EP0265598B1 - Verfahren zur Entsalzung von Steinkohlenteeren und -pechen - Google Patents

Verfahren zur Entsalzung von Steinkohlenteeren und -pechen Download PDF

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Publication number
EP0265598B1
EP0265598B1 EP87110278A EP87110278A EP0265598B1 EP 0265598 B1 EP0265598 B1 EP 0265598B1 EP 87110278 A EP87110278 A EP 87110278A EP 87110278 A EP87110278 A EP 87110278A EP 0265598 B1 EP0265598 B1 EP 0265598B1
Authority
EP
European Patent Office
Prior art keywords
water
pitches
coal
tar
pitch
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 - Lifetime
Application number
EP87110278A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0265598A1 (de
Inventor
Herbert Dr. Beneke
Arnold Dr. Alscher
Rudolf Dr. Oberkobusch
Siegfried Prof. Dr. Peter
Wolfgang Jaumann
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.)
Ruetgers Germany GmbH
Original Assignee
Ruetgerswerke AG
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 Ruetgerswerke AG filed Critical Ruetgerswerke AG
Publication of EP0265598A1 publication Critical patent/EP0265598A1/de
Application granted granted Critical
Publication of EP0265598B1 publication Critical patent/EP0265598B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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 separating 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.
  • the water wash can also be carried out at elevated temperature under elevated pressure and in several stages (GB-A 849 987). 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 prevent the ammonium chloride from going into the gas phase. This is generally done by metering in an amount of an aqueous NaOH or Na z COs solution adapted to the chloride content of the tar.
  • the salts formed like all other ash formers, remain in the respective distillation residue during tar processing, that is to say 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 gas containing carbon dioxide, 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 object of the present invention is not achieved by the known method, since the tar is not selectively ashed. It is also not recommended to use supercritical carbon dioxide for water washing.
  • 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 system of pitch or tar, water and CO 2 -containing gas is 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 that. To run wash water in countercurrent and to filter off the insoluble salts that occur during relaxation.

Landscapes

  • 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)
  • Epoxy Compounds (AREA)
  • Epoxy Resins (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
  • Detergent Compositions (AREA)
EP87110278A 1986-10-28 1987-07-16 Verfahren zur Entsalzung von Steinkohlenteeren und -pechen Expired - Lifetime EP0265598B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3636560 1986-10-28
DE19863636560 DE3636560A1 (de) 1986-10-28 1986-10-28 Verfahren zur entsalzung von steinkohlenteeren und -pechen

Publications (2)

Publication Number Publication Date
EP0265598A1 EP0265598A1 (de) 1988-05-04
EP0265598B1 true EP0265598B1 (de) 1990-09-19

Family

ID=6312587

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87110278A Expired - Lifetime EP0265598B1 (de) 1986-10-28 1987-07-16 Verfahren zur Entsalzung von Steinkohlenteeren und -pechen

Country Status (13)

Country Link
US (2) US4831101A (da)
EP (1) EP0265598B1 (da)
JP (1) JPS63122786A (da)
AU (1) AU593399B2 (da)
CA (1) CA1285897C (da)
CS (1) CS264297B2 (da)
DE (2) DE3636560A1 (da)
DK (1) DK561287A (da)
ES (1) ES2002257B3 (da)
IN (1) IN170362B (da)
PL (1) PL151418B1 (da)
SU (1) SU1512486A3 (da)
ZA (1) ZA876675B (da)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5274160A (en) * 1991-08-22 1993-12-28 Syracuse University Method and apparatus for synthesis of highly isomerically pure stereoisomers of glycidol derivatives
US5194637A (en) * 1991-08-22 1993-03-16 Syracuse University Method and apparatus for synthesis of highly isomerically pure stereoisomers of glycidol derivatives
US5576362A (en) * 1992-04-20 1996-11-19 Denki Kagaku Kogyo Kabushiki Kaisha Insulating material and a circuit substrate in use thereof
US5578740A (en) * 1994-12-23 1996-11-26 The Dow Chemical Company Process for preparation of epoxy compounds essentially free of organic halides
MY122050A (en) 1998-05-29 2006-03-31 Sumitomo Chemical Co Highly purified epoxy resin
JP5245274B2 (ja) * 2007-04-02 2013-07-24 三菱化学株式会社 タール又はタールエマルジョンからの水除去方法、タールエマルジョンのタール化方法、及びタール中の含水率低減方法
CN104910944B (zh) * 2015-06-10 2018-03-20 山东宝塔新能源有限公司 煤焦油脱盐工艺
CN106701157B (zh) * 2015-11-12 2018-04-10 中国石油化工股份有限公司 一种高温煤焦油脱金属方法

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US32120A (en) * 1861-04-23 Floor-clamp
US2572583A (en) * 1948-12-21 1951-10-23 Phillips Petroleum Co Improved liquid-liquid contacting process using di(beta-cyanoethyl)-amine
FR1038775A (fr) * 1950-06-20 1953-10-01 Collin F J Ag Perfectionnements apportés aux procédés et dispositifs d'épuration du goudron etdes produits goudronneux
GB849987A (en) * 1957-12-02 1960-09-28 Allied Chem Process for treating coke oven tar
US3202605A (en) * 1962-06-06 1965-08-24 Badger Co Propane deaspihalting process
GB1482690A (en) * 1974-12-19 1977-08-10 Coal Ind Hydrogenation of coal
US4101416A (en) * 1976-06-25 1978-07-18 Occidental Petroleum Corporation Process for hydrogenation of hydrocarbon tars
JPS6041111B2 (ja) * 1976-11-26 1985-09-13 新日鐵化学株式会社 コ−クス製造原料の調整方法
US4208267A (en) * 1977-07-08 1980-06-17 Exxon Research & Engineering Co. Forming optically anisotropic pitches
DE2810332C2 (de) * 1978-03-10 1982-08-05 Rütgerswerke AG, 6000 Frankfurt Verfahren zur Abtrennung von chinolinunlöslichen Bestandteilen aus Steinkohlenteerpech
US4219404A (en) * 1979-06-14 1980-08-26 Exxon Research & Engineering Co. Vacuum or steam stripping aromatic oils from petroleum pitch
DE3017876A1 (de) * 1980-05-09 1982-05-19 Peter, Siegfried, Prof.Dr., 8520 Erlangen Verfahren zur abtrennung von feststoffen aus oelen
US4402824A (en) * 1981-03-25 1983-09-06 Sumitomo Metal Industries, Limited Process for refining coal-based heavy oils
USRE32120E (en) 1981-04-01 1986-04-22 Phillips Petroleum Company Hydrotreating supercritical solvent extracts in the presence of alkane extractants
DE3135368A1 (de) * 1981-09-07 1983-03-31 Siemens AG, 1000 Berlin und 8000 München Verfahren und anordnung zur funktionspruefung einer programmierbare logikanordnung
US4482453A (en) * 1982-08-17 1984-11-13 Phillips Petroleum Company Supercritical extraction process
JPS5941387A (ja) * 1982-08-30 1984-03-07 Osaka Gas Co Ltd ピッチの製造方法
US4503026A (en) * 1983-03-14 1985-03-05 E. I. Du Pont De Nemours And Company Spinnable precursors from petroleum pitch, fibers spun therefrom and method of preparation thereof
US4502943A (en) * 1983-03-28 1985-03-05 E. I. Du Pont De Nemours And Company Post-treatment of spinnable precursors from petroleum pitch
US4447598A (en) * 1983-04-07 1984-05-08 The Dow Chemical Company Method of preparing epoxy resins having low hydrolyzable chloride contents
DE3335316A1 (de) * 1983-09-29 1985-04-11 Rütgerswerke AG, 6000 Frankfurt Verfahren zur abtrennung harzartiger stoffe aus kohlestaemmigen schweroelen und verwendung der gewonnenen fraktion
US4485221A (en) * 1983-11-03 1984-11-27 Ciba-Geigy Corporation Process for making epoxy novolac resins with low hydrolyzable chlorine and low ionic chloride content
US4604184A (en) * 1983-11-16 1986-08-05 Domtar Inc. Modified coal-tar pitch
JPS60200816A (ja) * 1984-03-26 1985-10-11 Kawasaki Steel Corp 炭素材料の製造方法
US4578177A (en) * 1984-08-28 1986-03-25 Kawasaki Steel Corporation Method for producing a precursor pitch for carbon fiber
US4575412A (en) * 1984-08-28 1986-03-11 Kawasaki Steel Corporation Method for producing a precursor pitch for carbon fiber
DE3539432A1 (de) * 1984-11-09 1986-06-05 Instytut Chemii Przemysłowej, Warschau/Warszawa Verfahren zur trennung von kohlenteeren

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Erdöl und Kohle, Erdgas; Bd. 34, Heft 7, Juli 1981, Seiten 296-300 *

Also Published As

Publication number Publication date
ZA876675B (en) 1988-03-16
DE3765079D1 (de) 1990-10-25
SU1512486A3 (ru) 1989-09-30
US4831101A (en) 1989-05-16
ES2002257A4 (es) 1988-08-01
EP0265598A1 (de) 1988-05-04
DK561287D0 (da) 1987-10-27
CS264297B2 (en) 1989-06-13
ES2002257B3 (es) 1991-04-01
US4871443A (en) 1989-10-03
DK561287A (da) 1988-04-29
DE3636560A1 (de) 1988-05-05
AU8017487A (en) 1988-05-05
AU593399B2 (en) 1990-02-08
CA1285897C (en) 1991-07-09
CS642487A2 (en) 1988-09-16
PL151418B1 (en) 1990-08-31
JPS63122786A (ja) 1988-05-26
PL268457A1 (en) 1988-11-24
IN170362B (da) 1992-03-21

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