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EP0510315B1 - Brai de goudron de houille, sa préparation et son utilisation - Google Patents

Brai de goudron de houille, sa préparation et son utilisation Download PDF

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Publication number
EP0510315B1
EP0510315B1 EP92102398A EP92102398A EP0510315B1 EP 0510315 B1 EP0510315 B1 EP 0510315B1 EP 92102398 A EP92102398 A EP 92102398A EP 92102398 A EP92102398 A EP 92102398A EP 0510315 B1 EP0510315 B1 EP 0510315B1
Authority
EP
European Patent Office
Prior art keywords
coal tar
pitch
evaporator
distillation
benzo
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
EP92102398A
Other languages
German (de)
English (en)
Other versions
EP0510315A1 (fr
Inventor
Winfried Dr. Boenigk
Hans-Dieter Behrens
Hans Dr. Spengler
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.)
Rain Carbon 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
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First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=6430010&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0510315(B1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Ruetgerswerke AG filed Critical Ruetgerswerke AG
Publication of EP0510315A1 publication Critical patent/EP0510315A1/fr
Application granted granted Critical
Publication of EP0510315B1 publication Critical patent/EP0510315B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • 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
    • C10C1/04—Working-up tar by distillation
    • 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 new coal tar pitch, a process for its production and its use.
  • a soft pitch or normal pitch is obtained as a residue, from which hard pitches are produced by further distillation, if appropriate with introduction of a carrier gas or application of low pressures.
  • the pitches are also mixed with one another or with coal tar fractions.
  • Coal tar pitches contain substances that can cause health damage if used improperly.
  • One of the longest known and best researched compounds in coal tar pitch is the carcinogen benzo [a] pyrene (3,4-benzopyrene).
  • the Legislators have taken this hazard potential into account by specifying that coal tar pitches with a benzo [a] pyrene (BaP) content of more than 50 ppm must be labeled as hazardous substances and handled with appropriate caution.
  • the BaP content of normal pitches is between 10,000 and 14,000 ppm.
  • Hard pitches obtained by oxidation or distillation contain about 4,000 to 12,000 ppm BaP.
  • coal tar pitches are replaced in some areas by other bituminous distillation residues or resins, despite the poorer property profiles of the products manufactured.
  • bitumen as a binder for hard coal briquettes or stones in road construction or phenolic resins as a binder in the refractory industry.
  • coal tar which contains about 50% by weight of normal pitch.
  • the aim should be to utilize the beneficial application potential of pitch while reducing the risk to humans during processing.
  • coal tar pitch which contains less than 50 ppm of benzo [a] pyrene.
  • Such evaporators are, for example, trickle film evaporators, thin-film evaporators and evaporators with rotating inserts, as are described in EP 0 299 222 A1.
  • the mean residence time of the pitch material must be very short. For this reason, the average residence time in Example 1 at the lowest treatment temperature is also less than 1 min. Similar short residence times are also observed in the other examples, as a comparison of the throughputs shows.
  • the pitch according to Example 2 still contains 140 ppm benzo [a] pyrene and is therefore subject to labeling. Since the pressure here was 1 mbar and the distillation temperature at 361 ° C was in the range from 300 to 380 ° C, the result shows the importance of the residence time for the removal of benzo [a] pyrene.
  • optical anisotropy was determined on pieces of pitch embedded in epoxy resin after grinding and polishing with the overhead polarizing microscope using a suitable video camera with automatic image analysis.
  • thermomechanical analysis to characterize the softening behavior of the pitches was carried out on pressed pitch powders (diameter 7 mm, height 1.2 mm) with the Mettler combination TA3000 / TMA40 with a contact force of 0.05 N and a heating rate of 5 K / min under N2- Shielding gas.
  • the characteristic temperatures given were defined as follows: the start of melting corresponds to a penetration of the penetration probe of 5 ⁇ m; the melting end of a 1 mm penetration.
  • the resulting pitch is characterized by the following analysis data: TI 50.5% QI 10.2% ⁇ -resins 40.3% Coking residue 83.3% BaP content 35 ppm Start of melting (TMA) 156 ° C Melting end (TMA) 194 ° C optical anisotropy 0.0%
  • Example 1 The pitch from Example 1 is distilled under the same conditions as in Example 1 but with a distillation temperature of 340 ° C.
  • the resulting pitch is characterized by the following analysis data: TI 62.7% QI 12.2% ⁇ -resins 50.5% Coking residue 88.5% BaP content 20 ppm Start of melting (TMA) 193 ° C Melting end (TMA) 237 ° C optical anisotropy 0.0%
  • Example 1 The pitch from Example 1 is distilled under the same conditions as in the previous examples but with a distillation temperature of 380 ° C.
  • the resulting pitch is characterized by the following analysis data: TI 70.8% QI 14.6% ⁇ -resins 56.2% Coking residue 92.3% BaP content 20 ppm Start of melting (TMA) 220 ° C Melting end (TMA) 266 ° C optical anisotropy 0.0%
  • the pitches from Examples 1 to 3 can be used directly as binders if an appropriate mixing temperature is set. Direct use as an impregnating agent for porous structures (e.g. composites) is also possible. In pyrolysis, the pitches result in an isotropic binder coke structure and thus high strength of the end products. If direct use is not possible for technical reasons, the viscosity of the pitches from Examples 1 to 3 can be reduced with compatible BaP-poor oils.
  • Example 2 72 parts by weight of the coal tar pitch from Example 1 are dissolved in 28 parts by weight of anthracene oil (40 ppm benzo [a] pyrene, boiling range 290 to 370 ° C.) at 200 ° C. to produce an electrode binder.
  • anthracene oil 40 ppm benzo [a] pyrene, boiling range 290 to 370 ° C.
  • the resulting binder pitch has the following properties: EPM 111.5 ° C TI 38.5% QI 7.7% ⁇ -resins 30.8% Coking residue 63.8% BaP content 40 ppm Start of melting (TMA) 50 ° C Melting end (TMA) 85 ° C optical anisotropy 0.0%
  • the ⁇ -resins are usually in the range between 20 and 25% for electrode binders.
  • the coking residue is higher than expected.
  • this new pitch has an extremely low content of only 40 ppm.
  • binders can also be produced, for example, for the briquetting of hard coal, for taphole fillings and for refractory compounds and impregnating agents.
  • a benzo [a] low pyrene oil u. a. a fraction from the residual oil of the pyrolysis of petroleum fractions can be used for the production of olefins.
  • Example 2 60 parts by weight of the coal tar pitch from Example 1 are dissolved in 25 parts by weight of coal tar oil with a boiling range of 230 to 290 ° C. and 15 parts by weight of a toluene / xylene mixture. In this way, a fungicidal, fast-drying coating for waterproofing structures with high root resistance is obtained.

Landscapes

  • 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)
  • Compositions Of Macromolecular Compounds (AREA)
  • Paints Or Removers (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
  • Fats And Perfumes (AREA)

Claims (6)

  1. Brai de goudron de houille présentant une anisotropie optique inférieure à 2%, caractérisé en ce qu'il contient moins de 50 ppm de benzo[a]pyrène.
  2. Procédé de fabrication d'un brai de goudron de houille selon la revendication 1 par distillation de goudron de houille dans une première étape de distillation à la pression normale ou sous pression réduite et distillation du résidu de la première étape de distillation dans un évaporateur sous une pression non supérieure à 1 mbar, caractérisé en ce que la température dans l'évaporateur se situe dans la plage de température de 300 à 380°C et que le temps de séjour moyen du résidu s'élève de 2 à 10 min., l'évaporateur présentant une surface d'évaporation spécifique de 330 à 10.000 m²/m³.
  3. Procédé selon la revendication 2, caractérisé en ce que le résidu de distillation issu de l'évaporateur est mélangé avec une huile fortement aromatique, pauvre en benzo[a]pyrène.
  4. Utilisation du brai de goudron de houille selon la revendication 1 en tant que liant ou agent d'imprégnation.
  5. Utilisation du brai de goudron de houille selon la revendication 1 pour la fabrication de peintures.
  6. Utilisation du brai de goudron de houille selon la revendication 1 pour la fabrication d'agents d'étanchéité pour le bâtiment résistant au percement des racines.
EP92102398A 1991-04-20 1992-02-13 Brai de goudron de houille, sa préparation et son utilisation Expired - Lifetime EP0510315B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4112955 1991-04-20
DE4112955A DE4112955A1 (de) 1991-04-20 1991-04-20 Steinkohlenteerpech, seine herstellung und verwendung

Publications (2)

Publication Number Publication Date
EP0510315A1 EP0510315A1 (fr) 1992-10-28
EP0510315B1 true EP0510315B1 (fr) 1994-08-31

Family

ID=6430010

Family Applications (1)

Application Number Title Priority Date Filing Date
EP92102398A Expired - Lifetime EP0510315B1 (fr) 1991-04-20 1992-02-13 Brai de goudron de houille, sa préparation et son utilisation

Country Status (8)

Country Link
US (1) US5262043A (fr)
EP (1) EP0510315B1 (fr)
JP (1) JP3105997B2 (fr)
AT (1) ATE110765T1 (fr)
DE (2) DE4112955A1 (fr)
DK (1) DK0510315T3 (fr)
ES (1) ES2034934T3 (fr)
GR (1) GR920300121T1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3326982A1 (fr) 2016-11-29 2018-05-30 RÜTGERS Germany GmbH Corps de moule réfractaires liés au carbone et procédé de fabrication correspondant

Families Citing this family (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5746906A (en) * 1995-08-10 1998-05-05 Koppers Industries, Inc. Coal tar pitch blend having low polycyclic aromatic hydrocarbon content and method of making thereof
FR2760637B1 (fr) * 1997-03-11 1999-05-28 Fabre Pierre Dermo Cosmetique Extrait de goudron de houille a teneur reduite en hydrocarbures aromatiques, procede d'obtention et preparations dermo-cosmetiques
EP0957150A1 (fr) * 1998-05-15 1999-11-17 Carbochimica S.p.A. Goudron et/ou huile de brai ayant une faible teneur à des substances aromatiques polycycliques et procédé de préparation
US6352637B1 (en) 1998-12-31 2002-03-05 Marathon Ashland Petroleum, Llc High coking value pitch
US6361591B1 (en) 1998-12-31 2002-03-26 Marathon Ashland Petroleum Llc Sealer from asphalt and pitch
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
DE102004002561B4 (de) 2004-01-17 2009-09-17 Rütgers Chemicals AG Herstellung von umweltfreundlichen kohlenstoffgebundenen Feuerfesterzeugnissen im Kaltmischverfahren
US8226816B2 (en) * 2006-05-24 2012-07-24 West Virginia University Method of producing synthetic pitch
US20080072476A1 (en) * 2006-08-31 2008-03-27 Kennel Elliot B Process for producing coal liquids and use of coal liquids in liquid fuels
AT505227B1 (de) * 2007-05-09 2012-07-15 Siemens Vai Metals Tech Gmbh Verfahren zur herstellung von formlingen
US8597382B2 (en) 2007-05-24 2013-12-03 West Virginia University Rubber material in coal liquefaction
US8449632B2 (en) 2007-05-24 2013-05-28 West Virginia University Sewage material in coal liquefaction
US8465561B2 (en) 2007-05-24 2013-06-18 West Virginia University Hydrogenated vegetable oil in coal liquefaction
US20120097580A1 (en) 2007-05-24 2012-04-26 Quantex Research Corporation Method of Obtaining a High Quality Coke from Low Rank Coal Liquefaction
BRPI0800466B1 (pt) * 2008-03-05 2016-05-17 Saint Gobain Cerâmicas & Plásticos Ltda processo de desenvolvimento de um sistema de ligação ecológico para uma massa refratária
EP2703523B1 (fr) 2012-08-31 2016-10-12 RÜTGERS Germany GmbH Fabrication d'une électrode de carbone améliorée
CN104593032B (zh) * 2015-01-12 2018-07-06 中钢集团鞍山热能研究院有限公司 一种环保沥青及其制备方法
CN104593033B (zh) * 2015-01-12 2018-05-08 中钢集团鞍山热能研究院有限公司 一种高性能环保沥青的制备方法
CN109135789B (zh) * 2018-08-16 2021-09-28 中钢集团鞍山热能研究院有限公司 一种中低温煤焦油制备针状焦的方法
US11248172B2 (en) 2019-07-23 2022-02-15 Koppers Delaware, Inc. Heat treatment process and system for increased pitch yields
EP4110886A4 (fr) 2020-02-24 2024-03-13 Carbon Holdings Intellectual Properties, LLC Systèmes et procédés de fabrication d'hydrocarbures à haut point de fusion à partir du charbon
EP4215481A1 (fr) * 2022-01-24 2023-07-26 Rain Carbon bv Matériau précurseur de carbone amélioré

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2066386A (en) * 1930-10-03 1937-01-05 Barrett Co Distillation product
GB616730A (en) * 1946-09-10 1949-01-26 Thomas Owston Wilton Improvements in the production of hard pitch and oils from medium soft coal tar pitch
CA1236789A (fr) * 1985-01-08 1988-05-17 Carbochem Inc. Brais faible volatilite
DE3702720A1 (de) * 1987-01-30 1988-08-11 Bergwerksverband Gmbh Pechmaterial aus kohleteerpech, verfahren zu dessen herstellung sowie verwendung des pechmaterials

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3326982A1 (fr) 2016-11-29 2018-05-30 RÜTGERS Germany GmbH Corps de moule réfractaires liés au carbone et procédé de fabrication correspondant
WO2018099853A1 (fr) 2016-11-29 2018-06-07 Rütgers Germany GmbH Procédé pour produire un corps moulé réfractaire à liaison carbone, et corps moulé réfractaire

Also Published As

Publication number Publication date
GR920300121T1 (en) 1993-03-16
ES2034934T1 (es) 1993-04-16
JPH05125366A (ja) 1993-05-21
DE4112955A1 (de) 1992-10-22
JP3105997B2 (ja) 2000-11-06
ATE110765T1 (de) 1994-09-15
DE59200428D1 (de) 1994-10-06
US5262043A (en) 1993-11-16
ES2034934T3 (es) 1994-12-16
EP0510315A1 (fr) 1992-10-28
DK0510315T3 (da) 1994-10-03

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