EP0744452B1 - Verfahren zur Herstellung von Basisschmierölen - Google Patents

Verfahren zur Herstellung von Basisschmierölen Download PDF

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Publication number
EP0744452B1
EP0744452B1 EP19960201148 EP96201148A EP0744452B1 EP 0744452 B1 EP0744452 B1 EP 0744452B1 EP 19960201148 EP19960201148 EP 19960201148 EP 96201148 A EP96201148 A EP 96201148A EP 0744452 B1 EP0744452 B1 EP 0744452B1
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EP
European Patent Office
Prior art keywords
range
process according
weight
dewaxing
hydrowax
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
EP19960201148
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English (en)
French (fr)
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EP0744452A3 (de
EP0744452A2 (de
Inventor
Philippe Marie Rivoalen
Bob Scheffer
Peter James Wardle
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Shell Internationale Research Maatschappij BV
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Shell Internationale Research Maatschappij BV
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Publication of EP0744452A3 publication Critical patent/EP0744452A3/de
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G65/00—Treatment of hydrocarbon oils by two or more hydrotreatment processes only
    • C10G65/02—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only
    • C10G65/10—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including only cracking steps
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
    • C10G2400/10—Lubricating oil

Definitions

  • the present invention relates to a process for producing lubricating base oils. More specifically, the present invention relates to a process for producing lubricating base oils having a high viscosity index (VI) using a hydrowax obtained as the bottom fraction of a hydrocracking treatment as the feedstock.
  • VI viscosity index
  • lubricating base oils having a very high VI can be produced from feedstocks containing relatively high amounts of waxy molecules, i.e. linear and slightly branched paraffins as well as long chain alkyl-aromatics and -naphthenics.
  • waxy molecules i.e. linear and slightly branched paraffins as well as long chain alkyl-aromatics and -naphthenics.
  • Such waxy molecules namely, have a very high VI of their own and accordingly, positively influence the VI of the product in which they are present.
  • high wax content feedstocks are slack waxes and synthetic waxes produced by Fischer-Tropsch synthesis reactions. Slack waxes usually contain 50% by weight or more of wax, whilst synthetic waxes even have a wax content of 80% by weight or more.
  • the present invention aims to provide a process wherein lubricating base oils having such high VI's are produced from a feedstock having a relatively low wax content, i.e. a wax content of less than 50% by weight, even of less than 30% by weight. More specifically, the present invention aims to provide a process for producing such lubricating base oils using a hydrocracker bottom fraction or hydrowax as the feedstock.
  • the process of the present invention accordingly, can be very suitably integrated in a refinery having hydrocracking capacity.
  • the final hydrogenation step increases the amount of saturated components present, whereby the hydrogenation of olefins into paraffinic and isoparaffinic components is favourable for the VI of the base oil finally obtained.
  • the aromatic components present which are also hydrogenated have no or hardly any impact on the VI of the final base oil and consequently do not contribute to a high VI.
  • base oils having a VI of 125 or higher cannot be obtained by the process according to EP-A-0,272,729.
  • the present invention aims to provide a process wherein lubricating base oils having a VI of 125 or higher can be produced in an effective way starting from a hydrowax obtained as the bottom fraction of a hydrocracked effluent.
  • the present invention relates to a process for producing lubricating base oils, which process comprises the steps of:
  • the feed used in the process according to the present invention is the bottom fraction of a hydrocracked effluent, which effluent in return is obtained from a hydrocracking operation.
  • the expression "bottom fraction” indicates the fraction recovered from the effluent obtained from the hydrocracking operation at the bottom of the separation device wherein said effluent is separated. Accordingly, said bottom fraction -commonly referred to as hydrowax- is that fraction of the hydrocracked effluent containing the heaviest components.
  • the hydrowax used as the feed in the process of the present invention is suitably obtained from the hydrocracked effluent at an effective cutpoint in the range of from 300 to 450 °C, preferably 310 to 380 °C.
  • the effective cutpoint is the temperature above which at least at least 85% by weight and preferably at least 90% by weight, of the hydrocarbons present in the hydrowax recovered has its boiling point.
  • Hydrocracking is a conversion process which is well known in the art and basically involves catalytically converting hydrocarbon molecules into smaller hydrocarbon molecules in the presence of hydrogen.
  • feedstocks can be used for hydrocracking operations, including inter alia distillate fractions, vacuum flashed distillates obtained from other hydrocarbon conversion processes and atmospheric residues.
  • Hydrocracking conditions usually comprise temperatures in the range of from 250 to 500 °C, hydrogen partial pressures in the range of from 1 to 300 bar, weight hourly space velocities of from 0.1 to 10 kg feed per litre of catalyst per hour and gas/feed ratios of from 100 to 5000 Nl of gas per kg of feed.
  • Hydrocracking catalysts are also known in the art and include both amorphous and zeolite-based catalysts.
  • a hydrocracking catalyst comprises at least one hydrogenation component of a Group VI metal and/or at least one hydrogenation component of a Group VIII metal and a carrier comprising an amorphous material, such as amorphous silica-alumina, silica or alumina, and/or a zeolite.
  • amorphous material such as amorphous silica-alumina, silica or alumina, and/or a zeolite.
  • Zeolites particularly useful in this connection comprise zeolite Y or a modification thereof, such as ultra-stable zeolite Y. The latter type of zeolites is most suitably applied. Combinations of amorphous materials and zeolites may also be applied.
  • Suitable Group VI metals are tungsten (W) and molybdenum (Mo), whilst suitable Group VIII metals are the non-noble metals nickel (Ni) and cobalt (Co) as well as the noble metals platinum (Pt) and palladium (Pd).
  • suitable amorphous catalysts are those comprising as the hydrogenation component(s) NiMo, CoMo, NiW, CoW, Pt, Pd or PtPd.
  • the hydrocracking operation may be a single stage operation, involving the use of one bed catalyst, or a two-stage operation, wherein two different catalyst beds are employed.
  • the hydrowax used as the feed in the process of the present invention can in principle be obtained from any arbitrary hydrocracking operation.
  • step (a) of the process according to the present invention the hydrowax is contacted with a catalyst comprising platinum and/or palladium on a refractory oxide carrier in the presence of hydrogen under such conditions that a 370 °C+ conversion of at least 10% by weight, preferably at least 25% by weight and even more preferably at least 35% by weight is attained.
  • the 370 °C+ conversion is kept below 80% by weight and more suitably below 70% by weight, as at too high conversion levels the yield of lubricating base oil product having a VI of 125 or higher is becoming less interesting from an economical point of view.
  • a highly preferred 370 °C+ conversion is in the range of from 40 to 70% by weight.
  • 370 °C+ conversion refers to the weight percentage of hydrocarbons present in the hydrowax having a boiling point of 370 °C or higher, which is converted into hydrocarbons having a lower boiling point. This implies that in step (a) both hydrogenation and hydrocracking reactions take place.
  • Suitable reaction conditions include a reaction temperature in the range of from 350 to 550 °C, preferably from 365 to 500 °C, a hydrogen partial pressure in the range of from 10 to 300 bar, preferably 25 to 250 bar, a weight hourly space velocity in the range of from 0.1 to 10 kg/l/hr, preferably from 0.2 to 5 kg/l/hr, and a hydrogen to feed ratio in the range of from 100 to 5,000 Nl/kg, preferably from 250 to 2,000 Nl/kg.
  • the catalyst used in step (a) is a noble metal-based catalyst comprising platinum and/or palladium supported on a refractory oxide carrier.
  • the total amount of platinum and/or palladium present in the catalyst is suitably in the range of from 0.1 to 5.0% by weight calculated as element based on total weight of carrier, more suitably in the range of from 0.2 to 2.0% by weight. If both present, the weight ratio of platinum to palladium (calculated as element) may vary within wide limits, but suitably is in the range of from 0.05 to 10, more suitably 0.1 to 5.
  • the catalyst comprises platinum as the sole catalytically active metal, whilst in another preferred embodiment of the present invention the catalyst comprises a combination of platinum and palladium. Platinum and palladium may be present as element, as oxide and/or as sulphide.
  • the catalyst used in step (a) may also comprise at least one Group VIB metal component.
  • a Group VIB metal component particularly when palladium is used as the noble metal, the presence of a Group VIB metal component may be beneficial.
  • Suitable Group VIB metal components include the oxides and sulphides of chromium, molybdenum or tungsten, but also these metals in elemental form. Of these, the tungsten and chromium components are preferred. If present, a Group VIB metal component is suitably present in an amount of from 1 to 35% by weight, more suitably from 5 to 30% by weight, calculated as element and based on total weight of carrier. Examples of very suitable noble metal-based catalysts, accordingly, are those comprising palladium and tungsten or palladium and chromium.
  • the carrier used comprises a refractory oxide.
  • Suitable refractory oxides include zeolites, alumina, amorphous silica-alumina, fluorinated alumina or mixtures of two or more of these. Of these, amorphous silica-alumina, zeolites and mixtures of these are preferred, whereby the use of amorphous silica-alumina is particularly preferred.
  • Suitable zeolites are the same as those described above to be suitably applied in hydrocracking catalysts, i.e. (modified) zeolite Y.
  • Suitable amorphous silica-alumina carrier materials comprise in the range of from 10 to 70% by weight of alumina and are commercially available.
  • the carrier comprises an amorphous silica-alumina and/or zeolite as the refractory oxide, it may also contain a binder.
  • binder materials in catalysts are well known in the art. Typical binder materials are silica and alumina. In general, the mutual weight ratio of binder to refractory oxide may vary between wide limits, but suitably is in the range of from 0 (i.e. no binder) to 5, suitably 0 to 4.
  • a particularly preferred catalyst comprises platinum and palladium on an amorphous silica-alumina carrier.
  • step (b) The product obtained from step (a) is subsequently separated in step (b) into at least one lighter distillate fraction and a heavy distillate fraction having a VI of 125 or higher, preferably of 135 or higher, and a kinematic viscosity at 100 °C (Vk100) of a least 3.5 centiStokes, whereby the Vk100 preferably does not exceed 12.0 centiStokes.
  • Vk100 kinematic viscosity at 100 °C
  • the dewaxing carried out in step (c) may in principle be carried out via any known dewaxing process.
  • suitable dewaxing operations are the conventional solvent dewaxing processes, particularly those wherein methylethylketone, toluene or a mixture thereof is used as the dewaxing solvent, and the catalytic dewaxing processes. Both types of dewaxing operations are well known in the art.
  • the most commonly applied solvent dewaxing process is the methyl ethyl ketone (MEK) solvent dewaxing route, wherein MEK is used as the dewaxing solvent, possibly in admixture with toluene.
  • MEK methyl ethyl ketone
  • Catalytic dewaxing generally involves cracking and/or isomerising linear and slightly branched paraffinic hydrocarbon molecules -which negatively influence the cold flow properties of the base oil- in the presence of hydrogen and a dewaxing catalyst.
  • Suitable dewaxing catalysts which mainly favour cracking of paraffinic hydrocarbons are those comprising ZSM-5, ferrierite and/or silicalite and optionally a hydrogenation component.
  • Examples of catalysts which mainly favour isomerisation of linear or slightly branched hydrocarbons include catalysts comprising a silicoaluminophosphate (SAPO), such as e.g. SAPO-11, SAPO-31 and SAPO-41, ZSM-23 and SSZ-32.
  • SAPO silicoaluminophosphate
  • a catalytic dewaxing step may suitably be followed by a hydrofinishing step to hydrogenate any unsaturated species (olefins, aromatics) still left.
  • a hydrofinishing step to hydrogenate any unsaturated species (olefins, aromatics) still left.
  • solvent dewaxing or catalytic dewaxing by isomerisation i.e. catalytic hydro-isomerisation.
  • a hydrowax having a boiling point distribution as indicated in Table I was contacted with a catalyst comprising 1.0% by weight of palladium and 0.3% by weight of platinum (both weight percentages being based on total weight of carrier) on an amorphous silica-alumina carrier having an alumina content of 45% by weight.
  • Operating conditions were such that the 370 °C+ conversion was 49.5% by weight. This corresponded with an operating temperature of 390 °C, a hydrogen pressure of 190 bar, a weight hourly space velocity (WHSV) of 1.0 kg/l/hr and a gas rate of 750 Nl/kg.
  • WHSV weight hourly space velocity
  • the cracked effluent was separated at an effective cutpoint of 400 °C and the 400 °C+ fraction was solvent dewaxed via the conventional MEK/toluene dewaxing process.
  • the dewaxed product had a VI of 140.1, a Vk40 (kinematic viscosity at 40 °C) of 23.8 cSt and a Vk100 of 4.98 cSt at a yield of 36.7% by weight on feed.
  • a hydrowax having a boiling point distribution as indicated in Table I was contacted with the same catalyst as described in Example 1. Operating conditions were such that the 370 °C+ conversion was 28.8% by weight. This corresponded with an operating temperature of 380 °C, a hydrogen pressure of 190 bar, a weight hourly space velocity (WHSV) of 1.0 kg/l/hr and a gas rate of 750 Nl/kg.
  • the cracked effluent was separated into a 385 °C- fraction, a 385-450 °C fraction and a 450 °C+ fraction.
  • the 385-450 °C fraction and the 450 °C+ fraction were solvent dewaxed via the conventional MEK/toluene dewaxing process.
  • Table II shows that a product having a VI of above 135 having good kinematic viscosity's at 40 and 100 °C is obtained, whilst the other dewaxed product obtained also has attractive properties as a lubricating base oil for those applications that do not require extra high VI values, i.e. a VI of 125 or higher.

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

Claims (10)

  1. Verfahren zur Herstellung von Schmiermittelgrundölen, welches Verfahren die folgenden Stufen umfaßt:
    (a) Inkontaktbringen eines Hydrowachses, das als Sumpffraktion eines hydrogecrackten Abstroms erhalten worden ist, mit einem Katalysator, der Platin und/oder Palladium auf einem feuerfesten Oxidträger umfaßt, in Gegenwart von Wasserstoff unter solchen Bedingungen, daß wenigstens 10 Gew.-%, vorzugsweise wenigstens 25 Gew.-% der Kohlenwasserstoffe mit einem Siedepunkt von 370°C und darüber, die in dem Hydrowachs vorliegen, in Kohlenwasserstoffe mit einem niedrigeren Siedepunkt umgewandelt werden,
    (b) Auftrennen des in Stufe (a) erhaltenen Produktes in wenigstens eine leichtere Destillatfraktion und eine schwere Destillatfraktion mit einem VI von 125 oder darüber und mit einer kinematischen Viskosität bei 100°C von wenigstens 3,5 Centistoke und
    (c) Entwachsen der in Stufe (b) erhaltenen schweren Destillatfraktion.
  2. Verfahren nach Anspruch 1, worin die schwere Destillatfraktion von Stufe (b) einen VI von 135 oder darüber aufweist.
  3. Verfahren nach einem der Ansprüche 1 - 2, worin das Hydrowachs aus dem hydrogecrackten Abstrom bei einem effektiven Cutpoint im Bereich von 300 bis 450°C erhalten wird.
  4. Verfahren nach Anspruch 3, worin der Cutpoint im Bereich von 310 bis 380°C liegt.
  5. Verfahren nach einem der Ansprüche 1 - 4, worin der feuerfeste Oxidträger ein amorphes Siliciumoxid-Aluminiumoxid, ein Träger auf Zeolith Y-Basis oder ein Gemisch hievon ist.
  6. Verfahren nach Anspruch 5, worin der in Stufe (a) verwendete Träger Platin und Palladium auf einem amorphen Siliciumoxid-Aluminiumoxidträger umfaßt.
  7. Verfahren nach einem der Ansprüche 1 - 6, worin die Stufe (a) bei einer Temperatur im Bereich von 350 bis 550°C, einem Wasserstoffpartialdruck im Bereich von 10 bis 300 bar, einer gewichtsbezogenen Raumgeschwindigkeit im Bereich von 0,1 bis 10 kg/l/h und bei einem Wasserstoff/Einsatzmaterial-Verhältnis im Bereich von 100 bis 5000 Nl/kg ausgeführt wird.
  8. Verfahren nach Anspruch 7, worin die Stufe (a) bei einer Temperatur im Bereich von 365 bis 500°C, einem Wasserstoffpartialdruck im Bereich von 25 bis 250 bar, einer gewichtsbezogenen Raumgeschwindigkeit im Bereich von 0,2 bis 5 kg/l/h und bei einem Wasserstoff/Einsatzmaterial-Verhältnis im Bereich von 250 bis 2000 Nl/kg ausgeführt wird.
  9. Verfahren nach einem der Ansprüche 1 - 8, worin das Entwachsen in Stufe (c) durch Lösungsmittelentwachsen ausgeführt wird.
  10. Verfahren nach einem der Ansprüche 1 - 8, worin das Entwachsen in Stufe (c) durch eine katalytische Hydroisomerisationsbehandlung ausgeführt wird, auf die gegebenenfalls eine Hydrofinishingstufe folgt.
EP19960201148 1995-04-28 1996-04-26 Verfahren zur Herstellung von Basisschmierölen Expired - Lifetime EP0744452B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP19960201148 EP0744452B1 (de) 1995-04-28 1996-04-26 Verfahren zur Herstellung von Basisschmierölen

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP95400991 1995-04-28
EP95400991 1995-04-28
EP19960201148 EP0744452B1 (de) 1995-04-28 1996-04-26 Verfahren zur Herstellung von Basisschmierölen

Publications (3)

Publication Number Publication Date
EP0744452A2 EP0744452A2 (de) 1996-11-27
EP0744452A3 EP0744452A3 (de) 1997-01-22
EP0744452B1 true EP0744452B1 (de) 1999-12-29

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0912243B1 (de) * 1996-07-15 2001-12-05 Chevron U.S.A. Inc. Schwefelbeständiger katalysator zur hydrokonversion und wasserstoffbehandlung von wasserstoffbehandlung von schwefelhältigen schmiermittelausgangsstoffen
WO1998002502A1 (en) * 1996-07-16 1998-01-22 Chevron U.S.A. Inc. Base stock lube oil manufacturing process
US6383366B1 (en) * 1998-02-13 2002-05-07 Exxon Research And Engineering Company Wax hydroisomerization process
FR2798136B1 (fr) * 1999-09-08 2001-11-16 Total Raffinage Distribution Nouvelle huile de base hydrocarbonee pour lubrifiants a indice de viscosite tres eleve

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3874510T2 (de) * 1987-12-18 1993-03-18 Exxon Research Engineering Co Verfahren zur stabilisierung von hydroisomeraten.
NO885605L (no) * 1987-12-18 1989-06-19 Exxon Research Engineering Co Fremgangsmaate for fremstilling av smoereolje.
US5275719A (en) * 1992-06-08 1994-01-04 Mobil Oil Corporation Production of high viscosity index lubricants

Also Published As

Publication number Publication date
EP0744452A3 (de) 1997-01-22
EP0744452A2 (de) 1996-11-27

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