EP0097755B1 - Verfahren zum Verändern von Kohlenteer - Google Patents

Verfahren zum Verändern von Kohlenteer Download PDF

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Publication number
EP0097755B1
EP0097755B1 EP82850147A EP82850147A EP0097755B1 EP 0097755 B1 EP0097755 B1 EP 0097755B1 EP 82850147 A EP82850147 A EP 82850147A EP 82850147 A EP82850147 A EP 82850147A EP 0097755 B1 EP0097755 B1 EP 0097755B1
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EP
European Patent Office
Prior art keywords
tar
coal
solvent
pitch
fraction
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP82850147A
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English (en)
French (fr)
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EP0097755A1 (de
Inventor
Samuel Cukier
Henry A.F.L. Kremer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Carbochem Inc
Original Assignee
Carbochem Inc
Domtar Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Carbochem Inc, Domtar Inc filed Critical Carbochem Inc
Priority to EP82850147A priority Critical patent/EP0097755B1/de
Priority to DE8282850147T priority patent/DE3275737D1/de
Publication of EP0097755A1 publication Critical patent/EP0097755A1/de
Application granted granted Critical
Publication of EP0097755B1 publication Critical patent/EP0097755B1/de
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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
    • C10C1/18—Working-up tar by extraction with selective solvents

Definitions

  • the present invention relates to a method of modifying coal-tars. More particularly it relates to a method of decreasing and/or modifying the quinoline insoluble content therein.
  • Coal-tar is usually obtained as a by-product of the distillation of coal in coke ovens, e.g. in the manufacture of metallurgical coke. It comprises a mixture of a number of hydrocarbon compounds which can be separated by distillation of the tar.
  • Pitch which is the residue in the still following such a distillation is a viscous material which softens and flows when heated. Pitches are conventionally classified according to their softening points and their solubility in various solvents eg. quinoline, benzene and dimethylformamide. The latter characteristic is usually indicated by the proportion of the pitch which is insoluble in the solvent eg. the proportion of the pitch which is quinoline-insoluble (Q.I.) is a widely-used pitch characteristic.
  • the pitch is preferably treated at an elevated temperature with a tar solvent and the residue mechanically separated.
  • the improvement in a process for obtaining a pitch material from an undistilled coal-tar material, the improvement essentially consists in decreasing the content of quinoline-insolubles (Q.I.) of said pitch material prior to distilling said coal-tar material by mixing said undistilled coal-tar material with a solvent which consists of at least one of the following: n-methyl-2-pyrrolidone and the fraction of a coal-tar distillate which boils between 100 and 350°C, said mixing being carried out at a temperature such as to form a solvent-dissolved fraction and a solvent-undissolved fraction, separating and removing said solvent-undissolved fraction of said undistilled coal-tar material, said undissolved fraction containing Q.I.
  • the process comprises the additional step of recovering the solvent.
  • the present invention relates to the production of pitch material by the distillation of the aforesaid solvent-dissolved fraction where the pitch has a reduced and modified Q.I.
  • the present invention relates to a process whereby the content of quinoline-insolubles (Q.I.) in coal-tar material can be decreased.
  • the coal-tar material which has been thus treated can be distilled in order to obtain a pitch having a diminished Q.I.
  • the Q.I. contained in the pitch so obtained will usually have a size distribution different from a conventionally obtained pitch having the same Q.1. This latter attribute of the present invention is referred to as the "modification" of the Q.I.
  • the present invention additionally relates to a novel coal tar pitch material having a significantly reduced viscosity and a lower average particle size.
  • the process of the present invention comprises a solvent extraction of coal-tar material in order to separate the quinoline-soluble from the quinoline-insoluble components; where the solvent chosen for this procedure contains at least one of n-methyl-2-pyrrolidone and the fraction of the coal-tar distillate which boils between 100 and 350°C, preferably between 200 and 350°C.
  • the latter solvent will be referred to as wash oil, a term which is widely used in the art.
  • the pitch material thus produced has a number of characteristics and uses that are associated with a low Q.I., a substantially reduced viscosity, and a relatively low average size of particulate matter.
  • the distillation which serves to separate the higher boiling components from the pitch residue, also serves to separate the n-methyl-2-pyrrolidone from the higher boiling components with which it distils over.
  • the n-methyl-2-pyrrolidone has a lower boiling point than the light boilers contained in the distillate and can be separated therefrom.
  • the wash oil fraction of the distillate can be permitted to distil over with the n-methyl-2-pyrrolidone and can equivalently (individually, or in combination with the n-methyl-2-pyrrolidone) be used as a solvent in this solvent extraction process. This will permit some flexibility in the distillation procedure.
  • the n-methyl-2-pyrrolidone and/or the wash oil fraction which will be contained in the distillate can then be recycled for use in the extraction of more coal-tar material.
  • the amount of solvent employed for this extraction will be partially determined by the viscosity of the resultant coal-tar-solvent mixture required for the separation technique (and which is also dependent upon the temperature of this process) and by the amount required to dissolve substantially all the quinoline soluble material.
  • the proportion of the solvent in the mixture will usually range from about 20 to 80% of the mixture, ie. the solvent: tar ratio will be in the range 1:4 to 4:1.
  • n-methyl-2-pyrrolidone which is introduced via line 01, can be mixed with recycled solvent which can additionally contain some light boilers and is introduced to the mixing tank 10, via line 02 where it is mixed with the untreated tar which has been introduced to the tank via line 04, at a temperature high enough to facilitate its handling and further processing.
  • the mixture then passes via line 06 to the separation step 20 where the solvent-dissolved fraction and the fraction insoluble in the solvent are separated, possibly by differences in specific gravity or by filtration, as a result of which the former fraction leaves this step via line 08 and the latter fraction via line 07.
  • the former fraction which contains a tar with a depleted Q.I.
  • the pitch residue obtained from this distillation via line 09 will have a substantially reduced viscosity, a lower average particle size of insolubles, in addition to a reduced Q.I. content.
  • a surprising outcome of this process is the manner in which the viscosity of the pitch and the size distribution of the Q.I. is affected.
  • the size distribution of a pitch derived from an unextracted tar, or one extracted with a solvent different from that of the present invention is often characterized by a greater degree of particulate agglomeration.
  • the pitch material thus obtained is characterized by a viscosity lower than that of pitches obtained by the distillation of the untreated coal tar. This is particularly important where the particulate size of the pitch is important e.g. in applications such as the impregnation of prebaked electrodes.
  • This example illustrates how the Q.I. of a conventional coal tar material can be decreased by the present invention using the light boilers of coal tar distillation (wash oil) as the solvent.
  • This example illustrates the use of n-methyl-2-pyrrolidone as the solvent in the extraction of the Q.I. from the tar.
  • This example presents a qualitative comparison of particle sizes of insolubles in tar which has been extracted using a conventional solvent (in this case quinoline), and that which is residual in pitch after an extraction of the precursor tar according to the present invention.
  • a conventional solvent in this case quinoline
  • Figure 2(a) is a scanning electron microscope (S.E.M.) photograph of residual tar Q.I. following an extraction using quinoline.
  • Figure 2(b) is a S.E.M. photograph of the insolubles in a pitch prepared from an identical tar after extraction with n-methyl-2-pyrrolidone.
  • the difference in the particle size distribution is all the more substantial when we note that the particles in the latter photograph include not only the insolubles following the extraction of the tar, but additionally include the "secondary" Q.I. produced during the tar distillation to produce the pitch, where the original Q.I. is concentrated and function as nuclei for the growth of Q.I. particles.

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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)

Claims (8)

1. Verfahren zum Gewinnung eines pechartigen Stoffes aus undestilliertem Steinkohlenteer, dadurch gekennzeichnet, daß man den Gehalt an Chinolin-unlöslichen Bestandteilen (Q.I.) des pechartigen Stoffes vor der Destillation des Steinkohlenteers verringert, indem man den undestillierten Steinkohlenteer mit einem Lösungsmittel mischt, welches mindestens aus einem der Bestandteile N-Methyl-2-pyrrolidon und einer zwischen 100 und 350°C siedenden Fraktion eines Steinkohlenteer-Destillates besteht, wobei das Mischen bei einer solchen Temperatur durchgeführt wird, daß eine im Lösungsmittel gelöste Fraktion und eine im Lösungsmittel ungelöste Fraktion entsteht, und man die im Lösungsmittel ungelöste Fraktion des undestillierten Steinkohlenteers abtrennt und entfernt, wobei die das Q.I. enthaltende ungelöste Fraktion einen hohen Gehalt an aschebildenden Verunreinigungen hat, und man die im Lösungsmittel gelöste Fraktion zur Gewinnung eines Steinkohlenteers mit verringertem Q.I. und geringeren Verunreinigungen verwendet, wobei man die im Lösungsmittel gelöste Fraktion des undestillierten Steinkohlenteers destilliert und dabei aus dem in Lösungsmittel gelösten Produkt einen pechartigen Stoff erhält, der einen niedrigen Gehalt an Q.I. und weniger Verunreinigungen enthält als ein pechartiger Stoff, wie er typischerweise erhalten wird durch übliche Destillation des Steinkohlenteers.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das abgetrennte Lösungsmittel zur Extraktion zusätzlichen Steinkohlenteers verwendet wird.
3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Verhältnis des Lösungsmittel zum Steinkohlenteermaterial im Bereich von etwa 4:1 bis etwa 1:4 liegt.
4. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Misch- und Abtrennungsschritte bei einer Temperatur im Bereich von 75 bis 95°C durchgeführt werden.
5. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Abtrennungsschritt in einer Filtration des Gemisches besteht.
6. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Abtrennungsschritt in einer Zentrifugierung des Gemisches besteht.
7. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Trennung durch Gravitation erfolgt.
8. Von Steinkohlenteer abgeleitetes Produkt, erhalten nach dem Verfahren gemäß Anspruch 1.
EP82850147A 1982-06-29 1982-06-29 Verfahren zum Verändern von Kohlenteer Expired EP0097755B1 (de)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP82850147A EP0097755B1 (de) 1982-06-29 1982-06-29 Verfahren zum Verändern von Kohlenteer
DE8282850147T DE3275737D1 (en) 1982-06-29 1982-06-29 Process for modifying coal tar materials

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP82850147A EP0097755B1 (de) 1982-06-29 1982-06-29 Verfahren zum Verändern von Kohlenteer

Publications (2)

Publication Number Publication Date
EP0097755A1 EP0097755A1 (de) 1984-01-11
EP0097755B1 true EP0097755B1 (de) 1987-03-18

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EP82850147A Expired EP0097755B1 (de) 1982-06-29 1982-06-29 Verfahren zum Verändern von Kohlenteer

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EP (1) EP0097755B1 (de)
DE (1) DE3275737D1 (de)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9222034B2 (en) 2013-11-19 2015-12-29 Uop Llc Process for removing a product from coal tar

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1189517B (de) * 1957-04-03 1965-03-25 Verkaufsvereinigung Fuer Teere Verfahren zur Herstellung eines Spezialkokses aus Steinkohlenteerprodukten

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2810332C2 (de) * 1978-03-10 1982-08-05 Rütgerswerke AG, 6000 Frankfurt Verfahren zur Abtrennung von chinolinunlöslichen Bestandteilen aus Steinkohlenteerpech
FR2467835B1 (fr) * 1979-10-25 1985-06-21 Inst Chemii Przemyslowej Procede de separation et d'epuration de l'anthracene de l'huile d'anthracene

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1189517B (de) * 1957-04-03 1965-03-25 Verkaufsvereinigung Fuer Teere Verfahren zur Herstellung eines Spezialkokses aus Steinkohlenteerprodukten

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Publication number Publication date
EP0097755A1 (de) 1984-01-11
DE3275737D1 (en) 1987-04-23

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