US2031204A

US2031204A - Method for producing lubricating oil

Info

Publication number: US2031204A
Application number: US486725A
Authority: US
Inventors: Ulric B Bray
Original assignee: Union Oil Company of California
Current assignee: Union Oil Company of California
Priority date: 1930-10-06
Filing date: 1930-10-06
Publication date: 1936-02-18
Anticipated expiration: 1953-02-18

Description

Feb. 18, 1936. u. B. BRAY METHOD FOR PRODUCING LUBRICA'IING OIL 2 Sheets-Sheet 1 Filed Oct. 6, 1930 INVENTOR Ulric .5. Bray BY ATTORNEY Feb. 18, 1936. u. B. BRAY 2,031,204

Y METHOD FOR PRODUCING LUBRICATING 011.

Filed 00;. 6. 1930 2 Sheets-Sheet 2 INVENTOR. Ulric .5. Ez-ay BY f ATTORNEY Patented Feb. 18, 1936 Ulric B. Bray, Talon Vardes 2,031,204 sm'rnon roa raogi r omc unmcarmo Estates, minor to Union Oil Company of California, Los'lingeles, Callf., a corporation of Oaflfosnia ApplicationOctobcr e, um, Serial no. mass 15 Claim. (01. 196-18) This invention relates to the production of lubricating oils from crude oils containing asphalt and wax. 1

It has been discovered that superior lubricating 1 "5 oil and asphalt can be obtained-from crude oil bycausing separation of the lubricating 11 from the asphalt at temperatures below that a which deleterious changes are induced in the oil.

It has been found that if oil containing asphalt is heated in the presence of the asphalt, thelatter catalyzes certain reactions in the oil which result in the destruction of those characteristics of the lubricating oils which are most desirable.

It has been found advisable do cause the soll oration of the asphalt from the oil by means of volatile solvents which are capable of dissolving the oil and any wax and which do not dissolve the asphalt. Such solvents are light petroleum fractions, such as caslnghead gasoline. and

" naphtha and also petroleum fractions normally gaseous at ordinary temperature and pressure. Other solvents which may be used are alcohol, I ether, mixtures of alcohol and ether, acetone, etc. We prefer to use as our volatile solvent a 35 petroleum fraction obtained by the rectification of natural gasoline. The fractions are composed in the main of propane and isobutane. A typical analysis of such a fraction is 6.72% ethane, 72.2% propane, 19.91% lsobutane and 1.17%, normal. butane. It will be understood however that these merely illustrate the type of fractions used and the composition may vary. This fraction will hereinafter be referred to as propane for purposes of simplicity.

In order to cause extraction with this liquid fraction the solution is maintained at a pressure sufllcient to maintain the propane liquid at ordinary temperatures. The fraction above described is liquid at ordinary "temperatures at about 125 pounds pressure. The extraction of the oil from the asphalt at such pressure results in an asphalt substantially free of oil and a solution of oil in the liquid petroleum fraction, This solu-' tion contains substantially all the wax present in the crude oil. a It has also been found that oil containing asphalt and impurities such as wax may be first I freed from the asphalt-by a primary extraction with a light solventisuch as the solvent described 0 above and that the impurities such as wax may then be removed by the aid of a heavier solvent such as naphtha. By heavier solvent I mean one of higher boiling point than the light solvent previously described.

propane after separation from the oil. all or a substantial part of the propane is vaporized from the solvent oil solution "mder'a pressure sufflciently high to permit condensation with the cooling medium available. .The oil freed of this a solventisthentreatedtoremovewax. Theoil may also be purified by acid treatment, either before or after removal of the propane. By acid treatment I intend to include treatment with acid followed by the step of neutralization and/or 1. clay treatment. Since the oil will be too viscous at the low temperatures necessary for the removal of wax, naphtha is added to the all prior to the wax treatment. Naphta may also be added prior to chemical treatment in order to avoid s those difliculties usually encountered in chemical- 1y treating oils of high viscosity. By naphtha. I

(ethylene or the like, or mixtures of benzol with acetone or other ketones. or mixtures of bonsai and hut'anol or other alcohols. V 30 In addition to the'power which the'naphtha has of reducing the viscosity of the asphalt-free -oil, it also is used as an extracting-medium for wax or other material whose presence is deleterious in a finished, high grade lubricating oil. The naphtha if used in suflleient quantities at low .temperature acts as a solvent for the oil during the removal of the wax or other impurities in a manner similar to the action of the propane solution during the removal of the asphalt. By regu- 4o lating the quantity and temperature substantially oil free wax may be precipitated. In comparing their volatility and specific gravity, the propane is. considered to be the llflht solvent and the naphtha is the heavier solvent. An advan- 5 tage in using both light and heavy sdvents resides inthefactthatthedewaxingmaytakeplacein the presence of the heavier solvent after the lighter, more volatile solvent has been removed.

Hie crudeoil containing asphalt and wax is first topped to a temperature of about 600-625 1.

to remove thegaaoline, kerosene and all or a portion of the light lubricating oil, and the topped 1 residuum is then treated by the process hereinafter described.

It is, therefore, an object of my invention to produce lubricating oil from oil containing asphalt and wax by mixing this oil with a light solvent, said solvent being capable of separating the oil and wax from the asphalt, removing substantially all the solvent from the oil and wax, adding a heavier solvent such as naphtha to the oil and wax substantially free of the light solvent, and subsequently dewaxing the oil in the presence of the heavier solvent.

It is a further object of my invention to produce lubricating oil from the type of 011 above described by mixing this oil with a volatile solvent under pressure thereby separating the asphalt from the oil and wax, removing at least a substantial portion of the solvent from the .oil and wax under pressure, adding naphtha to the oil and wax substantially free of the solvent, and subsequently dewaxing the oil in the presence of the naphtha.

Another object of my invention is to include chemical treatment of the oil in the processes outlined above, said chemical treatment being either before or after the removal of the propane from the asphalt free oil.

The process will be more adequately understood by reference to the drawings which show schematic arrangements of the apparatus to carry out the process described herein.

Fig. 1 is a schematic arrangement of apparatus in which the oil is first made asphalt free and then is chemically treated under pressure following which the propane is distilled oil under pressure and then the oil is dewaxed in the presence of naphtha. 1

Fig. 2 is a schematic arrangement ef apparatus in which the oil is first made asphalt free and then a substantial portion of the propane is removed under pressure, following which the remaining propane is removed under released pres- I sure; the oil is chemically treated and finally dewaxed in the presence of naphtha.

Referring more particularly to Fig. 1, the topped residuum which has been produced from the selected crude by a suitable topping operation, preferably at GOO-625 F., is stored in tank I from which it is sent by pump 2 through line I to T 4 where it meets liquid propane containing a small amount of oil coming through line i. The mixture of propane and residuum pass from T 4 through mixing coil I into decanter I, where the asphalt in the topped residiuum isprecipitated and settles rapidly as a slurry. From the bottom of decanter I, the asphalt slurry is sent by pump 8 through line 8 to line III where fresh liquid propane is introduced by pump II from liquid propane storage l2. The asphalt slurry and fresh liquid propane are sent through mixing coil ll into decanter i4.

The asphalt-propane slurry from the bottom of decanter i4 is drawn off through expansion valve II and line it and discharged at a lower pressure into coil ll set in furnace ll, where heat is supplied for the purpose of vaporizing the propane and melting the asphalt. The heated materials are passed from coil ll through pressure reduction valve is into evaporator which operates at a lower pressure. superheated steam is introduced via 2i into evaporator 20 to supply additional heat and to reduce the asphalt to proper specifications as to flre and flash points. The asphalt is taken from the bottom of evaporator 20 and sent through the rundown line ill by pump 22 to asphalt storage II. The vapors in evaporator 20 pass through mist extractor 24 and are then sent through line 25 to cooler 28 and to separator 21. The uncondensed propane from separator 21 is sent through line 28 to line 29 and to propane compressor I! where its pressure is raised to the pressure in the high pressure system. The propane is then sent through line I I to propane cooler 32 where it liquefles and runs down into propane storage tank If.

The overflow from decanter i4, containing the oil and wax washed from the asphalt slurry taken from decanter I, is sent by pump 33 through line 5 to T 4 where it is mixed with the topped residuum and sent into decanter 1 as explained above. The overflow from decanter 1, consisting of propane and lubricating oil stock, is sent through pump 35 and line 38 to turbulence or mixing coilfl where the acid and alkali treatment of the extracted lubricating 011 stock begins. The countercurrent washing of the precipitated asphalt illustrated by the above method of operating decanters l and I4 may be extended to as many steps as desired, but in general two decanters giving two countercurrent washings will be sufficient to give an asphalt of satisfactory wax content.

To the propane solution of extracted lubricating stock, acid from tank 38 is added through line ll by means of pump 4|. The propane solution and acid are forced by the pumps 35 and 40 through mixing coil 31 into decanter 4i where the sludge is allowed to settle. The acid sludge is removed via 42. The oil containing some acid flows from decanter 4| through line 43 by pump 44 into decanter 45 where water is introduced as a spray through line 44, from water storage 41 through pump 48 and valve 49. The water washed oil overflows from decanter 4i and is sent by pump 50 to line II where caustic soda solution is introduced by pump 52 through line 53 from tank 54. The wash water is removed from decanter 4| via 56. The mixture of oil solution and aqueous alkali solution is forced through mixing coil 58 into decanter 51 where thespent caustic solution separates from the propane solution of the oil and is withdrawn via 58.

The overflow from decanter 51 goes through line I via pump 60 to decanter 6i where water is introduced as a spray through line 02 and valve 63 by pump 48. The continuous and rapid treatment of lubricating oil stocks as described above is made possible by operating in the presence of propane, and is a distinct advantage of the process. Wash water is removed from decanter 0| via 01. The neutralized and water washed oil solution overflowing from decanter BI is carried by pump 84 through-line 65 to the surge tank 88 which acts as a reservoir between the acid treating and propane recovery operations.

Decanters I, I4, 4|, 45, 51 and CI together with propane storage I! and surge tank 66 are maintained at the same pressure by means of equilibrium lines 10 controlled by valves H. The pressure that is maintained is 'suflicient to keep the solvent in liquid state at ordinary temperatures. For the solvent given above, this is about 125 lbs. per sq. in. at about 70 F.

The treated oil solution in tank 4! is sent through valve 15, line II and pump I1 into the high pressure exhausting column III, which preferably consists of plates Ii carrying closed steam coils 82. The pressure in II! is maintained at a sufficient point to cause condensation in condenser 32 without-applying additional pressure in the condenser.

As the oil in propane solution travels down column 80, the propane is vaporized, passes through mist extractor 83 and exits through line 84 to line 3| from which the vapors pass to cooler 32 where they are liquefied and allowed to run down into liquid propane storage I2. The bottoms from column 80 consist of treated lubricating oil containing a small amount of dissolved propane. These bottoms are drawn off through pressure release valve 85 and line 86 into which naphtha from tank 81 is introduced through pump 89 and line 89 controlled by valve 90. The naphtha and oil pass through mixing coil 9I into blending or storage tank 92. The use oi additional heat or agitation in tank 92 may or may not be necessary. The blended oil-naphtha mixture is then'passed from tank 92 through line 93 by pump 94 into cooling chamber 95 where the mixtureis chilled at a proper rate to a suitable dewaxing temperature by means of cooling coil 96. The chilled mixture passes through line 91, pump 98 and valve 89 into centrifuge I driven by motor NH. The dewaxed oil solution discharged from the center of the centrifuge is then sent through line I02 to dewaxed naphtha-oil storage I03.

The dewaxed oil solution is sent from storage' I03 through pump' I04 and line I05 to heat interchanger I06 where heat is absorbed from naphtha vapors and steam from column I01 as described below. Leaving heat interchanger I06, the oilnaphtha mixture passes into exhausting column I01 in which open steam may be introduced via I08. The bottoms from column I01 consist of acid treated and dewaxed oil which has been reduced by steaming to flash and flre characteristics determined in the main by the extent oi.'- topping oi the crude residuum stored in tank I. The bottoms from column I01 are removed via line I09 and may be cooled by heat exchange in heat exchanger H0 in a manner to be described below. The oil'leaving the heat exchanger 0' is sent by line I I I to treated oil storage I I2, from which it may be sent to a clay treating plant or the like.

The overhead from column I01 is sent through mist extractor H5 and then to heat exchanger I06 by line II6 where heat is imparted to the incoming naphtha-oil solution as described above. The partially condensed overhead vapors next pass from heat exchanger I06 through line I" to cooler H8 and then to separator II 9. The naphtha condensate in separator H9 is sent by pump I through line I2I to naphtha storage 81.

The uncondensed propane fromseparator II9 passes through line I22 to line 29 where it is admitted to the suction of propane compressor 30, which discharges into the high pressure propane vapor line 3| as describedabove.

The wax discharged from the centrifuge through line I25 is melted by hot water introduced through line I26. The hot water and melted wax in line I25 pass into wax separator I21 from which the wax is removed via I28 into storage I29.

The water settling in wax separator I21 is withdrawnthrough line I30 by pump I3I into water storage I32 from which it may be withdrawn through line I33 by pump I34 into line I26 which passes through heat exchanger 0. Before recycling into pipe I25 the water is thereby heated by heat exchange in H0 with the bottoms from column I01 which are correspondingly cooled.

Referring more particularly to Fig. 2, this embodiment relates to the aforesaid process in which a modification is made whereby the chemical treatment takes place in the absence oi substantial quantities of the solvent due to a preliminary removal or the solvent irom the oil and wax.

The topped residuum from tank I is carried through line 2 to pump 3 and thence to line 4 where it meets a propane solution of lubricating oil coming through line I5. The propane and residuum pass through the turbulence or mixing coil 5 into decanter 6. The asphalt in the residuum is precipitated by the propane and settles to the bottom of decanter 6. The asphaltpropane slurry from decanter 6 is passed through pump 8 in line 1 to line 9 where iresh liquid propane irom storage I0 coming through pump I0 and line 9 is added and the mixture then passes through mixing coil II into decanter I2. In this second extractionthe asphaltic bodies are freed of substantially all the oil and wax contained in the asphaltic material. The mixed oil and propane is passed through line I3, pump I4 and line I5 into line 4 for treatment as previously described. Decanters 6 and I2 and tank I0 are connected by pressure equalizing lines I6 controlled by valves I1. The pressuresin 6-, I2, and I0 are sufliciently high to maintain the solvent in liquid condition. For the solvent described above the pressure is about .125 lbs. at about 70 F.

The asphalt slurry from decanter I2 is drawn oil through the pressure release valve I1 and sent through'to coil I8 positioned in furnace I9 where suiiicient heat is supplied to cause vaporization of the propane and to melt the asphalt. The heated mixture of asphalt and propane is now sent through line 20 to the evaporator 2I where superheated steam is introduced via 22 in order to complete the vaporization of the propane and reduce the asphalt to satisfactory flash and fire specifications. The pressure in the vapor 'izer 2I is substantially atmospheric. vThe overhead from the evaporator 2I is sent through line 23 to condenser 24 and into separator 26 via line 25. The uncondensed propane from separator 26 is carried through line 21 to propane compressor 28.

The compressed propane from compressor 28 passes through line 29, line 30, pump 3I and line 32. .It is then condensed in condenser 33, the condensed propane passing to storage I0. The condensed oil which has been entrained inthe asphalt slurry and vaporized in 2I is withdrawn through 26a and the condensed steam through 261). The reduced asphalt is sent through-line 3 to asphalt storage 36 via pump 34.

The clear overflow from decanter 6 containin a higher percentage of dissolved lubricating oil passes through line 31. pump 38 and line 39 to heat exchange 40 where its temperature is raised somewhat before passing through line H into high pressure evaporator or dephlegmator 42. The object at this point is to add suflicient heat to the liquid propane solution to cause substantially complete vaporization of the liquid propane at a pressure somewhat higher than that qbeing maintained in cooler 33.v Heat may be applied at this point by any desired means. but

in the drawing a steam coil is shown in thebottom of the dephlegmator. The pressure in 42 is maintained by controlling the temperature in the dephlegmator by proper manipulation of valve 44a, in vapor line 44. The pressurein 42 is maintained at a sufiicient point to cause condensation in the condenser 33 without applying additional pressure in the condenser. When heat is applied to the propane solution under pressure,

the propane vaporizes and travels through 44, line 30, line 32 and cooler 33 where the propane condenses and passes back to liquid propane storage ill. The temperature and pressure employed in dephlegmator 42 will determine towhat extent the propane is completely removed from the oil remaining in the bottom of the dephlegmator, but in general there will be suilicient propane remaining in the oil drawn from the bottom of the dephlegmator to Justify a further recovery of propane under reduced pressure.

The oil leaving the dephlegrnator 42 then passes through the pressure release valve 4| and line 46 into the low pressure dephlegmator 41. Additional heat may or may not be needed at this point, but in order to insure more complete recovery of propane, steam may be introduced into dephlegmator 41, via 48. The overhead from dephlegmator 41 passes through line 40 to condenser ill and then into separator ii. The uncondensed propane from separator BI is carried through line 52 to propane compressor I. Canpressor II raises the pressure of the propane to that being carried in the high pressure evaporator 42 and the compressed propane is then passed through line 30 going eventually to propane storage Hi as described above. The water condensed in 5| is withdrawn through line 55 and any oil evaporated in 41 and condensed in MI is withdrawn through 54.

The hot lubricating oil stock in the bottom of the low pressure dephlegmator 41 is passed through line 56 by pump 51 to heat exchanger 46 where it imparts heat to the propane solution in line 4! as described above. Leaving the heat exchanger 4|! the oil passes through line I! to lubricating oil stockstorage 60 from which it is withdrawn by pump 6|.

If it is desired to chemically treat the lubricating stock in the presence of naphtha, the lubrieating oil stock passing through valve 62 in line It is admixed with naphtha passing from tank 63 via pump 04 by proper operation of valves 6! and 85 and 85. The mixture of oil and naphthe. passes through line 06 to agitator 61 where it is treated with sulfuric acid received from tank I by operation of pump is and valve II. The decanted oil-naphtha solution is drawn 03 through valved draw ofl lines 12, and carried through 13 into agitator 14. The acid sludge is withdrawn via draw off line H. The oil is then washed with water, treated with caustic 'and again washed in 14, in separate stages with intermediate withdrawal of water and caustic. Water is supplied from tank I5 by operation of pump (8 and valve 11, and caustic is supplied from tank 18 by operation of pump 80 and valve 8|.

The water and caustic are separately withdrawn via 82. The treated oil in agitator I4 is drawn oil through valve 83 and sent through line 86 by pump 81 to refrigeration machine 88. In case additional naphtha is needed for the dewaxing operation, this may be supplied through line '4 by opening valve ii.

If it is not desired to chemically treat the lubricating oil stock in the presence of naphtha, the

coll ll, compressor Ii, cooling coils l2, tank I! and expansion valve I. The refrigerant may be ammonia or a volatile product such as is used in the extraction operation described above. The operation of this refrigerating equipment will be understood by those skilled in the art.

The chilled solution is taken from the cooling vessel It by line 04 and passed into centrifuge II of conventional design. Wax is discharged from the centrifuge through line Ila. The discharged wax may be worked up by any convenient means for the recovery of naphtha and oil. Dewaxed naphtha solution is discharged from the centrifuge through line 06 into surge tank I1 and is sent through pump as and line II into heat exchanger Ill where it absorbs heat from condensing naphtha vapors coming through line I, as explained below. Instead of interchanging" the cold naphtha solution with naphtha vapors as in Ill, the cold naphtha solution may be inter- 1 changed with the incoming naphtha solution in line. before the naphtha solution is sent to chilling vessel ll.

The naphtha solution leaving heat exchanger III passes through line III to coil III in furnace I! and thence into evaporator I44 via line I". Suillcient heat is absorbed in coil III to raise the temperature sufliciently to distill the naphtha with aid of steam introduced via III into evaporator I44. The naphtha is taken overhead through line I to heat exchanger ill and to condenser ill via line I". The condensed naphtha is sent to separator I" and then passes through line H0, pump Ill and line H2 into naphtha storage tank 63. The condensed steam exits through l'illa. The bottom from evaporator il4, consisting of dewaxed oil are now passed through line H3, pump H4, cooler Hi and line I" into acid treated dewaxed oil storage tank Ill.

It is to be understood that the above is merely illustrative of preferred embodiments of the invention of which many variations may be made ing oil from an 011 containing asphalt and wax" which comprises mixing said oil with liquid propane, separating the asphalt from the oil, wax and liquid propane, acid treating the oil, wax and liquid propane, separating the propane from the acid treated oil and wax, adding a wax extracting solvent to the acid treated oil and'wax, separating the wax from the oil and wax extracting solvent and separating the wax extracting solvent 3. A process for the production of lubricating oil from an oil containing asphalt and wax which comprises mixing said oil with liquid propane, separating the asphalt from the oil, wax and liquid propane, acid and alkali treating the oil, wax and liquid propane, separating the propane from the treated oil and wax, adding a heavy solvent to the treated oil and wax, separating the wax from the oil and heavy solvent and separating the heavy solvent from the oil.

4. A process for the production of lubricating oil from an oil containing asphalt and wax which 1 comprises mixing said 011 with liquid propane under superatmospheric pressure to separate asphalt, separating the asphalt from the oil, wax

and liquid propane under superatmospheric presseparating the precipitated wax from the oil and 6. A process for the production of lubricating oil from an oil containing asphalt and wax which comprises mixing said'oil in liquid propane under superatmospheric pressure to separate asphalt. separating the asphalt from the oil, wax and liquid propane, separating the propane from the oil and wax under superatmospheric pressure, chemically treating the oil and wax, adding a heavy solvent to the oil and wax, separating the wax from the oil and heavy solvent and separating the heavy solvent from the oil.

7. A process for the production 0! lubricating oil from an oil containing wax which comprises mixing said oil with liquid propane, acid treating the oil, wax and liquid propane, separating the propane from the acid treated oil and wax, adding naphtha to the acid treated oil and wax, sep-. arating the wax from the oil and naphtha and separating the naphtha from the oil.

'8. A process for the production of lubricating oil from an oil containing wax which comprises mixing said oil in liquid propane under superatmospheric pressure, acid treating said oil, wax and liquid propane, separating the propane from the acid treated oil and wax under superatmospheric pressure, adding naphtha to the acid treated oil and wax, cooling thenaphtha, oil and wax, separating the wax from the cooled oil and naphtha and separating the naphtha from the oil.

9. A process for the production of lubricating oil from an oil containing wax which comprises mixing said oil in a volatile solvent, .acid and alkali treating said oil, wax and volatile'solvent,

separating the volatile solvent from the treated oil and wax, adding naphtha to the treated oil and wax, cooling the naphtha, oil and wax, separating the wax from the cooled naphtha and oil and separating the naphtha from the oil.

10. A method for the separation 01. asphalt and wax from oil which comprises commingling said oil with a normally gaseous liquid hydrocarbon solvent to separate asphalt, separating the asphalt from the oil and wax dissolved in said solvent, removing the solvent from the oil -and wax, adding a heavier solvent to the oil and wax, cooling the heavy solvent solution of oil and wax to precipitate wax and separating the precipitated wax from the oil and heavy solvent.

11. A method for the separation of asphalt and wax from oil which. comprises commingling said oil with a normally gaseous liquid hydrocarbon solvent to separate asphalt, separating the asphalt from the oil and wax dissolved in said solvent, separating the solvent trom the oil and wax, dissolving said oil and wax in a heavy hydrocarbon solvent, cooling said heavy hydrocarbon solution of oil and wax to precipitate wax and separating the precipitated wax from the oil dissolved in said heavy hydrocarbon solvent.

12. A method for the separation of asphalt and wax from oil which comprises commingling said oil in a liquefied normally gaseous hydrocarbon solvent, the major portion of which is propane to separate asphalt, separating the asphalt from the oil and wax dissolved in said solvent, removing the solvent from the oil and wax, dissolving said oil and wax in a heavier solvent than said first mentioned solvent, cooling the oil and wax dissolved in said heavy solvent to precipitate wax and separating the precipitated wax from the oil dissolved in said heavy solvent.

13. A method for the separation of asphalt and wax from oil which comprises commingling said oil in a liquefied normally gaseous hydrocarbon solvent, the major portion of which is propane, to separate asphalt, separating the asphalt from the ofl and wax dissolved in said solvent, separating'the solvent from the oil and wax, dissolving said oil and wax in naphtha, cooling the naphtha solution or oil and wax to precipitate wax and separate asphalt, separating the asphalt from the oil and wax dissolved in said solvent, separating said solvent from the oil and wax, dissolving said oil and wax in naphtha, cooling the naphtha solution of oil and wax to precipitate wax and separating the precipitated wax from the oil dissolved in naphtha.

15. A method for the separation of asphalt and wax from oil which comprises commingling said 011 with a liquefied normally gaseous hydrocarbon solvent containing a major portion of hydrocarbons having less than three carbon atomsto separate asphalt, separating the asphalt from the oil and wax dissolved in said solvent, removing the solvent from the oil and wax, dissolving said oil and wax in a heavier hydrocarbon solvent than said first mentioned solvent, cooling the heavy solvent solution or oil and waxto precipitate wax and separating the precipitated wax from the oil dissolved in said heavy solvent.

' ULRIC B. BRAY.