EP0471461A2 - Verfahren zur Herstellung von Schmierölen mit niedrigem Stockpunkt und hohem Viskositätsindex durch Lösungsmittelentparaffinierung - Google Patents

Verfahren zur Herstellung von Schmierölen mit niedrigem Stockpunkt und hohem Viskositätsindex durch Lösungsmittelentparaffinierung Download PDF

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Publication number
EP0471461A2
EP0471461A2 EP91306827A EP91306827A EP0471461A2 EP 0471461 A2 EP0471461 A2 EP 0471461A2 EP 91306827 A EP91306827 A EP 91306827A EP 91306827 A EP91306827 A EP 91306827A EP 0471461 A2 EP0471461 A2 EP 0471461A2
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Prior art keywords
oil
boiling
dewaxing
low
point
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EP91306827A
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English (en)
French (fr)
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EP0471461B1 (de
EP0471461A3 (de
Inventor
James David Bell
Patrick Charles Ewener
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ExxonMobil Technology and Engineering Co
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Exxon Research and Engineering Co
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
    • C10M101/02—Petroleum fractions
    • 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
    • C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
    • C10G73/02—Recovery of petroleum waxes from hydrocarbon oils; Dewaxing of hydrocarbon oils
    • C10G73/06—Recovery of petroleum waxes from hydrocarbon oils; Dewaxing of hydrocarbon oils with the use of solvents

Definitions

  • Solvent dewaxing of waxy lube oils has long been known. It has also been known that lighter oils, oils of lower boiling point and VI of about 90-105/110 are more miscible in dewaxing solvents of a given composition than are higher boiling-higher VI oils. It is also widely accepted that good yields of dewaxed oils are obtained when the dewaxing procedure is practiced under oil/solvent miscible conditions. To this end, conditions of solvent to oil ratios, dewaxing temperatures and solvent/cosolvent ratios have been adjusted to achieve oil-solvent miscibility at the dewaxing temperature (filter temperature). All too often, however, a compromise must be struck between yield of dewaxed oil and pour point, that is low pour points are achieved at the expense of product yield or conversely high yields are achieved at the price of higher pour point.
  • U.S. Patent 3,365,390 describes a lube oil production process involving hydrocracking a heavy oil feed, separating hydrocracked wax from a hydrocracked lubricating oil portion of the products and hydroisomerizing the hydrocracked wax using an active reforming catalyst.
  • An isomerized lubricating oil fraction so produced can be dewaxed separately, to recover ultra high VI isomerized lube oil, or the isomerized lube oil fraction is dewaxed in admixture with a hydrocracked lubricating oil fraction.
  • the wax recovered is a mixture of hydrocracked wax and isomerized wax and the properties of the recovered lube oil are upgraded due to the presence of the isomerate lube oil portion.
  • High boiling-high VI wax isomerate and natural waxy oil distillates are difficult to dewax to achieve pour point in the region of about -20°C and lower.
  • Such oils when solvent dewaxed to low temperature typically encounter oil/solvent miscibility problems resulting in poor dewaxed oil yields.
  • high boiling high VI oils can be solvent dewaxed to low pour point under miscible conditions when using low miscibility dewaxing solvents, e.g. C3-C6 ketone based dewaxing solvents such as methyl ethyl ketone, methyl isobutyl ketone, acetone, etc. and mixtures thereof such as MEK/MIBK by combining a quantity of low boiling conventional VI waxy oil with the high boiling high VI oil and coprocessing the mixture under conventional solvent dewaxing conditions.
  • the addition of the low boiling conventional VI waxy oil to the high boiling high VI oil permits dewaxing to be conducted under miscible conditions resulting in the production of acceptable yields of low pour point dewaxed oil.
  • the low pour point dewaxed oil mixture may be subsequently fractioned into fractions whose specifications are very close to the parent materials in terms of boiling point and VI and that both such fractions possess the low pour point of the mixture.
  • the yield of the low pour-high boiling-high VI oil fraction achieved by the co-processing procedure is higher than that achieved when the high boiling high VI oil is dewaxed by itself.
  • Figure 1 compares the miscibility of heavy, high boiling high VI wax isomerate oil to that of a mixture of said heavy oil with a light oil at a 2/1 ratio in ketone dewaxing solvents of varying proportions at different temperatures.
  • Figure 2 shows the yield of -21°C pour dewaxed oil derived from Fischer-Tropsch isomerate, the yield being normalized to 100 barrels of Fischer-Tropsch isomerate feed to the dewaxer on the basis of both neat Fischer-Tropsch isomerate and a Fischer-Tropsch isomerate/150N blend.
  • Heavy, high boiling, high VI waxy oils be they waxy oils obtained by wax isomerization or conventional oils, such as deasphalted 600N hydrocracked oil, or Bright Stocks which are immiscible in typical low miscibility dewaxing solvents such as C3-C6 ketones at the low dewaxing temperature used when low pour points of about -21°C are sought can be solvent dewaxed to a target pour point of about -21°C and lower, preferably about -24°C, most preferably about -27°C using conventional solvents under miscible conditions (e.g.
  • a filter temperature of no less than about -35°C so as to have a pour/filter ⁇ T of about 3-4°C or less) by adding to the heavy, high boiling, high VI waxy oil a quantity of lower boiling conventional VI waxy oil distillate and processing this mixture through the solvent dewaxing process under miscible conditions.
  • the light lower boiling conventional VI waxy oil added to the heavy, high boiling high VI waxy oil will be such that it can be easily separated from the heavy oil by distillation, therefore it will be characterized by possessing a 90% off point about 50-300°F, preferably 50-100°F, lower than the 10% off point of the heavy oil.
  • the bulk of the light oil is substantially lighter and lower boiling than the bulk of the heavy oil.
  • the light oil is added to the heavy oil in an amount sufficient to render the mixture miscible in the low miscibility dewaxing solvent used at a filter temperature which permits the waxy oil to possess a pour point of at least -21°C, preferably about -24°C, most preferably about -27°C.
  • the amount of added light oil can range between about 5 to 50% by vol. of the oil mixture, preferably about 20 to 40 vol.%.
  • the solvent dewaxing process which is benefited by operating on the dual component waxy feed stock is any typical solvent dewaxing process including those identified as dilution indirect chilling processes, pre-dilution direct chilling processes or just direct chilling processes.
  • Indirect chilling processes include, for example, scraped surface chilling processes wherein the waxy oil charge is diluted with solvent to produce a solution which is passed through the scraped surface chiller wherein a refrigerant is passed through the outer jacket of the heat exchanger while a rotating scraper blade prevents wax build up in the inner surface of the chiller.
  • Direct chilling processes can employ either no dilution or predilution of the waxy charge.
  • the waxy charge with or without dilution is then chilled by the injection of cold solvent directly into the waxy charge.
  • a preferred embodiment of dilution chilling is the DILCHILL process wherein the waxy charge is passed through a chilling tower divided into stages and cold solvent is injected into a number of said stages. In those stages into which cold solvent is injected, a high level of agitation is maintained so that substantially instantaneous mixing of the chilling solvent and waxy oil is achieved thereby avoiding detrimental shock chilling.
  • This procedure is described in greater detail in U.S. Patent 3,773,650.
  • the waxy oil is chilled to a temperature about 35°F above the filter temperature in the apparatus described above, with chilling down to the filter temperature being performed in a subsequent scraped surface chiller. This embodiment is described in U.S. Patent 3,775,288.
  • the low miscibility dewaxing solvents which are typically used in solvent dewaxing processes and which are the same solvents which are used in the process of the present invention include C3-C6 ketones such acetone, methyl ethyl ketone (MEK), methyl isobutyl ketone (MIBK) and mixtures thereof, such as MEK/MIBK.
  • the heavy high boiling high VI waxy oil can be that material obtained by isomerizing wax either synthetic wax as is obtained from Fischer-Tropsch synthesis or natural wax as is obtained by dewaxing hydrocarbon oils, commonly called slack wax or a natural petroleum material such as hydrocracked oil, deasphalted 600N or, Bright Stock oil.
  • the waxy oil to be dewaxed is a heavy high boiling high VI wax isomerate
  • heavy-high boiling-high VI materials be they isomerates natural oils, or hydrocracked oils are those materials having a viscosity in the range 6 to 12 cSt @ 100°C, preferably 8 to 10 cSt @ 100°C, a mid LV% boiling point of 450 to 550°C, preferably 475 to 525°C and a VI of at least 120, preferably at least 140.
  • the light, lower boiling lower VI oil is one having a viscosity of about 3 to 7 cSt @ 100°C, preferably about 4 to 6 cSt @ 100°C, a 90% off point about 0 to 300°F, preferably about 50 to 100°F, lower than the 10% off point of the heavy oil and a VI of less than about 110, preferably less than about 100.
  • the heavy oil is mixed with a volume of light oil to permit operation of the solvent dewaxing process under miscible conditions at a filter temperature low enough to produce an oil having a pour point of at least -21°C.
  • the resulting dewaxed oil product is fractionated into fractions corresponding very closely to the original parent materials (i.e. a light oil fraction of conventional VI and a heavy oil fraction of high VI). Each of these fractions possesses a pour point of at least about -21°C, the pour point of the mixture.
  • the yield of heavy oil of -21°C pour obtained by this co-processing technique is higher than that achievable by processing the heavy oil by itself.
  • the wax which is isomerized may come from any of a number of sources. Synthetic waxes from Fischer-Tropsch processes may be used, as may be waxes recovered from the solvent or autorefrigerative dewaxing of conventional hydrocarbon oils as well as mixtures of these waxes. Waxes from dewaxing conventional hydrocarbon oils are commonly called slack waxes and usually contain an appreciable amount of oil. The oil content of these slack waxes can range anywhere from 0 to 45% or more, usually 5 to 30% oil. For the purposes of this application, the heavy waxes recovered from the dewaxing of Bright Stock and the heavy Fischer-Tropsch waxes are the feeds of choice.
  • Hydroisomerization may be performed over any of the standard hydroisomerization catalysts which contain a hydrogenation metal selected from Group VIB and Group VIII and mixtures thereof, preferably the Group VIII metals, more preferably the noble Group VIII metals, most preferably platinum.
  • Metal loading ranges between 0.1 to 5.0 wt% metal, preferably 0.1 to 1.0 wt% metal, most preferably 0.2 to 0.6 wt% metal.
  • the hydrogenation metal component is supported on a refractory inorganic metal oxide support, preferably alumina or silica-alumina, most preferably the transition aluminas, e.g., gamma alumina.
  • a refractory inorganic metal oxide support preferably alumina or silica-alumina, most preferably the transition aluminas, e.g., gamma alumina.
  • the support is halogenated.
  • the halogen is usually chlorine or fluorine or mixture thereof, preferably fluorine, with net halogen content in the range 1 to 10 wt%, preferably 2 to 8 wt%.
  • Isomerization is conducted under conditions of temperature between about 250 to 400°C, preferably 270-360°C, pressures of 500 to 3000 psi H2, preferably 1000-1500 psi H2, hydrogen gas rates of 1000 to 10,000 SCF/bbl, and a space velocity in the range 0.1-10 v/v/hr, preferably 1-2 v/v/hr.
  • Preferred catalysts are the subject of U.S. Patent 4,959,337, U.S. Patent 4,906,601 and U.S. Patent 4,900,707.
  • a most preferred catalyst is the subject of U.S. Patent 4,906,601.
  • the use of that catalyst for wax isomerization is the subject of U.S. Patent 4,923,588.
  • That catalyst comprises a noble Group VIII metal on low fluoride content small particle size refractory metal oxide base.
  • the catalyst is characterized by having a fluoride content in the range of 0.1 to up to but less than 2 wt%, preferably 0.1 to 1.5 wt%, more preferably 0.2 to 1.0 wt%, a particle diameter of less than 1/16 inch and a preferred noble Group VIII metal loading in the range of 0.1 to 2.0 wt%.
  • the preferred small particle support is 1/20 inch trilobe alumina.
  • noble metal isomerization catalysts are extremely susceptible to deactivation by the presence of heteroatom compounds (i.e. N, O or S compounds) in the wax feed so care must be exercised to remove such heteroatom materials from the wax feed charges.
  • heteroatom compounds i.e. N, O or S compounds
  • such precautions may not be necessary. In such cases, subjecting such waxes to very mild hydrotreating may be sufficient to insure protection for the isomerization catalyst.
  • waxes obtained from natural petroleum sources contain quantities of heteroatom compounds as well as appreciable quantities of oil which contain heteroatom compounds.
  • the slack waxes should be hydrotreated to reduce the level of heteroatom compounds to levels commonly accepted in the industry as tolerable for feeds to be exposed to isomerization catalysts. Such levels will typically be a N content of about 1 to 5 ppm and a S content of about 1 to 20 ppm, preferably 2 ppm or less nitrogen and 5 ppm or less sulfur. Similarly, such slack waxes prior to hydrotreating should be deoiled to an oil content in the range of 0 to 35% oil, preferably 5 to 25% oil.
  • the hydrotreating step will employ a typical hydrotreating catalyst such as Co/Mo or Ni/Mo on alumina under standard, commercially acceptable conditions, e.g., temperature of 280 to 400°C, space velocity of 0.1 to 2.0 V/V/hr, pressure of from 500 to 3000 psig H2 and hydrogen gas rates of from 500 to 5000 SCF/bbl.
  • a typical hydrotreating catalyst such as Co/Mo or Ni/Mo on alumina under standard, commercially acceptable conditions, e.g., temperature of 280 to 400°C, space velocity of 0.1 to 2.0 V/V/hr, pressure of from 500 to 3000 psig H2 and hydrogen gas rates of from 500 to 5000 SCF/bbl.
  • Figure 1 shows how the miscibility of a Fischer-Tropsch 8.7 cSt @100°C isomerate fraction boiling in the 550 to 575°C range (about equivalent to a 250N viscosity grade) can be improved about 10°C with the addition of 33% of a conventional 150N basestock. Filtration studies were performed with this combined feedstock and compared with base case evaluation of the neat Fischer-Tropsch 8.7 cSt @100°C wax isomerate.
  • the isomerate was made by isomerizing a Fischer-Tropsch 150 wax as feed over an isomerization catalyst comprising 0.6 Pt/5.6% F/Al2O3 at a temperature between 365 to 375°C, a pressure of 1000 psig, a H2 flow rate of 7500 SCF H2/bbl and a LHSV of 1.
  • the dewaxing data are given in Table 1.
  • the filter temperature can be lowered below the target pour without immiscibility occurring. Low pours (-21°C) were achieved at good yields.
  • the lower filtration rate of 5.2 m3/M2d is not necessarily cause for concern as plants running 600N stocks are typically designed for filter rates of 4 to 6 m3/m2d and techniques to handle these rates are known.
  • the product from the dewaxer is a mixture of conventional and non-conventional lube.
  • Crucial to the process is the successful separation of the light dewaxed oil from the heavy dewaxed oil e.g. the light conventional oil from the heavier isomerate oil. While any separation process (distillation, extraction, membranes, etc.) could be considered, the simplest and most straight forward process is distillation. For that reason low boiling conventional lubes are co-processed with the relatively high boiling isomerate oils. It is interesting to note that this does not imply a wide difference in viscosity grades. Due to the highly paraffinic nature of the isomerate oil it has a much higher boiling point than equivalent viscosity conventional stocks. This difference in the viscosity/boiling point relationship makes the separation of a 5.0 cSt 150N oil and a 8.7 cSt Fischer Tropsch wax isomerate quite feasible as demonstrated in Table 2.
  • dewaxed oil product from the co-processing was cut into fractions which were then reblended to roughly the same specifications as would be possessed by individually processed dewaxed oil fractions (See Table 2).
EP19910306827 1990-07-30 1991-07-29 Verfahren zur Herstellung von Schmierölen mit niedrigem Stockpunkt und hohem Viskositätsindex durch Lösungsmittelentparaffinierung Expired - Lifetime EP0471461B1 (de)

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US55977990A 1990-07-30 1990-07-30
US559779 1990-07-30

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EP0471461A2 true EP0471461A2 (de) 1992-02-19
EP0471461A3 EP0471461A3 (de) 1992-03-18
EP0471461B1 EP0471461B1 (de) 1994-08-24

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EP (1) EP0471461B1 (de)
JP (1) JPH04233996A (de)
CA (1) CA2047075A1 (de)
DE (1) DE69103598T2 (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1993004147A1 (en) * 1991-08-27 1993-03-04 Mobil Oil Ag Carburetor fuel additive
US9587184B2 (en) 2011-09-21 2017-03-07 Exxonmobil Research And Engineering Company Lubricant base oil hydroprocessing and blending
CN114437815A (zh) * 2020-10-30 2022-05-06 中国石油化工股份有限公司 一种制备光亮油的方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7655132B2 (en) * 2004-05-04 2010-02-02 Chevron U.S.A. Inc. Process for improving the lubricating properties of base oils using isomerized petroleum product

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3365390A (en) * 1966-08-23 1968-01-23 Chevron Res Lubricating oil production
DE2625635A1 (de) * 1976-06-08 1977-12-22 Texaco Development Corp Verfahren zur herstellung eines schmieroels mit hohem viskositaetsindex

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3365390A (en) * 1966-08-23 1968-01-23 Chevron Res Lubricating oil production
DE2625635A1 (de) * 1976-06-08 1977-12-22 Texaco Development Corp Verfahren zur herstellung eines schmieroels mit hohem viskositaetsindex

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1993004147A1 (en) * 1991-08-27 1993-03-04 Mobil Oil Ag Carburetor fuel additive
US9587184B2 (en) 2011-09-21 2017-03-07 Exxonmobil Research And Engineering Company Lubricant base oil hydroprocessing and blending
CN114437815A (zh) * 2020-10-30 2022-05-06 中国石油化工股份有限公司 一种制备光亮油的方法
CN114437815B (zh) * 2020-10-30 2023-10-10 中国石油化工股份有限公司 一种制备光亮油的方法

Also Published As

Publication number Publication date
DE69103598T2 (de) 1994-12-22
CA2047075A1 (en) 1992-01-31
DE69103598D1 (de) 1994-09-29
EP0471461B1 (de) 1994-08-24
EP0471461A3 (de) 1992-03-18
JPH04233996A (ja) 1992-08-21

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