US3516928A - Method of preparation of lubricating oils - Google Patents

Method of preparation of lubricating oils Download PDF

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Publication number
US3516928A
US3516928A US617593A US3516928DA US3516928A US 3516928 A US3516928 A US 3516928A US 617593 A US617593 A US 617593A US 3516928D A US3516928D A US 3516928DA US 3516928 A US3516928 A US 3516928A
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United States
Prior art keywords
gas
pressure
critical
feedstock
temperature
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Expired - Lifetime
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US617593A
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English (en)
Inventor
William Ronald King
William Llewelyn Thomas
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BP PLC
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BP PLC
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G31/00Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0403Solvent extraction of solutions which are liquid with a supercritical fluid
    • B01D11/0407Solvent extraction of solutions which are liquid with a supercritical fluid the supercritical fluid acting as solvent for the solute

Definitions

  • This invention relates to a method of preparation of lubricating oil base stocks, using a super-critical gas phase separation technique.
  • Dutch published patent application No. 6404125 refers to the use of a gas at super-critical temperature and pressure to separate the constituents of a mixture of liquid and/or solid substances. These constituents may be absorbed to varying extents in the super-critical gas, and may be separated therefrom by lowering the pressure and/or increasing the temperature.
  • Lubricating oils may desirably have a high content of naphthenes and the present process therefore provides a means by which base stocks suitable for the preparation of lubricating oils and greases may be prepared. Since.
  • n-parafiins may be absorbed preferentially to naphthenes by a gas under super-critical conditions of temperature and pressure
  • the feedstock should have a low n-paraftin or wax content.
  • it should have a cloud point of less than 30 F. If necessary reduction in wax or n-paraffin content to this level may be. achieved by conventional solvent or catalytic dewaxing procedures, or by the technique using a gas under super-critical conditions of temperature and pressure disclosed in our co-pending British patent application No. 7,682/66.
  • the method of the invention produces a material of reduced sulphur content compared to the original feedstock. If a product of low sulphur content is required, then a low sulphur feedstock should be. used. Conversely, a material of moderate sulphur content may be desirable as a base stock for certain lubricant applications, and in this case a feedstock having a suitably higher sulphur content should [be chosen. The materials obtained will boil within the range 350-590 C., depending on the boiling range of the feedstock.
  • the invention accordingly consists in a method of preparing a petroleum material of greater naphthene content than the original feedstock which comprises contacting a naphthenic feedstock boiling above 300 C. and, of low nparaflin content with a gas under super-critical conditions of temperature and pressure, removing the gas phase product, and separating therefrom a material enriched in naphthenes.
  • the feedstock may be a crude petroleum or a fraction derived therefrom.
  • the fraction treated may be derived from the crude petroleum by conventional distillation, or super-critical means may be employed. In the latter case the crude petroleum may be separated into light and heavy fractions and the latter contacted with super-critical gas at lower pressure and higher temperature than in the initial separation.
  • the choice of gas used in a super-critical separation process, and the. temperature and pressure at which it is used, will depend on the components to be separated. Thus, the gas must be inert with respect to the components to be separated. Since absorbability is greater the nearer the process temperature is to the critical temperature of the gas and the greater is the process pressure, it is desirable. that a gas be chosen whose critical temperature is near, but below, the desired working temperature, and whose critical pressure is, as far as possible, much below the desired working pressure.
  • the working temperature should not be more than C. above the critical temperature. In addition it is preferable that the working temperature should be within the range -100 C. to +300 C., and that the boiling point of the feedstock should be at least 100 C. above the critical temperature of the gas.
  • suitable gases for use in the method of the present invention include the lower alkanes and alkenes and their halogenated derivatives, and inorganic gases such as carbon dioxide and ammonia. Mixtures of one or more of these gases may be used provided that they are inert with respect to the feedstock.
  • gases ethane, ethylene, propane, and propylene are especially preferred.
  • This comprises a visual cell 1 of 180 ml. capacity which is a flanged stainless steel cylinder capable of withstanding pressures of up to 10,000 p.s.i., and fitted with a sight glass along its entire length, connected at its top via nylon tubing and a valve 3 to a small glass graduated receiver 4, fitted with a side arm and a valve 5.
  • the side arm is connected to a gas meter 13, the gas from which is vented to atmosphere, or compressed and recirculated to the system.
  • the bottom of the cell is connected by high pressure small bore tubing via a valve 2 and another valve 8 to the top of a gas cell 7 containing mercury.
  • the gas cell is connected via a valve 9 to a mercury pump '10 fitted with a pressure gauge 11. Gas is supplied from cylinder 12.
  • the pump is an electrically driven positive displacement device of conventional design.
  • the visual cell and the receiver, together with the associated valves 2, 3' and 5, are located in an electrically heated and thermostatically controlled air oven 6 fitted with a window and means for applying slight agitation to the cell.
  • valve 2 was closed and valve 3 gradually opened so as to bring the pressure in the visual cell down to atmospheric.
  • the residue remaining in the cell was fluid it was drained through valve 2 after disconnecting from valve 8. Otherwise the top flange of the visual cell was removed and the material dissolved in a low boiling hydrocarbon solvent and removed. With this material was combined material, if any, which had collected in the receiver during de-pressurisation of the visual cell. The solvent was stripped otf conventionally in a stream of nitrogen.
  • a material balance for each experiment was made by weighing the quantity of feedstock charged to the cell, and also each of the gas phase fractions and the residue.
  • the product rate was expressed as the weight of material vaporised per unit volume of gas measured at NTP.
  • the super-critical gas phase products have slightly lower sulphur contents than the corresponding distillates and they also have low asphaltene contents.
  • their colour was better than that of the distillate fractions. All these characteristics are desirable in a lubricating oil base stock, and such a stock can be obtained as has been described without the need to use large quantities of liquid solvents or catalytic methods using relatively arduous conditions.
  • a method of obtaining naphthenic lubricating oil base stock having a greater naphthene content than the original feedstock from a naphthenic feedstock having a low n-paraflln content in one stage without any need for further processing which comprises contacting the naphthenic feedstock boiling above 300 C. and having a low n-paraffin content and a cloud point of less than 30 F., with a gas selected from the group consisting of lower alkanes, lower alkenes, and halogenated derivatives thereof at a working temperature and a working pressure'above the critical temperature and the critical pressure of said gas, said working temperature being within the range C. to 300 C. and not more than 100 C.
  • a method of obtaining naphthenic lubricating oil base stock having a greaternaphthene content than the original feedstock from a naphthenic feedstock having a low n-parafiin content in one stage without any need for further processing which comprises contacting the naphthenic feedstock boiling above 300 C. and having a low n-paraffin content and a colud point of less than --30 F., with a gas selected from the group consisting of ethane, ethylene, propane, propylene, carbon dioxide, ammonia, and their inert mixtures thereof at a working temperature and a working pressure above the critical temperature and the critical pressure of said gas, said working temperature being within the range 100 C. to 300 C. and not more than 100 C.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Lubricants (AREA)
US617593A 1966-02-22 1967-02-21 Method of preparation of lubricating oils Expired - Lifetime US3516928A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB7684/66A GB1173746A (en) 1966-02-22 1966-02-22 Method of preparation of Lubricating Oils

Publications (1)

Publication Number Publication Date
US3516928A true US3516928A (en) 1970-06-23

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US617593A Expired - Lifetime US3516928A (en) 1966-02-22 1967-02-21 Method of preparation of lubricating oils

Country Status (7)

Country Link
US (1) US3516928A (de)
BE (1) BE694436A (de)
DE (1) DE1645695A1 (de)
FR (1) FR1512061A (de)
GB (1) GB1173746A (de)
NL (1) NL6702628A (de)
SE (1) SE341436B (de)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4191639A (en) * 1978-07-31 1980-03-04 Mobil Oil Corporation Process for deasphalting hydrocarbon oils
US4536283A (en) * 1984-08-20 1985-08-20 Exxon Research And Engineering Co. Integrated process for deasphalting heavy oils using a gaseous antisolvent
US4565623A (en) * 1984-08-20 1986-01-21 Exxon Research And Engineering Co. Method for deasphalting heavy oils using a miscible solvent at a low treat ratio and a carbon dioxide antisolvent
US9200211B2 (en) 2012-01-17 2015-12-01 Meg Energy Corp. Low complexity, high yield conversion of heavy hydrocarbons
US9481835B2 (en) 2010-03-02 2016-11-01 Meg Energy Corp. Optimal asphaltene conversion and removal for heavy hydrocarbons
US9976093B2 (en) 2013-02-25 2018-05-22 Meg Energy Corp. Separation of solid asphaltenes from heavy liquid hydrocarbons using novel apparatus and process (“IAS”)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2910973A1 (de) * 1979-03-21 1980-10-09 Krupp Koppers Gmbh Verfahren zur gewinnung von reinen dicarbonsaeuren, deren anhydriden und/oder estern
US5340268A (en) * 1992-02-20 1994-08-23 Dowty Alvis E Article handling mechanism for attachment to warehouse trucks

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2391576A (en) * 1942-09-05 1945-12-25 Phillips Petroleum Co High pressure separation
US2391607A (en) * 1942-10-05 1945-12-25 Phillips Petroleum Co High pressure separation process

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2391576A (en) * 1942-09-05 1945-12-25 Phillips Petroleum Co High pressure separation
US2391607A (en) * 1942-10-05 1945-12-25 Phillips Petroleum Co High pressure separation process

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4191639A (en) * 1978-07-31 1980-03-04 Mobil Oil Corporation Process for deasphalting hydrocarbon oils
US4536283A (en) * 1984-08-20 1985-08-20 Exxon Research And Engineering Co. Integrated process for deasphalting heavy oils using a gaseous antisolvent
US4565623A (en) * 1984-08-20 1986-01-21 Exxon Research And Engineering Co. Method for deasphalting heavy oils using a miscible solvent at a low treat ratio and a carbon dioxide antisolvent
US9481835B2 (en) 2010-03-02 2016-11-01 Meg Energy Corp. Optimal asphaltene conversion and removal for heavy hydrocarbons
US9890337B2 (en) 2010-03-02 2018-02-13 Meg Energy Corp. Optimal asphaltene conversion and removal for heavy hydrocarbons
US9200211B2 (en) 2012-01-17 2015-12-01 Meg Energy Corp. Low complexity, high yield conversion of heavy hydrocarbons
US9944864B2 (en) 2012-01-17 2018-04-17 Meg Energy Corp. Low complexity, high yield conversion of heavy hydrocarbons
US9976093B2 (en) 2013-02-25 2018-05-22 Meg Energy Corp. Separation of solid asphaltenes from heavy liquid hydrocarbons using novel apparatus and process (“IAS”)
US10280373B2 (en) 2013-02-25 2019-05-07 Meg Energy Corp. Separation of solid asphaltenes from heavy liquid hydrocarbons using novel apparatus and process (“IAS”)

Also Published As

Publication number Publication date
GB1173746A (en) 1969-12-10
DE1645695A1 (de) 1970-07-16
BE694436A (de) 1967-08-22
SE341436B (de) 1971-12-27
FR1512061A (fr) 1968-02-02
NL6702628A (de) 1967-08-23

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