EP0276711B1 - Pechmaterial aus Kohleteerpech, Verfahren zu dessen Herstellung sowie Verwendung des Pechmaterials - Google Patents

Pechmaterial aus Kohleteerpech, Verfahren zu dessen Herstellung sowie Verwendung des Pechmaterials Download PDF

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Publication number
EP0276711B1
EP0276711B1 EP88100584A EP88100584A EP0276711B1 EP 0276711 B1 EP0276711 B1 EP 0276711B1 EP 88100584 A EP88100584 A EP 88100584A EP 88100584 A EP88100584 A EP 88100584A EP 0276711 B1 EP0276711 B1 EP 0276711B1
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EP
European Patent Office
Prior art keywords
pitch
content
filter
coal tar
material according
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
EP88100584A
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German (de)
English (en)
French (fr)
Other versions
EP0276711A1 (de
Inventor
Ingo Dr. Romey
Rudolf Dipl.-Ing. Geier
Rolf Helmut Joest
Wilhelm Dipl.-Ing. Wüllscheidt
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.)
Deutsche Voest Alpine Industrieanlagenbau GmbH
Bergwerksverband GmbH
Original Assignee
Deutsche Voest Alpine Industrieanlagenbau GmbH
Bergwerksverband GmbH
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 Deutsche Voest Alpine Industrieanlagenbau GmbH, Bergwerksverband GmbH filed Critical Deutsche Voest Alpine Industrieanlagenbau GmbH
Priority to AT88100584T priority Critical patent/ATE62924T1/de
Priority to IN46/DEL/88A priority patent/IN171347B/en
Publication of EP0276711A1 publication Critical patent/EP0276711A1/de
Application granted granted Critical
Publication of EP0276711B1 publication Critical patent/EP0276711B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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.
  • a pitch material which corresponds to the pitch material according to the application in three characteristics, namely the content of mesophase (a), the content of quinoline-insoluble material (c) and the softening point ( d), namely for the partial range up to 274 ° C from the application range of 200 - 300 ° C.
  • the characteristics b) (content of toluene-insoluble material), e) (volatile components) and f) (ash content) are different.
  • the new material is excellent to process without the risk of early 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 filtration, practically all quinoline-insoluble constituents were 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.
EP88100584A 1987-01-30 1988-01-16 Pechmaterial aus Kohleteerpech, Verfahren zu dessen Herstellung sowie Verwendung des Pechmaterials Expired - Lifetime EP0276711B1 (de)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AT88100584T ATE62924T1 (de) 1987-01-30 1988-01-16 Pechmaterial aus kohleteerpech, verfahren zu dessen herstellung sowie verwendung des pechmaterials.
IN46/DEL/88A IN171347B (el) 1987-01-30 1988-01-19

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19873702720 DE3702720A1 (de) 1987-01-30 1987-01-30 Pechmaterial aus kohleteerpech, verfahren zu dessen herstellung sowie verwendung des pechmaterials
DE3702720 1987-01-30

Publications (2)

Publication Number Publication Date
EP0276711A1 EP0276711A1 (de) 1988-08-03
EP0276711B1 true EP0276711B1 (de) 1991-04-24

Family

ID=6319832

Family Applications (2)

Application Number Title Priority Date Filing Date
EP88901243A Pending EP0346347A1 (de) 1987-01-30 1988-01-16 Pechmaterial aus kohleteerpech, verfahren zu dessen herstellung sowie verwendung des pechmaterials
EP88100584A Expired - Lifetime EP0276711B1 (de) 1987-01-30 1988-01-16 Pechmaterial aus Kohleteerpech, Verfahren zu dessen Herstellung sowie Verwendung des Pechmaterials

Family Applications Before (1)

Application Number Title Priority Date Filing Date
EP88901243A Pending EP0346347A1 (de) 1987-01-30 1988-01-16 Pechmaterial aus kohleteerpech, verfahren zu dessen herstellung sowie verwendung des pechmaterials

Country Status (12)

Country Link
US (1) US5128021A (el)
EP (2) EP0346347A1 (el)
JP (1) JPH02502648A (el)
CN (1) CN88100544A (el)
AT (1) ATE62924T1 (el)
AU (1) AU601020B2 (el)
DD (1) DD279892A5 (el)
DE (2) DE3702720A1 (el)
ES (1) ES2022467B3 (el)
GR (1) GR3001859T3 (el)
RU (2) RU1826985C (el)
WO (1) WO1988005806A1 (el)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0358086B1 (de) * 1988-09-03 1992-02-05 Akzo Faser Aktiengesellschaft Verfahren zur Erhöhung des Mesophasenanteils in Pech
DE8900473U1 (el) * 1989-01-17 1990-05-23 Hoogovens Aluminium Huettenwerk Gmbh, 4223 Voerde, De
AT395316B (de) * 1991-03-14 1992-11-25 Voest Alpine Stahl Linz Steinkohlenteerpech
DE4112955A1 (de) * 1991-04-20 1992-10-22 Ruetgerswerke Ag Steinkohlenteerpech, seine herstellung und verwendung
US5534137A (en) * 1993-05-28 1996-07-09 Reilly Industries, Inc. Process for de-ashing coal tar
US5695631A (en) * 1993-06-04 1997-12-09 Mitsubishi Chemical Corporation Process for producing petroleum needle coke
US5656041A (en) * 1996-06-05 1997-08-12 Rochester Gas & Electric Co. Method for detoxifying coal-tar deposits
DE19703703B4 (de) * 1996-09-27 2007-02-01 Steel Authority Of India Ltd. Verfahren zur Produktion von geeignetem Pech zum Imprägnieren von Graphitelektroden für Lichtbogenöfen
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 (zh) * 2008-06-30 2008-11-12 邯郸市鑫宝煤化工有限公司 用于生产煤系针状焦的沥青的制备方法
CN103666513B (zh) * 2013-11-29 2015-02-04 中国五环工程有限公司 高含尘量煤焦油分离提质工艺及系统
CN105462602A (zh) * 2015-11-19 2016-04-06 贵州大学 一种煤沥青制备泡沫碳的方法
CN108291151A (zh) * 2015-11-20 2018-07-17 理查德·斯通 单级沥青工艺和产品
CN109355084B (zh) * 2018-12-17 2024-04-02 陕西延长石油（集团）有限责任公司 一种脱除煤焦油中水分和固体物质的系统及方法
US11248172B2 (en) 2019-07-23 2022-02-15 Koppers Delaware, Inc. Heat treatment process and system for increased pitch yields

Family Cites Families (25)

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Publication number Priority date Publication date Assignee Title
GB206885A (en) * 1922-06-20 1923-11-20 Turner Tanning Mach Co Ltd Improvements in or relating to leather working machines
GB850880A (en) * 1957-10-16 1960-10-12 Gelsenkirchener Bergwerks Ag Process and apparatus for the continuous production of pitch
US2956944A (en) * 1958-02-10 1960-10-18 Allied Chem Process for filtering tar
US3190812A (en) * 1960-01-22 1965-06-22 Ruetgerswerke Ag Device for the continuous production of hard pitch
JPS4917848B1 (el) * 1968-06-12 1974-05-04
FR2268857B1 (el) * 1974-04-25 1978-01-27 Sofresid
US3928169A (en) * 1974-05-06 1975-12-23 Domtar Ltd Production of pitch substantially soluble in quinoline
US4046690A (en) * 1976-04-01 1977-09-06 The United States Of America As Represented By The United States Energy Research And Development Administration Filtering coal-derived oil through a filter media precoated with particles partially solubilized by said oil
JPS6057478B2 (ja) * 1978-06-28 1985-12-14 呉羽化学工業株式会社 炭素繊維用ピツチの製造法
DE2828976C2 (de) * 1978-07-01 1983-06-01 Bergwerksverband Gmbh, 4300 Essen Anschwemmkerzenfilter-Vorrichtung für Trockenaustrag und Verfahren zur Reinigung der Vorrichtung
AU516280B2 (en) * 1978-12-21 1981-05-28 Mitsui Coke Co. Ltd. Production of carbon fibres
US4277324A (en) * 1979-04-13 1981-07-07 Exxon Research & Engineering Co. Treatment of pitches in carbon artifact manufacture
US4517072A (en) * 1981-05-18 1985-05-14 Domtar Inc. Process for modifying coal tar materials
US4497789A (en) * 1981-12-14 1985-02-05 Ashland Oil, Inc. Process for the manufacture of carbon fibers
US4448670A (en) * 1982-02-08 1984-05-15 Exxon Research And Engineering Co. Aromatic pitch production from coal derived distillate
US4522701A (en) * 1982-02-11 1985-06-11 E. I. Du Pont De Nemours And Company Process for preparing an anisotropic aromatic pitch
JPS58220805A (ja) * 1982-06-15 1983-12-22 Nippon Oil Co Ltd 炭素繊維用前駆体ピツチの製造方法
DE3305431A1 (de) * 1983-02-17 1984-08-23 Bergwerksverband Gmbh, 4300 Essen Verfahren zur reinigung von hochfeststoffhaltigen kokereiteeren
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DE3509861C2 (de) * 1984-03-26 1986-03-06 Idemitsu Kosan Co. Ltd., Tokio/Tokyo Pechmaterial für einen kohlenstoffhaltigen Formkörper und Verfahren zu seiner Herstellung
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DE3441727A1 (de) * 1984-11-15 1986-05-15 Bergwerksverband Gmbh, 4300 Essen Verfahren zur herstellung von anisotropen kohlenstoffasern
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Also Published As

Publication number Publication date
ATE62924T1 (de) 1991-05-15
CN88100544A (zh) 1988-08-10
EP0346347A1 (de) 1989-12-20
RU1826985C (ru) 1993-07-07
DE3702720A1 (de) 1988-08-11
RU1838375C (ru) 1993-08-30
AU1189588A (en) 1988-08-24
DE3862472D1 (de) 1991-05-29
DD279892A5 (de) 1990-06-20
WO1988005806A1 (en) 1988-08-11
EP0276711A1 (de) 1988-08-03
US5128021A (en) 1992-07-07
ES2022467B3 (es) 1991-12-01
JPH02502648A (ja) 1990-08-23
GR3001859T3 (en) 1992-11-23
AU601020B2 (en) 1990-08-30
DE3702720C2 (el) 1990-04-26

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