EP0265598A1 - Process for desalting coal tar and coal pitch - Google Patents

Process for desalting coal tar and coal pitch Download PDF

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EP0265598A1
EP0265598A1 EP87110278A EP87110278A EP0265598A1 EP 0265598 A1 EP0265598 A1 EP 0265598A1 EP 87110278 A EP87110278 A EP 87110278A EP 87110278 A EP87110278 A EP 87110278A EP 0265598 A1 EP0265598 A1 EP 0265598A1
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Prior art keywords
pitches
gas
tars
water
coal
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German (de)
French (fr)
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EP0265598B1 (en
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Herbert Dr. Beneke
Arnold Dr. Alscher
Rudolf Dr. Oberkobusch
Siegfried Prof. Dr. Peter
Wolfgang Jaumann
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Ruetgers Germany GmbH
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Ruetgerswerke AG
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
    • C10C1/00—Working-up tar

Definitions

  • the invention relates to a process for the separation of salts, in particular sodium and ammonium chloride and zinc sulfide, from coal tars and pitches.
  • the ammonium chloride present in the raw tar causes severe corrosion damage in the distillation columns during the tar processing. Since the salt is water-soluble, the water contained in the raw tar is mechanically separated. However, up to 2% water remains in the tar (Franck / Collin: Coal tar, p. 27). An additional water wash can further reduce the ammonium chloride content. However, this measure is too complex if the chloride content is to be reduced to such an extent that chloride corrosion no longer takes place. Therefore, the chloride is usually bound to a stronger base to avoid that the ammonium chloride passes into the gas phase. This is generally done by metering in an amount adapted to the chloride content of the tar of an aqueous NaOH or Na2CO3 solution.
  • the salts formed like all other ash formers, remain in the respective distillation residue during tar processing, ie in normal pitch, hard pitch or pitch coke.
  • Metallic impurities are extremely undesirable, especially when using pitch as a binder or coke as a carbon material in the manufacture of anodes for aluminum electrolysis. Not only do they form additional slags, they also increase the burn-off of the anodes. This applies in particular to sodium, which acts as an oxidation catalyst (Light Metals, AIME 1981, 471-476).
  • the object was therefore to develop a process with which salts can be selectively removed from coal tars and pitches.
  • the object is achieved in that the coal tars or pitches with water and a carbon dioxide-containing gas, optionally with the addition of a solvent or / and entrainer, in a pressure vessel at a temperature and a pressure near the critical point of the gas used washed and decanted, the liquid or dissolved tars or pitches and the water being drawn off separately and then being released.
  • the zinc present as insoluble zinc sulfide in the tar dissolves to a considerable extent in the aqueous phase, precipitates out after the pressure has been let down, and can be filtered off. It is thus possible to circulate the washing water freed from the zinc salt and to enrich the sodium or ammonium chloride content to the extent that this makes sense for technical reasons. Thereafter, the wash water must be at least partially processed or renewed.
  • the pitch or tar, water and CO2-containing gas are preferably present in the supercritical state. If additional dragging or solvents are used, they can be separated from the pitch and reused by gradually releasing the pressure.
  • All known pitch solvents come into question as solvents, that is to say pure aromatics, such as, for. B. toluene, or aromatic oils, such as. B. washing oil, or tar bases such as pyridine and quinoline, which can also be used as an entrainer.
  • gases containing carbon dioxide are also mixtures, especially hydrocarbons containing 1 to 6 carbon atoms, such as propane, butane or liquid gas.
  • the phases are separated and drained.
  • the chlorine or chlorides are almost completely removed by a single-stage wash.
  • the content of zinc and other ash formers can be reduced even further by washing in several stages with more thorough mixing. It is advantageous to run the wash water in countercurrent and to filter off the insoluble salts that occur during relaxation.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Working-Up Tar And Pitch (AREA)
  • Detergent Compositions (AREA)
  • Epoxy Compounds (AREA)
  • Epoxy Resins (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)

Abstract

Steinkohlenteere und -peche lassen sich mit Wasser und einem Kohlendioxid enthaltenden Gas entsalzen, wenn das System im überkritischen Zustand vorliegt. Wird die Wäsche einstufig durchgeführt, so werden die Chloride nahezu vollständig und die Zinksalze zu mehr als 50 % entfernt. Dabei verbleiben alle Harze in den Teeren bzw. Pechen. Bei einem mehrstufigen Waschprozeß kann die Salzabscheidung noch verbessert werden.Hard coal tars and pitches can be desalinated with water and a gas containing carbon dioxide if the system is in a supercritical state. If the washing is carried out in one step, the chlorides are almost completely removed and the zinc salts are removed to more than 50%. All resins remain in the tars or pitches. In a multi-stage washing process, the salt separation can still be improved.

Description

Gegenstand der Erfindung ist ein Verfahren zur Abtrennung von Salzen, insbesondere von Natrium- und Ammoniumchlorid und Zinksulfid, aus Steinkohlenteeren und -pechen.The invention relates to a process for the separation of salts, in particular sodium and ammonium chloride and zinc sulfide, from coal tars and pitches.

Das im Rohteer vorhandene Ammoniumchlorid verursacht bei der Teeraufarbeitung starke Korrosionsschäden in den Destillationskolonnen. Da das Salz wasserlöslich ist, wird das im Rohteer enthaltene Wasser mechanisch abgeschieden. Im Teer verbleiben jedoch noch etwa bis zu 2 % Wasser (Franck/Collin: Steinkohlenteer, S. 27). Durch eine zusätzliche Wasserwäsche kann der Gehalt an Ammoniumchlorid weiter gesenkt werden. Diese Maßnahme ist jedoch zu aufwendig, wenn der Chloridgehalt soweit vermindert werden soll, daß keine Chlorid-Korrosion mehr stattfindet. Daher wird üblicherweise das Chlorid an einer stärkeren Base gebunden, um zu vermeiden, daß das Ammoniumchlorid in die Gasphase übergeht. Dies geschieht im allgemeinen durch Zudosierung einer dem Chloridgehalt des Teeres angepaßten Menge einer wäßrigen NaOH- oder Na₂CO₃-Lösung.The ammonium chloride present in the raw tar causes severe corrosion damage in the distillation columns during the tar processing. Since the salt is water-soluble, the water contained in the raw tar is mechanically separated. However, up to 2% water remains in the tar (Franck / Collin: Coal tar, p. 27). An additional water wash can further reduce the ammonium chloride content. However, this measure is too complex if the chloride content is to be reduced to such an extent that chloride corrosion no longer takes place. Therefore, the chloride is usually bound to a stronger base to avoid that the ammonium chloride passes into the gas phase. This is generally done by metering in an amount adapted to the chloride content of the tar of an aqueous NaOH or Na₂CO₃ solution.

Die gebildeten Salze bleiben wie auch alle anderen Aschebildner bei der Teeraufarbeitung in dem jeweiligen Destillationsrückstand, also im Normalpech, Hartpech oder Pechkoks.The salts formed, like all other ash formers, remain in the respective distillation residue during tar processing, ie in normal pitch, hard pitch or pitch coke.

Insbesondere bei der Verwendung des Pechs als Bindemittel bzw. des Kokses als Kohlenstoffmaterial bei der Herstellung von Anoden für die Aluminiumelektrolyse sind metallische Verunreinigungen äußerst unerwünscht. Sie bilden nicht nur zusätzliche Schlacken, sondern erhöhen auch den Abbrand der Anoden. Dies gilt insbesondere für Natrium, das als Oxidationskatalysator wirkt (Light Metals, AIME 1981, 471-476).Metallic impurities are extremely undesirable, especially when using pitch as a binder or coke as a carbon material in the manufacture of anodes for aluminum electrolysis. Not only do they form additional slags, they also increase the burn-off of the anodes. This applies in particular to sodium, which acts as an oxidation catalyst (Light Metals, AIME 1981, 471-476).

Für die Entfernung unlöslicher Aschebildner gibt es zahlreiche Verfahren wie Filtrieren, Zentrifugieren und promotorbeschleunigtes Absitzenlassen, gegebenenfalls auch unter Verwendung überkritischer Lösungsmittel. All diesen Verfahren ist gemeinsam, daß sie nicht selektiv wirken, sondern alle nicht löslichen oder spezifisch schwereren Partikel abtrennen, wie beispielsweise rußartige Teerharze, die in Chinolin unlöslich sind. Diese sogenannten Alpha-Harze sind wichtige Bestandteile des Steinkohlenteerpechs für die genannten Anwendungsbeispiele, da sie die Koksausbeute und die Anodenfestigkeit entscheidend beeinflussen.There are numerous methods for removing insoluble ash formers, such as filtering, centrifuging and promoter-accelerated settling, if appropriate also using supercritical solvents. All of these processes have in common that they do not act selectively, but separate all insoluble or specifically heavier particles, such as, for example, soot-like tar resins which are insoluble in quinoline. These so-called alpha resins are important components of coal tar pitch for the application examples mentioned, since they have a decisive influence on the coke yield and the anode strength.

Es bestand daher die Aufgabe, ein Verfahren zu entwickeln, mit dem Salze aus Steinkohlenteeren und -pechen selektiv entfernt werden können. Die Aufgabe wird erfindungsgemäß dadurch gelöst, daß die Steinkohlenteere oder -peche mit Wasser und einem Kohlendioxid enthaltenden Gas, gegebenenfalls unter Zusatz eines Lösungs- oder/und Schleppmittels, in einem Druckbehälter bei einer Temperatur und einem Druck in der Nähe des kritischen Punktes des verwendeten Gases gewaschen und dekantiert werden, wobei die flüssig oder gelöst vorliegenden Teere oder Peche und das Wasser getrennt abgezogen und danach entspannt werden.The object was therefore to develop a process with which salts can be selectively removed from coal tars and pitches. The object is achieved in that the coal tars or pitches with water and a carbon dioxide-containing gas, optionally with the addition of a solvent or / and entrainer, in a pressure vessel at a temperature and a pressure near the critical point of the gas used washed and decanted, the liquid or dissolved tars or pitches and the water being drawn off separately and then being released.

Durch den Zusatz von Lösungsmitteln kann die Temperatur des Waschprozesses und die Viskosität, insbesondere bei hochschmelzenden Pechen, gesenkt werden. Bei Teeren und Normalpechen ist dies nicht erforderlich, da sich das überkritische Kohlendioxid nicht nur im Wasser, sondern auch im Teer bzw. Pech gut löst. Zusätzliche Schleppmittel bieten die Möglichkeit, auch die Dichte der Phasen zu beeinflussen.The addition of solvents can reduce the temperature of the washing process and the viscosity, especially in the case of high-melting pitches. This is not necessary for tars and normal pitches, since the supercritical carbon dioxide dissolves well not only in water, but also in tar or pitch. Additional entraining agents offer the possibility to influence the density of the phases.

Überraschenderweise hat es sich gezeigt, daß das im Teer als unlösliches Zinksulfid vorliegende Zink sich zu einem erheblichen Teil in der wäßrigen Phase löst, nach dem Entspannen ausfällt und abfiltriert werden kann. So ist es möglich, das vom Zinksalz befreite Waschwasser im Kreislauf zu führen und den Gehalt an Natrium- bzw. Ammoniumchlorid soweit anzureichern, wie dies aus technischen Gründen sinnvoll ist. Danach muß das Waschwasser zumindest teilweise aufgearbeitet oder erneuert werden.Surprisingly, it has been found that the zinc present as insoluble zinc sulfide in the tar dissolves to a considerable extent in the aqueous phase, precipitates out after the pressure has been let down, and can be filtered off. It is thus possible to circulate the washing water freed from the zinc salt and to enrich the sodium or ammonium chloride content to the extent that this makes sense for technical reasons. Thereafter, the wash water must be at least partially processed or renewed.

Während des Waschprozesses liegt das Sy stem Pech oder Teer, Wasser und CO₂-haltiges Gas vorzugsweise im überkritischen Zustand vor. Werden zusätzliche Schlepp- oder Lösungsmittel verwendet, so können sie durch stufenweises Entspannen von dem Pech getrennt und wiederverwendet werden. Als Lösungsmittel kommen alle bekannten Pechlösungsmittel in Frage, also reine Aromaten, wie z. B. Toluol, oder aromatische Öle, wie z. B. Waschöl, oder auch Teerbasen, wie Pyridin und Chinolin, die teilweise auch als Schleppmittel verwendet werden können. Kohlendioxid enthaltende Gase sind neben reinem Kohlendioxid auch Mischungen vor allem mit 1 bis 6 Kohlenstoffatome enthaltende Kohlenwasserstoffe, wie beispielsweise Propan, Butan oder Flüssiggas.During the washing process, the pitch or tar, water and CO₂-containing gas are preferably present in the supercritical state. If additional dragging or solvents are used, they can be separated from the pitch and reused by gradually releasing the pressure. All known pitch solvents come into question as solvents, that is to say pure aromatics, such as, for. B. toluene, or aromatic oils, such as. B. washing oil, or tar bases such as pyridine and quinoline, which can also be used as an entrainer. In addition to pure carbon dioxide, gases containing carbon dioxide are also mixtures, especially hydrocarbons containing 1 to 6 carbon atoms, such as propane, butane or liquid gas.

Die Erfindung wird anhand der nachfolgenden Beispiele näher erläutert.The invention is illustrated by the following examples.

Beispiel 1example 1

400 g Steinkohlenteerpech mit einem Erweichungspunkt von 70 °C und einem Aschegehalt von 2600 ppm werden mit 500 g Wasser in einem Rührautoklaven gebracht, dieser verschlossen und auf 150 °C aufgeheizt.
Während des Aufdrückens des CO₂-Gases wird mit dem Durchmischen der beiden Phasen begonnen. Bis zur Beendigung des Versuchs nach 3 Stunden wird der CO₂-Druck auf 100 bar gehalten.400 g of coal tar pitch with a softening point of 70 ° C and an ash content of 2600 ppm are placed with 500 g of water in a stirred autoclave, which is closed and heated to 150 ° C.
While the CO₂ gas is being pressed on, the mixing of the two phases is started. The CO₂ pressure is kept at 100 bar until the end of the experiment after 3 hours.

Die Phasen werden getrennt und abgelassen.The phases are separated and drained.

Proben des Einsatzpechs und des gewaschenen Peches werden nach DIN 51719 verascht und auf ZnO und NaCl untersucht. Die Ergebnisse sind in Tabelle 1 gegenübergestellt.

Figure imgb0001
Samples of the pitch and the washed pitch are ashed according to DIN 51719 and examined for ZnO and NaCl. The results are compared in Table 1.
Figure imgb0001

Beispiel 2Example 2

400 g Steinkohlenteer mit einem Gehalt an 653 ppm Zink und 1652 ppm Chlor (nach DIN 51577) werden mit 400 g Wasser in einem Autoklaven gegeben, auf 80 °C aufgeheizt und durch Aufdrücken von CO₂ auf einen Druck von 100 bar gebracht.
Man rührt 4 Stunden lang intensiv, danach werden durch Stehenlassen beide Phasen wieder getrennt.400 g of coal tar containing 653 ppm zinc and 1652 ppm chlorine (according to DIN 51577) are placed with 400 g of water in an autoclave, heated to 80 ° C and brought to a pressure of 100 bar by pressing in CO₂.
The mixture is stirred vigorously for 4 hours, after which the two phases are separated again by standing.

Der Asche- und Zinkgehalt und das Chlor im Teer werden bestimmt. Die Ergebnisse sind in Tabelle 2 zusammengefaßt:

Figure imgb0002
The ash and zinc content and the chlorine in the tar are determined. The results are summarized in Table 2:
Figure imgb0002

Wie die Analysen zeigen, werden das Chlor bzw. die Chloride bereits durch eine einstufige Wäsche nahezu vollständig entfernt. Der Gehalt an Zink und anderen Aschebildnern kann durch eine mehrstufige Wäsche mit intensiverer Durchmischung noch weiter abgesenkt werden. Dabei ist es vorteilhaft, das Waschwasser im Gegenstrom zu führen und die beim Entspannen anfallenden unlöslichen Salze abzufiltrieren.As the analyzes show, the chlorine or chlorides are almost completely removed by a single-stage wash. The content of zinc and other ash formers can be reduced even further by washing in several stages with more thorough mixing. It is advantageous to run the wash water in countercurrent and to filter off the insoluble salts that occur during relaxation.

Der entscheidende Vorteil dieses selektiven Verfahrens ist darin zu sehen, daß der Anteil der Harze in den Teeren und Pechen unverändert bleibt. The decisive advantage of this selective process is that the proportion of resins in the tars and pitches remains unchanged.

Claims (7)

1. Verfahren zur Entsalzung von Steinkohlenteeren und -pechen, dadurch gekennzeichnet, daß die Steinkohlenteere oder -peche mit Wasser und einem Kohlendioxid enthaltenden Gas, gegebenenfalls unter Zusatz eines Lösungs- oder/und Schleppmittels, in einem Druckbehälter bei einer Temperatur und einem Druck in der Nähe des kritischen Punktes des verwendeten Gases gewaschen und dekantiert werden, wobei die flüssig oder gelöst vorliegenden Teere oder Peche und das Wasser getrennt abgezogen und danach entspannt werden.1. A process for the desalination of coal tars and pitches, characterized in that the coal tars or pitches with water and a gas containing carbon dioxide, optionally with the addition of a solvent or / and entrainer, in a pressure vessel at a temperature and a pressure in the Washed and decanted near the critical point of the gas used, the liquid or dissolved tars or pitches and the water being drawn off separately and then relaxed. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß als Gas Kohlendioxid verwendet wird.2. The method according to claim 1, characterized in that carbon dioxide is used as gas. 3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß als Gas ein Gemisch aus Kohlendioxid und 1 bis 6 Kohlenstoffatome enthaltende Kohlenwasserstoffe verwendet wird.3. The method according to claim 1, characterized in that a mixture of carbon dioxide and hydrocarbons containing 1 to 6 carbon atoms is used as the gas. 4. Verfahren nach den Ansprüchen 1 bis 3, dadurch gekennzeichnet, daß in dem System Pech oder Teer, während des Waschprozesses das CO₂-haltige Gas im überkritischen Zustand vorliegt.4. The method according to claims 1 to 3, characterized in that in the pitch or tar system, the CO₂-containing gas is present in the supercritical state during the washing process. 5. Verfahren nach den Ansprüchen 1 bis 4, dadurch gekennzeichnet, daß das Waschwasser nach dem Entspannen filtriert und im Kreislauf geführt wird.5. Process according to claims 1 to 4, characterized in that the washing water is filtered after relaxation and is circulated. 6. Verfahren nach den Ansprüchen 1 bis 5, dadurch gekennzeichnet, daß aus den Teeren oder Pechen nach dem Waschen die Lösungs- und Schleppmittel durch stufenweises Entspannen zurück gewonnen werden.6. Process according to claims 1 to 5, characterized in that the solvents and entraining agents are recovered from the tars or pitches after washing by stepwise relaxation. 7. Verfahren nach den Ansprüchen 1 bis 6, dadurch gekennzeichnet, daß es in mehreren Stufen durchgeführt wird.7. The method according to claims 1 to 6, characterized in that it is carried out in several stages.
EP87110278A 1986-10-28 1987-07-16 Process for desalting coal tar and coal pitch Expired - Lifetime EP0265598B1 (en)

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DE3636560 1986-10-28
DE19863636560 DE3636560A1 (en) 1986-10-28 1986-10-28 METHOD FOR THE DESALINATION OF CARBON TARES AND PITCHES

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DE3636560A1 (en) 1988-05-05
DE3765079D1 (en) 1990-10-25
ES2002257B3 (en) 1991-04-01
CA1285897C (en) 1991-07-09

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