EP0276711A1 - Pitch material form coal tar pitch, process for preparing it and its use - Google Patents

Pitch material form coal tar pitch, process for preparing it and its use Download PDF

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Publication number
EP0276711A1
EP0276711A1 EP88100584A EP88100584A EP0276711A1 EP 0276711 A1 EP0276711 A1 EP 0276711A1 EP 88100584 A EP88100584 A EP 88100584A EP 88100584 A EP88100584 A EP 88100584A EP 0276711 A1 EP0276711 A1 EP 0276711A1
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Prior art keywords
pitch
content
filter
pitch material
coal tar
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EP88100584A
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German (de)
French (fr)
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EP0276711B1 (en
Inventor
Ingo Dr. Romey
Rudolf Dipl.-Ing. Geier
Rolf Helmut Joest
Wilhelm Dipl.-Ing. Wüllscheidt
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Deutsche Voest Alpine Industrieanlagenbau GmbH
Bergwerksverband GmbH
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Deutsche Voest Alpine Industrieanlagenbau GmbH
Bergwerksverband GmbH
Didier Engineering GmbH
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Application filed by Deutsche Voest Alpine Industrieanlagenbau GmbH, Bergwerksverband GmbH, Didier Engineering GmbH filed Critical Deutsche Voest Alpine Industrieanlagenbau GmbH
Priority to AT88100584T priority Critical patent/ATE62924T1/en
Priority to IN46/DEL/88A priority patent/IN171347B/en
Publication of EP0276711A1 publication Critical patent/EP0276711A1/en
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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
    • 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
    • C10C1/19—Working-up tar by thermal treatment not involving distillation

Definitions

  • the invention relates to a pitch material made of coal tar pitch, a method for its production and uses of the pitch material.
  • Coal tar pitch is according to the prior art, for. B. processed by distillation, solvent treatment, air blowing or crosslinking reactions to a pitch material, the softening point is about 70 to 150 ° C.
  • This pitch material serves as a binder for high-quality carbon articles, e.g. B. electrodes, carbon brushes and the like, as well as for the production of high-strength moldings which can be processed into graphites by thermal treatment of the coked material.
  • It is disadvantageous that the molded bodies produced from the known pitch material in a first step by heat treatment have a relatively low density and have to be compressed by repeated impregnation and renewed coking.
  • the invention has for its object to find a pitch material made of coal tar pitch and a method for producing this pitch material from which high-quality carbon articles can be produced without additional treatment steps or with fewer treatment steps than according to the prior art and which can also serve as an impregnating agent and is also a high quality binder.
  • the material is excellent to process without the risk of premature coking or thermal decomposition.
  • the new pitch material also surprisingly has a very high coke yield of 80 to> 90%, which is extremely good for pitch material made from coal tar pitch, because it can be used to produce a denser coke and, with further processing, a denser graphite, with fewer processing steps and shorter residence times .
  • the new pitch material can surprisingly be made from common coal tar pitch with a softening point below 100 ° C, which can contain 1 to 10% solids, by first removing these solids as far as possible by filtration in a candle filter, if necessary using filter aids can consist of ashes, carbon particles and components that are not soluble in quinoline (primary ⁇ -resins).
  • filter aids can consist of ashes, carbon particles and components that are not soluble in quinoline (primary ⁇ -resins).
  • the pre-cleaned pitch can be processed in thin film evaporators under vacuum in 10 mbar and in the temperature range above 300 ° C without problems to the new pitch material, which is obtained as a concentrate.
  • the by-products separated off as distillates also have excellent properties which make them particularly suitable for use as an admixture component for tars, pitches and oils.
  • the method feature C) (filter stage) can be modified in such a way that a plate filter is used, to which a post-washing stage is assigned.
  • process stage C filter stage
  • a drum filter with a dry cake discharge is used.
  • the new pitch material can be used advantageously in the carbon processing industry because it is very easy to process.
  • a preferred type of use is the production of pitch coke because of the surprisingly very high coke yield of over 90%
  • shaped carbon bodies are, for example, good for electrodes, carbon brushes or the like. suitable.
  • Graphitized, the heat-treated product can also be used as reactor graphite.
  • the new pitch material can preferably be used as an impregnating agent because, surprisingly, it has an extremely favorable, dynamic viscosity as a function of the temperature.
  • carbon molded articles that have been produced from conventional pitch material can be converted into high-strength molded articles by a few impregnation steps.
  • the new pitch material is also very suitable as a binder for carbon-containing materials.
  • the raw coal tar or the raw coal pitch is, if necessary with the addition of a filter aid, a hot filter stage 1, which can consist of a candle filter with dry filter cake discharge or a plate filter with post-washing device.
  • a hot filter stage 1 which can consist of a candle filter with dry filter cake discharge or a plate filter with post-washing device.
  • the filter temperature is approximately 90 to 350 ° C.
  • the filtered product is fed to a storage container 2, from which it is introduced via a feed pump 3 into a thin-film evaporator 5, the rotor of which is connected to a drive unit 4.
  • the product is evenly distributed on the inner wall of the apparatus via the rotor, so that the more volatile components evaporate very quickly.
  • a condenser 6 is also accommodated in the evaporator 5, on which these more volatile components of the filtered material are deposited.
  • the operating temperatures in the evaporator are above 300 ° C and the operating pressure is less than or equal to 10 mbar.
  • the non-evaporated product portion (concentrate) reaches the intake area of the concentrate discharge pump 8, is led out of the evaporator 5 and collected in a concentrate storage container 10.
  • the vacuum in the container is generated via a vacuum system 11.
  • the concentrate can be used, for example, as a raw material for the production of high-quality pitch coke and graphite, as foundry pitch, as impregnation pitch for pitch coke, as a binder for molded carbon bodies or as clay pigeon pitch.
  • the distillate produced which can still be fractionated in the usual way, is suitable, for example, for the following applications: Admixture component for tars, in particular for tars containing solids; Admixture component for pitches (fluxes); Mixing component for oils.
  • pitch materials from coal-based pitch according to the method according to the invention each of which has its coal-soluble pitch freed from its insoluble constituents by filtration and then distilled under elevated temperature and under reduced pressure in order to remove the fractions with a low softening point and a concentrate pitch with a higher softening point.
  • Pitch with a softening point ⁇ 100 ° C (KS) is generally used as the starting pitch, but pitches with a higher softening point can in principle also be used, but the achievable filter performance then decreases.
  • a coal tar pitch with a softening point of 69 ° C and a quinoline-insoluble content of 6.9% was heated to 240 ° C and filtered in a candle filter at a steadily increasing differential pressure of 1-5 bar.
  • a filter aid based on diatomaceous earth, Celite or carbon of about 1 - 4% can be added to increase the filtration capacity. After the filtration, practically all of the quinoline-insoluble components had been removed to below the detection limit. The material could be fed directly to a thin film evaporator without further pretreatment.
  • the filtered starting soft pitch material which had a softening point of 69 ° C, was subjected to a one-stage, continuous heat treatment at a temperature of 328 ° C and an operating pressure of 1 mbar, the pitch being distributed in the evaporator by means of mechanically moved wiper blades and its direction of flow was determined.
  • the operating vacuum was generated by means of vacuum devices, preferably multi-stage systems are suitable.
  • the mean residence time of the pitch material in the evaporator was less than 1 min.
  • the distilled fractions were separated off via a condenser in the evaporator and removed from there.
  • the specific throughput of the evaporator reached 80.0 kg / (m2.h).
  • the yield of concentrate was 49.6% by weight.
  • the resulting concentrate had a softening point (KS) of 209 ° C.
  • the starting pitch material and the experimental setup were the same as in Example 1, but the temperature of the heat treatment was increased to 361 ° C.
  • the specific throughput reached 74.3 kg / (m2.h).
  • the yield was 33.7% by weight and the concentrate had a softening point of 253 ° C.
  • the specific throughput reached 70.8 kg / (m2.h).
  • the yield was 27.6% by weight and the concentrate had a softening point of 292 ° C.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Working-Up Tar And Pitch (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

PCT No. PCT/EP88/00031 Sec. 371 Date Aug. 3, 1989 Sec. 102(e) Date Aug. 3, 1989 PCT Filed Jan. 16, 1988 PCT Pub. No. WO88/05806 PCT Pub. Date Aug. 11, 1988.A novel pitch material made from coal tar pitch has: a) mesophase content of </=2%, b) content of toluene-insolubles ( beta -resin) between 58 and 75%, c) content of quinoline-insolubles of <2%, d) softening point in the 200 DEG to 300 DEG C. range, according to the Krämer-Sarnow (KS) measurement, e) content of volatile matter </=20% and f) ash content of </=0.06%. The pitch material of high coke yield (80 to beyond 90%) is suitable for the manufacture of molded carbonaceous shapes of high quality and of pitch coke. A further application would be as impregnation agent or bind. The method of making new pitch uses hot filtration in the presence of a filtration and followed by thin-film evaporation.

Description

Die Erfindung betrifft ein Pechmaterial aus Kohleteerpech, ein Verfahren zu dessen Herstellung sowie Verwendungen des Pechmaterials.The invention relates to a pitch material made of coal tar pitch, a method for its production and uses of the pitch material.

Kohleteerpech wird nach dem Stand der Technik z. B. durch Destil­lation, Lösungsmittelbehandlung, Luftverblasen oder Vernetzungs­reaktionen zu einem Pechmaterial verarbeitet, dessen Erweichungs­punkt etwa 70 bis 150° C beträgt. Dieses Pechmaterial dient als Bindemittel für hochwertige Kohlenstoffartikel, z. B. Elek­troden, Kohlebürsten und ähnliches, sowie zur Erzeugung von hochfesten Formkörpern, die durch thermische Weiterbehandlung des verkokten Materials zu Graphiten verarbeitbar sind. Nach­teilig ist, daß die aus dem bekannten Pechmaterial in einem ersten Schritt durch eine Wärmebehandlung hergestellten Form­körper eine relativ geringe Dichte aufweisen und durch mehr­maliges Imprägnieren und erneutes Verkoken verdichtet werden müssen.Coal tar pitch is according to the prior art, for. B. processed by distillation, solvent treatment, air blowing or crosslinking reactions to a pitch material, the softening point is about 70 to 150 ° C. This pitch material serves as a binder for high-quality carbon articles, e.g. B. electrodes, carbon brushes and the like, as well as for the production of high-strength moldings which can be processed into graphites by thermal treatment of the coked material. It is disadvantageous that the molded bodies produced from the known pitch material in a first step by heat treatment have a relatively low density and have to be compressed by repeated impregnation and renewed coking.

Der Erfindung liegt die Aufgabe zugrunde, ein Pechmaterial aus Kohleteerpech sowie ein Verfahren zur Herstellung dieses Pechmaterials zu finden, aus dem hochwertige Kohlenstoffar­tikel ohne zusätzliche Behandlungsschritte oder mit weniger Behandlungsschritten als nach dem Stand der Technik hergestellt werden können und das darüber hinaus auch als Imprägniermit­tel dienen kann und außerdem ein hochwertiges Bindemittel ist.The invention has for its object to find a pitch material made of coal tar pitch and a method for producing this pitch material from which high-quality carbon articles can be produced without additional treatment steps or with fewer treatment steps than according to the prior art and which can also serve as an impregnating agent and is also a high quality binder.

Diese Aufgabe wird durch ein Pechmaterial aus Kohleteerpech gelöst, das folgende Parameter aufweist:

  • a) einen Gehalt an Mesophase ≦ 2%,
  • b) einen Gehalt an in Toluol unlöslichem Material (β-Harze) von 58 bis 75%,
  • c) einen Gehalt an in Chinolin unlöslichem Material ≦ 2%,
  • d) einen Erweichungspunkt im Bereich von 200 bis 300° C, gemessen nach Krämer-Sarnow (KS),
  • e) einen Gehalt an flüchtigen Bestandteilen ≦ 20% und
  • f) einen Aschegehalt ≦ 0,06%.
This problem is solved by a pitch material made of coal tar pitch, which has the following parameters:
  • a) a mesophase content of ≦ 2%,
  • b) a content of toluene-insoluble material (β-resins) from 58 to 75%,
  • c) a content of quinoline-insoluble material ≦ 2%,
  • d) a softening point in the range from 200 to 300 ° C., measured according to Krämer-Sarnow (KS),
  • (e) a volatile content of ≦ 20% and
  • f) an ash content ≦ 0.06%.

Wegen des überraschenderweise für ein Kohleteerpech vergleichs­weise hohen Erweichungspunktes, der im Bereich von 200 bis 300° C (KS) liegt, ist das Material hervorragend verarbeit­bar, ohne daß die Gefahr einer frühzeitigen Verkokung oder thermischen Zersetzung besteht.Because of the surprisingly high softening point for coal tar pitch, which is in the range of 200 to 300 ° C (KS), the material is excellent to process without the risk of premature coking or thermal decomposition.

Das neue Pechmaterial hat außerdem überraschenderweise eine sehr hohe Koksausbeute von 80 bis > 90%, was für Pechmaterial aus Kohleteerpech außerordentlich gut ist, denn es läßt sich daraus ein dichterer Koks und bei einer Weiterbehandlung auch ein dichterer Graphit herstellen, mit weniger Verarbeitungs­stufen und kürzeren Verweilzeiten.The new pitch material also surprisingly has a very high coke yield of 80 to> 90%, which is extremely good for pitch material made from coal tar pitch, because it can be used to produce a denser coke and, with further processing, a denser graphite, with fewer processing steps and shorter residence times .

Die Herstellung des neuen Pechmaterials erfolgt mit Hilfe nach­folgender Verfahrensstufen, wobei

  • A) als Ausgangsmaterial ein Kohleteerpech verwen­det wird, das bis 10% Feststoffe, wie Asche, Kohlepartikel, in Chinolin Unlösliches (primä­re α-Harze) enthält und einen Erweichungs­punkt < 100° C aufweist,
  • B) dem Ausgangsmaterial 1 bis 10% Filterhilfsmittel, wie Kieselgur, Aktivkohle, o.ä. zugesetzt wird,
  • C) das Gemisch in einem Kerzenfilter mit trockenem Kuchenaustrag und Filteröffnungen im Bereich von 50 bis 150 µm heiß filtriert wird und
  • D) das Filtrat in einem Dünnschichtverdampfer im Temperaturbereich oberhalb 300° C bis etwa 425° C und unter einem Druck ≦ 10 mbar aufkonzentriert wird.
The production of the new pitch material takes place with the help of subsequent process stages, whereby
  • A) a coal tar pitch is used as the starting material, which contains up to 10% solids, such as ash, Contains carbon particles, which are insoluble in quinoline (primary α-resins) and have a softening point <100 ° C,
  • B) the starting material 1 to 10% filter aid, such as diatomaceous earth, activated carbon, or the like. is added
  • C) the mixture is filtered hot in a candle filter with a dry cake discharge and filter openings in the range from 50 to 150 μm and
  • D) the filtrate is concentrated in a thin film evaporator in the temperature range above 300 ° C to about 425 ° C and under a pressure ≦ 10 mbar.

Das neue Pechmaterial läßt sich überraschenderweise aus üb­lichem Kohleteerpech mit einem Erweichungspunkt unter 100° C herstellen, das 1 bis 10% Feststoffe enthalten kann, indem es zunächst durch Filtration in einem Kerzenfilter, ggf. unter Anwendung von Filterhilfsmitteln von diesen Feststoffen wei­testgehend befreit wird, die aus Asche, Kohlepartikel und Be­standteilen bestehen können, die nicht chinolinlöslich sind (primäre α-Harze). Überraschenderweise läßt sich das so vor­gereinigte Pech in Dünnschichtverdampfern unter Vakuum ≦ 10 mbar und im Temperaturbereich oberhalt 300° C störungsfrei zu dem neuen Pechmaterial verarbeiten, das als Konzentrat an­fällt.The new pitch material can surprisingly be made from common coal tar pitch with a softening point below 100 ° C, which can contain 1 to 10% solids, by first removing these solids as far as possible by filtration in a candle filter, if necessary using filter aids can consist of ashes, carbon particles and components that are not soluble in quinoline (primary α-resins). Surprisingly, the pre-cleaned pitch can be processed in thin film evaporators under vacuum in 10 mbar and in the temperature range above 300 ° C without problems to the new pitch material, which is obtained as a concentrate.

Weiterhin überraschend haben auch die als Destillate abgetrenn­ten Nebenprodukte hervorragende Eigenschaften, die sie ins­besondere zur Verwendung als Zumischkomponente für Teere, Peche und öle geeignet machen.Furthermore, surprisingly, the by-products separated off as distillates also have excellent properties which make them particularly suitable for use as an admixture component for tars, pitches and oils.

Alternativ kann das Verfahrensmerkmal C) (Filterstufe) in der Weise abgewandelt werden, daß ein Plattenfilter verwendet wird, dem eine Nachwaschstufe zugeordnet ist.Alternatively, the method feature C) (filter stage) can be modified in such a way that a plate filter is used, to which a post-washing stage is assigned.

Eine weitere Abwandlung der Verfahrensstufe C) (Filterstufe) besteht darin, daß ein Trommelfilter mit trockenem Kuchenaus­trag verwendet wird.Another modification of process stage C) (filter stage) is that a drum filter with a dry cake discharge is used.

Auch bei Anwendung der beiden vorgenannten alternativen Filter­schritte werden ausreichend feststofffreie Filtrate erzielt, die sich zur Weiterverarbeitung in einem Dünnschichtverdampfer eignen.When using the two alternative filter steps mentioned above, sufficiently solid-free filtrates are obtained which are suitable for further processing in a thin-film evaporator.

Das neue Pechmaterial läßt sich vorteilhaft in der kohlenstoff­verarbeitenden Industrie verwenden, weil es sehr gut verarbeit­bar ist.The new pitch material can be used advantageously in the carbon processing industry because it is very easy to process.

Eine bevorzugte Verwendungsart ist die Herstellung von Pechkoks, wegen der überraschenderweise sehr hohen Koksausbeute von über 90%A preferred type of use is the production of pitch coke because of the surprisingly very high coke yield of over 90%

Eine weitere bevorzugte Verwendung ist die Herstellung von Kohlenstofformkörpern. Diese Kohleformkörper sind beispiels­weise gut für Elektroden, Kohlebürsten o.ä. geeignet. Graphi­tiert läßt sich das wärmebehandelte Produkt auch vorzüglich als Reaktorgraphit anwenden.Another preferred use is the production of shaped carbon bodies. These shaped carbon articles are, for example, good for electrodes, carbon brushes or the like. suitable. Graphitized, the heat-treated product can also be used as reactor graphite.

Weiterhin läßt sich das neue Pechmaterial bevorzugt als Im­prägniermittel verwenden, weil es überraschenderweise eine überaus günstige, dynamische Viskosität in Abhängigkeit von der Temperatur hat. Beispielsweise können damit Kohleformkör­per, die aus herkömmlichem Pechmaterial hergestellt worden sind, durch wenige Imprägnierschritte in hochfeste Formkör­per überführen.Furthermore, the new pitch material can preferably be used as an impregnating agent because, surprisingly, it has an extremely favorable, dynamic viscosity as a function of the temperature. For example, carbon molded articles that have been produced from conventional pitch material can be converted into high-strength molded articles by a few impregnation steps.

Schließlich ist das neue Pechmaterial auch sehr gut als Binde­mittel für kohlenstoffhaltige Materialien geeignet.Finally, the new pitch material is also very suitable as a binder for carbon-containing materials.

Die Erfindung wird nachfolgend in einer Verfahrensbeschrei­bung näher erläutert, und zwar anhand eines Verfahrensfließ­bildes, das Fig. 1 zeigt.The invention is explained in more detail below in a process description, specifically using a process flow diagram which is shown in FIG. 1.

Der Steinkohlenrohteer bzw. das Steinkohlenrohpech wird, ggf. unter Zumischung eines Filterhilfsmittels, einer Heißfilter­stufe 1 aufgegeben, die aus einem Kerzenfilter mit trockenem Filterkuchenaustrag oder aus einem Plattenfilter mit Nachwasch­einrichtung bestehen kann. Die Filtertemperatur beträgt je nach Einsatzprodukt etwa 90 bis zu 350° C. Das filtrierte Pro­dukt wird einem Vorratsbehälter 2 zugeführt, aus dem es über eine Speisepumpe 3 in einen Dünnschichtverdampfungsapparat 5 eingebracht wird, dessen Rotor mit einer Antriebseinheit 4 verbunden ist. über den Rotor wird das Produkt gleichmäßig auf der inneren Apparatewand verteilt, so daß die leichter flüchtigen Komponenten sehr schnell verdampfen. In dem Ver­dampfungsapparat 5 ist weiterhin ein Kondensator 6 unterge­bracht, an dem sich diese leichter flüchtigen Komponenten des filtrierten Materials niederschlagen. Sie gelangen auf den Boden des Dünnschichtverdampfungsapparates 5 und werden von dort mit einer Destillataustragspumpe 7 abgezogen und einem Destillatvorlagebehälter 9 aufgegeben. Die Betriebstempera­turen im Verdampfungsapparat liegen oberhalb 300° C und der Betriebsdruck ist kleiner oder gleich 10 mbar. Der nicht ver­dampfte Produktanteil (Konzentrat) gelangt in den Einzugsbe­reich der Konzentrataustragspumpe 8, wird aus dem Verdampfungs­apparat 5 herausgeführt und in einem Konzentratvorlagebehäl­ter 10 gesammelt. Das Vakuum im Behälter wird über ein Vaku­umsystem 11 erzeugt.The raw coal tar or the raw coal pitch is, if necessary with the addition of a filter aid, a hot filter stage 1, which can consist of a candle filter with dry filter cake discharge or a plate filter with post-washing device. Depending on the product used, the filter temperature is approximately 90 to 350 ° C. The filtered product is fed to a storage container 2, from which it is introduced via a feed pump 3 into a thin-film evaporator 5, the rotor of which is connected to a drive unit 4. The product is evenly distributed on the inner wall of the apparatus via the rotor, so that the more volatile components evaporate very quickly. A condenser 6 is also accommodated in the evaporator 5, on which these more volatile components of the filtered material are deposited. They reach the bottom of the thin-film evaporator 5 and are drawn off from there with a distillate discharge pump 7 and placed in a distillate storage container 9. The operating temperatures in the evaporator are above 300 ° C and the operating pressure is less than or equal to 10 mbar. The non-evaporated product portion (concentrate) reaches the intake area of the concentrate discharge pump 8, is led out of the evaporator 5 and collected in a concentrate storage container 10. The vacuum in the container is generated via a vacuum system 11.

Das Konzentrat kann beispielsweise als Rohmaterial zur Herstel­lung von hochwertigem Pechkoks und -graphit, als Gießereipech, als Imprägnierpech für Pechkokse, als Bindemittel für Kohlen­stofformkörper oder als Tontaubenpech verwendet werden.The concentrate can be used, for example, as a raw material for the production of high-quality pitch coke and graphite, as foundry pitch, as impregnation pitch for pitch coke, as a binder for molded carbon bodies or as clay pigeon pitch.

Das erzeugte Destillat, das sich in üblicher Weise noch frak­tionieren läßt, eignet sich beispielsweise für folgende An­wendungsfälle:

Beimischkomponente für Teere, insbesondere für feststoffhal­tige Teere;
Beimischkomponente für Peche (Fluxmittel);
Beimischkomponente für öle.The distillate produced, which can still be fractionated in the usual way, is suitable, for example, for the following applications:

Admixture component for tars, in particular for tars containing solids;
Admixture component for pitches (fluxes);
Mixing component for oils.

Nachstehend sind drei Beispiele von Pechmaterialien aus kohle­stämmigen Pechen nach dem erfindungsgemäßen Verfahren darge­stellt, wobei jeweils ein kohlestämmiges Pech durch Filtrieren von seinen unlöslichen Bestandteilen befreit und anschließend unter erhöhter Temperatur und unter vermindertem Druck destil­liert wurde, um die Fraktionen mit niedrigem Erweichungspunkt zu entfernen und ein Konzentratpech mit höherem Erweichungs­punkt zu erhalten. Als Ausgangspeche werden im allgemeinen Peche mit einem Erweichungspunkt < 100° C (KS) verwendet, je­doch lassen sich grundsätzlich auch Peche mit höherem Erwei­chungspunkt einsetzen, wobei dann jedoch die erzielbare Fil­terleistung abnimmt.Below are three examples of pitch materials from coal-based pitch according to the method according to the invention, each of which has its coal-soluble pitch freed from its insoluble constituents by filtration and then distilled under elevated temperature and under reduced pressure in order to remove the fractions with a low softening point and a concentrate pitch with a higher softening point. Pitch with a softening point <100 ° C (KS) is generally used as the starting pitch, but pitches with a higher softening point can in principle also be used, but the achievable filter performance then decreases.

Beispiel 1example 1

Ein Steinkohlenteerpech mit einem Erweichungspunkt von 69° C und einem Gehalt an chinolinunlöslichen Bestandteilen von 6,9 % wurde auf 240° C erhitzt und in einem Kerzenfilter bei einem stetig steigenden Differenzdruck von 1 - 5 bar filtriert. Zur Erhöhung der Filtrationsleistung kann ggf. ein Filterhilfs­mittel auf Basis Kieselgur, Celite oder Kohlenstoff von etwa 1 - 4 % zugegeben werden. Nach der Filtration waren praktisch alle chinolinunlöslichen Bestandteile bis unter die Nachweis­grenze entfernt. Das Material konnte ohne weitere Vorbehandlung direkt einem Dünnschichtverdampfer zugeführt werden.A coal tar pitch with a softening point of 69 ° C and a quinoline-insoluble content of 6.9% was heated to 240 ° C and filtered in a candle filter at a steadily increasing differential pressure of 1-5 bar. For If necessary, a filter aid based on diatomaceous earth, Celite or carbon of about 1 - 4% can be added to increase the filtration capacity. After the filtration, practically all of the quinoline-insoluble components had been removed to below the detection limit. The material could be fed directly to a thin film evaporator without further pretreatment.

Das filtrierte Ausgangs-Weichpechmaterial, welches einen Erwei­chungspunkt von 69° C aufwies, wurde einer einstufigen, kon­tinuierlichen Wärmebehandlung bei einer Temperatur von 328° C und einem Betriebsdruck von 1 mbar unterworfen, wobei in dem Verdampfungsapparat das Pech mittels mechanisch bewegter Wischer­blätter verteilt und dessen Fließrichtung bestimmt wurde. Dabei erfolgte eine mechanische Selbstreinigung. Das Betriebsvakuum wurde mittels Vakuumapparate erzeugt, bevorzugt eignen sich mehrstufige Systeme.The filtered starting soft pitch material, which had a softening point of 69 ° C, was subjected to a one-stage, continuous heat treatment at a temperature of 328 ° C and an operating pressure of 1 mbar, the pitch being distributed in the evaporator by means of mechanically moved wiper blades and its direction of flow was determined. This involved mechanical self-cleaning. The operating vacuum was generated by means of vacuum devices, preferably multi-stage systems are suitable.

Die mittlere Verweilzeit des Pechmaterials im Verdampfungsappa­rat betrug unter 1 min. Die abdestillierten Fraktionen wurden über einen im Verdampfer befindlichen Kondensator abgeschieden und von dort abgeführt.The mean residence time of the pitch material in the evaporator was less than 1 min. The distilled fractions were separated off via a condenser in the evaporator and removed from there.

Der spezifische Durchsatz des Verdampfungsapparates erreichte 80,0 kg/(m².h). Die Ausbeute an Konzentrat betrug 49,6 Gew.-%. Das anfallende Konzentrat wies einen Erweichungspunkt (KS) von 209° C auf.The specific throughput of the evaporator reached 80.0 kg / (m².h). The yield of concentrate was 49.6% by weight. The resulting concentrate had a softening point (KS) of 209 ° C.

Die weiteren stoffspezifischen Eigenschaften des Konzentrates mit 209° C Erweichungspunkt waren folgende:

- Verkokungsrückstand (Alcan):      81,5 %
- sekundärunlösliche Bestandteile:      0,14 %
- β-Harze:      58 %
- chinolinunlösliche Bestandteile:      0,78 %
- Dynamische Viskosität in Abhängigkeit von der Temperatur gemäß Kurve A in Fig. 2
- Flüchtige Bestandteile      18,5 %
- Asche      0,05 %The other substance-specific properties of the concentrate with a softening point of 209 ° C were as follows:

- Coking residue (Alcan): 81.5%
- secondary insoluble components: 0.14%
- β-resins: 58%
- Quinoline-insoluble components: 0.78%
Dynamic viscosity as a function of temperature according to curve A in FIG. 2
- Volatile components 18.5%
- ash 0.05%

Beispiel 2Example 2

Das Ausgangspechmaterial und der Versuchsaufbau waren die glei­chen wie in Beispiel 1, jedoch wurde die Temperatur der Wärme­behandlung auf 361° C erhöht.The starting pitch material and the experimental setup were the same as in Example 1, but the temperature of the heat treatment was increased to 361 ° C.

Der spezifische Durchsatz erreichte 74,3 kg/(m².h). Die Ausbeute betrug 33,7 Gew.-% und das Konzentrat wies einen Erweichungs­punkt von 253° C auf.The specific throughput reached 74.3 kg / (m².h). The yield was 33.7% by weight and the concentrate had a softening point of 253 ° C.

Die weiteren stoffspezifischen Eigenschaften waren folgende:

- Verkokungsrückstand (Alcan):      86,2 %
- sekundärunlösliche Bestandteile      0,9 %
-β-Harze:      69%
- chinolinunlösliche Bestandteile:      1,55 %
- Dynamische Viskosität in Abhängigkeit von der Temperatur gemäß Kurve B in Fig. 2
- Flüchtige Bestandteile      13,8 %
- Asche      0,06 %The other substance-specific properties were as follows:

- Coking residue (Alcan): 86.2%
- secondary insoluble components 0.9%
-β resins: 69%
- Quinoline-insoluble components: 1.55%
Dynamic viscosity as a function of temperature according to curve B in FIG. 2
- volatile constituents 13.8%
- ash 0.06%

Beispiel 3Example 3

Das Ausgangspechmaterial und der Versuchsaufbau waren wiederum die gleichen wie im Beispiel 1, jedoch wurde die Temperatur nunmehr auf 395° C erhöht.The starting pitch material and the experimental setup were again the same as in Example 1, but the temperature was now increased to 395 ° C.

Der spezifische Durchsatz erreichte 70,8 kg/(m².h). Die Ausbeute betrug 27,6 Gew.-% und das Konzentrat wies einen Erweichungspunkt von 292° C auf.The specific throughput reached 70.8 kg / (m².h). The yield was 27.6% by weight and the concentrate had a softening point of 292 ° C.

Die weiteren stoffspezifischen Eigenschaften waren folgende:

- Verkokungsrückstand (Alcan)      90,8 %
- sekundärunlösliche Bestandteile:      1,01 %
- βiHarze:       75%
- chinolinunlösliche Bestandteile:      1,95 %
- Dynamische Viskosität in Abhängigkeit von der Temperatur gemäß Kurve C in Fig. 2
- Flüchtige Bestandteile      9,2 %
- Asche      0,06 %The other substance-specific properties were as follows:

- Coking residue (Alcan) 90.8%
- secondary insoluble components: 1.01%
- βi resins: 75%
- Quinoline-insoluble components: 1.95%
Dynamic viscosity as a function of the temperature according to curve C in FIG. 2
- volatile components 9.2%
- ash 0.06%

Claims (9)

1. Pechmaterial aus Kohleteerpech, gekennzeichnet durch die folgenden Parameter: a) einen Gehalt an Mesophase ≦ 2 %, b) einen Gehalt an in Toluol unlöslichem Material (β-Harze) von 58 bis 75 %, c) einen Gehalt an in Chinolin unlöslichem Material ≦ 2 %, d) einen Erweichungspunkt im Bereich von 200 bis 300° C, gemessen nach Krämer-Sarnow (KS) e) einen Gehalt an flüchtigen Bestandteilen ≦ 20 % und f) einen Aschegehalt ≦ 0,06 %. 1. Coal tar pitch material characterized by the following parameters: a) a mesophase content of ≦ 2%, b) a content of toluene-insoluble material (β-resins) from 58 to 75%, c) a content of quinoline-insoluble material ≦ 2%, d) a softening point in the range from 200 to 300 ° C, measured according to Krämer-Sarnow (KS) (e) a volatile content of ≦ 20% and f) an ash content ≦ 0.06%. 2. Verfahren zur Herstellung eines Pechmaterials gemäß Anspruch 1, dadurch gekennzeichnet, daß A) als Ausgangsmaterial ein Kohleteerpech verwendet wird, das bis 10 % Feststoffe, wie Asche, Kohlepartikel, in Chinolin Unlösliches (primäre -Harze) enthält und einen Erweichungspunkt ≦ 100° C aufweist, B) dem Ausgangsmaterial 1 bis 10 % Filterhilfsmittel, wie Kieselgur, Aktivkohle, o. ä. zugesetzt wird, C) das Gemisch in einem Kerzenfilter mit trockenem Kuchen­austrag und Filteröffnungen im Bereich von 50 bis 150 µm heiß filtriert wird und D) das Filtrat in einem Dünnschichtverdampfer im Temperatur­bereich oberhalb 300° C bis etwa 425° C und unter einem Druck ≦ 10 mbar aufkonzentriert wird. 2. A method for producing a pitch material according to claim 1, characterized in that A) a coal tar pitch is used as the starting material, which contains up to 10% solids, such as ash, carbon particles, which are insoluble in quinoline (primary resins) and has a softening point ≦ 100 ° C, B) 1 to 10% of filter aids, such as diatomaceous earth, activated carbon, or the like, are added to the starting material, C) the mixture is filtered hot in a candle filter with a dry cake discharge and filter openings in the range from 50 to 150 μm and D) the filtrate is concentrated in a thin film evaporator in the temperature range above 300 ° C to about 425 ° C and under a pressure ≦ 10 mbar. 3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß in der Filterstufe (C) ein Plattenfilter verwendet wird, dem eine Nachwaschstufe zugeordnet ist.3. The method according to claim 2, characterized in that a plate filter is used in the filter stage (C), which is assigned a post-washing stage. 4. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß in der Filterstufe (C) ein Trommelfilter mit trockenem Kuchen­austrag verwendet wird.4. The method according to claim 2, characterized in that a drum filter with dry cake discharge is used in the filter stage (C). 5. Verwendung des Pechmaterials nach Anspruch 1 in der kohlen­stoffverarbeitenden Industrie.5. Use of the pitch material according to claim 1 in the carbon processing industry. 6. Verwendung des Pechmaterials nach Anspruch 1 zur Herstellung von Pechkoks.6. Use of the pitch material according to claim 1 for the manufacture of pitch coke. 7. Verwendung des Pechmaterials nach Anspruch 1 zur Herstel­lung von Kohlenstofformkörpern.7. Use of the pitch material according to claim 1 for the production of carbon molded articles. 8. Verwendung des Pechmaterials nach Anspruch 1 als Impräg­niermittel.8. Use of the pitch material according to claim 1 as an impregnating agent. 9. Verwendung des Pechmaterials nach Anspruch 1 als Bindemittel.9. Use of the pitch material according to claim 1 as a binder.
EP88100584A 1987-01-30 1988-01-16 Pitch material form coal tar pitch, process for preparing it and its use Expired - Lifetime EP0276711B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AT88100584T ATE62924T1 (en) 1987-01-30 1988-01-16 PITCH MATERIAL FROM COAL TAR PITCH, PROCESS FOR PRODUCTION AND USE OF THE PITCH MATERIAL.
IN46/DEL/88A IN171347B (en) 1987-01-30 1988-01-19

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19873702720 DE3702720A1 (en) 1987-01-30 1987-01-30 CARBONED PECH MATERIAL, METHOD FOR THE PRODUCTION THEREOF AND USE OF THE PECH MATERIAL
DE3702720 1987-01-30

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EP0276711B1 EP0276711B1 (en) 1991-04-24

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EP88901243A Pending EP0346347A1 (en) 1987-01-30 1988-01-16 Pitch material made of coal tar pitch, process for producing and using the same

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US5534137A (en) * 1993-05-28 1996-07-09 Reilly Industries, Inc. Process for de-ashing coal tar
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US7033485B2 (en) * 2001-05-11 2006-04-25 Koppers Industries Of Delaware, Inc. Coal tar and hydrocarbon mixture pitch production using a high efficiency evaporative distillation process
CN101302431A (en) * 2008-06-30 2008-11-12 邯郸市鑫宝煤化工有限公司 Preparation of asphalt for producing coal-based needle coke
CN103666513B (en) * 2013-11-29 2015-02-04 中国五环工程有限公司 High-dust-content coal tar separation and upgrading purification process and system
CN105462602A (en) * 2015-11-19 2016-04-06 贵州大学 A method of preparing foamy carbon from coal-tar pitch
CN108291151A (en) * 2015-11-20 2018-07-17 理查德·斯通 Single-stage pitch technique and product
CN109355084B (en) * 2018-12-17 2024-04-02 陕西延长石油（集团）有限责任公司 System and method for removing water and solid matters in coal tar
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EP0346347A1 (en) 1989-12-20
JPH02502648A (en) 1990-08-23
RU1826985C (en) 1993-07-07
DE3702720A1 (en) 1988-08-11
CN88100544A (en) 1988-08-10
WO1988005806A1 (en) 1988-08-11
DE3862472D1 (en) 1991-05-29
ES2022467B3 (en) 1991-12-01
EP0276711B1 (en) 1991-04-24
GR3001859T3 (en) 1992-11-23
DE3702720C2 (en) 1990-04-26
ATE62924T1 (en) 1991-05-15
AU601020B2 (en) 1990-08-30
RU1838375C (en) 1993-08-30
DD279892A5 (en) 1990-06-20
US5128021A (en) 1992-07-07
AU1189588A (en) 1988-08-24

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