EP0181066A2 - Procédé pour déparaffiner des distillats lourds et des liquides résiduels - Google Patents

Procédé pour déparaffiner des distillats lourds et des liquides résiduels Download PDF

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Publication number
EP0181066A2
EP0181066A2 EP85306342A EP85306342A EP0181066A2 EP 0181066 A2 EP0181066 A2 EP 0181066A2 EP 85306342 A EP85306342 A EP 85306342A EP 85306342 A EP85306342 A EP 85306342A EP 0181066 A2 EP0181066 A2 EP 0181066A2
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EP
European Patent Office
Prior art keywords
zsm
dewaxing
stage
waxes
reactor
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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.)
Withdrawn
Application number
EP85306342A
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German (de)
English (en)
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EP0181066A3 (fr
Inventor
Philip Varghese
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.)
ExxonMobil Oil Corp
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Mobil Oil Corp
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Publication date
Application filed by Mobil Oil Corp filed Critical Mobil Oil Corp
Publication of EP0181066A2 publication Critical patent/EP0181066A2/fr
Publication of EP0181066A3 publication Critical patent/EP0181066A3/fr
Withdrawn legal-status Critical Current

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    • 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
    • C10G65/04—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including only refining steps
    • C10G65/043—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including only refining steps at least one step being a change in the structural skeleton
    • 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
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/58—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins
    • C10G45/60—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used
    • C10G45/64—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used containing crystalline alumino-silicates, e.g. molecular sieves
    • 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
    • C10G55/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by at least one refining process and at least one cracking process
    • C10G55/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by at least one refining process and at least one cracking process plural serial stages only
    • C10G55/06—Treatment of hydrocarbon oils, in the absence of hydrogen, by at least one refining process and at least one cracking process plural serial stages only including at least one catalytic cracking step

Definitions

  • Catalytic dewaxing of hydrocarbon oils to reduce the temperature at which precipitation of waxy hydrocarbons occurs is a known process and is described, for example, in the Oil and Gas Journal, January 6, 1975, pages 69-73.
  • U. S. Patent No. Re 28,398 describes a process for catalytic dewaxing with a catalyst comprising ZSM-5 and a hydrogenation/dehydrogenation component.
  • a process for hydrodewaxing a gas oil with'ZSM-5 is described in U. S. Patent No. 3,956,102.
  • a mordenite catalyst containing a Group VI or Group VIII metal may be used to dewax a distillate from a waxy crude, as described in U. S. Patent No. 4,100,056.
  • U. S. Patent No. 3,755,138 describes a process for mild solvent dewaxing to remove high quality wax from a lube stock, which is then catalytically dewaxed to specification pour point
  • Catalytic dewaxing processes may be followed by other processing steps such as hydrodesulfurization and de- nitrogenation in order to improve the qualities of the product U.
  • S. Patent No. 3,668,113 describes a catalytic dewaxing process employing a mordenite dewaxing catalyst which is followed by a catalytic hydrodesulfurization step over an alumina-based catalyst U.
  • S. Patent No. 4,400,265 describes a catalytic dewaxing/hydrodewaxing process using ZSM-5 wherein gas oil is catalytically dewaxed followed by hydrodesulfurization in a cascade system.
  • the waxy components are cracked by the zeolite into lighter products, such as paraffins, olefins and aromatics, some of which remain in the lube oil boiling range.
  • lighter products are produced in the naphtha boiling range (boiling at less than 204°C (4000F)).
  • Olefinic fragments are unstable to oxidation so the dewaxed oil may be subsequently hydrogenated over catalysts to saturate the olefins and improve the oxididation stability of the oil.
  • the hydrogenation catalysts generally used are mild hydrogenation catalysts, such as a CoMo/Al 2 O 3 type. The color of the oil may also be improved in this hydrofinishing.
  • U. S. Patent No. 4,428,819 to Shu et aI discloses a process for hydrofinishing a catalytically dewaxed oil in which the residual wax content of the dewaxed oil is isomerized over a hydroisomerization catalyst
  • heavier lube fractions (boiling above 316°C (600°F)) contain waxy components comprising normal paraffins, branched paraffins and cyclo paraffins.
  • a shape-selective catalyst such as HZSM-5, is used to dewax these feeds, the normal paraffins crack much faster than the branched paraffins and cycloparaffins.
  • mid-methyl branched paraffins and larger sterically hindered high molecular weight waxes are harder to convert than n-parrafin or end-methyl branched paraffins.
  • the conversion of the harder' to convert waxes is inhibited by the presence of large quantities of the easier to convert waxes and the lower molecular weight analogs (primary products) derived from the molecular cracking of the easier to convert waxes. These primary products appear to be able to interact with remaining high molecular weight materials to cause rapid catalyst aging.
  • small amounts of easy to convert light hydrocarbons such as paraffins and olefins derived from primary conversion of n-paraffins and end-methyt branched paraffins, substantially inhibit the conversion of the less easily converted poly-branched and mid-methyl branched paraffin waxes.
  • the present process is applicable to feedstocks, including lube stocks, when a low wax content is desired in the final product. This process is especially useful for feeds with pour points higher than 21 °C (70°F).
  • the feeds may be whole crudes or fractions, and may have been subjected to other refinery processes.
  • First stage dewaxing unit 4 operates at a temperature of 204 to 427°C (400° to 800°F), and pressure of 1,500 to 7,000 kPa (200 to 1000 psig), and liquid hourly space velocity (LHSV) between 0.5 and 3 hr.1 .
  • the feedstock 2 comprises n-paraffin waxes, end methyl branched waxes, poly-branched waxes and mid-methyl branched waxes.
  • the easily converted waxes such as the n-paraffin waxes and end-methyl branched waxes
  • lighter products such as C-, gases and light paraffinic and olefinic fragments, some of which remain in the lube oil boiling range, but most of which are in the naphtha range.
  • An effluent stream 6 from the dewaxing unit 4 discharges into separator 8.
  • Separator 8 separates stream 6 into a vapor stream 10 and a liquid stream 12. The separation may be accomplished by lowering the pressure and flashing the effluent stream 6 or by distilling the effluent stream 6 or by allowing vapor liquid separation to occur at an elevated pressure and temperature.
  • the separator removes those materials boiling below 204°C (400°F), and preferably those boiling below 371 °C (700°F).
  • the composition of the liquid stream 12 and vapor stream 10 can be adjusted by adjusting the temperature and pressure in separator 8.
  • the vapor stream 10 may be sent to downstream processing, such as distillation, while the liquid stream 12 passes into the second stage dewaxing unit 14 which may operate within the same ranges of temperature and pressure specified for the first dewaxing unit.
  • the relative operating conditions in the second stage dewaxing unit 14 are preferably more severe than those of the first stage dewaxing unit 4, to obtain a product stream 16 that meets pour point specifications by cracking the difficult to convert waxes, such as the poly-branched waxes and mid-methyl branched waxes, in liquid stream 12.
  • the ratio of LHSV in the first stage dewaxing unit 4 relative to dewaxing unit 14 will be 5:1 to about o.5:1.
  • the second stage dewaxing unit 14 then produces the product stream 16 which is passed to downstream processing, such as hydrofinishing into final product.
  • the primary reaction products inhibit the cracking of remaining uncracked stock. It is also theorized that the primary products react with the remaining uncracked stock because the primary reaction products are often olefins which can cyclize and/or alkylate to heavier components in the stock.
  • the primary reaction products such as light hydrocarbons, especially naphtha boiling range products, may inhibit the reaction of the heavier uncracked stock because they are more rapidly absorbed into catalyst volume, thus in effect accelerating the measured rate of catalyst aging for dewaxing to the desired product.
  • the catalysts employed in the first and second stage dewaxing units 4, 14 may be the same type or different. Preferably, they possess shape-selective paraffin cracking ability. Catalysts that have shape-selective qualities include crystalline zeolite catalysts and crystalline silica alumina phosphate (SAPO) catalysts. These materials may be bound in a variety of matrices, such as silica alumina or silica and alumina alone.
  • SAPO crystalline silica alumina phosphate
  • the catalysts should contain a hydrogenation/dehydrogenation component hereafter.
  • the preferred hydrogenation components are the noble metals of Group VIII, especially platinum and palladium, but other noble metals, such as irridium, ruthenium or rhodium, may also be used. Combinations of noble metals with non-noble metals, such as nickel, rhenium, tungsten, chromium and molybdenum are of interest.
  • Base metal hydrogenation components may also be used, especially nickel, cobalt, molybdenum, tungsten, copper or zinc. Up to 15% metal may be added, though usually much less noble metal promoter is needed.
  • the metal may be incorporated into the catalyst by any suitable method such as impregnation or exchange onto the zeolite.
  • the metal may be incorporated in the form of a cationic, anionic or a neutral complex, such as Pt(NH,) 9-and cationic complexes of this type will be found convenient for exchanging metals onto a zeolite.
  • Anionic complexes are also useful for impregnating metals into the zeolites.
  • a portion of zeolites useful herein are termed medium pore zeolites and are characterized by an effective pore size of generally less than about 7 angstroms, and/or pore windows in a crystal formed by 10-membered rings.
  • the medium pore zeolites include ZSM-5, ZSM-11, ZSM-23, ZSM-35, ZSM-38, ZSM-48 and TMA Offretite.
  • zeolites important to the present invention are large pore zeolites. These have a pore size sufficiently large to admit the vast majority of components normally found in a feedstock, generally in excess of 7.5 angstroms and/or formed by 12-membered rings.
  • the large pore zeolites are represented by ZSM-4, ZSM-12, ZSM-20, Zeolite Beta, Mordenite, TEA Mordenite, Dealuminized Y, and Rare Earth Y. Additionally, the large pore component may include a low sodium Ultrastable Y molecular sieve (USY).
  • ZSM-4 is described in U. S. 3,923,639.
  • ZSM-5 is described in U. S. 3,702,886.
  • ZSM- 11 is described in U. S. 3,709,976.
  • ZSM-23 is described in U. S. 4,076,842.
  • ZSM-35 is described in U. S. 4,016,245.
  • ZSM-48 is described in U. S. 4,397,827.
  • Zeolite Beta is described in U. S. 3,308,069 and Re. 28,341.
  • the first and second stage dewaxing units 4, 14 respectively may be part of the same reactor, may be in separate vessels, or may each consist of a plurality of vessels.
  • a preferred embodiment, as shown in Fig. 2 comprises a series of two or more reactors 40, 42, 44, 46 and 48 for each stage.
  • the first stage dewaxing unit 4 comprises two reactors 40, 42
  • the second stage dewaxing unit 14 comprises two other reactors 44, 46.
  • the units 4, 14 could operate with only one reactor per unit.
  • the reactors 40, 42, 44 and 46 contain dewaxing catalysts and are operated in series.
  • a solid line shown in Fig. 2, represents the path of hydrocarbons through the reactors 40, 42, 44 and 46.
  • a feedstock passes into the first reactor 40 to produce an outlet stream 50 which passes into the second reactor 4 2.
  • the outlet stream 52 from the second reactor 42 becomes an effluent stream 6 which passes into the separation unit 8 to form a vapor stream 10 and a liquid stream 12.
  • the liquid stream 12 passes into the third reactor 44 to produce an outlet stream 54 which passes into the fourth reactor 46 to produce an outlet stream 56 which forms the product stream 16.
  • headers 24, 26 and 28 are provided so that the reactors may be rotated, thus allowing for on-line reactivation/regeneration of catalysts in any one of the reactors.
  • the headers 24, 26 and 28 allow flashing or distillation between any two or the reactors 40, 42, 44, 46 and 48.
  • the feedstock 2 feeds the feed header 24 which is attached to each of the reactors 40, 42, 44, 46 and 48.
  • the outlets 50, 52, 54, 56 and 58 from each reactor 40, 42, 44, 46 and 48, respectively, can feed either the product header 28 or the separation unit header 26.
  • the effluent 6 from the first stage dewaxing unit passes into the separation header 26 and subsequently into the separation unit 8.
  • the product stream 16 passes into the product header 28 and subsequently to downstream processing.
  • This arrangement will have an added benefit because catalysts that age far enough to be unsuitable for use in the more severe second stage dewaxing unit 14 could be switched to duty in the first stage dewaxing unit 4, allowing another reactor with its catalyst charge to be freed for rotational reactivation/regeneration.
  • Appropriate valving (not shown) would be provided to direct flow to the correct headers and units.
  • Fig. 3 shows an alternative embodiment of the invention, in which a feedstock 2 passes into a dewaxing unit 30 under the first set of operating conditions outlined above.
  • the effluent 6 then passes to a separation unit to form a vapor stream 10 and a liquid stream 12.
  • the liquid stream 12 is then stored in tankage 18, such as any suitable tankage storage area located on a plant site.
  • tankage 18 such as any suitable tankage storage area located on a plant site.
  • an effluent 20 comprising the hydrocarbons from the liquid stream 12 is catalytically dewaxed in the dewaxing unit 30, which operates at the second set of operating conditions outlined above.
  • the effluent 6 would then form a product stream 16 which passes to downstream processing.
  • FIG. 4 An alternate embodiment of the invention is shown in Fig. 4 , in which a feedstock 2 and a recycle stream 22 are catalytically dewaxed in a dewaxing unit 30 to produce an effluent 6.
  • the dewaxing unit 30 temperature is 204 to 426°C (400°F to 800°F).
  • dewaxing may be accomplished by an easy conversion step and a relatively more difficult conversion step.
  • Example 1 shown in Fig. 5, is a plot of pour point versus days on stream and compares feed run by itself over catalyst against feed run, with 3% and 6% added hydrocarbons boiling below 204°C (400 °F). These were mixtures of paraffins boiling in the naphtha range, i.e., liquids boiling below 204°C.These tests were run at a temperature of 354°C (670°F), a pressure of 2,900 kPa (400 psig) and a space velocity of 1 hr- 1.
  • Example 2 shown in Fig. 6, compares the pour point versus days on stream at constant space velocity and temperature of a feed dewaxed in a single dewaxing stage as opposed to a feed dewaxed at the same overall space velocity, temperature and pressure in two. stages with separation and removal of a vapor stream in between the two stages.
  • the test was run at 299°C (570°F), pressure of 2,900 kPa (400 psig) and 1.0 LHSV for the single stage unit and 2.0 LHSV per stage for the two-stage units. Both the one-stage and two-stage units contain the same amount of catalyst.
  • the catalyst was a Ni-ZSM-5.
  • the separation was a laboratory fractionation, to remove 204°C (400°F) and lighter material from the liquid feed to the second stage. This shows lower pour points and extended catalyst life when two stages and a separation stage are used.

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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)
  • Crystallography & Structural Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
EP85306342A 1984-10-29 1985-09-06 Procédé pour déparaffiner des distillats lourds et des liquides résiduels Withdrawn EP0181066A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US66579384A 1984-10-29 1984-10-29
US665793 1984-10-29

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EP0181066A2 true EP0181066A2 (fr) 1986-05-14
EP0181066A3 EP0181066A3 (fr) 1988-07-20

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EP85306342A Withdrawn EP0181066A3 (fr) 1984-10-29 1985-09-06 Procédé pour déparaffiner des distillats lourds et des liquides résiduels

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EP (1) EP0181066A3 (fr)
JP (1) JPS61108693A (fr)
AU (1) AU586980B2 (fr)
CA (1) CA1253107A (fr)
ZA (1) ZA856718B (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0202744A2 (fr) * 1985-04-18 1986-11-26 Mobil Oil Corporation Procédé de déparaffinage catalytique
EP0234123A1 (fr) * 1986-01-03 1987-09-02 Mobil Oil Corporation Méthode et appareil de déparaffinage
EP0304251A1 (fr) * 1987-08-20 1989-02-22 Mobil Oil Corporation Procédé de déparaffinage catalytique
US4908120A (en) * 1987-08-20 1990-03-13 Mobil Oil Corporation Catalytic dewaxing process using binder-free zeolite
US4921593A (en) * 1987-08-20 1990-05-01 Mobil Oil Corporation Catalytic dewaxing process
EP0264158B1 (fr) * 1986-10-17 1991-08-21 Shell Internationale Researchmaatschappij B.V. Conversion d'un courant contenant des hydrocarbures lourds en un courant contenant des hydrocarbures ayant un domaine d'ébullition inférieur
WO1999029810A1 (fr) * 1997-12-10 1999-06-17 Chevron U.S.A. Inc. Procede de deparaffinage

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3431194A (en) * 1966-10-14 1969-03-04 Exxon Research Engineering Co Process for lowering the pour point of a middle distillate
EP0072220A1 (fr) * 1981-08-07 1983-02-16 Mobil Oil Corporation Procédé en deux étapes de déparaffinage et d'hydrotraitement d'hydrocarbures

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4211634A (en) * 1978-11-13 1980-07-08 Standard Oil Company (Indiana) Two-catalyst hydrocracking process
US4428819A (en) * 1982-07-22 1984-01-31 Mobil Oil Corporation Hydroisomerization of catalytically dewaxed lubricating oils
US4597854A (en) * 1985-07-17 1986-07-01 Mobil Oil Corporation Multi-bed hydrodewaxing process

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3431194A (en) * 1966-10-14 1969-03-04 Exxon Research Engineering Co Process for lowering the pour point of a middle distillate
EP0072220A1 (fr) * 1981-08-07 1983-02-16 Mobil Oil Corporation Procédé en deux étapes de déparaffinage et d'hydrotraitement d'hydrocarbures

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0202744A2 (fr) * 1985-04-18 1986-11-26 Mobil Oil Corporation Procédé de déparaffinage catalytique
EP0202744A3 (fr) * 1985-04-18 1988-08-17 Mobil Oil Corporation Procédé de déparaffinage catalytique
EP0234123A1 (fr) * 1986-01-03 1987-09-02 Mobil Oil Corporation Méthode et appareil de déparaffinage
EP0264158B1 (fr) * 1986-10-17 1991-08-21 Shell Internationale Researchmaatschappij B.V. Conversion d'un courant contenant des hydrocarbures lourds en un courant contenant des hydrocarbures ayant un domaine d'ébullition inférieur
EP0304251A1 (fr) * 1987-08-20 1989-02-22 Mobil Oil Corporation Procédé de déparaffinage catalytique
US4908120A (en) * 1987-08-20 1990-03-13 Mobil Oil Corporation Catalytic dewaxing process using binder-free zeolite
US4921593A (en) * 1987-08-20 1990-05-01 Mobil Oil Corporation Catalytic dewaxing process
WO1999029810A1 (fr) * 1997-12-10 1999-06-17 Chevron U.S.A. Inc. Procede de deparaffinage

Also Published As

Publication number Publication date
AU586980B2 (en) 1989-08-03
EP0181066A3 (fr) 1988-07-20
ZA856718B (en) 1987-04-29
CA1253107A (fr) 1989-04-25
JPS61108693A (ja) 1986-05-27
AU4685985A (en) 1986-05-08

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