EP0455504B1 - Verkokung von Dekantieröl und anderen Schwerölen zur Herstellung von Nadelkoks höherer Qualität - Google Patents

Verkokung von Dekantieröl und anderen Schwerölen zur Herstellung von Nadelkoks höherer Qualität Download PDF

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Publication number
EP0455504B1
EP0455504B1 EP91304022A EP91304022A EP0455504B1 EP 0455504 B1 EP0455504 B1 EP 0455504B1 EP 91304022 A EP91304022 A EP 91304022A EP 91304022 A EP91304022 A EP 91304022A EP 0455504 B1 EP0455504 B1 EP 0455504B1
Authority
EP
European Patent Office
Prior art keywords
coking
coke
temperature
threshold
drum
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
EP91304022A
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English (en)
French (fr)
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EP0455504A1 (de
Inventor
Harry A. Adams
Stephen C. Paspek
Jeffrey B. Hauser
Sim Romero
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Standard Oil Co
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Standard Oil Co
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Filing date
Publication date
Application filed by Standard Oil Co filed Critical Standard Oil Co
Publication of EP0455504A1 publication Critical patent/EP0455504A1/de
Application granted granted Critical
Publication of EP0455504B1 publication Critical patent/EP0455504B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B55/00—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material

Definitions

  • the invention relates to a process for production of needle-coke used in the manufacture of graphite electrodes for the steel industry. More particularly, this invention relates to a process for making needle-coke having the purity and physical properties necessary to meet the stringent quality criteria of graphite electrodes. Specifically, a low coefficient of thermal expansion (CTE) is one of the most critical parameters of quality coke.
  • CTE coefficient of thermal expansion
  • the needle-coke obtained in practice of the process of the present invention is particularly well-suited for use as graphite electrodes in the steel industry.
  • the low coefficient of thermal expansion found in the coke obtained in practice of the present invention allows for the construction of superior graphite electrodes.
  • references will be made to the use of the needle-coke as used in the production of graphite electrodes for the steel industry, and certain prior art coke cases will be discussed. However, it should be realized that the invention could be used in the production of other coke materials, as well as high quality needle-coke.
  • US Patent No.4,822,479 describes a process that involves calculating a minimum coking severity level based upon the percentage of aromatic-form carbon atoms in the feedstock. An expression is then used to identify minimum coking temperatures, soaking temperatures and reaction times that satisfy the required severity level, and produces coke having CTE and VBD values in the premium coke range.
  • the generally accepted route to needle-coke from an oil is a series of carbonization reactions that first transforms the oil into a pitch, which then forms a liquid crystal called mesophase, which subsequently orients and solidifies into a needle structure. This process is explained in "Optimum Carbonization Conditions Needed to Form Needle-Coke", Mochida, I., Oil and Gas Journal , May 2, 1988.
  • Mochida indicates that to produce low CTE needle-coke, the proper feedstock and proper operating conditions for that feedstock are important. He proposes that to form low CTE content needle-coke it is important to first form small spheres of mesophase pitch, to maintain a sufficiently low viscosity to allow the mesophase spheres to coalesce into large domains, and to produce sufficient gas evolution at the right time in the reaction cycle to orient the mesophase domains into the desired needle-like structure. Failure to meet all of these conditions will lead to a more amorphous structure which has a significantly higher CTE.
  • a new process for making coke has been found by Applicants, wherein unique temperature and reaction times i.e., time at temperature, have been developed to form low CTE needle-coke.
  • Applicants have learned that there is a specific threshold temperature range, above which, coking will result in unexpectedly high CTE values.
  • Applicants have discovered a minimum threshold reaction time, above which further reaction time does not significantly effect the CTE value of the coke. Accordingly, Applicants have established a new and improved coking process, wherein, a high quality low CTE value coke is produced by utilizing temperatures below the threshold temperature range for reaction time sufficient to achieve a low CTE value.
  • One use would then be its conversion into high quality graphite electrodes for the steel industry.
  • a still further object of the present invention is to provide a unique process which operates at the temperature and the time conditions newly discovered which produce high yields of suitable quality needle-coke.
  • the process of this invention comprises introducing a heated petroleum feedstock into a coking drum, maintaining the temperature of the drum contents in a range near but below the CTE threshold temperature during the balance of the filling cycle, and maintaining the temperature of the drum contents at about the same temperature during the post-fill portion of the cycle by passing a heated vapor through the coke drum for sufficient time to allow the drum contents to properly react, orient, and solidify into a solid product with the desired properties.
  • the time at temperature during fill in combination with the vapor introduction time should be at least the threshold reaction time.
  • the threshold temperature basically encompasses the highest temperature at which coke can be produced while maintaining an acceptable CTE.
  • the temperature at which a rapid CTE increase occurs will vary with the feedstock. Generally, however, the magnitude of increase would include a 100% increase in CTE value over a 20°C temperature rise.
  • the drum contents continue to react and orient, forming a product with improved physical properties such as a lower CTE.
  • the time-at-temperature exceeds the threshold reaction time, further improvements in CTE with increasing time are minimal.
  • the process results in more uniform coke, i.e., more consistent CTE values throughout the drum because of a more narrow residence time distribution. Also, the process minimizes reaction time by operating at the highest temperature possible while meeting coke product quality specifications. Accordingly, economic advantages are realized.
  • the generally accepted route to form needle-coke from a hydrocarbon feedstock is a series of carbonization reactions that first transform the oil to a pitch, which then forms a liquid crystal called mesophase, which subsequently orients and solidifies into a needle structure.
  • the present invention is a new and improved process for coke production.
  • the process comprises heating a petroleum feedstock to a temperature necessary to maintain the temperature of the drum contents at a level sufficient for coking but below the threshold temperature and introducing the heated feedstock to a coking drum.
  • a temperature necessary to maintain the temperature of the drum contents at a level sufficient for coking but below the threshold temperature
  • introducing the heated feedstock to a coking drum.
  • This process is enhanced by filling the coking drum as rapidly as the physical constraints of the system allow.
  • a heated vapor is introduced to the coke drum.
  • the vapor is introduced at a temperature sufficient to maintain the contents of the coke drum at a temperature near to but below the threshold temperature.
  • the introduction of the vapor is conducted for at least the threshold reaction time.
  • the formed coke can be stripped using steam, light hydrocarbons, or other solvents and removed from the drum as is known in the art.
  • the feed can be any type of petroleum feedstock.
  • the feedstock is a fluid cat cracker decanted oil, a heavy cycle oil, or a filtered decanted oil.
  • the feedstock is a fluid cat cracker decanted oil.
  • blends of the above feedstocks can be utilized.
  • the temperature to which the feed is heated is determined for each particular feed depending on the desired temperature range of the drum contents to obtain sufficiently low CTE in the product coke to meet product specifications.
  • the threshold temperature is the point at which increased temperature leads to rapidly increasing CTE values.
  • the threshold temperature can in fact cover a range of temperatures of about 10°-20°C over which the CTE value of the coke begins its rapid increase, and above which CTE rapidly increases.
  • the threshold temperature for a given feedstock is also a function of the drum pressure, recycle ratios and other parameters known to one skilled in the art.
  • the coking temperature is preferably in the range of about 400°C to about 600°C. More preferably, the coking temperature is between 420°C and 510°C. Most preferably, the temperature is in the range of about 460°C to about 500°C. However, the temperature is dependent upon the feedstock and must be determined for each individual feedstock. This determination can be accomplished by the process described in the following examples.
  • the temperature in the coke drum is maintained after drum fill by sending a vapor with a low coking tendency through the coke drum.
  • the vapor is a hydrocarbon, steam, nitrogen, refinery gas, carbon dioxide or any inert gases or mixtures thereof. More preferably, the vapor is a refinery derived light hydrocarbon stream for example fluid cat cracker light cycle oil, coker heavy gas oil, or mixtures thereof.
  • the vapor is recycled within the process, wherein the vapor stream is obtained from a bubble tower which is in combination with the coking drum system.
  • the vapor is recycled outside the coker unit operation, i.e., a fractionation tower not in combination vith the coking system.
  • the vapor is used on a once through basis.
  • reaction time is a crucial factor to the production of low CTE value coke. It has been found that insufficient reaction times can lead to insufficient development and solidification of the coke structure leading to significant amounts of sparsely condensed solid pitch which form poor quality coke in a calciner. This material will not meet typical needle-coke specifications. Furthermore, it has been determined that CTE values are not strongly influenced by additional time-at-temperature exceeding a certain minimum reaction time, herein described as the threshold reaction time. More particularly, longer time-at-temperature results in little change in CTE once the threshold reaction time for a particular feedstock at a particular temperature is reached.
  • the reaction time can be adjusted. For example, since the drum is filled gradually, the upper portion of the coke experiences a shorter coking time. Accordingly, it is up to the individual operation to determine if the most beneficial procedure involves coking only a portion of the coke for the threshold reaction time. For example, the lower 90% of the drum, which is filled first, may be coked for the threshold reaction time and form higher quality coke, while the upper 10% of the drum is coked for less than the threshold time and is of lesser quality. The upper 10% may be sacrificed in quality to obtain the lower 90% in a shorter period of time.
  • the experimentation was performed in a micro-coker system.
  • This system consists of a glass tube sealed at one end and filled with the desired coking feedstock.
  • This filled tube is placed in a custom-built 100cc stainless steel pressure vessel.
  • the top of the vessel is sealed by deforming a copper gasket when the screw cap is tightened.
  • the vessel is then connected to a gas/liquid separator and a back pressure regulator.
  • the system is pressurized to the desired operating pressure, and the vessel is placed in a fluidized sandbath set to the desired operating temperature. Gases and vaporized liquids exit through the top of the vessel and are separated in the gas/liquid separator.
  • the 1/8 inch tube connecting the vessel and the separator serves as a heat exchanger to condense the liquids. Gases leave the system through the regulator as it maintains a constant pressure.
  • the six feedstocks as described in Table 1, consisting of decanted oil fractions and blends thereof, were coked at a temperature range of 460°C-525°C for 16 hours.
  • Table II displays the results for the various feedstocks. All of the feedstocks display about the same low CTE value at 480°C or below and about the same high CTE value at 510°C or above.
  • Table II shows a dramatic increase in CTE at temperatures above the threshold temperature.
  • Coke from feedstock 3 shows a dramatic CTE increase from 0.1 to 1.05 X 10 ⁇ 6/°C over only a 15°C temperature increase. This suggests that for feedstock 3, 490°C is already past the threshold maximum coking temperature, while 475°C is below the threshold temperature.
  • the results from the other feedstocks indicate a threshold temperature less than 510°C.
  • the particular threshold temperature for any given feedstock can be determined by this method using micro-coker experiments. More particularly, coking operations can be conducted on a feedstock at gradually increasing temperatures, and the resulting needle-coke can be analyzed to determine CTE values.
  • the threshold temperature point or range will appear as that temperature or temperatures where CTE values rapidly increase with increasing temperature.
  • Reaction time effects on CTE were determined for feedstocks 1 am 2 using the above described micro-coker system.
  • the feedstocks were subjected to varying coking times at at 460°C and 480°C.
  • Three sets of time behavior micro-coking experiments were run, including 8, 16, 64 hour coking times at 460°C coking temperature for feedstock 1.
  • 12 and 16 hour coking time experiments were run for feedstock 2 at a 460°C coking temperature.
  • 8, 10, and 16 hour coking times were tested for feedstock 2 at 480° coking temperature. The results are displayed in Table III.
  • the experiments with feedstock 1 were conducted at short (8-hour) and long (64-hour) coking times at 460°C.
  • the 8 hour experiment was chosen to simulate the coke at the point when solidification was just about complete.
  • the 64 hour experiment was chosen to see if any changes occur to the coke long after solidification.
  • the 8-hour, 460°C run with feedstock 1 did not develop sufficient coke structure and had significant amounts of partially-condensed solid pitch present which formed into low quality coke in the calciner. This is unacceptable for producing quality needle coke, therefore, 8 hours is below the necessary minimum coking time at 460°C for feedstock 1.
  • the threshold reaction time can be determined for any particular feedstock by coking the feedstock at a particular temperature, preferably just below the threshold temperature for various periods of time and analyzing the resultant needle-coke to determine CTE values.
  • the CTE values should decrease over time to the threshold reaction time, at which point, CTE values will change only slightly with increasing time-at-temperature.
  • TABLE III Effect of time at 460°C, and 480°C For Two Feeds Feedstock No. Temperature °C Time (Hours) CTE x 10 ⁇ 6/°C 1 460 8 >1 1 460 16 -.04 1 460 64 -.34 2 460 12 .34 2 460 16 .10 2 480 8 .04 2 480 10 .21 2 480 16 .08

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Coke Industry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Claims (13)

  1. Verfahren zur Bildung von Koks, umfassend
    (a) die Bestimmung der Schwellentemperatur für das Erdöl-Einsatzprodukt durch Messung des thermischen Ausdehnungskoeffizienten des aus dem Einsatzprodukt bei verschiedenen Verkokungs-Temperaturen gebildeten Kokses, wobei die Schwellentemperatur die Verkokungs-Temperatur ist, bei der der thermische Ausdehnungskoeffizient in Verbindung mit einem engen Bereich der Verkokungs-Temperatur schnell ansteigt;
    (b) das Erhitzen des Erdöl-Einsatzproduktes und das Einführen des Erdöl-Einsatzproduktes in eine Verkokungstrommel;
    (c) das Halten des Inhaltes der Verkokungstrommel bei einer Temperatur unterhalb der Schwellentemperatur;
    (d) das Einleiten eines erhitzten Dampfstroms in die Verkokungstrommel, um den Koks bei einer Temperatur zu halten, die ausreichend zum Verkoken ist, aber unterhalb der Schwellentemperatur liegt;
    (e) das Beibehalten des Einleitens des heißen Dampfes für einen Zeitraum, der zum Erreichen einer Schwellen-Reaktionszeit für den Trommelinhalt notwendig ist; und
    (f) das Austragen des Kokses aus der Verkokungstrommel.
  2. Verfahren nach Anspruch 1, wobei das Erdöl-Einsatzprodukt aus der Gruppe, die aus dekantierten Ölen, schweren Kreislaufölen oder Mischungen davon besteht, ausgewählt ist.
  3. Verfahren nach Anspruch 2, wobei das Erdöl-Einsatzprodukt dekantiertes Öl ist.
  4. Verfahren nach einem der vorhergehenden Ansprüche, wobei die Schwellentemperatur zwischen 400 °C und 600 °C liegt.
  5. Verfahren nach Anspruch 4, wobei die Schwellentemperatur zwischen 460 °C und 500 °C liegt.
  6. Verfahren nach einem der vorhergehenden Ansprüche, wobei der Dampf aus der Gruppe ausgewählt ist, die aus einem Kohlenwasserstoff mit geringer Verkokungstendenz, Stickstoff, Inertgasen, Kohlendioxid, Raffineriegas, Wasserdampf oder Mischungen daraus besteht.
  7. Verfahren nach Anspruch 6, wobei der Kohlenwasserstoff mit einer geringen Verkokungstendenz leichtes Fluid-Catcracker-Kreislauföl umfaßt.
  8. Verfahren nach Anspruch 6, wobei der Kohlenwasserstoff mit einer geringen Verkokungstendenz schweres Gasöl aus dem Verkokungsprozeß umfaßt.
  9. Verfahren nach einem der vorhergehenden Ansprüche, wobei der Dampf durch einen Blasenturm in Kombination mit der Verkokungsanlage zurückgeführt wird.
  10. Verfahren nach einem der vorhergehenden Ansprüche, wobei der Dampf aus einem Fraktionierturm erhalten wird, der mit der Verkokungsanlage nicht verbunden ist.
  11. Verfahren nach einem der vorhergehenden Ansprüche, wobei der Schwellen-Reaktionszeitraum zwischen 8 Stunden und 16 Stunden liegt.
  12. Verfahren nach einem der vorhergehenden Ansprüche, wobei die Schwellen-Reaktionszeit um nicht mehr als ungefähr eine Stunde überschritten wird.
  13. Verfahren nach einem der vorhergehenden Ansprüche, wobei ein beträchtlicher Teil des Inhalts der Verkokungstrommel für die Schwellenreaktions-Zeitdauer bei einer Temperatur gehalten wird, die ausreichend zum Verkoken ist, aber unterhalb der Schwellentemperatur liegt.
EP91304022A 1990-05-04 1991-05-03 Verkokung von Dekantieröl und anderen Schwerölen zur Herstellung von Nadelkoks höherer Qualität Expired - Lifetime EP0455504B1 (de)

Applications Claiming Priority (2)

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US51905690A 1990-05-04 1990-05-04
US519056 2000-03-03

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EP0455504A1 EP0455504A1 (de) 1991-11-06
EP0455504B1 true EP0455504B1 (de) 1995-03-29

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EP (1) EP0455504B1 (de)
AT (1) ATE120479T1 (de)
CA (1) CA2041436A1 (de)
DE (1) DE69108440T2 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7371317B2 (en) 2001-08-24 2008-05-13 Conocophillips.Company Process for producing coke

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102295943B (zh) * 2011-08-12 2013-06-26 中石油东北炼化工程有限公司葫芦岛设计院 一种大循环比油系针状焦焦化的方法
CN105733631B (zh) * 2014-12-06 2020-01-10 中国石油化工股份有限公司 一种针状焦的制备方法及其装置
CN105733630B (zh) * 2014-12-06 2019-03-19 中国石油化工股份有限公司 一种均质针状焦的制备方法及其装置
US20240352320A1 (en) * 2023-04-18 2024-10-24 Chevron U.S.A. Inc. Method for producing needle coke from renewable and circular feedstocks

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4547284A (en) * 1982-02-16 1985-10-15 Lummus Crest, Inc. Coke production
US4822479A (en) * 1986-11-21 1989-04-18 Conoco Inc. Method for improving the properties of premium coke

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7371317B2 (en) 2001-08-24 2008-05-13 Conocophillips.Company Process for producing coke

Also Published As

Publication number Publication date
EP0455504A1 (de) 1991-11-06
ATE120479T1 (de) 1995-04-15
DE69108440T2 (de) 1995-07-27
CA2041436A1 (en) 1991-11-05
DE69108440D1 (de) 1995-05-04

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