EP1739153B1 - Method for the production of brea from tar and the distillates thereof arising from coal tar by oxidative thermal treatment - Google Patents

Method for the production of brea from tar and the distillates thereof arising from coal tar by oxidative thermal treatment Download PDF

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Publication number
EP1739153B1
EP1739153B1 EP05708091A EP05708091A EP1739153B1 EP 1739153 B1 EP1739153 B1 EP 1739153B1 EP 05708091 A EP05708091 A EP 05708091A EP 05708091 A EP05708091 A EP 05708091A EP 1739153 B1 EP1739153 B1 EP 1739153B1
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EP
European Patent Office
Prior art keywords
thermal treatment
pitch
tar
distillation
oxygen
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.)
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Application number
EP05708091A
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German (de)
English (en)
French (fr)
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EP1739153A2 (en
Inventor
Manuel Olivo Gonzalez Garcia
Manuel José GONZALEZ CIMAS
Juan José FERNANDEZ RODRIGUEZ
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.)
Industrial Quimica del Nalon SA
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Industrial Quimica del Nalon SA
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Priority to PL05708091T priority Critical patent/PL1739153T3/pl
Publication of EP1739153A2 publication Critical patent/EP1739153A2/en
Application granted granted Critical
Publication of EP1739153B1 publication Critical patent/EP1739153B1/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10CWORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
    • C10C1/00Working-up tar
    • C10C1/04Working-up tar by distillation
    • C10C1/16Winning of pitch

Definitions

  • the invention relates to a process for producing pitches, in particular those suitable for use as carbon precursors, from coal tars and distillates thereof, through a sequential and combined operation in three steps:
  • coal tar is a byproduct from coke batteries makes this raw material a highly inconsistent product, and this drawback is only compensable through the formulation of suitable tar blends.
  • all types of tars and, consequently, pitches obtained thereby have solid particles in suspension (primary and secondary QI, and carry-over), besides different types of metallic sludge identifiable by its ashes content. Both pollutants prejudice pitch quality and/or decrease its potential application in advanced carbon materials.
  • Anthracene oil is obtained along distillation of coal tar and is characterized by its distillation range, which is comprised from about 260° C until the corresponding temperature for adjusting the softening point of the pitch obtained as a final product (generally 400-410° C).
  • Anthracene oil is mostly constituted by aromatic hydrocarbons of 2-4 benzene rings and the corresponding heterocyclics with O, N and S, phenanthrene, anthracene, fluoranthene, carbazole and pyrene being the main components.
  • Patent US 4892642 discloses the production of pitches from coal tars in three steps: an oxidative thermal treatment by 350-400° C and 1-3 atm, a thermal treatment under inert atmosphere and a fractional distillation.
  • Patent EP-A-0167046 discloses the production of a pitch with low content in solids by means of oxidation with air or oxygen of a distillation fraction selected from coal tar or a heavy oil derived thereof, while heated at preferred temperatures of 315-385° C, though the possibility of operating at a lower temperature (149° C) is mentioned, until obtaining a desired intermediate product.
  • This intermediate product is then submitted to distillation by stripping with steam or an inert gas, although said distillation could be avoided by using higher temperatures in the oxidation phase.
  • the result is an impregnating pitch especially useful in the manufacture of electrodes.
  • the process according to the invention in comparison with the prior art, starts with a wider range of raw materials, including petrochemical aromatic fractions.
  • Pitches obtained in accordance with the invention when compared with those of the prior art, present a higher intrinsic quality and improved properties in relation to health (carcinogenesis) and environment.
  • the resulting pitch can generate cokes which when observed under optical microscopy with polarized light, can appear as 100% anisotropic or 100% isotropic, depending on the properties of the pitch receiving interest.
  • pitches are suitable for applications belonging to the field of carbon precursors and in particular are useful in the manufacture of electrodes for aluminium industry, graphite electrodes and synthetic graphite in general, binders for refractory industry, waterproof materials and electrometallurgical paste.
  • anthracene oil may be directly put in commerce, in accordance with the usual applications of said raw material obtained by tar distillation. Additionally, the increase of anthracene/phenanthrene concentration, as a consequence of these being poorly reactive components, would provoke that said fraction could promote the actual interest in the manufacture of anthracene paste.
  • raw material it is used anthracene oil arising from coal tar distillation with the following average characteristics (non-limitative aspect):
  • Raw material Anthracene oil Origin Distillation of high temperature tar Distillation range (BS144) > 260° C Density (ASTM D1298) > 1.120 g/cm 3 (20° C) Ashes (ASTM D482) ⁇ 0.02% Toluene insolubles (BS144) ⁇ 0.1% C/H atomic ratio (ASTM D5291) > 1.30
  • different carbochemical fractions can be used by means of widening or narrowing the proposed distillation range, with no inconvenient for the quality of the product.
  • the sole substantial variation to be obtained will be that derived from a higher or lower yield in the process.
  • reaction must be conducted under vigilance in order to avoid the formation of gums and cross-linked structures. It is recommendable to maximize the temperature and reduce the conversion to a single step.
  • the resulting pitch would be suitable for its application as a binder pitch for electrodes in aluminium industry.
  • a greater ratio of quinoline insolubles is required, it is possible to prepare blends with a carbochemical pitch with high insolubles content, in which case there would be obtained a pitch with improved beta-resin and fixed carbon (normalized to the insolubles level) parameters.
  • Example 2 Standard pitch Example 4 Softening point (ASTM D3104) °C, Mettler 90 90 90 Flash point (ASTM D92) °C, COC 276 250-270 272 Toluene insolubles (ISO 6376) % 25.3 15.0 23.8 Quinoline insolubles (ASTM D2318) % 0.4 0.8 0.5 Beta-resin % 24.9 14.2 23.3 Fixed carbon (CRDG-B10) %, Sers 43.1 40.1 42.0 Filtration rate g, 80 min 59 (6 min) 15-20 67 (55 min) Ashes (ASTM D2415) % ⁇ 0.01 0.1 ⁇ 0.01

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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)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Carbon And Carbon Compounds (AREA)
EP05708091A 2004-02-20 2005-02-17 Method for the production of brea from tar and the distillates thereof arising from coal tar by oxidative thermal treatment Active EP1739153B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL05708091T PL1739153T3 (pl) 2004-02-20 2005-02-17 Sposób wytwarzania paku ze smoły oraz jej destylatów powstałych ze smoły węglowej przez tlenową obróbkę termiczną

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ES200400421A ES2238931B1 (es) 2004-02-20 2004-02-20 Procedimiento de obtencion de breas a partir de alquitranes y sus destilados procedentes del alquitran de hulla, mediante tratamiento termico oxidativo.
PCT/ES2005/000079 WO2005079136A2 (es) 2004-02-20 2005-02-17 Procedimiento de obtención de breas a partir de alquitranes y sus destilados procedentes del alquitrán de hulla, mediante tratamiento térmico oxidativo

Publications (2)

Publication Number Publication Date
EP1739153A2 EP1739153A2 (en) 2007-01-03
EP1739153B1 true EP1739153B1 (en) 2011-09-07

Family

ID=34878432

Family Applications (1)

Application Number Title Priority Date Filing Date
EP05708091A Active EP1739153B1 (en) 2004-02-20 2005-02-17 Method for the production of brea from tar and the distillates thereof arising from coal tar by oxidative thermal treatment

Country Status (11)

Country Link
EP (1) EP1739153B1 (pl)
JP (1) JP2007525578A (pl)
KR (1) KR20070044800A (pl)
CN (1) CN1957061A (pl)
AT (1) ATE523579T1 (pl)
BR (1) BRPI0507215B1 (pl)
CA (1) CA2556482C (pl)
DK (1) DK1739153T3 (pl)
ES (2) ES2238931B1 (pl)
PL (1) PL1739153T3 (pl)
WO (1) WO2005079136A2 (pl)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11248172B2 (en) 2019-07-23 2022-02-15 Koppers Delaware, Inc. Heat treatment process and system for increased pitch yields

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
US8747651B2 (en) * 2008-05-22 2014-06-10 Graftech International Holdings Inc. High coking value pitch
RU2477744C1 (ru) * 2011-11-29 2013-03-20 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Башкирский государственный университет" Способ получения нефтяных пеков
JP6076147B2 (ja) * 2013-03-11 2017-02-08 株式会社クレハ 高軟化点ピッチの製造方法
KR102207835B1 (ko) * 2013-12-23 2021-01-26 재단법인 포항산업과학연구원 콜타르의 증류 유분을 이용한 탄소소재용 핏치의 제조방법 및 이를 이용하여 제조된 탄소소재용 핏치
CN108003910B (zh) * 2016-10-27 2020-06-19 宝武炭材料科技有限公司 一种高软化点环保沥青的制备方法、沥青及应用
CN107446606B (zh) * 2017-08-30 2024-01-23 西北大学 一种煤焦油生产改质沥青、脂肪烃与芳香烃的工艺及装置
KR102202219B1 (ko) * 2018-12-13 2021-01-12 재단법인 한국탄소융합기술원 카본블록 밀도화 방법
CN111518583B (zh) * 2020-04-20 2021-03-05 华中科技大学 一种固废热解液相产物熔盐梯级处理除杂提质装置
RU2744579C1 (ru) * 2020-06-01 2021-03-11 Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" Способ получения связующего пека

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4146048A (en) * 1977-05-02 1979-03-27 Prefco Productions, Inc. Fire damper and method of fabrication
GB2115437B (en) * 1982-02-15 1985-10-02 Nippon Oil Co Ltd Pitch for carbon fibers
US4664774A (en) * 1984-07-06 1987-05-12 Allied Corporation Low solids content, coal tar based impregnating pitch
US4892642A (en) * 1987-11-27 1990-01-09 Conoco Inc. Process for the production of mesophase

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11248172B2 (en) 2019-07-23 2022-02-15 Koppers Delaware, Inc. Heat treatment process and system for increased pitch yields
US11624029B2 (en) 2019-07-23 2023-04-11 Koppers Delaware, Inc. Heat treatment process for increased pitch yields

Also Published As

Publication number Publication date
JP2007525578A (ja) 2007-09-06
WO2005079136A2 (es) 2005-09-01
KR20070044800A (ko) 2007-04-30
ES2238931B1 (es) 2007-06-16
PL1739153T3 (pl) 2012-03-30
EP1739153A2 (en) 2007-01-03
DK1739153T3 (da) 2012-01-09
WO2005079136A3 (es) 2005-12-29
CA2556482C (en) 2012-11-27
ES2376938T3 (es) 2012-03-21
CA2556482A1 (en) 2005-09-01
CN1957061A (zh) 2007-05-02
ES2238931A1 (es) 2005-09-01
BRPI0507215B1 (pt) 2015-05-26
BRPI0507215A (pt) 2007-06-19
ATE523579T1 (de) 2011-09-15

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