EP0284501B1 - Imprägnierpech mit verbesserter Filtrierbarkeit und dessen Herstellung - Google Patents

Imprägnierpech mit verbesserter Filtrierbarkeit und dessen Herstellung Download PDF

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Publication number
EP0284501B1
EP0284501B1 EP19880400643 EP88400643A EP0284501B1 EP 0284501 B1 EP0284501 B1 EP 0284501B1 EP 19880400643 EP19880400643 EP 19880400643 EP 88400643 A EP88400643 A EP 88400643A EP 0284501 B1 EP0284501 B1 EP 0284501B1
Authority
EP
European Patent Office
Prior art keywords
pitch
equal
quinoline
weight
content
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
EP19880400643
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English (en)
French (fr)
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EP0284501A1 (de
Inventor
Pierre Couderc
Serge Buche
Jean Louis Saint-Romain
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.)
Arkema France SA
Original Assignee
Elf Atochem SA
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Publication date
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Application filed by Elf Atochem SA filed Critical Elf Atochem SA
Priority to AT88400643T priority Critical patent/ATE58549T1/de
Publication of EP0284501A1 publication Critical patent/EP0284501A1/de
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Classifications

    • 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
    • C10C1/19Working-up tar by thermal treatment not involving distillation

Definitions

  • the present invention relates to pitches, in particular the pitches of coal tar, which are intended to be used as impregnating agents for carbon or graphite parts, with the aim of increasing their density and their mechanical strength.
  • pitches in particular the pitches of coal tar, which are intended to be used as impregnating agents for carbon or graphite parts, with the aim of increasing their density and their mechanical strength.
  • these pitches will be designated by the expression "impregnation pitches”.
  • the essential criterion for the success of an impregnation pitch is constituted by another measure specific to pitches of this type because it reflects the quality of impregnation of the pitch, namely, the filtration speed (or index of filterability).
  • the filterability indices have here been determined by the following method:
  • the present invention firstly relates to an impregnation pitch having a softening point KS of between approximately 60 ° and 80 ° C., and a content of substances insoluble in quinoline less than or equal to 7% by weight approximately by weight , characterized in that its filterability index is greater than or equal to 4.5.
  • the impregnation pitch according to the invention has a fixed carbon content at least equal to 46% by weight, and the substances insoluble in quinoline comprise a substantial proportion of mesophase particles of size between 8 and 10 ⁇ m.
  • the invention also relates to a method of manufacturing an impregnation pitch as defined above, characterized in that one submits in tar or else a soft pitch, that is to say a pitch having a softening point KS at most equal to 60 ° C, and a content of substances insoluble in quino leine at most equal to 7% by weight, to a heat treatment capable of eliminating a substantial part of its constituents of molecular mass less than 1200, said heat treatment being carried out at a temperature between 350 and 430 ° C and for a period from 1 to 50 hours.
  • a soft pitch that is to say a pitch having a softening point KS at most equal to 60 ° C, and a content of substances insoluble in quino leine at most equal to 7% by weight
  • the above-mentioned treatment is followed by flash distillation.
  • the duration will be chosen the longer the lower the temperature.
  • the temperature will be in particular between 400 ° C and 420 ° C and the duration of treatment will be in particular between 2 and 7 hours.
  • impregnation pitches are prepared as follows: the pitch of Example 1 (comparative) is obtained by direct distillation of the coal tar, without heat treatment; the pitches of Examples 2 to 5 (in accordance with the invention) are prepared by subjecting the pitch of Example 1 to a heat treatment at temperature T (expressed in ° C) and for the duration t (expressed in hours) indicated in the table below, then a flash distillation.
  • T expressed in ° C
  • t expressed in hours
  • the molar masses of the pitches are determined by gel permeation chromatography in 1,2,4-trichloro benzene at 135 ° C.
  • the calibration is carried out using pitch fractions which have been collected by preparative CPG and whose molecular weights have been determined by osmometry.
  • the area S obtained is then calculated by integrating the peak (s) of the curve in FIG. 1c and the corresponding curves for the pitches of Examples 2 to 4, between the values 300 and 1200 of the molecular masses; these surfaces are plotted on the ordinate, with, on the abscissa, in a corresponding manner, the filterability indices I, which makes it possible to plot the curve of FIG. 2. It can be seen that the improvement in the filterability index of a pitch is all the greater as the elimination of the aforementioned products is important.
  • the percentages of the largest particles are plotted on the ordinate for each of the pitches analyzed, and, on the abscissa, the filterability indices I correspondingly, which gives the curve of the figure. 3. It can thus be seen that the filterability index 1 gradually increases with the percentage of these particles, which are representative of the mesophase.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Working-Up Tar And Pitch (AREA)
  • Filtering Materials (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Ceramic Products (AREA)
  • Reinforced Plastic Materials (AREA)
  • Inorganic Fibers (AREA)
  • Stringed Musical Instruments (AREA)
  • Materials For Medical Uses (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Claims (5)

1. lmprägnierpech, welches einen Erweichungspunkt KS zwischen einschließlich 60°C und 80°C und einen Gehalt an in Chinolin unlöslichen Substanzen unterhalb oder gleich 7 Gew.-% aufweist, dadurch gekennzeichnet, daß sein Filtrierbarkeitsindex größer oder gleich 4,5, sein Gehalt an nach der ISO 6998 Norm bestimmten festen Kohlenstoff mindestens 46 Gew.-% ist und die in Chinolin unlöslichen Substanzen einen wesentlichen Anteil an Mesophasenteilchen mit einer Größe zwischen einschließlich 8 und 10 wm umfassen.
2. Imprägnierpech nach Anspruch 1, dadurch gekennzeichnet, dass es frei von Produkten mit einer Molekülmasse zwischen einschließlich 300 und 1200 ist.
3. Verfahren zur Herstellung eines Imprägnierpechs nach einem der Ansprüche 1 und 2, dadurch gekennzeichnet, dass man ein Pech, welches einen Erweichungspunkt KS von höchstens gleich 60°C und einen Gehalt an in Chinolin unlöslichen Substanzen unterhalb oder gleich 7 Gew.-% aufweist, einer Wärmebehandlung unterwirft, die geeignet ist, einen wesentlichen Teil seiner Bestandteile mit einer Molekülmasse unter 1200 zu entfernen, wobei die genannte Wärmebehandlung bei einer Temperatur zwischen einschließlich 350°C und 430°C und während eines Zeitraumes von 1 bis 50 h durchgeführt wird.
4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, daß die genannte Behandlung bei einer Temperatur zwischen einschließlich 400° und 420°C durchgeführt wird.
5. Verfahren nach einem der Ansprüche 3 und 4, dadurch gekennzeichnet, daß die genannte Behandlung während eines Zeitraumes von 2 bis 7 h durchgeführt wird.
EP19880400643 1987-03-20 1988-03-18 Imprägnierpech mit verbesserter Filtrierbarkeit und dessen Herstellung Expired - Lifetime EP0284501B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88400643T ATE58549T1 (de) 1987-03-20 1988-03-18 Impraegnierpech mit verbesserter filtrierbarkeit und dessen herstellung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8703927A FR2612525B1 (fr) 1987-03-20 1987-03-20 Brai d'impregnation a filtrabilite amelioree et son procede de fabrication
FR8703927 1987-03-20

Publications (2)

Publication Number Publication Date
EP0284501A1 EP0284501A1 (de) 1988-09-28
EP0284501B1 true EP0284501B1 (de) 1990-11-22

Family

ID=9349268

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19880400643 Expired - Lifetime EP0284501B1 (de) 1987-03-20 1988-03-18 Imprägnierpech mit verbesserter Filtrierbarkeit und dessen Herstellung

Country Status (10)

Country Link
US (1) US4997542A (de)
EP (1) EP0284501B1 (de)
JP (1) JPS6414296A (de)
AT (1) ATE58549T1 (de)
BR (1) BR8801342A (de)
CA (1) CA1304198C (de)
DE (1) DE3861103D1 (de)
ES (1) ES2018618B3 (de)
FR (1) FR2612525B1 (de)
GR (1) GR3001462T3 (de)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5326457A (en) * 1992-08-06 1994-07-05 Aristech Chemical Corporation Process for making carbon electrode impregnating pitch from coal tar
US5695631A (en) * 1993-06-04 1997-12-09 Mitsubishi Chemical Corporation Process for producing petroleum needle coke
JP6274390B2 (ja) * 2012-10-24 2018-02-07 東海カーボン株式会社 リチウム二次電池負極材用黒鉛粉末の製造方法

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3835024A (en) * 1971-03-19 1974-09-10 Osaka Gas Co Ltd Method for manufacturing pitch
US3692663A (en) * 1971-03-19 1972-09-19 Osaka Gas Co Ltd Process for treating tars
US3970542A (en) * 1971-09-10 1976-07-20 Cindu N.V. Method of preparing electrode pitches
NL7305172A (de) * 1973-04-13 1974-10-15
US4086156A (en) * 1974-12-13 1978-04-25 Exxon Research & Engineering Co. Pitch bonded carbon electrode
NL183771C (nl) * 1976-06-23 1989-01-16 Cindu Chemie Bv Werkwijze voor de bereiding van een bindmiddelpek, alsmede gevormd voorwerp, verkregen onder toepassing van een volgens de werkwijze bereid bindmiddelpek.
JPS533764A (en) * 1976-07-01 1978-01-13 Seiko Instr & Electronics Ltd Low power consumption oscillating circuit
US4096056A (en) * 1976-10-21 1978-06-20 Witco Chemical Corporation Method of producing an impregnating petroleum pitch
JPS5360927A (en) * 1976-11-12 1978-05-31 Nippon Oil Co Ltd Continuous method of manufacturing petroleum pitch
JPS5944352B2 (ja) * 1978-02-28 1984-10-29 ユニオン・カ−バイド・コ−ポレ−シヨン ピツチの製造法
US4369171A (en) * 1981-03-06 1983-01-18 Great Lakes Carbon Corporation Production of pitch and coke from raw petroleum coke
GB2110232B (en) * 1981-11-18 1986-05-08 Nippon Oil Co Ltd Process for the production of ethane
US4664774A (en) * 1984-07-06 1987-05-12 Allied Corporation Low solids content, coal tar based impregnating pitch

Also Published As

Publication number Publication date
FR2612525A1 (fr) 1988-09-23
EP0284501A1 (de) 1988-09-28
JPS6414296A (en) 1989-01-18
US4997542A (en) 1991-03-05
BR8801342A (pt) 1988-11-01
FR2612525B1 (fr) 1989-05-19
ES2018618B3 (es) 1991-04-16
CA1304198C (fr) 1992-06-30
ATE58549T1 (de) 1990-12-15
DE3861103D1 (de) 1991-01-03
GR3001462T3 (en) 1992-10-08

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