EP2184334A1 - Method and device for recycling materials containing hydrocarbons - Google Patents
Method and device for recycling materials containing hydrocarbons Download PDFInfo
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- EP2184334A1 EP2184334A1 EP08019151A EP08019151A EP2184334A1 EP 2184334 A1 EP2184334 A1 EP 2184334A1 EP 08019151 A EP08019151 A EP 08019151A EP 08019151 A EP08019151 A EP 08019151A EP 2184334 A1 EP2184334 A1 EP 2184334A1
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- reactor
- tubular reactor
- materials
- tubular
- pyrolysis
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- 239000000463 material Substances 0.000 title claims abstract description 54
- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 36
- 150000002430 hydrocarbons Chemical class 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000004064 recycling Methods 0.000 title description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 23
- 239000007787 solid Substances 0.000 claims abstract description 20
- 238000000197 pyrolysis Methods 0.000 claims abstract description 17
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 14
- 238000003763 carbonization Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 229920001971 elastomer Polymers 0.000 claims description 20
- 239000005060 rubber Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000010924 continuous production Methods 0.000 claims description 2
- 239000010920 waste tyre Substances 0.000 claims description 2
- 230000003750 conditioning effect Effects 0.000 abstract 1
- 239000007858 starting material Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 5
- 238000007670 refining Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000004071 soot Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 150000002830 nitrogen compounds Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920001059 synthetic polymer Polymers 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000237858 Gastropoda Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
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Classifications
-
- 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
- C10G1/10—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal from rubber or rubber waste
Definitions
- the invention relates to processes and systems for hydrocarbon-containing materials, in particular rubber-based materials (such as. Waste tires) to recycle by means of pyrolysis.
- WO92 / 0176 a process for the recycling of car tires, in which in the presence of an oxygen-containing atmosphere at temperatures between 180 and 260 ° C car tires are pyrolyzed to form liquid and gaseous hydrocarbons.
- This document further discloses a plant for carrying out this process, wherein the pyrolysis reactor is arranged vertically and is heated by partial combustion of the starting material autothermally.
- US5505008 a discontinuous process for recycling hydrocarbon-containing materials, eg. Car tires, in which under inert atmosphere, reduced pressure of 0.1 - 40 mbar and temperatures of at least 200 ° C, the starting materials are reacted discontinuously.
- This document further discloses a plant for carrying out this process, wherein the pyrolysis reactor is not specified more precisely.
- GB2278606 also discloses a process for recycling rubber waste in which comminuted particles are reacted in the presence of 16-80% by weight of additives at 100-200 ° C in a stirred reactor to yield a rubber-like material as the final product. This Process causes no decomposition of the starting material but a return to reusable rubbery material. This document further discloses a plant for carrying out this process, wherein the reactor is designed as a stirred tank.
- the present invention is therefore based on the object of providing an improved process for recycling hydrocarbon-containing materials, in particular rubber-based materials, and systems suitable therefor.
- the invention relates to a continuous process for the pyrolysis of hydrocarbonaceous materials to form solid carbon (especially soot) and volatile hydrocarbons, characterized in that a) the hydrocarbonaceous materials under inert atmosphere, at normal or Underpressure in a tubular reactor containing means for conveying and mixing, subjected to a time and temperature graded treatment; b) the volatile hydrocarbons formed in step a) are removed at one or more points along the longitudinal axis of said tubular reactor; c) the solid carbon formed in step a) is removed after cooling at the end of said tubular reactor.
- the inventive method is designed continuously, i. Starting material is constantly fed to the tubular reactor at one end and products (solid carbon and volatile hydrocarbons) are continuously withdrawn from the tube reactor.
- the starting material is fed comminuted.
- the method according to the invention is carried out in a time scale, i. the residence time of the materials in the various steps is predetermined and adapted to the particular situation.
- the residence time can be determined or varied by the design of the tubular reactor, such as its dimenization or the design of a screw conveyor.
- the process according to the invention is particularly suitable for recycling rubber-based materials, in particular rubber-based, vulcanized materials, for example old tires.
- the inventive method is also particularly suitable for recycling hydrocarbon-containing materials, such as PS fittings.
- An advantage of the process according to the invention is the resulting product mix of volatile hydrocarbons and solid carbon. Furthermore, it is to be regarded as advantageous that the method according to the invention is very flexible with regard to further components. Thus, the method is feasible with and without the addition of catalysts and with and without the addition of other auxiliaries.
- the residence time in the tubular reactor can be varied within a wide range and can in principle be determined in simple series experiments. Residence times of from 0.5 to 24 hours, preferably from 4 to 10 hours, have proved to be advantageous. The residence times can be adjusted by the means for conveying and sizing the reactor.
- the reaction temperatures in the reactor can be varied within a wide range.
- the heating of the reactor takes place e.g. allothermic, preferably by means of a circulating carrier oil.
- the temperatures realized are in the range between 20 ° C (room temperature) and about 1100 ° C (preferably: 20 - 500 ° C).
- Reaction in the reactor is "temperature-graded", i. the temperature is varied along the reactor longitudinal axis.
- the temperatures are selected so that the steps "carbonization", “finishing” and “post-treatment” occur in successive zones of the tubular reactor.
- the temperature is chosen so that the refining takes place at higher temperatures and the aftertreatment at lower temperatures than the carbonization.
- the following temperature ranges have proven to be advantageous: For the carbonization to 500 ° C (preferably: 350 ° C); for refining up to 1100 ° C (preferably: 450 ° C).
- the aftertreatment is conducted in an advantageous embodiment so that the solid reaction product leaves the reactor at a maximum of 100.degree. Suitable reaction temperatures are naturally related to the (sub) pressure of the plant, wherein a lower pressure in the system also allows lower reaction temperatures.
- a temperature profile can likewise be impressed, for example, fluctuating between 80 and 300 ° C. during the carbonization and continuously decreasing from 400 ° C. to 80 ° C. in the after-treatment.
- the reaction pressure in the reactor can be varied in a wider range.
- a suitable reaction pressure the range of -100 - +800 mbar, in particular 400 - 600 mbar has been found.
- the reaction pressure can be generated by vacuum pumps, which with the Points communicate to remove the liquid hydrocarbons.
- the invention in a second aspect , relates to a plant for the pyrolysis of rubber-based materials, comprising one or more tubular reactors, these tubular reactors being equipped with i) means for supplying comminuted rubber-based materials; ii) means for conveying and mixing said rubber-based materials through the tubular reactor; iii) means for removing formed gaseous hydrocarbons disposed along the longitudinal axis of the tubular reactor; (iv) means of removal of solid carbon formed; v) means for indirect temperaturgraduften heating and wherein said tubular reactors are designed so that they can be operated under inert atmosphere, at normal or negative pressure.
- Suitable reactors are known per se, for example rotary kilns or screw reactors. Particularly suitable are screw reactors. Such reactors may have baffles which cause a promotion and mixing. In the case of screw reactors, mixing and conveying takes place exclusively or additionally through the central auger. The pitch of the screw can be constant over the entire length or vary, so as to adjust the residence time.
- the supply of the starting material and the removal of the solid carbon can be done by common devices, such as cyclo and other equipment.
- the removal of the volatile hydrocarbons can also be done by conventional devices, for example. Via valves that communicate with capacitors and vacuum pumps. Suitable devices and equipment are known in the art and may be selected and designed by those skilled in the art.
- the tubular reactor is arranged horizontally or nearly horizontally (i.e., +/- 10 °). Such an arrangement has the advantage over a vertical arrangement that a controlled homogenized process is achieved.
- the tubular reactor is subdivided into three or more interconnected partial reactors.
- the subdivision preferably takes place in three partial reactors.
- the carbonization is carried out in the first part reactor, the refining in the second part reactor and the aftertreatment in the third part reactor.
- means for removing volatile hydrocarbons are provided only in the first and second part of the reactor. Further, only the first part reactor contains means for feeding crushed rubber-based materials and only the third part reactor means for removing formed solid carbons.
- the tubular reactor is subdivided into three or more interconnected partial reactors (phases), these partial reactors being arranged one below the other, such that the feed takes place at the upper part reactor and the removal takes place at the lower part reactor.
- the pyrolysis plant according to the invention are assigned further secondary plants in order to carry out the process described here. Particular mention should be made of: devices for generating the desired reaction pressure (over-, under-, normal pressure); Apparatus for isolating and separating the generated liquid hydrocarbons; Storage container for the starting material; Reservoir for the generated solid carbon. These individual devices are known per se and can be designed and adapted by the person skilled in the art.
- means for recovering energy e.g., heat exchangers
- the energy for heating the plant can be obtained from the recovered volatile hydrocarbons.
- FIG. 1 Showing: 1 Pyrolysis plant for rubber-based materials 2 Screw reactor consisting of three partial reactors, Schwelung 21, finishing 22 and after-treatment 23 24 Volatile hydrocarbon removal agent and vacuum connection 25 Means for feeding shredded rubber-based materials 26 Snail for conveying and mixing 27 Means for removing formed solid carbons 28 Double-walled version for indirect heating 3 Plant for the supply of rubber-based materials 31 reservoir 32 conveyor belt 33 intermediate container 4 Plant for storage and delivery of the soot formed 41 reservoir 42 Auger 43 Auger
- a corresponding plant for the processing of hydrocarbon-containing materials is similar to the one in Fig. 1 shown construction, wherein (3) and (25) are modified accordingly.
- a plant according to Fig. 1 In a plant according to Fig. 1
- two identically dimensioned tubular reactors in each case 10 tons of shredded old tires, are continuously converted per day. This typically gives: 7 t of soot; 10 t volatile hydrocarbons (1 t gas, 9 t liquid hydrocarbons); 3 t of waste steel. While preferred embodiments of the invention are described in the present application, it is to be understood that the invention is not limited thereto and may be embodied otherwise within the scope of the following claims.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
Description
Die Erfindung betrifft Verfahren und Anlagen um kohlenwasserstoff-haltige Materialien, insbesondere gummibasierte Materialien (wie bspw. Altreifen), mittels Pyrolyse zu recyclieren.The invention relates to processes and systems for hydrocarbon-containing materials, in particular rubber-based materials (such as. Waste tires) to recycle by means of pyrolysis.
Es sind bereits verschiedene Verfahren zur Aufarbeitung, Wiedergewinnung und / oder Recycling von kohlenwasserstoff-haltigen Materialien bekannt.Various processes for working up, recovering and / or recycling hydrocarbon-containing materials are already known.
So offenbart
Ferner offenbart
Die bekannten Recyclingmethoden für kohlenwasserstoff-haltige Materialien, insbesondere gummibasierten Materialien zeigen verschiedene Nachteile, so sind die Anlagen aufwändig bzw. ineffizient, und / oder die entstehenden Produkte /Produktgemische von nachteiliger Zusammensetzung.The known recycling methods for hydrocarbon-containing materials, in particular rubber-based materials show various disadvantages, so the systems are complex or inefficient, and / or the resulting products / product mixtures of disadvantageous composition.
Der vorliegenden Erfindung liegt daher die Aufgabe zugrunde, ein verbessertes Verfahren zum Recyclieren von kohlenwasserstoff-haltigen Materialien, insbesondere gummibasierten Materialien, und dafür geeignete Anlagen zur Verfügung zu stellen.The present invention is therefore based on the object of providing an improved process for recycling hydrocarbon-containing materials, in particular rubber-based materials, and systems suitable therefor.
Diese Aufgabe wird durch das Verfahren gemäss Anspruch 1 gelöst. Weitere Aspekte der Erfindung sind in den unabhängigen Ansprüchen und der Beschreibung angegeben, vorteilhafte Ausführungsformen sind den abhängigen Ansprüchen und der Beschreibung zu entnehmen.This object is achieved by the method according to claim 1. Further aspects of the invention are set forth in the independent claims and the description, advantageous embodiments are given in the dependent claims and the description.
Die vorliegende Erfindung wird im Folgenden im Detail beschrieben. Im Rahmen dieser Erfindung können die verschiedenen Ausführungsformen, Bevorzugungen und Bereiche dabei beliebig miteinander kombiniert werden. Ferner können, je nach Ausgestaltung, einzelne Definitionen, Ausführungsformen oder Bereiche entfallen.The present invention will be described below in detail. In the context of this invention, the various embodiments, preferences and areas can be combined as desired. Furthermore, depending on the configuration, individual definitions, embodiments or areas can be omitted.
Sofern sich aus dem Zusammenhang nichts anderes ergibt, sollen die folgenden Definitionen gelten:
- Der Begriff "kohlenwasserstoff-haltige Materialien" bezeichnet natürliche und synthetische Polymere Materialien im weitesten Sinne. Insbesondere synthetische Polymere, einschliesslich Co-Polymere, Blends und Composites. Beispielhaft seine Polymerisate und Polykondensate genannt. Bevorzugt sind Materialien enthaltend oder bestehend aus Polyester (wie PET), Polyolefine (wie PE, PP), Polystyrol, Polyurethan. Gummibasierte Materialien wie nachfolgend beschrieben bilden eine weitere bevorzugte Gruppe von kohlenwasserstoff-haltigen Materialien.
- Der Begriff "gummibasierten Materialien" bezeichnet polymere Materialien mit weichelastischen (gummiartigen) Eigenschaften. Insbesondere betrifft er Materialien, welche natürlichen, naturidentischen oder synthetischen Kautschuk enthalten ("kautschukhaltige Materialien"). Beispielhaft seien kautschukhaltige Formstücke, insbesondere Fahrzeugreifen und zerkleinerte Fahrzeugreifen genannt ("Altreifen").
- Der Begriff "fester Kohlenstoff" bezeichnet das bei der Reaktion entstehende feste Reaktionsprodukt, welches im Wesentlichen aus Kohlenstoff besteht. Die Zusammensetzung und Qualität hängt vom eingesetzten Ausgangsmaterial und den Reaktionsbedingungen ab. Typischerweise enthält der "feste Kohlenstoff" >90 Gew-%, bevorzugt >95 Gew-%, besonders bevorzugt >99 Gew-% Kohlenstoff. Der "feste Kohlenstoff" fällt feinteilig an, typischerweise in Reinheitsgraden und Partikelgrössen, die den Qualitätskriterien von Russ entsprechen.
- Der Begriff "flüchtige Kohlenwasserstoffe" ist allgemein bekannt. Er bezeichnet insbesondere die bei der Reaktion gebildeten, verdampfbaren Kohlenwasserstoffe mit Siedepunkten <500°C (bei Normaldruck). Solche flüchtigen Kohlenwasserstoffe liegen typischerweise als Gemisch verschiedener Verbindungen vor und kann Verunreinigungen wie Wasser, Schwefel- und Stickstoffverbindungen enthalten.
- Der Begriff "inerte Atmosphäre" bezeichnet eine Atmosphäre, die bei gegebenen Bedingungen nicht mit dem Ausgangsmaterial oder den gebildeten Produkten reagiert. Geeignet sind insbesondere sauerstoffarme oder sauerstofffreie Gase, wie Stickstoff, Kohlendioxid oder die bei der Reaktion gebildeten Gase.
- The term "hydrocarbon-containing materials" refers to natural and synthetic polymers materials in the broadest sense. In particular, synthetic polymers, including co-polymers, blends and composites. Exemplary his polymers and polycondensates called. Preference is given to materials containing or consisting of polyester (such as PET), polyolefins (such as PE, PP), polystyrene, polyurethane. Rubber based materials as described below form another preferred group of hydrocarbonaceous materials.
- The term "rubber-based materials" refers to polymeric materials having soft elastic (rubbery) properties. In particular, it relates to materials which contain natural, nature-identical or synthetic rubber ("rubber-containing materials"). Examples include rubber-containing fittings, in particular vehicle tires and crushed vehicle tires called ("old tires").
- The term "solid carbon" refers to the solid reaction product formed in the reaction which consists essentially of carbon. The composition and quality depends on the starting material used and the reaction conditions. Typically, the "solid carbon"contains> 90% by weight, preferably> 95% by weight, more preferably> 99% by weight of carbon. The "solid carbon" is finely divided, typically in purities and particle sizes that meet Russ's quality criteria.
- The term "volatile hydrocarbons" is well known. It refers in particular to the vaporizable hydrocarbons formed in the reaction with boiling points <500 ° C (at normal pressure). Such volatile hydrocarbons are typically present as a mixture of various compounds and may contain impurities such as water, sulfur and nitrogen compounds.
- The term "inert atmosphere" refers to an atmosphere that does not react with the starting material or products under given conditions. Particularly suitable are oxygen-poor or oxygen-free gases, such as nitrogen, carbon dioxide or the gases formed during the reaction.
In einem ersten Aspekt betrifft die Erfindung daher ein kontinuierliches Verfahren zur Pyrolyse von kohlenwasserstoff-haltigen Materialien unter Bildung von festem Kohlenstoff (insbesondere Russ) und flüchtigen Kohlenwasserstoffen, dadurch gekennzeichnet, dass a) die kohlenwasserstoff-haltige Materialien unter inerter Atmosphäre, bei Normal- oder Unterdruck in einem Rohrreaktor welcher Mittel zur Förderung und Mischung enthält, einer Zeit- und Temperaturgestuften Behandlung unterworfen werden; b) die im Schritt a) gebildeten flüchtigen Kohlenwasserstoffe an einer oder mehreren Stellen entlang der Längsachse des besagten Rohrreaktors entnommen werden; c) der im Schritt a) gebildete feste Kohlenstoff nach Abkühlung am Ende des besagten Rohrreaktors entnommen wird.In a first aspect , therefore, the invention relates to a continuous process for the pyrolysis of hydrocarbonaceous materials to form solid carbon (especially soot) and volatile hydrocarbons, characterized in that a) the hydrocarbonaceous materials under inert atmosphere, at normal or Underpressure in a tubular reactor containing means for conveying and mixing, subjected to a time and temperature graded treatment; b) the volatile hydrocarbons formed in step a) are removed at one or more points along the longitudinal axis of said tubular reactor; c) the solid carbon formed in step a) is removed after cooling at the end of said tubular reactor.
Ohne sich an eine Theorie gebunden zu fühlen, wird davon ausgegangen, dass beim erfindungsgemässen Verfahren die Umsetzung des Ausgangsmaterials in den Schritten Schwelung - Veredelung - Nachbehandlung erfolgt. Während der Schwelung werden im wesentlichen ggf. vorliegende Disulfid-Brücken im Ausgangsmaterial gebrochen sowie leicht flüchtige Komponenten ausgetrieben. Während der Veredelung werden höher siedende Kohlenwasserstoffe entfernt und die Bildung des festen Kohlenstoffs setzt ein. Während der Veredelung wird die Struktur des gebildeten festen Kohlenstoffs verbessert und dieser auf eine lagerfähige Temperatur abgekühlt.Without being bound to any theory, it is assumed that in the process according to the invention the reaction of the starting material takes place in the steps of smelting - finishing - aftertreatment. During the carbonization essentially existing disulfide bridges are broken in the starting material and expelled volatile components. During refining, higher boiling hydrocarbons are removed and the formation of solid carbon begins. During refining, the structure of the solid carbon formed is improved and cooled to a storable temperature.
Das erfindungsgemässe Verfahren ist kontinuierlich ausgelegt, d.h. Ausgangsmaterial wird dem Rohrreaktor an einem Ende ständig zugeführt und Produkte (fester Kohlenstoff und flüchtige Kohlenwasserstoffe) werden dem Rohreaktor kontinuierlich entnommen. Vorteilhaft wird das Ausgangsmaterial zerkleinert zugeführt.The inventive method is designed continuously, i. Starting material is constantly fed to the tubular reactor at one end and products (solid carbon and volatile hydrocarbons) are continuously withdrawn from the tube reactor. Advantageously, the starting material is fed comminuted.
Das erfindungsgemässe Verfahren wird Zeitgestuft durchgeführt, d.h. die Verweilzeit der Materialien in den Verschiedenen Schritten vorbestimmt und an die jeweilige Situation angepasst ist. Die Verweilzeit kann durch die Ausgestaltung des Rohrreaktors, wie dessen Dimenisionierung oder die Gestaltung einer Förderschnecke festgelegt bzw. Variiert werden.The method according to the invention is carried out in a time scale, i. the residence time of the materials in the various steps is predetermined and adapted to the particular situation. The residence time can be determined or varied by the design of the tubular reactor, such as its dimenization or the design of a screw conveyor.
Das erfindungsgemässe Verfahren ist besonders geeignet zum Recyclieren von gummibasierten Materialien, insbesondere gummibasierten, vulkanisierten Materialien bspw. Altreifen. Das erfindungsgemässe Verfahren ist ferner besonders geeignet zum Recyclieren kohlenwasserstoff-haltiger Materialien, wie PS-Formstücken.The process according to the invention is particularly suitable for recycling rubber-based materials, in particular rubber-based, vulcanized materials, for example old tires. The inventive method is also particularly suitable for recycling hydrocarbon-containing materials, such as PS fittings.
Als vorteilhaft beim erfindungsgemässen Verfahren ist der entstehende Produktmix aus flüchtigen Kohlenwasserstoffen und festem Kohlenstoff anzusehen. Ferner ist als vorteilhaft zu werten, dass das erfindungsgemässe Verfahren in Bezug auf weitere Komponenten sehr flexibel ist. So ist das verfahren mit und ohne den Zusatz von Katalysatoren sowie mit und ohne den Zusatz von anderen Hilfsstoffen durchführbar.An advantage of the process according to the invention is the resulting product mix of volatile hydrocarbons and solid carbon. Furthermore, it is to be regarded as advantageous that the method according to the invention is very flexible with regard to further components. Thus, the method is feasible with and without the addition of catalysts and with and without the addition of other auxiliaries.
Die Verweilzeit im Rohrreaktor kann in einem breiten Bereich variiert werden und kann im Prinzip in einfachen Reihenversuchen bestimmt werden. Als vorteilhaft haben sich Verweilzeiten von 0.5 - 24 Stunden, bevorzugt von 4 - 10 Stunden erwiesen. Die Verweilzeiten können durch das Mittel zur Förderung und die Dimensionierung des Reaktors eingestellt werden.The residence time in the tubular reactor can be varied within a wide range and can in principle be determined in simple series experiments. Residence times of from 0.5 to 24 hours, preferably from 4 to 10 hours, have proved to be advantageous. The residence times can be adjusted by the means for conveying and sizing the reactor.
Die Reaktionstemperaturen im Reaktor können in einem breiten Bereich variiert werden. Die Beheizung des Reaktors erfolgt z.B. allotherm, bevorzugt mittels eines umlaufenden Trägeröls. Die realisierten Temperaturen liegen im Bereich zwischen 20°C (Raumtemperatur) und ca. 1100°C (bevorzugt: 20 - 500°C). Die Umsetzung im Reaktor erfolgt "temperaturgestuft", d.h. die Temperatur wird entlang der Reaktorlängsachse variiert. Die Temperaturen werden dabei so gewählt, dass die Schritte "Schwelung", "Veredelung" und "Nachbehandlung" in aufeinander folgenden Zonen des Rohrreaktors ablaufen. Dabei wird die Temperatur so gewählt, dass die Veredelung bei höheren Temperaturen und die Nachbehandlung bei tieferen Temperaturen als die Schwelung erfolgt. Die folgenden Temperaturbereiche haben sich als vorteilhaft erwiesen: Für die Schwelung bis 500°C (bevorzugt: 350°C); für die Veredelung bis 1100°C (bevorzugt: 450°C). Die Nachbehandlung wird in einer vorteilhaften Ausgestaltung so geführt, dass das feste Reaktionsprodukt bei maximal 100°C den Reaktor verlässt. Geeignete Reaktionstemperaturen hängen naturgemäss mit dem (Unter)druck der Anlage zusammen, wobei ein geringerer Druck in der Anlage auch niedrigere Reaktionstemperaturen ermöglicht. Innerhalb der einzelnen Reaktionszonen (Schwelung, Veredelung, Nachbehandlung) kann ebenfalls ein Temperaturprofil aufgeprägt werden, bspw. schwankend zwischen 80 und 300°C bei der Schwelung und kontinuierlich sinkend von 400°C auf 80°C in der Nachbehandlung.The reaction temperatures in the reactor can be varied within a wide range. The heating of the reactor takes place e.g. allothermic, preferably by means of a circulating carrier oil. The temperatures realized are in the range between 20 ° C (room temperature) and about 1100 ° C (preferably: 20 - 500 ° C). Reaction in the reactor is "temperature-graded", i. the temperature is varied along the reactor longitudinal axis. The temperatures are selected so that the steps "carbonization", "finishing" and "post-treatment" occur in successive zones of the tubular reactor. The temperature is chosen so that the refining takes place at higher temperatures and the aftertreatment at lower temperatures than the carbonization. The following temperature ranges have proven to be advantageous: For the carbonization to 500 ° C (preferably: 350 ° C); for refining up to 1100 ° C (preferably: 450 ° C). The aftertreatment is conducted in an advantageous embodiment so that the solid reaction product leaves the reactor at a maximum of 100.degree. Suitable reaction temperatures are naturally related to the (sub) pressure of the plant, wherein a lower pressure in the system also allows lower reaction temperatures. Within the individual reaction zones (carbonization, refinement, aftertreatment), a temperature profile can likewise be impressed, for example, fluctuating between 80 and 300 ° C. during the carbonization and continuously decreasing from 400 ° C. to 80 ° C. in the after-treatment.
Der Reaktionsdruck im Reaktor kann in einem weiteren Bereich variiert werden. Als geeigneter Reaktionsdruck hat sich der Bereich von -100 - +800 mbar, insbesondere 400 - 600 mbar erwiesen. Der Reaktionsdruck kann durch Vakuumpumpen erzeugt werden, welche mit den Stellen zur Entnahme der flüssigen Kohlenwasserstoffe kommunizieren.The reaction pressure in the reactor can be varied in a wider range. As a suitable reaction pressure, the range of -100 - +800 mbar, in particular 400 - 600 mbar has been found. The reaction pressure can be generated by vacuum pumps, which with the Points communicate to remove the liquid hydrocarbons.
In einem zweiten Aspekt betrifft die Erfindung eine Anlage zur Pyrolyse von gummibasierten Materialien, umfassend einen oder mehrere Rohrreaktoren wobei diese Rohrreaktoren ausgestattet sind i) mit Mitteln zur Zufuhr von zerkleinerten gummibasierten Materialien; ii) mit Mitteln zur Förderung und Mischung besagter gummibasierter Materialien durch den Rohrreaktor; iii) mit Mitteln zur Entnahme gebildeter gasförmiger Kohlenwasserstoffe angeordnet entlang der Längsachse des Rohrreaktors; iv) mit Mitteln zur Entnahme gebildeter fester Kohlenstoffe; v) mit Mitteln zur indirekten temperäturgestuften Beheizung und wobei besagte Rohrreaktoren so ausgelegt sind, dass sie unter inerter Atmosphäre, bei Normal- oder Unterdruck betrieben werden können.In a second aspect , the invention relates to a plant for the pyrolysis of rubber-based materials, comprising one or more tubular reactors, these tubular reactors being equipped with i) means for supplying comminuted rubber-based materials; ii) means for conveying and mixing said rubber-based materials through the tubular reactor; iii) means for removing formed gaseous hydrocarbons disposed along the longitudinal axis of the tubular reactor; (iv) means of removal of solid carbon formed; v) means for indirect temperaturgraduften heating and wherein said tubular reactors are designed so that they can be operated under inert atmosphere, at normal or negative pressure.
Geeignete Reaktoren sind an sich bekannt, bspw. Drehrohröfen oder Schneckenreaktoren. Geeignet sind insbesondere Schneckenreaktoren. Solche Reaktoren können Leitbleche aufweisen, welche eine Förderung und Mischung bewirken. Im Fall von Schneckenreaktoren erfolgt die Mischung und Förderung ausschliesslich oder zusätzlich durch die zentrale Förderschnecke. Die Steigung der Schnecke kann über die gesamte Länge konstant sein oder variieren, um so die Verweilzeit anzupassen. Die Zufuhr des Ausgangsmaterials und die Entnahme des festen Kohlenstoffes kann durch gängige Vorrichtungen, wie Zyklo- und anderen Anlagen erfolgen. Die Entnahme der flüchtigen Kohlenwasserstoffe kann ebenfalls durch gängige Vorrichtungen, bspw. über Ventile, welche mit Kondensatoren und Vakuumpumpen kommunizieren, erfolgen. Geeignete Vorrichtungen und Anlagenteile sind im Stand der Technik bekannt und können vom Fachmann ausgewählt und ausgelegt werden. Vorrichtungen zur indirekten temperaturgestuften Beheizung von Rohrreaktoren sind allgemein bekannt. Möglich ist bspw. eine Gas und elektrische Beheizung. Als vorteilhaft hat sich die indirekte Beheizung mittels einer Trägerflüssigkeit erwiesen, wobei der Reaktor doppelwandig ausgeführt wird. Eine Beheizung kann so ausgelegt werden, dass sie segmentweise angesteuert wird um einen optimalen Verfahrensablauf sicher zu stellen. Eine indirekte Beheizung ist der direkten Beheizung vorzuziehen.Suitable reactors are known per se, for example rotary kilns or screw reactors. Particularly suitable are screw reactors. Such reactors may have baffles which cause a promotion and mixing. In the case of screw reactors, mixing and conveying takes place exclusively or additionally through the central auger. The pitch of the screw can be constant over the entire length or vary, so as to adjust the residence time. The supply of the starting material and the removal of the solid carbon can be done by common devices, such as cyclo and other equipment. The removal of the volatile hydrocarbons can also be done by conventional devices, for example. Via valves that communicate with capacitors and vacuum pumps. Suitable devices and equipment are known in the art and may be selected and designed by those skilled in the art. Devices for the indirect temperature-controlled heating of tubular reactors are well known. Is possible for example, a gas and electric heating. The indirect heating by means of a carrier liquid has proved to be advantageous, the reactor being designed to be double-walled. A heating can be designed so that it is controlled segment by segment to ensure optimal process flow. Indirect heating is preferable to direct heating.
In einer vorteilhaften-Ausführungsform der erfindungsgemässen Pyrolyseanlage ist der Rohrreaktor waagerecht oder nahezu waagerecht (d.h. +/-10°) angeordnet. Eine solche Anordnung hat gegenüber einer senkrechten Anordnung den Vorteil, dass ein kontrollierter homogenisierter Ablauf erreicht wird.In an advantageous embodiment of the pyrolysis plant according to the invention, the tubular reactor is arranged horizontally or nearly horizontally (i.e., +/- 10 °). Such an arrangement has the advantage over a vertical arrangement that a controlled homogenized process is achieved.
In einer weiteren vorteilhaften Ausführungsform der erfindungsgemässen Pyrolyseanlage ist der Rohrreaktor unterteilt in drei oder mehrere miteinander verbundenen Teilreaktoren. Bevorzugt erfolgt die Unterteilung in drei Teilreaktoren. In dieser Ausführungsform wird im ersten Teilreaktor die Schwelung, im zweiten Teilreaktor die Veredelung und im dritten Teilreaktor die Nachbehandlung durchgeführt. In dieser Ausführungsform sind nur im ersten und zweiten Teilreaktor Mittel zur Entnahme flüchtiger Kohlenwasserstoffe vorgesehen. Ferner enthält nur der erste Teilreaktor Mittel zur Zufuhr von zerkleinerten gummibasierten Materialien und nur der dritte Teilreaktor Mittel zur Entnahme gebildeter fester Kohlenstoffe.In a further advantageous embodiment of the inventive pyrolysis plant, the tubular reactor is subdivided into three or more interconnected partial reactors. The subdivision preferably takes place in three partial reactors. In this embodiment, the carbonization is carried out in the first part reactor, the refining in the second part reactor and the aftertreatment in the third part reactor. In this embodiment, means for removing volatile hydrocarbons are provided only in the first and second part of the reactor. Further, only the first part reactor contains means for feeding crushed rubber-based materials and only the third part reactor means for removing formed solid carbons.
In einer weiteren vorteilhaften Ausführungsform der erfindungsgemässen Pyrolyseanlage ist der Rohrreaktor unterteilt in drei oder mehr miteinander verbundenen Teilreaktoren (Phasen), wobei diese Teilreaktoren untereinander angeordnet sind, derart, dass die Zufuhr am oben gelegenen Teilreaktor und die Entnahme am unten gelegenen Teilreaktor erfolgt.In a further advantageous embodiment of the pyrolysis plant according to the invention, the tubular reactor is subdivided into three or more interconnected partial reactors (phases), these partial reactors being arranged one below the other, such that the feed takes place at the upper part reactor and the removal takes place at the lower part reactor.
Der erfindungsgemässen Pyrolyseanlage sind weitere Nebenanlagen zugeordnet um das hier beschriebene Verfahren durchzuführen. Dabei sind insbesondere zu nennen: Vorrichtungen zur Erzeugung des Gewünschten Reaktionsdruckes (Über-, Unter-, Normal-druck); Vorrichtungen zur Isolierung und Trennung der erzeugten flüssigen Kohlenwasserstoffe; Vorratsbehälter für das Ausgangsmaterial; Vorratsbehälter für den erzeugten festen Kohlenstoff. Diese einzelnen Vorrichtungen sind an sich bekannt und können vom Fachmann ausgelegt und angepasst werden.The pyrolysis plant according to the invention are assigned further secondary plants in order to carry out the process described here. Particular mention should be made of: devices for generating the desired reaction pressure (over-, under-, normal pressure); Apparatus for isolating and separating the generated liquid hydrocarbons; Storage container for the starting material; Reservoir for the generated solid carbon. These individual devices are known per se and can be designed and adapted by the person skilled in the art.
Weiterhin können in der Pyrolyseanlage Vorrichtungen zur Rückgewinnung von Energie (z.B. Wärmetauscher) vorgesehen werden. Die Energie zum Beheizen der Anlage kann aus dem gewonnenen flüchtigen Kohlenwasserstoffen bezogen werden.Further, in the pyrolysis plant, means for recovering energy (e.g., heat exchangers) may be provided. The energy for heating the plant can be obtained from the recovered volatile hydrocarbons.
Die einzelnen im Zusammenhang mit der erfindungsgemässen Pyrolyseanlage beschriebenen Anlagenteile (Reaktor, Nebenanlagen, ...) können jeweils einfach oder mehrfach ausgeführt sein, um so die die Betriebssicherheit und/oder Flexibilität zu erhöhen. Beispielsweise ist ein paralleler Betrieb mehrerer Reaktoren möglich. Ebenso können die genannten Teilreaktoren nochmals in einzelne Phasen unterteilt werden. Solche Variationen sind von der vorliegenden Erfindung mit umfasst.The individual plant parts described in connection with the pyrolysis plant according to the invention (reactor, ancillary plants,...) Can each be designed to be single or multiple, so as to increase the operational safety and / or flexibility. For example, a parallel operation of several reactors is possible. Likewise, the sub-reactors mentioned can be divided into individual phases again. Such variations are included in the present invention.
Weitere Vorteile und Anwendungen der Erfindung ergeben sich aus der nun folgenden Beschreibung anhand der
Eine entsprechende Anlage für die Verarbeitung von kohlenwasserstoff-haltigen Materialien gleicht dem in
In einer Anlage gemäss
Claims (9)
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| EP08019151A EP2184334A1 (en) | 2008-10-31 | 2008-10-31 | Method and device for recycling materials containing hydrocarbons |
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| EP08019151A EP2184334A1 (en) | 2008-10-31 | 2008-10-31 | Method and device for recycling materials containing hydrocarbons |
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| WO2013187788A2 (en) | 2012-06-12 | 2013-12-19 | DAGAS Sp. z.o.o. | The method of conducting a pyrolysis process of plastic waste and/or rubber waste and/or organic waste and the installation to carry out this method |
| CN106701131A (en) * | 2015-11-13 | 2017-05-24 | 张瑞永 | Continuous thermal desorption and cracking equipment with three-section type reaction furnace system |
| CN112973578A (en) * | 2021-03-16 | 2021-06-18 | 江西诺邦生物科技有限公司 | Disinfectant production is with low temperature dry distillation extraction element |
| IT202100033044A1 (en) | 2021-12-30 | 2023-06-30 | Versalis Spa | PROCEDURE FOR THE PYROLYSIS OF SUBSTANTIALLY PLASTIC MATERIAL OF NON-CONSTANT COMPOSITION, RELATED REACTOR, APPARATUS AND PRODUCT OBTAINED |
| IT202100033059A1 (en) | 2021-12-30 | 2023-06-30 | Versalis Spa | METHOD FOR MONITORING A CONTROL PARAMETER ON A SUBSTANTIALLY PLASTIC MATERIAL, RELATED APPARATUS AND PYROLYSIS PROCESS WHICH USES SAID METHOD |
| IT202100033053A1 (en) | 2021-12-30 | 2023-06-30 | Versalis Spa | PYROLYSIS PROCESS FOR THE PRODUCTION OF A PYROLYSIS OIL SUITABLE FOR CLOSED LOOP RECYCLING, RELATED APPARATUS, PRODUCT AND USE THEREOF |
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