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
  • C10C1/19—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.
• Koh leteerpech is z. 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 shaped 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 made of coal tar pitch which has the following parameters: a) a mesophase content of ⁇ 2%,
• the material is outstandingly processable without the risk of premature coking or thermal decomposition.
• the new pitch material also surprisingly has a very high coke yield of 80 to> 90%, which is extraordinarily good for pitch material made of 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 .
• coal tar pitch is used as the starting material, which contains up to 10% solids, such as ash, Charcoal particles containing quinoline insoluble (primary ⁇ -resins) and a softening point ⁇ 100 o C,
• filter aid such as diatomaceous earth, activated carbon, or the like.
• the filtrate is concentrated in a thin film evaporator in the temperature range above 300 ° C. to approximately 425 ° C. and under a pressure of ⁇ 10 mbar.
• the new pitch material can surprisingly be produced from conventional 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, optionally using filter aids can consist of ash, carbon particles and components that are not quinoline-soluble (primary ⁇ -resins), surprisingly, the so-cleaned pitch can be processed in thin-film evaporators under vacuum ⁇ 10 mbar and in the temperature range above 300 ° C without problems to the new pitch material, which as Concentrate is produced.
• the by-products separated as distillates also have excellent properties which make them particularly suitable for use as an admixture component for tars, pitches and oils.
• the process 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 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 good, for example, 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 which have been produced from conventional pitch material can be converted into high-strength molded articles by means of a few impregnants.
• the new pitch material is also very suitable as a binder for carbon-containing materials.
• the raw coal tar or the hard 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 a washing device.
• a hot filter stage 1 which can consist of a candle filter with dry filter cake discharge or a plate filter with a 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 non-evaporated product portion 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 impregnating pitch for pitch coke, as a binder for shaped carbon bodies or as clay pigeon pitch.
• distillate produced which can still be fractionated in the usual way, is suitable, for example, for the following applications:
• Admixture component for tars especially for solids-containing tars
• Admixture component for pitches for pitches (fluxing agents); Mixing component for oils.
• the following shows three examples of 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 obtain the fractions with low Remove softening point and get a concentrate pitch with 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 constantly 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 the filtration, practically all of the quinoline-insoluble components had been 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 their direction of flow was determined. This involved mechanical self-cleaning.
• 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 / (m 2 .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 experimental set-up were the same as in Example 1, but the temperature of the heat treatment was raised to 361 ° C.
• the specific throughput reached 74.3 kg / (m 2 .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 / (m 2 .h).
• the yield was 27.6% by weight and the concentrate had a softening point of 292 ° C.
• the other substance-specific properties were as follows:

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• 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)
• Carbon And Carbon Compounds (AREA)
• Compositions Of Macromolecular Compounds (AREA)

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• 1987
  • 1987-01-30 DE DE19873702720 patent/DE3702720A1/de active Granted
• 1988
  • 1988-01-16 AT AT88100584T patent/ATE62924T1/de not_active IP Right Cessation
  • 1988-01-16 DE DE8888100584T patent/DE3862472D1/de not_active Expired - Fee Related
  • 1988-01-16 JP JP63501454A patent/JPH02502648A/ja active Pending
  • 1988-01-16 AU AU11895/88A patent/AU601020B2/en not_active Ceased
  • 1988-01-16 US US07/397,486 patent/US5128021A/en not_active Expired - Fee Related
  • 1988-01-16 ES ES88100584T patent/ES2022467B3/es not_active Expired - Lifetime
  • 1988-01-16 EP EP88901243A patent/EP0346347A1/de active Pending
  • 1988-01-16 WO PCT/EP1988/000031 patent/WO1988005806A1/de not_active Application Discontinuation
  • 1988-01-16 EP EP88100584A patent/EP0276711B1/de not_active Expired - Lifetime
  • 1988-01-27 DD DD88312468A patent/DD279892A5/de not_active IP Right Cessation
  • 1988-01-30 CN CN198888100544A patent/CN88100544A/zh active Pending
• 1989
  • 1989-07-28 RU SU894614698A patent/RU1826985C/ru active
• 1991
  • 1991-04-25 GR GR91400522T patent/GR3001859T3/el unknown
  • 1991-12-27 RU SU915010830A patent/RU1838375C/ru active

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