US3470089A - Separation of solvent from raffinate phase in the solvent refining of lubricating oil stocks with n-methyl-2-pyrrolidone - Google Patents

Separation of solvent from raffinate phase in the solvent refining of lubricating oil stocks with n-methyl-2-pyrrolidone Download PDF

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Publication number
US3470089A
US3470089A US648533A US3470089DA US3470089A US 3470089 A US3470089 A US 3470089A US 648533 A US648533 A US 648533A US 3470089D A US3470089D A US 3470089DA US 3470089 A US3470089 A US 3470089A
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solvent
oil
water
mix
percent
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Herbert C Morris
John I Nixon
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Texaco Inc
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Texaco Inc
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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
    • C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
    • C10G21/28—Recovery of used solvent

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  • Solvent is separated from rainate-mix by adding water in an amount of at least 2.0 weight percent of the N-methyl- Z-pyrrolidone dissolved therein effecting separation of an oil phase and a wet solvent phase comprising at least 2.0 weight percent water. Refined oil is separated by distilling remaining solvent therefrom. Wet solvent is recycled with solvent of lower water content to comprise at least a part of the solvent charged in contact with said lubricating oil charge stock.
  • This invention is directed to the solvent refining of lubricating oil charge stocks with N-methyl-Z-pyrrolidone hereinafter referred to as NMP.
  • NMP N-methyl-Z-pyrrolidone
  • the lubricating oil charge stock is contacted with a solvent stream comprising NMP and not more than about 1.0 Weight percent water forming a railinate-mix comprising a major portion of oil with a minor portion of NMP dissolved therein.
  • An extract-mix is also separated comprising a major portion of solvent with the extract constituents dissolved therein.
  • This invention relates to an improved method of separating the NMP dissolved in the raffinate-mix.
  • NMP has been known as a solvent for the separation of olelins, dioleiins, and aromatic hydrocarbons.
  • the usual method of separation of solvent from the resulting extract and rainate-mix has been by simple distillation. Disadvantages of simple distillation are that the entire raffinate-mix must be subjected to distillation thereby subjecting the refined oil to an additional distillation step and requiring relatively large distillation facilities.
  • Solvent extraction with NMP may be applied to parain base oils for example, oils used in the manufacture of crankcase lubricants for internal combustion engines, and naphtenic oils for example, oils used in the manufacture of turbine lubricating oils.
  • an extraction temperature within the range of about to 250 F. and preferably within the range of about to 180 F. is employed and a solvent dosage within the range of about 50 to 450 percent and preferably about 100 to 340 percent is employed.
  • the corresponding extraction temperatures and dosages when relining naphthene oils are within the range of about 50 to 200 F., preferably within the range of about 75 to 150 F. and about 50 to 300 percent, and preferably about 75 to 200 percent respectively.
  • the dosage of solvent employed is only about half that employed with furfural, a widely used selective solvent.
  • the viscosity index of parain base lubricating oil charge stocks is within the range of about 40 to 105 and the viscosity index of the refined lubricating oil stock is at least ten units higher.
  • water in an amount within the range of about 2 to 20 weight percent and preferably about 5.0 weight percent of the NMP in the raflinate-mix is added thereto to effect separation of a wet solvent phase.
  • the effect of water addition to a rainate-mix containing 30 weight percent NMP produced in the treatment of a wax distillate at F. is shown in the following Table I.
  • the amount of wet solvent layer separated may be increased by cooling the diluted rafiinate-mix to a temperature below the treating temperature.
  • the degree of sepation of wet solvent from the refined oil phase is a function of the boiling range of the charge stock, the temperature of the raffinate-mix leaving the extractor, the amount of water added, and the degree of cooling.
  • the lower the boiling range of the charge stock and the higher the raffinate-mix temperature leaving the extractor the greater is the amount of solvent soluble in the oil phase.
  • operating with the lowest possible raffinate-mix outlet temperature necessary to obtain the desired quality and the lowest practical wet solvent separation temperature minimizes the volume of solvent remaining in the oil phase and permits the separation of the desired amount of wet solvent with a minimum of water.
  • the use of a minimum amount of dilution water permits the use of the largest volume of wet solvent from other processing steps while controlling the water content to 1.0 weight percent maximum.
  • the volume of aromatic oil contained in the wet solvent is less than 0.3 weight percent of the recycled solvent which does not have any significant effect on the solvent power of the solvent recycled in the extraction step.
  • the aromatic oil dissolved in the wet solvent is similar to the extract oil and does not build up in the recycle solvent since it is, in effect, displaced into the extract oil.
  • Dissolved water has a substantial effect upon the solvent refining characteristics of NMP.
  • the effect is shown in a series of tests wherein a vacuum distillate :from crude distillation referred to as a Wax Distillate 7 and having a refractive index at 70 of 1.4741 is solvent refined with NMP at constant conditions of solvent dosage and extract outlet temperature with varying amounts of water dissolved in the NMP solvent. Results of this series of ltests are shown in Table II following:
  • Solvent dosage volume percent 200 200 200 200 200 200 Extraction temperature
  • the raffinate mix is produced by refining a Vacuuml Distillate 20 with NMP at a solvent dosage of volume percent, .an extract-mix outlet temperature of F. and a raffinate-mix outlet temperature of 190 F.
  • the resulting raffinate-mix comprises 19.3 weight percent oil which upon stripping produces a stripped oil having a refractive index at 70 C. of 1.4605.
  • Other portions of said raffinate-mix are treated by water addition, Water addition with cooling, or by cooling alone to effect separation of two phases, an upper oil layer containing dissolved solvent and water and .a bottom solvent layer containing dissolved oil and water.
  • Table III The yields and cornpositions of the resulting layers are shown in Table III following:
  • Solvent dosage volume percent charge 200 414 107 411 Extraction temperature, F 200 200 200 200 Refined oil yield, volume percent... 45. 2 50. 5 60. 0 66. 2 Refined oil quality: RI at 70 C 1, 4622 1, 4620 1, 4665 1,4667
  • FIG. 1 is a flow diagram of a solvent refining system employing the process of this invention.
  • the figure illustrates particular arrangements of apparatus in which the invention may be pracdisc contactor, and it may include mechanical means to improve contacting such as sonic generators or pulsing means.
  • Solvent is introduced in the top of extractor 2 through line 26.
  • the charge oil constituents soluble in the solvent leave the extractor as extract-mix through into the rainate-mix and controlling the temperature to which this phase is cooled in balance with the amount of atmospheric ash tower overhead split to the recycle stream. y
  • Atmospheric flash tower bottoms of reduced solvent line 3 at a temperature of about 185 F. with the bulk 5 content is withdrawn through line 41, through heating of the solvent.
  • the charge stock constituents insoluble coil 42 in furnace 43 where it is heated to about 538 in the solvent leave the extractor through line 4 at a F. and discharged through line 44 to pressure hash tower temperature of about 190 F. as ra'inate-mix containing 45 at a top tower pressure of about 55 pounds per square some dissolved solvent. Water in an amount of about 5 10 inch absolute. About 90 percent of the solvent remaining weight percent of the dissolved solvent in line 5 in inin the extract-mix is removed as dry distillate through jected into the raffinate-mix .and the mixture passed to line 46.
  • This stream is passed through heat exchanger 32 cooler 7. Cooled, diluted raffinate-mix at about 130 F. and line 47 to comprise the dry solvent combined with is passed through line 8 to separator 9.
  • Separator 9 is the wet solvent in line 25. Extract oil with a small amount divided into two compartments by wier 10. Wet solvent of remaining solvent is Withdrawn through line 50 and phase having an upper level 11 is separated in the compassed at about 523 F. to vacuum flash tower 51 which partmcnt behind wier 10 and is withdrawn through line is operated at a top tower pressure of about 2 pounds per 12, and recycled with dry solvent through lines and square inch absolute so that about 95 percent of the re- 26 to extractor 2. Separated oil phase, having an upper maining solvent is flashed overhead through line 52.
  • vacuum steam stripper 56 comprising steam and solvent Reiined oil product is withdrawn from stripper 18 through is combined with the wet streams in lines 38 .and 21 and line 20, passed through line to solvent dryer 61.
  • Solvent dryer yExtract-mix at a temperature of about F, leaving 61 is a fractional distillation tower which is operated at extractor 2 through line 3 is passed through exchanger a OP OWCI PreSSure 0f about 18 Pounds per Square inch 30, line 31, exchanger 32 and line 33 to atmospheric Hash 35 absolute to remove water as distillate which is discharged tower 34 operated at a top tower pressure of about 20 through line 62.
  • Dry solvent is withdrawn from the botpounds per square inch absolute, Heat supplied by extoni of solvent dryer 61 through line 63 .and is recycled changers 30 and 32 raises the extract-mix temperature to i0 eXraCOl' 2 through lines 53 and 26 With the dry solabout 418 F. and effects vaporization of about 40 per- Vent from lines 52 and47.
  • a vacuum distillate heat to exchanger 30 1s Passed through hhe 36 to Supply from crude distillation is rened with NMP in the appaheat tf exehehger 16 and 1S 'heh passed throhgh 37' ratus and at the conditions described in connection with The distillate in line 37 comprising solvent and dissolved 45 FIGURE l, NMP Solvent containing 1.0 weight percent Water 1S f heh, Spht betWeeh the Solvent recycled to eX water is employed at a solvent dosage of 151 volume perh'aetor z 1h hhe 2 5 and fed to the s olveht drylhg :tower cent.
  • a yield of refined oil of 68.9 weight percent is ob- 1r1 1111@ 38 1n afatlo Controlled t0 mamfam the maXlmum tained which refined sii has a gravity API of 31.1, and a WaCI desired 111 the recycled Solvent AS 'die Wafer COH- viscosity index before dewaxing of 105.0.
  • a material baltent and volume of the stream in line 12 is increased, 50 ance Showing the distribution of NM1), Water, and Oil less of the atmospheric flash tower distillate in line 37 fractions in the refining of 10,000 barrels per day of the is included in the recycled solvent passed through line Wax Distillate 20 charge stock is shown in Table V, 25. Recovery is optimized by injecting a volume of water following.
  • said lubricating oil charge stock is a parafiinic base oil having a viscosity index within the range of about 40 to 105 and the viscosity index of said refined oil is at least l0 units higher than said lubricating oil charge stock.

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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)
  • Pyrrole Compounds (AREA)
US648533A 1967-06-20 1967-06-20 Separation of solvent from raffinate phase in the solvent refining of lubricating oil stocks with n-methyl-2-pyrrolidone Expired - Lifetime US3470089A (en)

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US (1) US3470089A (enrdf_load_stackoverflow)
ES (1) ES413874A3 (enrdf_load_stackoverflow)
FR (1) FR1579639A (enrdf_load_stackoverflow)
GB (1) GB1166975A (enrdf_load_stackoverflow)
NL (1) NL147778B (enrdf_load_stackoverflow)

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2709679A1 (de) * 1976-03-26 1977-09-29 Exxon Research Engineering Co Verfahren zur wiedergewinnung von n-methyl-2-pyrrolidon bei kw-extraktionsverfahren
US4168226A (en) * 1977-04-08 1979-09-18 Exxon Research & Engineering Co. Thermal stabilization of N-methyl-2-pyrrolidone
DE2918853A1 (de) * 1978-05-10 1979-11-15 Lummus Co Verfahren zur wiedergewinnung von loesungsmitteln beim aufarbeiten von kohlenwasserstoffen
US4294689A (en) * 1980-02-14 1981-10-13 Texaco, Inc. Solvent refining process
DE3107360A1 (de) * 1980-03-07 1982-02-18 Texaco Development Corp., 10650 White Plains, N.Y. "verfahren zur loesungsmittelraffinierung von kohlenwasserstoffgemischen"
US4390418A (en) * 1982-05-12 1983-06-28 Texaco Inc. Recovery of solvent in hydrocarbon processing systems
US4419227A (en) * 1982-05-12 1983-12-06 Texaco Inc. Recovery of solvent from a hydrocarbon extract
US4422923A (en) * 1980-01-29 1983-12-27 Edeleanu Gesellschaft Mbh Process for recovering solvents from solvent-containing hydrocarbon phases in hydrocarbon raffination systems
US4781820A (en) * 1985-07-05 1988-11-01 Union Carbide Corporation Aromatic extraction process using mixed polyalkylene glycols/glycol ether solvents
US9512369B1 (en) 2013-03-14 2016-12-06 James Joseph Noble Process for removing color bodies from used oil
US11479736B1 (en) 2021-06-04 2022-10-25 Afton Chemical Corporation Lubricant composition for reduced engine sludge

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA950851A (en) * 1970-03-16 1974-07-09 Ian D. Campbell Stability of hydrocracked lubricating oils to air and light
EP2882830B1 (en) * 2012-08-09 2018-01-03 Council of Scientific & Industrial Research A process for production of benzene lean gasoline by recovery of high purity benzene from unprocessed cracked gasoline fraction containing organic peroxides

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2923680A (en) * 1956-12-31 1960-02-02 Exxon Research Engineering Co Extraction process for refining lubricating oils
US2963427A (en) * 1956-04-18 1960-12-06 Standard Oil Co Aromatics recovery system using butyrolactone in the first stage and propane in the second stage
CA610414A (en) * 1960-12-13 D. Morin Richard Separation of hydrocarbon mixtures

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA610414A (en) * 1960-12-13 D. Morin Richard Separation of hydrocarbon mixtures
US2963427A (en) * 1956-04-18 1960-12-06 Standard Oil Co Aromatics recovery system using butyrolactone in the first stage and propane in the second stage
US2923680A (en) * 1956-12-31 1960-02-02 Exxon Research Engineering Co Extraction process for refining lubricating oils

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2709679A1 (de) * 1976-03-26 1977-09-29 Exxon Research Engineering Co Verfahren zur wiedergewinnung von n-methyl-2-pyrrolidon bei kw-extraktionsverfahren
US4168226A (en) * 1977-04-08 1979-09-18 Exxon Research & Engineering Co. Thermal stabilization of N-methyl-2-pyrrolidone
DE2918853A1 (de) * 1978-05-10 1979-11-15 Lummus Co Verfahren zur wiedergewinnung von loesungsmitteln beim aufarbeiten von kohlenwasserstoffen
US4422923A (en) * 1980-01-29 1983-12-27 Edeleanu Gesellschaft Mbh Process for recovering solvents from solvent-containing hydrocarbon phases in hydrocarbon raffination systems
US4294689A (en) * 1980-02-14 1981-10-13 Texaco, Inc. Solvent refining process
DE3107360A1 (de) * 1980-03-07 1982-02-18 Texaco Development Corp., 10650 White Plains, N.Y. "verfahren zur loesungsmittelraffinierung von kohlenwasserstoffgemischen"
US4390418A (en) * 1982-05-12 1983-06-28 Texaco Inc. Recovery of solvent in hydrocarbon processing systems
US4419227A (en) * 1982-05-12 1983-12-06 Texaco Inc. Recovery of solvent from a hydrocarbon extract
US4781820A (en) * 1985-07-05 1988-11-01 Union Carbide Corporation Aromatic extraction process using mixed polyalkylene glycols/glycol ether solvents
US9512369B1 (en) 2013-03-14 2016-12-06 James Joseph Noble Process for removing color bodies from used oil
US11479736B1 (en) 2021-06-04 2022-10-25 Afton Chemical Corporation Lubricant composition for reduced engine sludge

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NL147778B (nl) 1975-11-17
DE1770368B1 (de) 1972-11-02
ES413874A3 (es) 1976-04-01
NL6808515A (enrdf_load_stackoverflow) 1968-12-23
GB1166975A (en) 1969-10-15
FR1579639A (enrdf_load_stackoverflow) 1969-08-29

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