EP0132612A1 - Process for the production of liquid hydrocarbons - Google Patents

Process for the production of liquid hydrocarbons Download PDF

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Publication number
EP0132612A1
EP0132612A1 EP84107378A EP84107378A EP0132612A1 EP 0132612 A1 EP0132612 A1 EP 0132612A1 EP 84107378 A EP84107378 A EP 84107378A EP 84107378 A EP84107378 A EP 84107378A EP 0132612 A1 EP0132612 A1 EP 0132612A1
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Prior art keywords
solvent
liquid hydrocarbons
pressure
waste
bar
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German (de)
French (fr)
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EP0132612B1 (en
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Hubert Dr. Coenen
Rainer Hagen
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Fried Krupp AG
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Fried Krupp AG
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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
    • C10G1/10—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 a process for the production of liquid hydrocarbons from used tires, cable, polyethylene and / or polypropylene waste.
  • the liquid hydrocarbons that are produced by this process include alkanes, cycloalkanes and aromatics, which have a boiling point of 20 to about 350 ° C and whose molecules contain 5 to about 30 carbon atoms.
  • the liquid hydrocarbons produced by the process can contain organic sulfur and chlorine compounds.
  • the liquid hydrocarbons can be used as heating oil or for blending heating oil or as a chemical raw material.
  • Used tires belong to the waste products of the automotive industry and consist of one or more rubber compounds, a bead ring and a fabric.
  • the rubber mixture contains rubber, soot, oils and resins, zinc oxide, vulcanization accelerators, anti-aging agents and sulfur.
  • the rubber is composed of chain-like macromolecules which interengage 29lun g en and are additionally linked by sulfur atoms.
  • the tires are manufactured using natural rubber and synthetic rubber, with the synthetic rubbers being polymerized by the polymerization of isoprene, butadiene, chlorobutadiene and the copolymerization of butadiene Styrene or iso-butene can be produced with isoprene.
  • the carbon black serves as a filler and to improve the rubber properties, because it forms a very close bond with the rubber during tire manufacture.
  • the oils and resins act as plasticizers and improve the processability of the rubber mixture.
  • the zinc oxide serves as a filler and as an activator for the vulcanization accelerators.
  • the bead ring stabilizes the tire against radial forces and is made of steel wire or steel cable.
  • the fabric in the tire consists of synthetic fibers or steel wires.
  • the weight proportion of the rubber compound in the old tires is usually between 75 and 80%.
  • Cable waste arises from the processing and renewal of cables that consist of a metallic electrical conductor, a plastic insulation and a plastic jacket and are used for the transmission of messages or electrical energy.
  • Polyethylene and polypropylene waste is produced in the manufacture and processing of plastics and accumulates there in a relatively pure form. These pure wastes can be processed into liquid hydrocarbons by the process according to the invention, while the polyethylene and polypropylene wastes contained in the household waste cannot be fed to the process according to the invention, since they are difficult to separate from the other plastics contained in the household waste, in particular polyvinyl chloride.
  • Polyethylene and polypropylene are produced by polymerizing ethene or propene and, in addition to the polymers, also contain fillers.
  • used tires are usually removed by incineration, which takes place either in specially designed ovens or in waste incineration plants.
  • the exhaust gases from the incineration plants, in which used tires are burned, must be dedusted and desulphurized, in particular due to the high ZnO and S0 2 content.
  • used tires can be removed by pyrolysis processes and processed into reusable products.
  • the pyrolysis of old tires produces a pyrolysis coke, a flammable pyrolysis gas that mostly serves to cover the energy requirements of the pyrolysis process, and a pyrolysis oil that is used as heating oil.
  • the polyethylene and polypropylene waste is mostly incinerated.
  • the cable waste is usually deposited in a landfill.
  • the combustion processes have the disadvantage that they are difficult to carry out due to the nature of the old tires and plastic waste and that the combustion exhaust gases have to be cleaned using complex processes.
  • the disadvantage of the pyrolysis process is that a very large part of the organic compounds, which are valuable per se, is coked and thus converted into a less valuable state.
  • the invention has for its object to provide a method with which old tires, cable, polyethylene and / or polypropylene waste can be removed without damage and processed into valuable reusable liquid hydrocarbons, the formation of gaseous and coke-like decomposition products should be largely avoided.
  • the object underlying the invention is achieved in that the shredded old tires, cable, polyethylene and / or polypropylene waste at a temperature of 150 to 500 ° C and a pressure of 20 to 300 bar with a liquid at 1 bar and 20 ° C.
  • Solvents are treated, that the solvent phase laden with the liquid hydrocarbons is separated off and broken down into its constituents by lowering the pressure or by lowering the pressure and temperature, and that the solvent is circulated.
  • the polymer molecules are cleaved under the influence of the high pressure and the high temperature, liquid hydrocarbons in particular having about 5 to 30 carbon atoms being formed without any noticeable coking occurring.
  • the liquid hydrocarbons are absorbed and removed comparatively quickly by the solvent.
  • the plasticizers and anti-aging agents are released from the solvent and only slightly decomposed under the influence of pressure and temperature.
  • the carbon black, the fillers, the metals and the fabric remain as a solid, insoluble residue, which also contains the small amounts of coking products that may arise during the process.
  • the process has the advantage that the majority of the organic compounds present in the waste materials are converted into liquid reusable hydrocarbons.
  • the process according to the invention can be carried out particularly successfully if gasoline, benzene, toluene, xylene, ethyl bezole and / or water is used as the solvent, the weight ratio of the waste materials to the solvent being between 1: 3 and 1:30.
  • the organic solvents to be used according to the invention have an optimal dissolving power for the liquid hydrocarbons formed, while the water to be used according to the invention provides products with a lower molecular weight.
  • the pressure and temperature are reduced in several stages and that the constituents of the loaded solvent phase are obtained in several fractions. This procedure allows the liquid hydrocarbons to be broken down into fractions suitable for various purposes.
  • a suitable fraction can be returned to the process according to the invention as a solvent.
  • the reactor 1 there is a bed of shredded old tires, cable, polyethylene and / or polypropylene waste.
  • the sulfur and chlorine content of the old tires is advantageously diluted by the polyethylene and polypropylene waste.
  • the solvent is heated in the heat exchanger 6 to the process temperature of 150 to 500 ° C and brought to a process pressure of 20 to 300 bar by the compressor 5 and conveyed into the reactor 1.
  • the solvent flows through the reactor 1 and removes the liquid hydrocarbons formed in the reactor 1 and the gaseous reaction products formed in a small amount.
  • the solvent phase laden with the liquid hydrocarbons is removed, expanded in the expansion valve 2, cooled in the heat exchanger 7, freed from the gaseous reaction products in the separation vessel 8 and then fed to the distillation column 3.
  • the higher-boiling hydrocarbons are taken off at the bottom of the distillation column 3, while the low-boiling hydrocarbons are taken off together with the solvent at the top of the distillation column 3.
  • the low-boiling fraction is then cooled in the heat exchanger 9 and, after liquefaction, is returned from the compressor 5 to the reactor 1. It is possible to carry out the expansion and cooling of the solvent phase laden with the liquid hydrocarbons in several stages, which is not shown in the drawing.
  • the solid residue which contains the insoluble constituents of the waste materials used and the coking products is removed from the reactor 1.
  • Used tires and cable waste were shredded so that particles with an edge length of approx. 2 cm were obtained. 602 g of these particles were treated with toluene at 350 ° C. and 80 bar for 4 hours.
  • the solvent phase laden with the liquid hydrocarbons was then separated off and let down to 10 bar and cooled to 310 ° C.
  • a separation was carried out into a toluene-containing liquid phase and into a gas phase, which mainly consisted of toluene.
  • the liquid phase which contained about 85% toluene, was distilled to remove the toluene and the low-boiling liquid hydrocarbons after relaxing to atmospheric pressure.
  • the solid residue obtained after the toluene treatment was powdery and mainly consisted of carbon black, ZnO, other tire fillers and pieces of metal. Its sulfur content was 2.37%, while the sulfur content of the particles used was 1.70%.
  • 12 kg of toluene were used for 1 kg of starting material, and these can largely be recovered and recycled.
  • the metals present in the starting material were found in the residue in unchanged form. This is an advantage over pyrolysis carried out at higher temperatures. There, the metals present in the old tires and cable waste melt together in an undesirable manner, while in the process according to the invention they can be reduced at a low rate with mechanical separation processes! Energy expenditure can be sorted out and recycled.

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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)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

A process for the production of liquid hydrocarbons from old tires, cable wastes, polyethylene wastes and/or polypropylene wastes, by which the waste products, in pulverized form, are treated at a temperature of 150 DEG to 500 DEG C. and a pressure 20 to 300 bar with a solvent which is liquid at 1 bar and 20 DEG C. to form a solvent phase charged with liquid hydrocarbons and a residue phase. The charged solvent phase is separated from the residue, and the separated charged solvent phase is resolved into its components by lowering of pressure and/or temperature, and by distillation.

Description

Verfahren zur Herstellung flüssiger KohlenwasserstoffeProcess for the production of liquid hydrocarbons

Die Erfindung bezieht sich auf ein Verfahren zur Herstellung flüssiger Kohlenwasserstoffe aus Altreifen, Kabel-, Polyäthylen- und/oder Polypropylenabfällen. Zu den flüssigen Kohlenwasserstoffen, die nach diesem Verfahren hergestellt werden, gehören Alkane, Cycloalkane und Aromaten, welche einen Siedepunkt von 20 bis ca. 350°C haben und deren Moleküle 5 bis ca. 30 Kohlenstoffatome enthalten. Die nach dem Verfahren hergestellten flüssigen Kohlenwasserstoffe können je nach dem Schwefel-und Chlorgehalt der Altreifen organische Schwefel-und Chlorverbindungen enthalten. Die flüssigen Kohlenwasserstoffe können als Heizöl bzw. zum Verschneiden von Heizöl oder als Chemierohstoff verwendet werden.The invention relates to a process for the production of liquid hydrocarbons from used tires, cable, polyethylene and / or polypropylene waste. The liquid hydrocarbons that are produced by this process include alkanes, cycloalkanes and aromatics, which have a boiling point of 20 to about 350 ° C and whose molecules contain 5 to about 30 carbon atoms. Depending on the sulfur and chlorine content of the old tires, the liquid hydrocarbons produced by the process can contain organic sulfur and chlorine compounds. The liquid hydrocarbons can be used as heating oil or for blending heating oil or as a chemical raw material.

Altreifen gehören zu den Abfallprodukten des Kraftfahrzeuggewerbes und bestehen aus einer oder mehreren Gummimischungen, einem Wulstring und einem Gewebe. Die Gummimischung enthält Kautschuk, Ruß, öle und Harze, Zinkoxid, Vulkanisationsbeschleuniger, Alterungsschutzmittel und Schwefel. Der Kautschuk besteht aus kettenförmigen Makromolekülen, die ineinander verschlungen und zusätzlich durch Schwefelatome verknüpft sind. Die Reifenherstellung erfolgt unter Verwendung von Naturkautschuk und synthetischem Kautschuk, wobei die synthetischen Kautschuksorten durch Polymerisation von Isopren, Butadien, Chlorbutadien und Copolymerisation von Butadien mit Styrol oder iso-Buten mit Isopren erzeugt werden. Der Ruß dient als Füllstoff und zur Verbesserung der Kautschukeigenschaften, denn er geht bei der Reifenherstellung mit dem Kautschuk eine sehr enge Bindung ein. Die öle und Harze wirken als Weichmacher und verbessern die Verarbeitbarkeit der Kautschukmischung. Das Zinkoxid dient als Füllstoff und als Aktivator für die Vulkanisationsbeschleuniger. Der Wulstring stabilisiert den Reifen gegen radiale Kräfte und besteht aus Stahldraht oder Stahlseil. Das im Reifen vorhandene Gewebe besteht aus Kunstfasern oder Stahldrähten. Der Gewichtsanteil der Gummimischung liegt in den Altreifen in der Regel zwischen 75 und 80%.Used tires belong to the waste products of the automotive industry and consist of one or more rubber compounds, a bead ring and a fabric. The rubber mixture contains rubber, soot, oils and resins, zinc oxide, vulcanization accelerators, anti-aging agents and sulfur. The rubber is composed of chain-like macromolecules which interengage verschlun g en and are additionally linked by sulfur atoms. The tires are manufactured using natural rubber and synthetic rubber, with the synthetic rubbers being polymerized by the polymerization of isoprene, butadiene, chlorobutadiene and the copolymerization of butadiene Styrene or iso-butene can be produced with isoprene. The carbon black serves as a filler and to improve the rubber properties, because it forms a very close bond with the rubber during tire manufacture. The oils and resins act as plasticizers and improve the processability of the rubber mixture. The zinc oxide serves as a filler and as an activator for the vulcanization accelerators. The bead ring stabilizes the tire against radial forces and is made of steel wire or steel cable. The fabric in the tire consists of synthetic fibers or steel wires. The weight proportion of the rubber compound in the old tires is usually between 75 and 80%.

Kabelabfälle entstehen bei der Verarbeitung und Erneuerung von Kabeln, die aus einem metallischen elektrischen Leiter, einer Kunststoffisolierung sowie einem Kunststoffmantel bestehen und zur Übertragung von Nachrichten oder elektrischer Energie verwendet werden.Cable waste arises from the processing and renewal of cables that consist of a metallic electrical conductor, a plastic insulation and a plastic jacket and are used for the transmission of messages or electrical energy.

Polyäthylen- und Polypropylenabfälle entstehen bei der Kunststoffherstellung und Kunststoffverarbeitung und fallen dort in verhältnismäßig reiner Form an. Diese reinen Abfälle können nach dem erfindungsgemäßen Verfahren zu flüssigen Kohlenwasserstoffen verarbeitet werden, während die im Hausmüll enthaltenen Polyäthylen- und Polypropylenabfälle dem erfindungsgemäßen Verfahren nicht zugeführt werden können, da sie nur schwer von den im Hausmüll enthaltenen anderen Kunststoffen, insbesondere Polyvinylchlorid, getrennt werden können. Polyäthylen und Polypropylen werden durch Polymerisation von Äthen bzw. Propen erzeugt und enthalten neben den Polymerisaten insbesondere noch Füllstoffe.Polyethylene and polypropylene waste is produced in the manufacture and processing of plastics and accumulates there in a relatively pure form. These pure wastes can be processed into liquid hydrocarbons by the process according to the invention, while the polyethylene and polypropylene wastes contained in the household waste cannot be fed to the process according to the invention, since they are difficult to separate from the other plastics contained in the household waste, in particular polyvinyl chloride. Polyethylene and polypropylene are produced by polymerizing ethene or propene and, in addition to the polymers, also contain fillers.

Die schadlose Beseitigung der Altreifen ist schwierig und teuer. Altreifen werden heute in der Regel durch Verbrennung beseitigt, was entweder in besonders konstruierten öfen oder in Müllverbrennungsanlagen erfolgt. Die Abgase der Verbrennungsanlagen, in denen Altreifen verbrannt werden, müssen insbesondere wegen des hohen ZnO- und S02-Gehalts entstaubt und entschwefelt werden. Außerdem ist bekannt, daß Altreifen durch Pyrolyseverfahren beseitigt und zu wiederverwendbaren Produkten verarbeitet werden können. Bei der Pyrolyse von Altreifen entsteht ein Pyrolysekoks, ein brennbares Pyrolysegas, das meist zur Deckung des Eigenenergiebedarfs des Pyrolyseverfahrens dient, und ein Pyrolyseöl, das als Heizöl eingesetzt wird. Die Polyäthylen- und Polypropylenabfälle werden meistens verbrannt. Die Kabelabfälle werden üblicherweise auf einer Mülldeponie abgelagert.It is difficult and expensive to remove used tires without damage. Today, used tires are usually removed by incineration, which takes place either in specially designed ovens or in waste incineration plants. The exhaust gases from the incineration plants, in which used tires are burned, must be dedusted and desulphurized, in particular due to the high ZnO and S0 2 content. It is also known that used tires can be removed by pyrolysis processes and processed into reusable products. The pyrolysis of old tires produces a pyrolysis coke, a flammable pyrolysis gas that mostly serves to cover the energy requirements of the pyrolysis process, and a pyrolysis oil that is used as heating oil. The polyethylene and polypropylene waste is mostly incinerated. The cable waste is usually deposited in a landfill.

Die Verbrennungsverfahren haben den Nachteil, daß sie wegen der Beschaffenheit der Altreifen und Kunststoffabfälle nur schwierig durchführbar sind und daß die Verbrennungsabgase mit aufwendigen Verfahren gereinigt werden müssen. Der Nachteil der Pyrolyseverfahren besteht darin, daß ein sehr großer Teil der an sich wertvollen organischen Verbindungen verkokt und damit in einen weniger wertvollen Zustand überführt wird.The combustion processes have the disadvantage that they are difficult to carry out due to the nature of the old tires and plastic waste and that the combustion exhaust gases have to be cleaned using complex processes. The disadvantage of the pyrolysis process is that a very large part of the organic compounds, which are valuable per se, is coked and thus converted into a less valuable state.

Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren zu schaffen, mit dem Altreifen, Kabel-,Polyäthylen- und/oder Polypropylenabfälle schadlos beseitigt und zu wertvollen wiederverwendbaren flüssigen Kohlenwasserstoffen verarbeitet werden können, wobei das Entstehen von gasförmigen und koksartigen Zersetzungsprodukten weitgehend vermieden werden soll.The invention has for its object to provide a method with which old tires, cable, polyethylene and / or polypropylene waste can be removed without damage and processed into valuable reusable liquid hydrocarbons, the formation of gaseous and coke-like decomposition products should be largely avoided.

Die der Erfindung zugrundeliegende Aufgabe wird dadurch gelöst, daß die zerkleinerten Altreifen, Kabel-, Polyäthylen- und/oder Polypropylenabfälle bei einer Temperatur von 150 bis 500 °C und einem Druck von 20 bis 300 bar mit einem bei 1 bar und 20 °C flüssigen Lösungsmittel behandelt werden, daß die mit den flüssigen Kohlenwasserstoffen beladene Lösungsmittelphase abgetrennt sowie durch Druckerniedrigung oder durch Druck- und Temperaturerniedrigung destillativ in ihre Bestandteile zerlegt wird und daß das Lösungsmittel im Kreislauf geführt wird. Unter dem Einfluß des hohen Drucks und der hohen Temperatur erfolgt eine Spaltung der polymeren Moleküle, wobei insbesondere flüssige Kohlenwasserstoffe mit ca. 5 bis 30 Kohlenstoffatomen gebildet werden, ohne daß dabei eine merkliche Verkokung eintritt. Die flüssigen Kohlenwasserstoffe werden vom Lösungsmittel vergleichsweise schnell aufgenommen und abtransportiert. Die Weichmacher und Alterungsschutzmittel werden vom Lösungsmittel gelöst und unter dem Einfluß des Drucks und der Temperatur nur in geringem Umfang zersetzt. Der Ruß, die Füllstoffe, die Metalle und das Gewebe bleiben als fester unlöslicher Rückstand zurück, der auch die beim Verfahren eventuell entstehenden geringen Mengen der Verkokungsprodukte enthält. Das Verfahren hat den Vorteil, daß der größte Teil der in den Abfallstoffen vorhandenen organischen Verbindungen in flüssige wiederverwenbare Kohlenwasserstoffe umgewandelt wird.The object underlying the invention is achieved in that the shredded old tires, cable, polyethylene and / or polypropylene waste at a temperature of 150 to 500 ° C and a pressure of 20 to 300 bar with a liquid at 1 bar and 20 ° C. Solvents are treated, that the solvent phase laden with the liquid hydrocarbons is separated off and broken down into its constituents by lowering the pressure or by lowering the pressure and temperature, and that the solvent is circulated. The polymer molecules are cleaved under the influence of the high pressure and the high temperature, liquid hydrocarbons in particular having about 5 to 30 carbon atoms being formed without any noticeable coking occurring. The liquid hydrocarbons are absorbed and removed comparatively quickly by the solvent. The plasticizers and anti-aging agents are released from the solvent and only slightly decomposed under the influence of pressure and temperature. The carbon black, the fillers, the metals and the fabric remain as a solid, insoluble residue, which also contains the small amounts of coking products that may arise during the process. The process has the advantage that the majority of the organic compounds present in the waste materials are converted into liquid reusable hydrocarbons.

Das erfindungsgemäße Verfahren kann besonders erfolgreich durchgeführt werden, wenn als Lösungsmittel Benzin, Benzol, Toluol, Xylol, Athylbehzol und/oder Wasser verwendet wird, wobei das Gewichtsverhältnis der Abfallstoffe zum Lösungsmittel zwischen 1:3 und 1:30 liegt. Die nach der Erfindung zu verwendenden organischen Lösungsmittel haben für die gebildeten flüssigen Kohlenwasserstoffe ein optimales Lösungsvermögen, während das nach der Erfindung zu verwendende Wasser Produkte mit niedrigerem Molekulargewicht liefert. In weiterer Ausgestaltung der Erfindung ist vorgesehen, daß die Druck- und Temperaturerniedrigung in mehreren Stufen erfolgt und daß die Bestandteile der beladenen Lösungsmittelphase in mehreren Fraktionen anfallen. Durch diese Verfahrensführung ist es möglich, die flüssigen Kohlenwasserstoffe in für verschiedene Anwendungszwecke geeignete Fraktionen zu zerlegen. Außerdem kann eine geeignete Fraktion dem erfindungsgemäßen Verfahren als Lösungsmittel wieder zugeführt werden.The process according to the invention can be carried out particularly successfully if gasoline, benzene, toluene, xylene, ethyl bezole and / or water is used as the solvent, the weight ratio of the waste materials to the solvent being between 1: 3 and 1:30. The organic solvents to be used according to the invention have an optimal dissolving power for the liquid hydrocarbons formed, while the water to be used according to the invention provides products with a lower molecular weight. In a further embodiment of the invention it is provided that the pressure and temperature are reduced in several stages and that the constituents of the loaded solvent phase are obtained in several fractions. This procedure allows the liquid hydrocarbons to be broken down into fractions suitable for various purposes. In addition, a suitable fraction can be returned to the process according to the invention as a solvent.

Der Gegenstand der Erfindung wird nachfolgend anhand der Zeichnung und mehrerer Ausführungsbeispiele näher erläutert.The object of the invention is explained in more detail below with reference to the drawing and several exemplary embodiments.

Im Reaktor 1 befindet sich eine Schüttung aus zerkleinerten Altreifen, Kabel-, Polyäthylen- und/ oder Polypropylenabfällen. Durch die Polyäthylen-und Polypropylenabfälle wird der Schwefel- und Chlorgehalt der Altreifen in vorteilhafter Weise verdünnt. Das Lösungsmittel wird im Wärmeaustauscher 6 auf die Verfahrenstemperatur von 150 bis 500°C erhitzt und vom Kompressor 5 auf den Verfahrensdruck von 20 bis 300 bar gebracht sowie in den Reaktor 1 gefördert. Das Lösungsmittel durchströmt den Reaktor 1 und führt die im Reaktor 1 gebildeten flüssigen Kohlenwasserstoffe sowie die in geringer Menge entstehenden gasförmigen Reaktionsprodukte ab. Am Kopf des Reaktors 1 wird die mit den flüssigen Kohlenwasserstoffen beladene Lösungsmittelphase abgenommen, im Entspannungsventil 2 entspannt, im Wärmeaustauscher 7 abgekühlt, im Trenngefäß 8 von den gasförmigen Reaktionsprodukten befreit und anschließend der Destillationskolonne 3 zugeführt. Am Fuß der Destillationskolonne 3 werden die höher siedenden Kohlenwasserstoffe abgenommen, während die niedrig siedenden Kohlenwasserstoffe zusammen mit dem Lösungsmittel am Kopf der Destillationskolonne 3 abgezogen werden. Die niedrig siedende Fraktion wird anschließend im Wärmeaustauscher 9 abgekühlt und nach der Verflüssigung vom Kompressor 5 in den Reaktor 1 zurückgeführt. Es ist möglich, die Entspannung und Abkühlung der mit den flüssigen Kohlenwasserstoffen beladenen Lösungsmittelphase in mehreren Stufen durchzuführen, was in der Zeichnung nicht dargestellt ist. Aus dem Reaktor 1 wird der feste Rückstand entnommen, der die unlöslichen Bestandteile der eingesetzten Abfallstoffe sowie die Verkokungsprodukte enthält.In the reactor 1 there is a bed of shredded old tires, cable, polyethylene and / or polypropylene waste. The sulfur and chlorine content of the old tires is advantageously diluted by the polyethylene and polypropylene waste. The solvent is heated in the heat exchanger 6 to the process temperature of 150 to 500 ° C and brought to a process pressure of 20 to 300 bar by the compressor 5 and conveyed into the reactor 1. The solvent flows through the reactor 1 and removes the liquid hydrocarbons formed in the reactor 1 and the gaseous reaction products formed in a small amount. At the top of the reactor 1, the solvent phase laden with the liquid hydrocarbons is removed, expanded in the expansion valve 2, cooled in the heat exchanger 7, freed from the gaseous reaction products in the separation vessel 8 and then fed to the distillation column 3. The higher-boiling hydrocarbons are taken off at the bottom of the distillation column 3, while the low-boiling hydrocarbons are taken off together with the solvent at the top of the distillation column 3. The low-boiling fraction is then cooled in the heat exchanger 9 and, after liquefaction, is returned from the compressor 5 to the reactor 1. It is possible to carry out the expansion and cooling of the solvent phase laden with the liquid hydrocarbons in several stages, which is not shown in the drawing. The solid residue which contains the insoluble constituents of the waste materials used and the coking products is removed from the reactor 1.

Beispiel 1example 1

Altreifen und Kabelabfälle wurden so zerkleinert, daß Teilchen mit einer Kantenlänge von ca. 2 cm anfielen. 602 g dieser Teilchen wurden 4 Stunden mit Toluol bei 350 °C und 80 bar behandelt. Anschließend wurde die mit den flüssigen Kohlenwasserstoffen beladene Lösungsmittelphase abgetrennt und auf 10 bar entspannt sowie auf 310 °C abgekühlt. Dabei erfolgte eine Trennung in eine toluolhaltige flüssige Phase und in eine Gasphase, die in der Hauptsache aus Toluol bestand. Die flüssige Phase, die ca. 85% Toluol enthielt, wurde zur Abtrennung des Toluols und der niedrig siedenden flüssigen Kohlenwasserstoffe nach Entspannen auf Atmosphärendruck destilliert. Nach der weitgehend quantitativen Abtrennung des Toluols blieb ein Extrakt in einer Menge zurück, die 65,1 Gew.-% der eingesetzten Teilchen betrug. Der Extrakt bestand überwiegend aus aliphatischen und aromatischen Kohlenwasserstoffen und hatte einen Schwefelgehalt von 1,43 Gew.-%. Weder im toluolfreien Extrakt noch im abdestillierten Toluol waren Kohlenwasserstoffe mit einer Molekülgröße unter C10 enthalten, wie eine gasschromatographische Analyse zeigte. Bei der IR-spektroskopischen Untersuchung des Extrakts wurden geringe Mengen Chlorkohlenwasserstoffe sowie organische Säuren und Ester identifiziert. Die Viskosität des Extrakts lag bei >200 000 cP, das mittlere Molekulargewicht betrug 240 g/mol und der Heizwert wurde mit 9000 kcal/kg bestimmt. Der nach der Toluolbehandlung anfallende feste Rückstand war pulverförmig und bestand in der Hauptsache aus Ruß, ZnO, anderen Reifen-Füllstoffen und Metallstücken. Sein Schwefelgehalt betrug 2,37%, während der Schwefelgehalt der eingesetzten Teilchen bei 1,70% lag. Bei der Toluolbehandlung wurden für 1 kg Ausgangsmaterial 12 kg Toluol eingesetzt, die weitgehend zurückgewonnen und im Kreislauf geführt werden können. Die im Ausgangsmaterial vorhandenen Metalle wurden im Rückstand in unveränderter Form gefunden. Dies ist ein Vorteil gegenüber einer Pyrolyse, die bei höheren Temperaturen durchgeführt wird. Dort schmelzen die in den Altreifen und Kabelabfällen vorhandenen Metalle in unerwünschter Weise zusammen, während sie beim erfindungsgemäßen Verfahren mit mechanischen Trennverfahren unter geringem ! Energieaufwand aussortiert und einer Verwertung zugeführt werden können.Used tires and cable waste were shredded so that particles with an edge length of approx. 2 cm were obtained. 602 g of these particles were treated with toluene at 350 ° C. and 80 bar for 4 hours. The solvent phase laden with the liquid hydrocarbons was then separated off and let down to 10 bar and cooled to 310 ° C. A separation was carried out into a toluene-containing liquid phase and into a gas phase, which mainly consisted of toluene. The liquid phase, which contained about 85% toluene, was distilled to remove the toluene and the low-boiling liquid hydrocarbons after relaxing to atmospheric pressure. After the largely quantitative removal of the toluene, an extract remained in an amount which was 65.1% by weight of the particles used. The extract consisted mainly of aliphatic and aromatic hydrocarbons and had a sulfur content of 1.43% by weight. Neither the toluene-free extract nor the distilled toluene contained hydrocarbons with a molecular size below C 10 , as a gas chromatographic analysis showed. When the extract was examined by IR spectroscopy, small amounts of chlorinated hydrocarbons as well as organic acids and esters were identified. The viscosity of the extract was> 200,000 cP, the average molecular weight was 240 g / mol and the calorific value was determined to be 9000 kcal / kg. The solid residue obtained after the toluene treatment was powdery and mainly consisted of carbon black, ZnO, other tire fillers and pieces of metal. Its sulfur content was 2.37%, while the sulfur content of the particles used was 1.70%. In the toluene treatment, 12 kg of toluene were used for 1 kg of starting material, and these can largely be recovered and recycled. The metals present in the starting material were found in the residue in unchanged form. This is an advantage over pyrolysis carried out at higher temperatures. There, the metals present in the old tires and cable waste melt together in an undesirable manner, while in the process according to the invention they can be reduced at a low rate with mechanical separation processes! Energy expenditure can be sorted out and recycled.

Beispiel 2Example 2

233 g zerkleinertes Polyäthylen wurde während 4 Stunden mit 3 kg/h Toluol bei 80 bar und 315 °C behandelt. Dabei wurde nahezu die gesamte Polyäthylenmenge von der Lösungsmittelphase aufgenommen. Die Lösungsmittelphase wurde anschließend auf 1 bar entspannt sowie auf 90 °C abgekühlt und zur Abtrennung des Toluols sowie der niedrig siedenden flüssigen Kohlenwasserstoffe destilliert. Das Toluol konnte bei der Destillation nahezu quantitativ zurückgewonnen werden.233 g of crushed polyethylene was treated with 3 kg / h of toluene at 80 bar and 315 ° C. for 4 hours. Almost the entire amount of polyethylene was absorbed by the solvent phase. The solvent phase was then let down to 1 bar and cooled to 90 ° C. and distilled to remove the toluene and the low-boiling liquid hydrocarbons. The toluene could be recovered almost quantitatively during the distillation.

Beispiel 3Example 3

193 g zerkleinertes Polypropylen wurde bei 100 bar und 310°C während 4 Stunden mit 3 kg/h Toluol behandelt. Nahezu das gesamte Polypropylen wurde dabei vom Lösungsmittel aufgenommen. Nach Abtrennung der beladenen Lösungsmittelphase wurde sie auf 1 bar entspannt sowie auf 85°C abgekühlt und dann zur Abtrennung des Toluols destilliert. Bei der Destillation konnte das Toluol nahezu quantitativ aus dem Extrakt entfernt und zurückgewonnen werden.193 g of crushed polypropylene was treated with 3 kg / h of toluene at 100 bar and 310 ° C. for 4 hours. Almost all of the polypropylene was absorbed by the solvent. After the loaded solvent phase had been separated off, it was let down to 1 bar and cooled to 85 ° C. and then distilled to remove the toluene. During the distillation, the toluene could be removed from the extract almost quantitatively and recovered.

Claims (3)

1. Verfahren zur Herstellung flüssiger Kohlenwasserstoffe aus Altreifen, Kabel-, Polyäthylen- und/ oder Polypropylenabfällen, dadurch gekennzeichnet, daß die zerkleinerten Altreifen, Kabel-, Polyäthylen- und/oder Polypropylenabfälle bei einer Temperatur von 150 bis 500 °C und einem Druck von 20 bis 300 bar mit einem bei 1 bar und 20 °C flüssigen Lösungsmittel behandelt werden, daß die mit den flüssigen Kohlenwasserstoffen beladene Lösungsmittelphase abgetrennt sowie durch Druckerniedrigung oder durch Druck-und Temperaturerniedrigung destillativ in ihre Bestandteile zerlegt wird und daß das Lösungsmittel im Kreislauf geführt wird.1. A process for the production of liquid hydrocarbons from used tires, cable, polyethylene and / or polypropylene waste, characterized in that the shredded used tires, cable, polyethylene and / or polypropylene waste at a temperature of 150 to 500 ° C and a pressure of 20 to 300 bar are treated with a solvent which is liquid at 1 bar and 20 ° C., that the solvent phase laden with the liquid hydrocarbons is separated off and broken down into its constituents by lowering the pressure or by lowering the pressure and temperature, and that the solvent is circulated . 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß als Lösungsmittel Benzin, Benzol, Toluol, Xylol, Äthylbenzol und/oder Wasser verwendet wird, wobei das Gewichtsverhältnis der Abfallstoffe zum Lösungsmittel zwischen 1:3 und 1:30 liegt.2. The method according to claim 1, characterized in that gasoline, benzene, toluene, xylene, ethylbenzene and / or water is used as the solvent, the weight ratio of the waste materials to the solvent being between 1: 3 and 1:30. 3. Verfahren nach den Ansprüchen 1 und 2, dadurch gekennzeichnet, daß die Druck- und Temperaturerniedrigung in mehreren Stufen erfolgt und daß die Bestandteile der beladenen Lösungsmittelphase in mehreren Fraktionen anfallen.3. Process according to claims 1 and 2, characterized in that the pressure and temperature reduction takes place in several stages and that the constituents of the loaded solvent phase are obtained in several fractions.
EP84107378A 1983-07-21 1984-06-27 Process for the production of liquid hydrocarbons Expired EP0132612B1 (en)

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US4642401A (en) 1987-02-10
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DE3326284C2 (en) 1985-08-14
JPS6040193A (en) 1985-03-02

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