EP4196552B1 - Apparatus and process for the catalytic production of diesel from organic materials - Google Patents

Description

The invention relates to a plant for the catalytic production of diesel oil from residual materials, such as plastics (PE, PP, PET, PVC, etc.), cellulose-containing materials and biomaterials according to the preamble of claim 1. Furthermore, the invention relates to a corresponding process according to the preamble of claim 12.

From the WO 2005/071043 A1 A plant is known in which hydrocarbon-containing residues or residues are heated, cracked and fractionated in a multi-stage process, whereby, among other things, diesel oil is obtained. Furthermore, the DE103 56 245 B4 A similar system is also known, whereby the main heat input occurs via the flow energy of the pumps, which are slowed down by a counter-rotating agitator as well as their friction and internal friction. However, it has turned out that these systems are still very susceptible to failure.

From the DE 103 16 969 A1 A process for the catalytic conversion of hydrocarbon-containing residues into oil in a liquid circuit is known, whereby ion-exchangeable catalysts, such as calcium aluminum silicate or sodium aluminum silicate, are used as catalysts in a heated oil bath circuit which is cleaned at the heat transfer points, whereby the oil bath circuit with the suspended catalysts is heated by electric heaters which are arranged concentrically around the reactor tubes.

From the US 2019/0330537 A1 A process for producing energy products is known. The DE 100 49 377 A1 concerns the catalytic production of diesel oil and gasoline from hydrocarbon-containing waste and oils. US 2013/0136665 A1 A system for producing oil from waste is known. From the WO 2010/003180 A1 A process for processing oil refinery waste is known. From the US 2015/0047962 A1 A device for the catalytic depolymerization of hydrocarbon-containing material is known. US 2015/0053592 A1 A process for treating hydrocarbon fuels with microwave energy is known.

The object of the invention is therefore to provide a system and a method that can be operated more easily and is less susceptible to faults.

This object is achieved by a system according to claim 1, which is characterized in that the central reactor, which receives the starting material in a carrier oil and in which the catalytic reaction takes place, is provided with at least one heater which is designed as a high-frequency wave heater with a solid-state generator (SSG high-frequency wave heater). A corresponding method is described according to claim 12.

In this case, all hydrocarbon-containing raw and residual materials are to be considered as starting materials, in particular residual and waste materials from the group of plastics (PE, PP, PET, PVC, etc.), cellulose-containing materials and biomaterials, such as wood, sawdust or wood shavings, paper, cardboard, plant parts and the like. Furthermore, a granular particle size is to be understood as free-flowing particles which, in their largest spatial extent, have an average of less than or equal to 20 mm, advantageously less than or equal to 10 mm. Ideally, these are formed as chips, flakes or comparable flat particles. In this case, diesel or diesel oil is to be understood as a kerosene mixture, the so-called middle distillate fractions in known fractionations of crude oil. The carrier oil, on the other hand, is a low-boiling heavy oil or heavy oil mixture. Such carrier oils are usually thermal oils which do not decompose at high operating temperatures, such as in the present case, for example, in the range of 280°C to 320°C. Furthermore, so-called secondary raffinates can be used. These are oils that do not lead to chemical reactions, outgassing or foaming.

This plant for the catalytic production of diesel oil from the aforementioned starting material comprises an inlet system for the starting material, a reaction unit, at least one single or multi-part separation and separating unit and at least one sediment treatment stage for solids and/or sediments, such as ash, tar substances, etc. The reaction unit generally comprises only one central reactor for treating a mixed phase consisting of a liquid carrier phase (carrier oil) and the solid starting material, whereby the reactor is often also called a melt reactor because the solids are catalytically converted into diesel oil in it. The reactor ideally has only one reactor interior, but in normal operation has a head space filled with gas or vapor and a product space filled with the mixed phase. It also comprises at least one inlet for the starting material, at least one head outlet for a gas or vapor phase, to which a separation column can be directly connected or attached. Furthermore, there is an outlet which is connected to the sediment treatment stage, as well as at least one motor-driven stirring unit for homogenizing and circulating the reactor contents, which protrudes into the product space with at least one stirring body.

The core of the invention is that a heating device is provided for the mixing phase, which is provided as a device on the outside of the reactor wall and acts on the fluid through the container wall; alternatively, such a heating device can be included in the reactor. These heating devices are designed and dimensioned in such a way that a filled mixing phase can be heated to over 200 °C, ideally to a temperature between 280 °C and 320 °C. According to the invention, an SSG high-frequency wave heater is used as the heating device, which is described in more detail below.

The heater includes a solid-state generator for electromagnetic waves in the high-frequency range. The frequencies are in the range of 0.9 to 300 GHz and a wavelength of approx. 30 cm to 1 mm. High-frequency waves used industrially are usually 915 MHz, 2450 MHz and 5.8 GHz. The so-called solid-state generator is characterized by the fact that the high frequency is not generated by a hollow chamber resonator (magnetron), but by semiconductor components. The magnetron is an electron tube with electrodes in a gas-filled glass bulb. The so-called solid-state semiconductor replaces the electron tubes.

One particular advantage has been shown to be that the age-related loss of performance of a magnetron does not occur with solid-state generators. A magnetron loses up to 30% of its output power within three to four years and must therefore be regularly replaced or serviced if the performance is to be maintained at a good level. Semiconductor components, on the other hand, are designed for a service life of over 10 years to 20 years in continuous operation. Another advantage is that the high voltage of up to 4 kV that a magnetron needs to generate frequencies is not necessary with solid-state generators. Solid-state generators work with direct voltages from 28 V. This means that components such as the oscillation source (oscillator), transformers and fans are significantly smaller for the respective performance class. The solid-state generator itself is also smaller in terms of its external dimensions and the entire high-frequency wave heating system can therefore be designed to save space. The high-frequency wave is therefore more efficient and has a longer service life and leads to lower operating costs.

The emitted high frequency is guided from the solid-state generator via waveguides into the reactor interior, where the thermal oil with the starting material and the additives are heated by the described interaction.

The waveguides are hollow aluminum profiles, usually rectangular hollow profiles, which allow versatile arrangements of reactors and solid-state generators from straight pieces and curves. The electromagnetic waves (high frequency waves) act on the molecules and cause them to vibrate and/or rotate. This increases the kinetic energy and thus the temperature of the fluid.

This has a very high level of efficiency and, unlike conventional heating surfaces, there is no thermal adhesion due to local overheating on the exchange surfaces or the emitting surfaces of the SSG high-frequency wave heater. At least one such SSG high-frequency wave heater is ideally arranged in the liquid-covered space of the reactor interior. The output of the solid-state vibration generator should be in the range of over 70 kW, ideally in the range of 80 kW to 250 kW. If necessary, the output can also be higher or more than one solid-state vibration generator can be provided.

The SSG high-frequency wave heater does not comprise a magnetron as the main component as mentioned above, but rather a generator, which in turn essentially consists of semiconductor components (solid-state) and a waveguide. On the input side, the SSG high-frequency wave heater comprises a powered signal generator (oscillator) which has an output strength in the mW range. The oscillation source of the signal generator can be, for example, a suitably excited quartz crystal, crystal or a comparable oscillation source. An intermediate amplifier for the oscillation signal can be provided in front of the actual solid-state amplifier, which in turn can be powered independently, for example in the range of 30 to 70 V. This is followed by the actual solid-state amplifier/generator, with the transistors arranged on one or both sides of the conductor track, in particular LDMOS (laterally-diffused metal-oxide semiconductor). A circulator for wrong-direction power is arranged in front of the dissipating waveguide. The waveguide mentioned generally comprises, among other things, at least one glass or Quartz glass pane, a tuner to minimize the reflected waves, a circulator and a water load (absorption component) as well as suitable detectors and directional couplers. In an improved embodiment, the product space is bordered not only by a glass or quartz glass pane, but also by a safety lock with a glass or quartz glass pane on both sides, the interior of which can be filled with an inert gas or through which an inert gas can flow. Both sides is understood to mean the direction of the main extension of the waveguide in which the high-frequency waves are guided. The advantage is that the interior can be evacuated and if the pane adjacent to the product space is damaged, no oxygen gets into the reactor and the other components of the SSG high-frequency wave heater remain protected.

An alternative design is that the reactor contents are not heated directly by the above-mentioned disk in the reactor wall or a mounting nozzle using SSG high-frequency wave heating, but the at least one SSG high-frequency wave heating acts on a side stream of the mixed phase through a glass or quartz glass tube. This side stream in a circulation line is advantageously driven by a suitable conveying means, such as a twin-screw pump.

To seal the safety panes of the safety lock in the hollow channel, paper seals or seals made of a copper material (soft copper) are advantageously provided so that a gas-tight separation is created. Surprisingly, it has been found that this gas-tight section from the central reactor functions as a very advantageous cooling section.

In an alternative variant, the SSG high-frequency wave heater is arranged in the lid and/or head space of the reactor. The advantage is that the thermal and mechanical influences are reduced by the location of the SSG high-frequency wave heater in the head space of the reactor. Furthermore, this ensures good accessibility in the event of maintenance.

Furthermore, it is particularly preferred to provide at least one motor-driven, rotationally driven cutting device for the impact and/or cutting comminution of the starting material, which has at least one cutting edge or one cutting section and projects into the product space of the reactor.

In one embodiment of the cutting device, it is attached to and driven by the same drive shaft as the at least one stirring body, whereby alternatively or additionally the at least one stirring body can also be designed as a cutting edge or with a cutting section. Another alternative is that the cutting device extends into the product space and has its own drive shaft and its own drive that is independent of the drive of the stirring unit.

One improvement consists in that at least one agitator body is arranged at a vertical height between two cutting units, so that they can work in a cutting and/or dividing manner directly above and below the agitator in the directed flow.

The drive must be designed in such a way that it enables permanent, complete mixing and multiple circulations per minute, which means that the stirring unit must be able to rotate at a speed of at least 400 to 500 rpm. A rotational speed of 440 to 470 rpm is advantageous. It is advantageous if the peripheral speed of the stirring unit is in the range of 10 to 20 m/s, and ideally a peripheral speed of 13 to 18 m/s can be achieved using the drive and adjusted during operation of the system. The same applies to the drive of the cutting unit, which should have a speed of at least 400 to 500 rpm, although a speed of over 440 to 470 rpm should be maintained during operation.

A further improvement is that the agitator, in particular its drive shaft, is arranged eccentrically in the reactor, which creates a particularly advantageous three-dimensional flow in the product space of the reactor. Axial eccentricity E of the agitator axis to the central axis of the reactor has proven to be advantageous, which lies in the range of 0.15 to 0.25.

The single or multi-part separation and separation unit downstream of the reactor comprises at least one condenser and/or a separation column for separating the diesel oil. Surprisingly, it has been found that it is sufficient to provide a simple separation column after the reactor - possibly directly on top of it - in order to subsequently provide one or two condensers for separating the product oil.

As indicated, the separation column then forms a structural unit with the reactor and is attached directly to the head space or is directly connected to it via a flange. The head space of the reactor extends directly into the lowest bottom or inlet area of the column and forms a single space.

A further improved variant consists in providing a recirculation inlet on the reactor, which is connected to the sediment treatment stage and via which partial flows or partial quantities that have been removed via an outlet can be returned to the reactor. The returned partial flows or partial quantities are usually liquid and depleted of solids such as lime, catalyst, ash or tar fractions.

The reactor inlet and/or the return inlet are shaped in such a way that a housing of an incoming conveyor screw is held and sealed thereon. Known flange or coupling elements can be provided for this purpose. It is particularly advantageous if there is no longer a separate pipe section between the reactor inlet and the outlet end of the incoming conveyor screw.

One improvement is that the housing of the incoming conveyor screw ends directly at the reactor with the outlet end or forms the reactor flange.

Process and auxiliary materials, such as a carrier oil to be supplemented, lime, catalyst can be introduced into one of the other feed or return streams. However, a separate feed unit for process and auxiliary materials is advantageously provided, which is connected to the reactor via a pipe, with a separate access nozzle being provided for this purpose in the reactor.

Not described in detail, because they are common practice for a specialist, are necessary line connections, connecting flanges, structural elements and the like, as well as the known and usual control and regulation units.

By using this plant and in particular the reactor, a process for the continuous production of diesel oil from the aforementioned starting material is possible, which is introduced as a granular solid phase into a liquid phase of the aforementioned carrier oil and catalytically converted.

The temperature in the mixing phase is between 200 and 400°C, and is ideally between 280°C and 350°C. The mixing phase also contains a proportion of lime of 1.5% to 10% by weight, whereby lime is understood here as a collective term for substances or mixtures of substances containing calcium or calcium carbonate. The mixing phase also contains a catalyst in a proportion of 1% to 15% by weight.

The gaseous or vaporous phase is continuously removed, ideally by means of at least one vacuum pump from the head space of the reactor. Downstream of the reactor, the diesel oil is separated from the more volatile gaseous or vaporous phase in at least one condenser. In parallel, in the mixing phase, the contained gaseous starting material is mechanically cut and/or crushed using at least one cutting edge or cutting section. For optimal mixing in the reactor interior and to avoid any sedimentation, the peripheral speed of the stirring unit is between 8 and 20 m/s, although it has been found that this should ideally be between 13 and 17 m/s.

The catalyst is advantageously a bentonite or zeolite, especially an aluminum silicate, which is in a powdery state. The pressure to be set in the head space of the reactor is less than or equal to 1 bar, ideally it is in the range of 25 to 60 mbar.

Not described in detail, because they are common practice for a specialist, are necessary line connections, connecting flanges, structural elements and the like, as well as the known and usual control and regulation units.

• Figur 1 als Blockdiagramm einen Verfahrensablauf und die wichtigsten Verfahrensschritte,
• Figur 2 die Anlage nach Figur 1 mit Einzelschritten zur Produktaufbereitungsstufe,
• Figur 3 ein erstes Ausführungsbeispiel des zentralen Reaktors,
• Figur 4 ein zweites Ausführungsbeispiel des zentralen Reaktors,
• Figur 5 den Aufbau der SSG-Hochfrequenzwellenheizung des zentralen Reaktors und
• Figur 6 eine alternative Ausführungsform zur Figur 5.

The invention is explained in more detail below by way of example, showing

• Figure 1 as a block diagram a process flow and the most important process steps,
• Figure 2 the system after Figure 1 with individual steps to the product preparation stage,
• Figure 3 a first embodiment of the central reactor,
• Figure 4 a second embodiment of the central reactor,
• Figure 5 the construction of the SSG high-frequency wave heating of the central reactor and
• Figure 6 an alternative embodiment to Figure 5 .

In the Figure 1 The entire plant 1 for the catalytic production of diesel oil 9 from the starting material 7 is shown schematically as a block diagram. The starting material 7 is fed via the inlet system 100 to the reaction unit 10, which has at least one reactor, but can also comprise two or more reactors connected in parallel (not shown). The starting material 7 is fed into the reactor 11 via the reactor inlet 12, as shown.

The process and auxiliary materials 8, such as carrier oil to be added, lime and catalyst, are also introduced via the introduction system 100. Alternatively, but not shown, this can be done via a separate feed unit that is connected to the reactor via a pipeline, with a separate access nozzle being provided in the reactor for this purpose. Furthermore, a product preparation stage 300 for the diesel oil 9 is connected via a pipeline to or to the head space 11.1 of the reactor 11 via the head outlet 13. In the product preparation stage 300, the diesel oil portion is separated from the lower-boiling aqueous phase in the gas and vapor phase. The diesel oil 9 is stored in the storage tank 24.

Close to the bottom with a connection to the product chamber 11.2, the reactor 11 is connected via the bottom outlet 14 and the outlet line 14.1 to a sediment processing stage 200, from which the return line 23.1 leads into the return inlet 23 so that a liquid phase can be fed back into the reactor 11. The system 1 also comprises a coupling and purification unit 400, which is optional and by means of which the diesel oil 9 can be desulfurized, for example, and/or the solid and sedimentation substances can be further processed and packaged. For this purpose, the product processing stage 300 and/or the sediment processing stage are connected to one another in a suitable manner via suitable conveying means and/or lines.

In Figure 1 and the following figures, common units for control, regulation, conveying, displays, etc. are not shown for reasons of clarity.

As continued in Figure 1 As can be seen, the reactor 11 has a stirring unit 15 with a drive 19, a drive shaft 17, a stirring body 16 and a cutting unit 18. The stirring body 16 is designed as a 2- to 4-bladed propeller in this and the following embodiments.

The Figure 2 shows Appendix 1 acc. Figure 1 in an embodiment in which the product preparation stage 300 for the gas and/or vapor phase leaving the headspace of the reactor 11 via the head outlet 13 comprises a separation and deposition unit 3, which includes a deposition column 4 and two condensers 5.1, 5.2 connected in series, which are connected via the steam lines 26.1 and 26.2. These condensers 5.1, 5.2 are operated at a temperature just above the boiling point of water at > 100°C, ideally in a temperature range of 101°C to 105°C. This process control enables the volatile vapor phase, which essentially contains remaining water vapor, to leave the product preparation stage 300 to the chimney 25 via the steam line 26.3. The condensed diesel oil 9 leaves the respective condenser 5.1, 5.2 via the product lines 27.1 and 27.2 and is fed to the storage tank 24 via the collecting product line 27. Starting from one of the product lines 27, 27.1, 27.2, diesel oil 9 is fed to the top of the separation column 4 via the return line 28 in order to ensure a reliable separation process.

The separation column 4 is filled with a bed 4.1 of inert shaped pieces, usually metallic shaped bodies, which are arranged on one or more sieve plates. In this case, a proportion of diesel oil of less than 15% of the total flow is returned to the separation column 4. The separation column 4 essentially does not serve as a distillation column, but rather serves the purpose of safely retaining entrained foreign or starting materials, rising foam and heavy oil droplets in the reactor 11.

Furthermore, the heating device 22, an SSG high-frequency wave heater, is shown schematically on the reactor 11 in the area of the product space 11.2, whereby, as stated above, usual power and/or data lines, fittings, valves, conveyors, etc. are not shown.

In the Figure 3 the reactor 11 is shown in more detail. The drive shaft 17 of the agitator 15 is arranged at the distance E1 parallel and eccentric to the central axis MA of the reactor 11 and is held by the fastening flange 19.1 on the upper dished bottom 30.1. The cutting device 18 has a diameter d1 which is slightly larger than the diameters d2 of the two agitator bodies 16.1 and 16.2, which are attached above and below the cutting device 18 on the same drive shaft 17 and are driven by it. The distance between the upper edge or flange of the lower dished bottom 30.2 to the lower edge or flange of the upper dished bottom 30.1 is the height H1. The height H2 is also measured up to the lower edge or flange of the upper dished bottom 30.1, but has the deepest extension of the lower dished bottom 30.2 as the lower reference point. The flange of the reactor inlet 12 is inclined upwards by the angle α of 30° with respect to the horizontal 29.2, with the horizontal 29.2 penetrating the opening at the reactor inlet 12 in the center of the flow area. The horizontal 29.2 thus forms a theoretical center line that runs parallel and centrally between an upper plane e1, which at the height h1 includes the highest point of the upper edge of the reactor inlet 12, and a lower plane e2, which at the height h2 includes the lowest point of the lower edge of the reactor inlet 12.

In the present embodiment, the reactor inlet 12 and the return inlet 23 are formed in such a way that a line or a conveyor unit can be directly flanged on, in particular that the housing of an introductory Conveyor screw is held and sealed thereon (not shown). Known flange or coupling elements can be provided for this purpose. It is particularly advantageous if there is no longer a separate pipe section between the reactor inlet and the outlet end of the incoming conveyor screw and these merge directly into one another. As in the Figure 3 As can be seen, the return inlet 23 is also inclined by an angle β to the horizontal, which should be in the range of 5° to 35°.

In general, it has been found that it is very advantageous if the space spanned by the cutting unit 18 during rotation lies below the horizontal 29.1 or encompasses it and ideally lies below the plane e2. In other words, ideally a theoretical cutting plane 31, as a theoretical middle plane of the space that results from the rotational movement of the cutting unit 18, lies at a height h3 that is smaller than the height h1 and in particular is also smaller than or equal to the height h2.

Surprisingly, it was found that a further improvement is achieved if the theoretical cutting plane 31 is located in the space between the horizontal 29.1 and the plane e2. This means that the supplied starting material is immediately subjected to cutting and impact processing upon entering the reactor 11, resulting in optimal distribution and comminution.

In the case of a very pronounced, strongly curved lower dished bottom 30.2, the analogous observation takes place starting from the lowest point of the dished bottom.

The motor power of the drive 19 is in the range of 9 to 15 kW motor with a speed of 1,300 to 2,000 rpm. Depending on the gear, a drive speed of 400 to 500 rpm is achieved on the stirring body 16 in the present embodiment.

As in the Figure 3 As can also be seen, the separating column 4 is attached to the top outlet 13 via a connecting flange directly to the upper dished bottom 30.1 on the reactor 11. The heating device is in the design according to Figure 3 a SSG high frequency wave heater 22.1, with an output of 100 kW, whose High frequency waves 22.2, indicated as cubic waves, act directly on the mixing phase. For this purpose, the SSG high frequency wave heater 22.1 is arranged in the interior of the reactor 11.

An alternative location of the SSG high-frequency wave heater 22.1 (not shown) is in the head space 11.1 of the reactor 11, because this reduces the thermal-mechanical influences and provides better accessibility in the event of maintenance.

In the present example, the actual solid-state amplifier of the high-frequency wave heater comprises 2, 3 or 4 LDMOS on one or both sides of the conductor track, each with a power of 200 to 500 W, i.e. it is equipped with a maximum of 8 LDMOS.

The output power is therefore 50 to 400 kW, depending on the number of LDMOS in the central solid-state amplifier. Common parts and components, as well as the necessary power supply, are not listed here for the sake of clarity.

In the version according to the Figure 4 The stirring unit 15 shown on the left essentially corresponds to the one shown in Figure 3 , with a stirring body 16.1 being provided on one drive shaft 17 and above the cutting mechanism 18. Furthermore, a second stirring device 15.1 with its own drive 21 and associated drive shaft 20 is provided, on which two further stirring bodies 16.3, 16.4 are arranged. The advantage is that the upward flow is supported and the drive 19 of the stirring device 15 can be made smaller. A further advantage is that even if one stirring device 15, 15.1 fails, the circulation in the reactor 11 can be maintained, if necessary with reduced or switched off supply of starting material. The second stirring device 15.1 is also arranged eccentrically by the distance E2, parallel to the central axis MA. Ideally, the two drive shafts and the central axis MA are in a vertical plane. The main flow direction is indicated by arrows.

The embodiments and arrangements according to the Figures 3 and 4 can be combined depending on the reactor dimensions, in particular the number of stirring elements and/or the cutting edges or cutting sections. For example, the second or a further Agitator may also be provided with a cutting or cutting section (not shown).

In the Figures 5 and 6 The installation situations and structure of the SSG high frequency wave heater 22.1 are shown in detail and are otherwise analogous to the design according to Figure 3 trained. The Figure 6 one of possibly several SSG high-frequency wave heaters 22.1, which are arranged directly on the outer wall of the central reactor 11.

The SSG high-frequency wave heater 22.1 comprises a signal generator 37, a solid-state generator 35, a waveguide 38 and a safety lock 36, which adjoins the reactor 11 with a first end and the safety disk 36.2 arranged there.

Conventional flange and connecting elements are provided, but not further developed. An inert gas, e.g. nitrogen, can be fed into the interior 36.1 of the safety lock 36 via the inlet 36.3. A further safety pane 36.4 is arranged at the second end of the safety lock 36; both safety panes 36.2, 36.4 are made of glass or quartz glass. Signal generator 37 generates the high-frequency waves, which are indicated as a strong arrow pointing in the direction of the reactor 11. Only mentioned, without detailed representation, are the known other elements of the SSG high-frequency wave heating, such as a tuner for minimizing the reflected high-frequency waves, which are indicated as a narrow arrow, a circulator, a water load or a suitable absorption component, as well as suitable detectors and a directional coupler.

In this advantageous embodiment, the product space 11.2 is bordered not only by a single glass or quartz glass pane 36.2, but also by a safety lock 36, whereby in a simplified design only a single safety pane 36.2 can be provided between the product space 11.2 of the reactor 11 and the SSG high-frequency wave heater 22.1.

Alternatively to Figure 5 shows Figure 6 an alternative design in which the mixed phase filled in the product chamber 11.2 is not heated directly. Instead, a line 58 is provided which leads in a circuit out of the reactor and back in and in which a conveying means 59, such as a double spindle pump, operates. Furthermore, a section of the line 58 is provided with a glass or quartz glass tube 39, via which the high-frequency waves from two SSG high-frequency wave heaters 22.1a, 22.1b act on the flowing mixed phase. To avoid excessive reflection of the high-frequency waves into the SSG high-frequency wave heaters, it can be advantageous to provide several glass or quartz glass tubes 39 on different sections of the line 58, each with a single SSG high-frequency wave heater 22.1a, 22.1b.

In the variant shown, the pipeline 58 has SSG high-frequency wave heaters 22.1a, 22.1b in two designs. The SSG high-frequency wave heater 22.1a arranged closer to the reactor 11 is constructed as in Figure 6 described, wherein the SSG high-frequency wave heater 22.1b arranged downstream for this purpose does not comprise a safety lock and only one or more windows made of glass or quartz glass are provided through which the high-frequency waves are guided into the interior of the pipe.

It has been found to be advantageous if, for example, a seal made of a copper material is provided on at least one side, ideally on both sides, as the sealing material for the first safety disk 36.2, which borders on the pipe interior and/or product space 11.2 that carries the mixing phase. On the second side of the safety channel 36 facing away from this, a fluororubber is provided to seal the inside of the safety disk and a cooling flange made of an aluminum material is provided on the outside facing the semiconductor high-frequency generator.

The units, some of which are not shown, can be provided individually or jointly as explained above, in particular with regard to the type, design and/or arrangement of the SSG high-frequency wave heater 22.1.

list of reference symbols

1

Attachment

2

supply of auxiliary materials

3

separation and separation unit

4

separation column
4.1 Filling

5

capacitors
5.1 capacitor
5.2 Capacitor

6

inert gas

7

starting material

8

auxiliary and process media
8.1 Tank
8.2 Funding

9

diesel oil/line

10

reactor unit

11

reactor
11.1 Headroom
11.2 Product space

12

reactor inlet
12.1 Inlet line

13

head outlet

14

floor outlet
14.1 Outlet line

15

stirring unit

16

stirring elements
16.1 Stirring body first
16.2 Stirring body second

17

drive shaft
17.1 Drive

18

cutting unit
18.1 Cutting edge or cutting section

19

drive
19.1 Mounting flange

20

drive shaft

21

drive

22

heating device
22.1 SSG high frequency wave heating
22.2 High-frequency wave

23

return inlet
23.1 Return line

24

storage tank

25

Chimney

26

steam line 26.1, 26.2, 26.3

27

Product Line 27.1, 27.2

28

return line

29

horizontal
29.1 Middle of H1
29.2 Middle of H2 ...

30

dished bottom
30.1 upper dished bottom
30.2 lower dished bottom

31

cutting plane

32

control and supply unit

34

data and/or power line

35

solid-state generator

36

security gate
36.1 Interior
36.2 Safety glass
36.3 Inlet
36.4 Safety glass

37

signal generator

38

waveguide

39

glass or quartz glass tube

58

Line

59

funding

100

inlet system

200

sediment processing stage (sediment) (new)

300

Product preparation stage (product) (new)

400

coupling and purification unit

e1

plane, horizontal

e2

plane, horizontal

E1

eccentricity

E2

eccentricity

H1

Height of reactor interior without dished bottom

H2

Height of reactor interior with lower dished bottom

h1

height of the upper edge of the inlet

h2

height of the lower edge of the inlet

h3

height of the cutting unit

α, β

angle

MA

central axis

Claims (15)

1. System (1) for the catalytic production of diesel oil (9) from a starting material (7) from the group of residues, such as plastics (PE, PP, pet, PVC, etc.), cellulose-containing substances and biomaterials, comprising at least one introduction system (100) for the starting material (7), a reaction unit (10), at least one single-part or multi-part separation and separator unit (3) and at least one sediment preparation stage (200) for solids and/or sediments, wherein the reaction unit (10) comprises at least one reactor (11) for treating a mixing phase of a liquid carrier phase (carrier oil) and the solid starting material (7), wherein the reactor (11)

   - in intended operation, has a gas- or steam-filled head chamber (11.1) and a product chamber (11.2) filled with the mixing phase, further comprising an inlet (12) for the starting material (7), a head outlet (13) for a gas or vapor phase, an outlet (14) connected to the sediment preparation stage (200) and at least one motor-driven agitation unit (15) for homogenizing and circulating the reactor content, which projects into the product chamber (11.2) with at least one agitator body (16), characterized in that the reactor (11) comprises at least one heating device (22) or a heating device (22) directly adjacent thereto, wherein the heating device (22) is an SSG high-frequency wave heater (22.1), which has a solid-state generator (35), and the at least one SSG high-frequency wave heater (22.1) has in particular a power of 80 to 200 kW or more, and which is separated from the product chamber (11.2) of the reactor (11) or the circulating line (58) carrying the mixing phase by at least one pane, window and/or pipe made of glass or quartz glass.
2. System (1) according to Claim 1, characterized in that the at least one SSG high-frequency wave heater (22.1) comprises a safety lock (36) as a waveguide section, which has an evacuatable inner chamber (36.1), in particular an inner chamber (36.1), on which glass or quartz glass panes (36.2, 36.4) are arranged on both sides.
3. System (1) according to any of the preceding claims, characterized in that the reactor (11) furthermore has at least one motor-driven rotary cutting mechanism (18) for impact and/or cutting comminution of the starting material (7), wherein optionally

   - it can be provided that the at least one cutting mechanism (18) has at least one cutting edge or a cutting section (18.1) and is attached to and driven by the same drive shaft (17) as the at least one agitator body (16) and/or that the at least one agitator body (16) is designed as a cutting edge or with a cutting section (18.1);

   - it can be provided that the cutting mechanism (18) has a drive shaft (20) and its own drive (21) independent of the drive (19) of the agitation unit (15); or

   - it can be provided that at least one cutting mechanism (18) is arranged at a vertical height between two agitator bodies (16.1, 16.2).
4. System (1) according to any of the preceding claims, characterized in that

   - the drive (19) enables the speed of the agitation unit (15) of at least 400 to 500 rpm, advantageously a rotational speed of 440 to 470 rpm and/or a circumferential speed of the agitation unit (15) of 10 to 20 m/s can be achieved, ideally a circumferential speed of 13 to 18 m/s can be achieved;
   and/or

   - the agitator (15) and/or its drive shaft (17) is arranged eccentrically in the reactor (9).
5. System (1) according to Claim 3, characterized in that the drive (21) of the cutting mechanism (18) allows a speed of at least 400 to 500 rpm, advantageously allows a speed of over 440 to 470 rpm.
6. System (1) according to any of the preceding claims, characterized in that the single- or multi-part separation and separator unit (3) comprises at least one condenser (5) and/or a separating column (4) for separating the diesel oil (9) .
7. System (1) according to any of the preceding claims, characterized in that

   - the separating column (4) and subsequently the at least one condenser (5), ideally two condensers (5.1, 5.2), are arranged downstream of the reactor (11);
   and/or

   - the separating column (4) forms a structural unit with the reactor (11) and is attached directly to or connected to the head chamber (11.1).
8. System (1) according to any of the preceding claims, characterized in that a recirculation inlet (23) is provided on the reactor (11), which is connected to the sediment preparation stage (200) and via which partial streams or partial quantities removed via the outlet (14) can be recirculated to the reactor (11).
9. System (1) according to any of the preceding claims, characterized in that the reactor inlet (12) and/or the return inlet (23) is shaped in such a way that a housing (42.1, 62.1) of an introducing screw conveyor (42, 62) is held and sealed against it.
10. System (1) according to any of the preceding claims, characterized in that the housing (42.1, 62.1) of the introducing screw conveyor (42, 62) is directly connected to an inlet (12, 23) or a flange of the reactor (11) and/or projects into the latter.
11. System (1) according to any of the preceding claims, characterized in that a supply unit (2) for process and auxiliary materials (8) is provided, which is connected by lines to the reactor (11).
12. Method for the continuous production of diesel oil from a starting material (7) from the group of residual materials, such as plastics (PE, PP, PET, PVC, etc.), cellulose-containing substances (sawdust, shredded material) and biomaterials, which is introduced as a granular solid phase into a liquid phase from a carrier oil and catalytically shaped, characterized in that a system (1) according to any of the preceding Claims 1 to 11 is provided, and wherein

    - the temperature in the mixing phase is between 200 and 400°C, ideally between 280°C and 350°C, and

    - the mixing phase still contains a proportion of lime of 1.5% by weight to 10% by weight (2-5) and a proportion of catalyst of 1% by weight to 15% by weight 2-10), and wherein

    - the gaseous or vaporous phase is continuously withdrawn from the head chamber (11.1) by means of at least one vacuum pump and, downstream of the reactor (11) in at least one condenser (5), the diesel oil (9) is separated from the highly volatile gaseous or vaporous phase.
13. Method according to Claim 12, characterized in that the starting material (7) contained in the mixing phase is mechanically comminuted in the reactor (11) by means of the at least one cutting edge or the cutting section (18.1).
14. Method according to any of Claims 12 or 13, characterized in that the catalyst is a bentonite or zeolite, in particular an aluminium silicate.
15. Method according to any of Claims 12 to 14, characterized in that

    - the circumferential speed of the agitation unit (15) is between 8 and 20 m/s, ideally between 13 and 17 m/s;
    and/or

    - the pressure in the head chamber (11.1) of the reactor (11) is less than or equal to 1 bar, ideally in the range of 25 to 60 mbar.

Images