oil-containing or bitumen-containing substances and additives is ensured, without a coupling to the manufacture of new asphalt being present, and wherein the additives and the oil-containing or bitumen-containing material is stored and when required, newly classified, can be fed to a new asphalt production. Moreover, the energy application should be as low as possible.
- A device according to the invention, for separating mixtures, which contain oil or bitumen and additives, includes a reaction vessel, into which the mixture and a solvent can be brought through a feed opening and/or a filling conduit, into a reaction space, further including a supply container with a vapor space, at least one capture container with a withdrawal conduit and with a riser conduit, and a condensation vessel. In some embodiments, the mixture is filled in through the feed opening while the solvent is introduced through the filling conduit, but also only one opening can be provided for this purpose for space-saving reasons. The opening in any case is closed via a valve.
- The solvent dissolves the oil-containing or bitumen-containing material from the additives, in the reaction space in an initial method step. Thus the additives to all intents and purposes are free from their encasing and purified and can be classified as newly manufactured material. This procedure can be carried out several times until the desired purity of the additives is achieved. This “washing procedure” may thereby take place at room temperature without any additional supply of heat.
- The solvent laden with oil or bitumen, in a further method step, is removed from the reaction space, while the additives remain in this. Thereafter, the material remaining in the reaction space is removed from this by way of a lock. Thereby, it can be advantageous to provide a transport belt below the lock, said transport belt immediately transporting away the additives. Alternatively, the material can be removed again through the feed opening, also by way of tilting the reaction vessel.
- The oil-laden or bitumen-laden solvent from the reaction space collects in the supply container as a sediment on a base, while the solvent in the upper part of the supply container, the vapor space, is located in the gas phase. At least one conduit, the withdrawal conduit, departs from the base of the supply container, to capture containers. If the withdrawal conduit is opened, for example by way of opening a valve contained therein, then the oil-laden or bitumen-laden solvent flows into the capture container. The capture container is heated in a further method step, in order to separate the solvent from the oil or bitumen. The evaporated solvent is transported away via the riser conduit which leads from the capture container into the vapor space of the supply vessel, while the oil or bitumen stays back in the capture container. In some embodiments, a filled capture container can be removed after closure of the valves, and be replaced by an empty one. The solvent is constantly kept in the vapor phase in the vapor space by way of a suitable temperature. Solvent can be supplied to the supply container through the riser conduit in a simple manner, without requiring separate pumps or other energy-consuming apparatus.
- The vapor space is connected to the reaction space which in turn is in connection with the condensation vessel. The solvent in one method step gets into the condensation vessel and is liquefied there. The liquefied solvent from here can either be filled into a reaction vessel again, in order to start a renewed washing procedure.
- The device according to the invention thus has the advantage of a significantly simpler construction compared to devices for separating stone chippings and bitumen, which are known from the state of the art. In particular, a device according to the invention requires no wash drum and achieves a reliable separation of oil or bitumen and additives, even without the support of ultrasound. Thus the energy consumption for carrying out the method is significantly reduced compared to methods and devices known from the state of the art.
- In one advantageous development, the reaction space at the discharge conduit includes a particle filter which prevents fine particles being sucked as well.
- Mixing devices such as stirrers or ultrasound cleaning devices for the improved through-mixing of the solvent can also be contained in the reaction space, for supporting the washing procedure.
- In order to ensure a continuous washing procedure, a device according to the invention may advantageously include several reaction spaces which are connected parallel to one another. A washing procedure then takes place in each reaction space, wherein the individual washing procedures particularly advantageously take place in staggered manner with regard to time, in order to ensure a uniform accumulation of the separated materials. Several capture containers can just as well be provided, in order to continuously capture oil or bitumen.
- One advantageous embodiment can envisage the reaction space including a discharge conduit which is connected to the supply container. In a particularly advantageous manner, the discharge conduit can be connected to the vapor space. A direct connection between the reaction space and the supply container is given by the discharge conduit, and this connection permits substances to be transported in a defined direction between the connected spaces.
- The discharge conduit out of the reaction space into the supply container is advantageously designed according to the principle of a siphon. Thus a discharge is effected alone on account of the rising solvent level.
- In a further embodiment, the vapor space can be connected via a conduit to the condensation vessel. Thus the solvent can be led directly out of the vapor space into the condensation vessel, condense more rapidly by way of this and also be brought more rapidly to the mixture for cleaning.
- One embodiment can envisage the condensation vessel being in connection with the reaction space via a further conduit. This has the advantage of a direct introduction of the condensed solvent into the reaction space, by which means the solvent can be brought onto the mixture to be cleaned or purified, in a more rapid manner.
- The device according to the invention, by way of a pump, can be maintained at a slight vacuum, thus e.g. between 5 mbar and 10 mbar below the atmospheric pressure. Thus one prevents solvent from exiting into the surroundings in the case of leaking locations. The pump or the blower which is used for this can be provided with an additional condenser which is cooled by a cooling device at a few degrees above 0° C. and condenses solvent vapors out of the discharge air, so that the solvent can be constantly reused and no exit of the solvent into the environment takes place.
- The vapor space by way of a heater can be kept at a temperature of 60° C. to 65° C., in order to maintain the solvent in the vapor space in the vapor phase, since a boiling delay occurs at greater temperatures.
- The capture container is advantageously held at a temperature of between 75° C. and 95° C. by way of a heating element for heating, but this range can be varied depending on the boiling point of the used solvent.
- The condensation vessel can be held at lower temperatures, such as between 10° C. and 15° C., for condensing the solvent and this can be effected by way of a cooling element. With the application of greater temperatures, a larger condensation vessel is required, whereas lower temperatures lead to an increasing condensation of water which again must be removed through a filter.
- A further embodiment can envisage the reaction space including a conveying device, on which the mixture containing oil and bitumen and additives, and the solvent are conveyed. The mixture for this is led in a counter-flow to the solvent, by which means a particularly efficient washing by the solvent takes place.
- In some embodiments, the solvent is dichloromethane. However chloroform, diesel, naphtha, acetone, methanol, tetrahydrofurane, butyl methyl ether, carbon tetrachloride, propane gas, benzene or toluene can be applied for this purpose.
- The separation of the oil-laden or bitumen-laden solvent from the additives in the reaction space can be controlled or regulated with regard to time, in order to increase the efficiency of the method. Thereby, a clouding of the solvent, determined by a measurement apparatus which carries out a turbidity measurement, can be used as a control variable or controlled variable.
- One advantageous further development can envisage a heating of the reaction space being carried out for drying the additives of the mixture and for removing the remaining solvent. The method becomes more efficient on account of this, since the additives can be removed in a completely dried manner, and the removed solvent can be used for the renewed washing
- A further advantageous development envisages the reaction space for heating being heated about 10 minutes at a temperature of 60° C. Alternatively, the reaction space can be heated for a shorter time at a temperature of over 100° C. in dependence on the applied material and the boiling point of the solvent, in order to shorten the drying times. For supporting this, the air can be sucked through the reaction space, which is particularly advantageous if the device is maintained at a vacuum.
- By the same token, air can be sucked or blown through the capture container for supporting the drying. This, as already mentioned, is particularly advantageous if the device is kept under a vacuum.
- In a particularly advantageous manner, the device and the method are applied with the treatment of asphalt containing bitumen.
- The end product of the method consists of bitumen or oil and additives, preferably mineral aggregates, and which were separated from one another by the method.
- Embodiment examples of the method are represented in sketched manner in
FIGS. 1 to 6 and are explained by way of these figures. - There are shown in:
-
FIG. 1 is a schematic view of a first embodiment example of a device according to the invention, with several reaction vessels, wherein different steps of the method are represented in the individual reaction vessels, -
FIG. 2 is an enlarged schematic view of one of the reaction vessels with a solvent feed conduit which is designed differently compared to the embodiment represented inFIG. 1 , -
FIG. 3 is a schematic view of a second embodiment example of a device according to the invention, with a single reaction vessel, in which a conveyor belt runs, -
FIG. 4 is a representation corresponding toFIG. 3 with an embodiment example of an alternative solvent feed onto the conveyor belt, -
FIG. 5 is a representation according toFIG. 3 , with a worm instead of the conveyor belt and -
FIG. 6 is a representation of the device, according toFIG. 5 , with the worm and the solvent feed through the worm. -
FIG. 1 shows a schematic view of a device according to the invention, with several reaction vessels, wherein different steps of the method are represented in the individual reaction vessels. - The reaction vessels 1-8 are each constructed identically, even if for reasons of an improved overview, not all components are represented on each reaction vessel 1-8. Each reaction vessel 1-8 includes a
reaction space 11 which via afeed opening 12 and a valve contained therein, can be filled with the material 14 to be purified. The material 14 to be purified in the present case is asphalt which contains bitumen or mineral additives. Moreover, liquid solvent 210, in the present case dichloromethane, can be filled into thereaction space 11 via a fillingconduit 19 by opening the valve 18 contained therein. - The solvent 210 dissolves the oil-containing or bitumen-containing constituents of the material 14 to be purified, from the additives, which is hereinafter indicated as the “washing procedure”. Finally, the oil-laden or bitumen-laden solvent 210, by way of the rising liquid level of the solvent 210, is removed via a
discharge conduit 16 in abend 20, out of thereaction space 11 and led into asupply container 100. Thisdischarge conduit 16 in the present embodiment example is a siphon and can be closed via a valve 17. This washing procedure can be repeated until the desired degree of purity of the material 14 to be cleaned has been achieved. Also a simultaneous separation of several products can be effected by way of the provision of several supply containers. - A mixing device 300 which includes a stirrer or an ultrasound cleaning device is attached for improving the mixing. A
measurement apparatus 310 which measures the clouding of the oil-laden or bitumen-laden solvent 210 and which controls or regulates the washing procedure in dependence on the measured clouding, is contained in thedischarge conduit 16. Thus additional solvent 210 is filled when the ascertained clouding is too high. Themeasurement apparatus 310 for this purpose contains a light source, for example an LED, and a detector, e.g. a bolometer and measures the absorption of the light emitted by the light source, in the laden solvent 210. Alternatively, another radiation source with a detector which matches this is also possible. Moreover, aparticle filter 320 is contained in thereaction space 11, below thebend 20 on thedischarge conduit 16, and this filter prevents fine particles being sucked as well. Thisparticle filter 320 is attached on a funnel-like widening which acts as a suction opening. - After the solvent 210 has flowed away out of the
reaction space 11, the reaction vessel is heated for about 10 minutes long to 60° C. or is heated for a shorter time to above 100° C., in order to dry the material 21 which has now been purified and to finally remove the remaining solvent residues. Air can also be sucked through thereaction space 11 for supporting the drying. - The material 21 which is now dried and purified is removed from the
reaction space 11 via alock 13 by way of opening a valve contained therein and can be transported further via a transport belt 15. - The reaction vessels 1-8 represented in
FIG. 1 are connected in parallel and permit a continuous purification of the material 14 to be purified. The material 14 to be purified is filled into thereaction vessel 1, whereas thematerial 14 has already been filled in thereaction vessel 2 and solvent 210 is now added. In thereaction vessel 3, the oil or bitumen is dissolved in the solvent 210 and flows via thedischarge conduit 16 into thesupply container 100, and the same procedure is represented in thereaction vessel 4, but here the clouding of the solvent 210 is already significantly reduced, since a large part of the oil or bitumen has already been washed out. In the same manner, a more extensive washing out of the solvent 210 is shown in thereaction vessel 5, and this is represented by way of a constantly reducing clouding of the laden solvent 210. The solvent is removed from thereaction space 11 in thereaction vessel 6 and only the purifiedmaterial 21 remains therein. This vessel is therefore heated for drying the purifiedmaterial 21 and for removing remaining solvent residues. A heater is applied on the outer walls of the reaction vessel for heating, for this. In the reaction vessel 7, thelock 13 is opened by way of opening the valve and the purifiedmaterial 21 falls onto a transport belt 15 running below the exit of thelock 13. Again then,new material 14 to be purified is filled into the reaction vessel 8. The washing procedure in the reaction vessels 1-8 is carried out at room temperature. - The solvent laden with oil or bitumen in the
supply vessel 100 forms a sediment 110 which collects on the base of thesupply vessel 100. From there, this solvent sediment 110 via the opening of avalve 102 of a withdrawal conduit 101 gets into acapture container 103, for example a barrel. Thecapture container 103 is heated to a temperature of 75° C. to 95° C., so that the solvent 210 evaporates and the bitumen or the oil remains in thecapture container 103. The vaporization can be accelerated by way of sucking or blowing air through the capture container. The selected temperature range is designed for the use of dichloromethane as a solvent 210 and can slightly change with the application of different materials. - The vaporized solvent 210 escapes via a
riser conduit 104 on opening thevalve 105 contained in theriser conduit 104, into avapor space 120. Thisvapor space 120 in thesupply container 100 is located above the sediment 110 and can be separated from this by way of separation elements. A temperature of 60° C. to 65° C. and which is produced by a heater prevails in thevapor space 120. This temperature region maintains the solvent 210 in the gas phase while a boiling delay occurring at even higher temperatures is prevented. - The
capture container 103 can be removed after heating and cooling the bitumen or oil and be replaced with a new one, wherein a continuous separation of bitumen or oil and a continuous exchange of thecapture container 103 are made possible by way of the provision ofseveral capture containers 103. - The
supply vessel 100, more specifically thevapor space 120 is connected to acondensation vessel 200 via aconduit 130. The gaseous solvent 210 via thisconduit 130 gets into a condenser or acondensation vessel 200 which is maintained at a temperature of 10° C. to 15° C. by way of a cooling device. An increasing condensation of water occurs below these temperatures, and this water must be removed through a filter which is not represented. The solvent 210 is liquefied in thecondensation vessel 200 by way of condensation and can be fed again to the respective reaction vessels 1-8 via a fillingconduit 19. - The device is maintained at a slight vacuum, approx. 5 mbar to 10 mbar below atmospheric pressure, by way of a
blower 190 or a pump. Due to this, it is impossible for solvent to exit into the surroundings on account of possibly present or occurring leakages. The through-blowing of thecapture container 103 and of thereaction spaces 11 is made possible by way of theblower 190 and the vacuum which is created by way of this. Thisblower 190 is connected to an additional condensation vessel orcondenser 180 which condenses solvent vapors out of the discharge air, so that the solvent is available for further washing procedure without an losses. For this, thecondenser 180 is cooled down to a few degrees above 0° C. - One of the reaction vessels 1-8, by way of example the
reaction vessel 1, is represented in an enlarged manner inFIG. 2 . In this figure as well as in the subsequent figures, identical elements are provided with identical reference numerals. In contrast to the embodiment example represented inFIG. 1 , thereaction vessel 1 now has no introduction of the solvent 210 effected from above into thereaction space 11, but the solvent 210 coming from thecondensation vessel 200 lying above thereaction vessel 1 is led through the fillingconduit 19 firstly past thereaction vessel 1. The fillingconduit 19 at its end includes a bend and runs out in a lower part of thereaction vessel 1. The fillingconduit 19 includes apump 23 for supporting a feed of solvent. The solvent 210 however can also get into thereaction space 1 also without the application of thepump 23 due to the position of thereaction space 1 below thecondensation vessel 200. An upwardly directed distributor head 22 which is formed in a hemispherical manner and includes openings on its surface, is attached at the end of the fillingconduit 19 in thereaction vessel 1, so that the solvent 210 can exit as uniformly as possible through the distributor head 22 and thus encompasses the material 14 to be purified. -
FIG. 3 in a schematic representation shows a further embodiment example of a device for carrying out the method according to the invention. The material 14 to be purified, in the represented embodiment example oil sand which contains bitumen and mineral additives, is introduced into areaction space 11 via afeed opening 12. In the represented embodiment example, thematerial 14 to be cleaned is introduced into afirst receiver container 260 and from there is led via a valve into asecond receiver container 270 which is opened or closed by way of thefeed opening 12. Alternatively, one may also provide only one container which is closed by way of thefeed opening 12. - The
reaction space 11 includes aconveyor belt 220 as a conveying device, onto which, when thefeed opening 12 is opened, thematerial 14 to be purified falls and is transported by theconveyor belt 220 in the direction of thecondensation vessel 200. Theconveyor belt 220 includes a multitude ofcapture grids 240 at uniform distances, on which thematerial 14 to be purified clings and is caught, for simplified transport. The solvent 210, in the present case acetone, as a condensate, is deposited through a discharge conduit out of thecondensation vessel 200 onto theconveyor belt 200, at an end of theconveyor belt 220 which is opposite to the feed opening. This discharge conduit for example can include a pipe conduit or a funnel system. - The
conveyor belt 220 starting from the end, at which thematerial 14 to be purified is deposited, runs in a rising manner up to the end, at which the solvent 210 is deposited, so that the solvent 210 flows counter to the transport direction of theconveyor belt 220. Hereby, the solvent 210 rinses through the material 14 to be purified in the counter-flow direction and dissolves the oil-containing or bitumen-containing constituents of the material 14 to be purified, from the additives, within the framework of the washing procedure. Thecapture grids 240 can be simply passed by the liquid solvent 210, while the solid constituents of the material 14 to be purified remain in thecapture grids 240 and are transported. Thereaction space 11 hereby is maintained at a temperature in the range of 15° C. to 25° C. In some embodiments, thereaction space 11 is maintained at a temperature in the range of 17° C. to 23° C. In some embodiments, thereaction space 11 is maintained at a temperature of 20° C., thus room temperature. This can be effected by way of heating elements or cooling elements which are not shown inFIG. 3 for reasons of a better overview. - With an increasing conveying path on the
conveyor belt 220, the sold constituents of the material 14 to be purified are thus purified or cleaned to an increasing extent and fall at the end of theconveyor belt 220 located below acondensation vessel 200, from which the solvent 210 is brought onto the conveyingbelt 220, into acapture device 280 provided with aheater 230. Thecapture device 280 is heated, for example about 10 minutes to a temperature of 60° C., in order to remove solvent residues remaining on the solid constituents. Subsequently, the purifiedmaterial 21 is removed out of the device through alock 13 and can be used again, or should the purification not have been effected to a satisfactory extent, is deposited onto theconveyor belt 220 again and the washing procedure is carried out once again. The solvent 210 which is conveyed into the gaseous condition by way of the heating of theheater 230 is fed via afurther riser conduit 290 to thecondensation vessel 200 where it condenses and is deposited afresh onto theconveyor belt 220. Thefurther riser conduit 290 for this can be opened and closed via a valve 390. Conduits are pipe conduits in the embodiment examples represented in the figures. - The solvent 210 which runs down on the
conveyor belt 220, at the end of theconveyor belt 220, at which end the feed opening is located, is emptied into asupply container 100. Thesupply container 100 is located directly below thefeed opening 12 and is in connection with thereaction space 11. Thereaction space 11 includes aparticle filter 320 below the end of theconveyor belt 220 which is situated below thefeed opening 12, in order to ensure that no solid constituents of the material 14 to be purified get into thesupply container 100. The solvent 210 forms a solvent sediment 110 at the base of thesupply container 100. Avapor space 120 is located above the sediment 110. The solvent 210 in thevapor space 120 is kept in the gaseous state by way of aheater 250 running around thesupply container 100, at a temperature of 60° C. to 65° C. - The base of the
supply container 100 is closed by avalve 102 of a withdrawal conduit 101. The withdrawal conduit 101 connects thesupply container 100 to acapture container 103. When thevalve 102 is open, the solvent 210 can get through the withdrawal conduit 101 into thecapture container 103. Thiscapture container 103 is connected via a further valve to a barrel, but in an embodiment which is not represented, thecapture container 103 may directly be a barrel and thus be separated from the device according to the invention and transported away, in a particularly simple manner. Thecapture container 103 is heated by theheater 250 to 60° C. so that solvent 210 thus acetone evaporates and the bitumen or the oil remains in thecapture container 103. Air can be blown through thecapture container 103 by way of a blower which is not shown, for accelerating the vaporization. - Vaporized solvent 210 escapes via a
riser conduit 104 on opening thevalve 105 contained in theriser conduit 104, into thevapor space 120. Since thereaction space 11 and thevapor space 120 are connected to one another, the vaporous solvent 210 can also get into thereaction space 11, condense there and settle again on theconveyor belt 220. The solvent vapor condenses at the latest on reaching thecondensation vessel 200, and the solvent 210 settles on theconveyor belt 220 in the liquid state. The connection between thevapor space 120 andcondensation vessel 200 in the represented embodiment example is effected via thereaction space 11 through the space above and below theconveyor belt 220, but can also be designed as a separate conduit. Thecondensation vessel 200 is kept at a temperature of 10° C. to 15° C. by way of a cooling device. - A
blower 190 attached on thecondensation vessel 200 maintains the device at a slight vacuum, thus roughly 5 mbar to 10 mbar below the atmospheric pressure. By way of this, an exit of solvent by way of leaks is avoided. Theblower 190 is connected to anadditional condenser 180 and this condenser condenses the solvent vapors out of the discharge air, for which it is cooled to a few degrees above 0° C., and 3° C. in the represented embodiment example. - Several devices of a second embodiment and which are represented in
FIG. 3 can also be operated parallel to one another, wherein for example acondensation vessel 200 can be all devices together. -
FIG. 4 in a schematic view corresponding toFIG. 3 represents a further embodiment example of the device for separating mixtures with aconveyor belt 220. However, the solvent 210 coming from thecondensation vessel 200 in the embodiment example shown inFIG. 4 is collected in acapture space 330 at the lower end of thecondensation vessel 200 and in contrast to the embodiment example shown inFIG. 3 can no longer get into thereaction space 11 in an uninhibited manner. Thecapture space 330 includes a run-over protection 340 so that given a filled level of the solvent 210 in thecapture space 330, said level rising above the run-over protection 340, the solvent 210 can run off into thereaction space 11 onto theconveyor belt 220 without intervention of a user. - The solvent 210 collected in the
capture space 330 is pumped via apump 23 into thereaction space 11. For this, an end-pipe 340 with openings in thereaction space 11 is attached between a lower end and an upper end of theconveyor belt 220. The openings are located on the upper side of the end-pipe 340, i.e. on a side which faces the material 14 to be purified. The solvent enters into thereaction space 11 through the openings of the end-pipe 340. The solvent 230 in the end-pipe 340 is under pressure due to thepump 23, so that the solvent 210 can be injected or sprayed out of the openings onto theconveyor belt 220. - A view of a device for separating mixtures with a
worm 350 running in the reaction space instead of theconveyor belt 220 is shown inFIG. 5 , in a manner corresponding toFIG. 3 . Theworm 350 is driven by adrive unit 360 and rotates about a longitudinal axis. Theworm 350 functions similarly to an Archimedean screw, i.e. the material 14 to be purified is deposited onto theworm 350 via thefeed opening 12 and is transported further in the direction of thecapture device 280 by aworm thread 400. The solvent 210 flows through the material 14 to be purified, in a counter-flow and can be deposited directly from thecondensation vessel 200 onto theworm 350. Thecondensation vessel 200 moreover yet includes aconduit 370 which departing from thecondensation vessel 200 ends with the end-pipe 340 at theworm 350. The end-pipe 340 includes openings, through which the solvent 210 is sprayed onto theworm 350. Thepump 23 is attached on theconduit 370 and sucks the solvent 210 out of thecondensation vessel 200 and pumps it through theconduit 370 up to the end-pipe 340. -
FIG. 6 in a view corresponding toFIG. 5 represents a further embodiment example of the device for separating mixtures. As with the embodiment example represented inFIG. 5 , the conveying device is theworm 350 which is set into rotation about its longitudinal axis by thedrive unit 360 and thus transports the material to be purified on theworm gear 400. Theconduit 370 from thecondensation vessel 200 into thereaction space 11 is however led through thedrive unit 360 into an interior of theworm shaft 380. Theworm shaft 380 includes openings extending in the direction of the rotation axis. The solvent 210 exits through these openings into thereaction space 11, wherein it is accelerated by the centrifugal force acting by way of the rotation of theworm 350, through the openings of theworm shaft 380 and flows in a counter-flow through the material 14 to be purified. - Further aspects which are encompassed by the invention are mentioned hereinafter. One aspect of the invention includes a device for separating
mixtures 14 which contain oil or bitumen and additives, wherein the device includes at least onereaction vessel 1 having areaction space 11, afeed opening 12 and adischarge conduit 16, further including asupply container 100 having avapor space 120, further including at least onecapture container 103 having a withdrawal conduit 101 and ariser conduit 104, and further including acondensation vessel 200, wherein thedischarge conduit 16 is in connection with thesupply container 100, thesupply container 100 via the withdrawal conduit 101 with thecapture container 103, thecapture container 103 via theriser conduit 104 with thevapor space 120, thevapor space 120 via aconduit 130 with thecondensation vessel 200, and thecondensation vessel 200 via afurther conduit 19 with thereaction space 11. - A further aspect relates to a device according to the preceding aspect, wherein the
reaction space 11 contains aparticle filter 320. - A further aspect relates to a device according to one of the preceding aspects, wherein stirrers or ultrasound cleaning devices 300 for improved mixing of a solvent 210 are contained in the
reaction space 11. - A further aspect relates to a device according to one of the preceding aspects, wherein
several reaction vessels - A further aspect relates to a device according to one of the preceding aspects, wherein the
discharge conduit 16 includes a siphon. - A further aspect relates to a device according to one of the preceding aspects, wherein the device has a slight vacuum of 5 to 10 mbar below atmospheric pressure.
- A further aspect relates to a device according to one of the preceding aspects, wherein the
vapor space 120 has a temperature of 60° C. to maximal 65° C. - A further aspect relates to a device according to one of the preceding aspects, wherein the
capture container 103 has a temperature of 75° C. to 95° C. - A further aspect relates to a device according to one of the preceding aspects, wherein the
condenser 200 has a temperature of 10° C. to 15° C. - One aspect of the invention relates to a method for separating
mixtures 14 which contain oil or bitumen and additives, having the following steps: -
- a) dissolving oil-containing or bitumen-containing constituents out of a mixture in a solvent 210 in a
reaction space 11; - b) separating the oil-laden or bitumen-laden solvent 210 from additives of the mixture and leading the oil-laden or bitumen-laden solvent 210 further into a
supply container 103; - c) heating the
reaction space 11 for drying the additives of the mixture and for removing the remaining solvent 210; - d) vaporizing the oil-laden or bitumen-laden solvent 210 in a
capture container 103 connected to thesupply container 100 and capturing the oil or bitumen in thecapture container 103, and the solvent vapor in avapor space 120 of thesupply container 100; - e) leading away the solvent vapor out of the
vapor space 120 and condensing the solvent in acondenser 200.
- a) dissolving oil-containing or bitumen-containing constituents out of a mixture in a solvent 210 in a
- A further aspect of the invention relates to a method according to the preceding aspect, wherein the solvent 210 includes dichloromethane, chloroform, diesel, naphtha, acetone, methanol, tetrahydrofurane, butyl methyl ether, carbon tetrachloride, propane gas, benzene or toluene.
- A further aspect relates to a method according to one of the preceding aspects, wherein the separation of the oil-laden or bitumen-laden solvent 210 is controlled or regulated in a temporal manner, preferably via a turbidity measurement of the solvent 210.
- A further aspect relates to a method according to one of the preceding claims, wherein the
reaction space 11 is heated for 10 minutes to 60° C. for heating. - A further aspect relates to a method according to one of the preceding aspects, wherein air is sucked or blown through the
capture container 103, for the accelerated vaporization of the solvent 210. - A further aspect relates to a method according to one of the preceding aspects, wherein bitumen-containing asphalt is used as a
mixture 14. -
- 1-8 reaction vessel
- 11 reaction space
- 12 feed opening
- 13 lock
- 14 material to be purified
- 15 transport belt
- 16 discharge conduit
- 17 valve
- 18 valve
- 19 filling conduit
- 20 bend
- 21 purified material
- 22 distributor head
- 23 pump
- 100 supply container
- 101 withdrawal conduit
- 102 valve
- 103 capture container
- 104 riser conduit
- 105 valve
- 110 solvent sediment
- 120 vapor space
- 130 conduit
- 180 additional condenser
- 190 blower
- 200 condensation vessel
- 210 solvent
- 220 conveyor belt
- 230 heater
- 240 capture grid
- 250 heater
- 260 first receiving container
- 270 second receiving container
- 280 capture device
- 290 further riser conduit
- 300 mixing device
- 310 measurement apparatus
- 320 particle filter
- 330 capture space
- 340 end-pipe
- 350 worm
- 360 drive unit
- 370 conduit
- 380 worm shaft
- 390 valve of the further riser conduit
- 400 worm thread
Claims (21)
1-20. (canceled)
21. A device for separating mixtures which contain oil or bitumen and additives, the device comprising:
at least one reaction vessel having a reaction space and a feed opening;
at least one capture container having a withdrawal conduit and a riser conduit;
a supply container having a vapor space, the supply container connected with the at least one capture container via the withdrawal conduit, the at least one capture container connected with the vapor space via the riser conduit; and
a condensation vessel connected with the reaction space, the reaction space connected with the supply container.
22. The device of claim 21 , further comprising a particle filter within the reaction space.
23. The device of claim 21 , further comprising stirrers or ultrasound cleaning devices within the reaction space in order to improve solvent mixing.
24. The device of claim 21 , wherein the at least one reaction vessel comprises several reaction vessels arranged in parallel.
25. The device of claim 21 , further comprising a discharge conduit connected with the supply container.
26. The device of claim 25 , wherein the discharge conduit comprises a siphon.
27. The device of claim 21 , wherein the vapor space is connected with the condensation vessel via a conduit.
28. The device of claim 27 , further comprising a filling conduit, the condensation vessel connected with the reaction space via the filling conduit.
29. The device of claim 21 , wherein the device has a slight vacuum of 5 to 10 mbar below atmospheric pressure.
30. The device of claim 21 , wherein the vapor space has a temperature of 60° C. to 65° C.
31. The device of claim 21 , wherein the capture container has a temperature of 75° C. to 95° C.
32. The device of claim 21 , wherein the condensation vessel has a temperature of 10° C. to 15° C.
33. The device of claim 21 , wherein the reaction space comprises a conveying device on which the mixture containing oil or bitumen and additives and solvent are led, the mixture led in a counter-flow to the solvent.
34. A method for separating mixtures which contain oil or bitumen and additives, the method comprising:
a) dissolving oil-containing or bitumen-containing constituents out of a mixture in a solvent, in a reaction space;
b) separating the oil-laden or bitumen-laden solvent from additives of the mixture and leading the oil-laden or bitumen-laden solvent into a supply container;
c) vaporizing the oil-laden or bitumen-laden solvent in a capture container connected to the supply container and capturing the oil or bitumen in the capture container, and capturing the solvent vapour in a vapor space of the supply container;
d) leading away the solvent vapor out of the vapour space and condensing the solvent in a condensation vessel.
35. The method of claim 34 , wherein solvent comprises dichloromethane, chloroform, diesel, naphtha, acetone, methanol, tetrahydrofurane, butyl methyl ether, carbon tetrachloride, propane gas, benzene or toluene.
36. The method of claim 34 , wherein separating the oil-laden or bitumen-laden solvent is controlled or regulated in a temporal manner.
37. The method of claim 34 , further comprising heating the reaction space for drying the additives of the mixture and for removing remaining solvent.
38. The method of claim 37 , wherein the reaction space is heated for 10 minutes at 60° C.
39. The method of claim 34 , further comprising sucking or blowing air through the capture container for accelerating solvent vaporization.
40. The method of claim 34 , wherein the mixture comprises bitumen-containing asphalt.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP10075333A EP2412783A1 (en) | 2010-07-30 | 2010-07-30 | Device and method for separating out mixtures containing oil or bitumen and additives |
EP10075333.4 | 2010-07-30 | ||
PCT/EP2011/003866 WO2012013363A1 (en) | 2010-07-30 | 2011-07-29 | Device and method for separating mixtures that contain oil or bitumen and additives |
Publications (1)
Publication Number | Publication Date |
---|---|
US20130240411A1 true US20130240411A1 (en) | 2013-09-19 |
Family
ID=43569537
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US13/813,251 Abandoned US20130240411A1 (en) | 2010-07-30 | 2011-07-29 | Device and method for separating mixtures which contain oil or bitumen and additives |
Country Status (6)
Country | Link |
---|---|
US (1) | US20130240411A1 (en) |
EP (1) | EP2412783A1 (en) |
CN (1) | CN103314077A (en) |
CA (1) | CA2806748A1 (en) |
DE (1) | DE112011102547A5 (en) |
WO (1) | WO2012013363A1 (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2018125952A1 (en) * | 2016-12-30 | 2018-07-05 | Stojan Kotefski | Methods for reclaiming or recycling asphalt and asphalt and asphalt components produced thereby |
US10640712B2 (en) | 2016-11-18 | 2020-05-05 | Stojan Kotefski | Methods for retrieving, reclaiming, or recycling petroleum-based products and byproducts |
CN112057884A (en) * | 2020-07-22 | 2020-12-11 | 江苏高速公路工程养护技术有限公司 | Method and system for recycling and treating flowing liquid for asphalt molecule testing |
US11549016B2 (en) | 2016-11-18 | 2023-01-10 | Stojan Kotefski | Hybrid crude oil and methods of making the same using petroleum-based waste stream products |
WO2024084358A1 (en) * | 2022-10-19 | 2024-04-25 | Russell Atlas James | System, method, and apparatus for recycling asphalt shingles |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108181196A (en) * | 2017-11-22 | 2018-06-19 | 中国石油天然气股份有限公司 | method for measuring oil content of shale |
CN107917873B (en) * | 2017-12-05 | 2020-05-19 | 南京林业大学 | Method for testing oil corrosion resistance of asphalt mixture |
DE102018213210A1 (en) | 2018-08-07 | 2020-02-13 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Process for cleaning mineral solids and wood materials, device for this process and its use |
CN111257159A (en) * | 2020-02-24 | 2020-06-09 | 成都理工大学 | Evaluation method for dispersion and removal effects of carbonaceous asphalt in carbonate reservoir |
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US3010893A (en) * | 1958-12-22 | 1961-11-28 | Consolidation Coal Co | Method for removing finely divided solid particles from low temperature carbonization tars |
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DE3443039A1 (en) * | 1984-11-26 | 1986-05-28 | Klöckner & Co KGaA, 4100 Duisburg | METHOD FOR THE EXTRACTION OF DETACHABLE ADDITIVES FROM NON-SOLUBLE Bulk Goods |
DE9302646U1 (en) * | 1992-10-24 | 1993-07-22 | Pitts, Martin, 31275 Lehrte | Device for the emission-free extraction of a substance from a mixture of substances |
DE4308149C2 (en) * | 1993-03-15 | 1997-04-10 | Horst Walterschen | Method and device for separating mineral solids from bituminous building materials |
DE4430951C1 (en) * | 1994-08-31 | 1996-05-23 | Bayer Ag | Method and device for separating a solid residue from its solution in a stirred material bed |
DE19506358A1 (en) * | 1995-02-23 | 1996-08-29 | Fhf Strassentest Gmbh | Quantitative recovery of bitumen binder from asphalt sample |
EP1022391B1 (en) | 1999-01-11 | 2004-05-12 | Heijmans Infrastructuur B.V. | Process for recycling tar and/or bitumen containing material which comprises asphaltic aggregate by thermal conversion in combination with the production of asphalt |
DE102006038614A1 (en) | 2006-08-17 | 2008-02-21 | Norddeutsche Mischwerke Gmbh & Co. Kg | Process for reuse of spent asphalts and production of bituminous mixtures |
CN200967805Y (en) * | 2006-11-25 | 2007-10-31 | 夏立元 | Oilstone segregator |
CN100531938C (en) * | 2007-12-12 | 2009-08-26 | 夏立元 | Device for separating oilstone |
-
2010
- 2010-07-30 EP EP10075333A patent/EP2412783A1/en not_active Withdrawn
-
2011
- 2011-07-29 CN CN2011800466345A patent/CN103314077A/en active Pending
- 2011-07-29 CA CA2806748A patent/CA2806748A1/en not_active Abandoned
- 2011-07-29 DE DE112011102547T patent/DE112011102547A5/en not_active Withdrawn
- 2011-07-29 US US13/813,251 patent/US20130240411A1/en not_active Abandoned
- 2011-07-29 WO PCT/EP2011/003866 patent/WO2012013363A1/en active Application Filing
Patent Citations (1)
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US3010893A (en) * | 1958-12-22 | 1961-11-28 | Consolidation Coal Co | Method for removing finely divided solid particles from low temperature carbonization tars |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10640712B2 (en) | 2016-11-18 | 2020-05-05 | Stojan Kotefski | Methods for retrieving, reclaiming, or recycling petroleum-based products and byproducts |
US11549016B2 (en) | 2016-11-18 | 2023-01-10 | Stojan Kotefski | Hybrid crude oil and methods of making the same using petroleum-based waste stream products |
WO2018125952A1 (en) * | 2016-12-30 | 2018-07-05 | Stojan Kotefski | Methods for reclaiming or recycling asphalt and asphalt and asphalt components produced thereby |
CN112057884A (en) * | 2020-07-22 | 2020-12-11 | 江苏高速公路工程养护技术有限公司 | Method and system for recycling and treating flowing liquid for asphalt molecule testing |
CN112057884B (en) * | 2020-07-22 | 2022-04-29 | 江苏高速公路工程养护技术有限公司 | Method and system for recycling and treating flowing liquid for asphalt molecule testing |
WO2024084358A1 (en) * | 2022-10-19 | 2024-04-25 | Russell Atlas James | System, method, and apparatus for recycling asphalt shingles |
Also Published As
Publication number | Publication date |
---|---|
CA2806748A1 (en) | 2012-02-02 |
WO2012013363A1 (en) | 2012-02-02 |
DE112011102547A5 (en) | 2013-05-02 |
EP2412783A1 (en) | 2012-02-01 |
CN103314077A (en) | 2013-09-18 |
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