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Publication numberUS2273846 A
Publication typeGrant
Publication dateFeb 24, 1942
Filing dateAug 25, 1941
Priority dateAug 25, 1941
Publication numberUS 2273846 A, US 2273846A, US-A-2273846, US2273846 A, US2273846A
InventorsDunmire Russell P
Original AssigneeBuckeye Lab Inc
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Process for treating hydrocarbons
US 2273846 A
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Description  (OCR text may contain errors)

Patented Feb. 24, 1942 PROCESS FOR TREATING HYDROOARBONS Russell P. Dunmire, Shaker-Heights, Ohio, as-

signor to The Buckeye poration of Ohio No Drawing.

Laboratories, Inc., a cor- Application August 25, 1941, Serial No, 408,260

- .14 Claims. (01.196-16) My invention relates generally to the treatment of hydrocarbons and has for one of its objects the refining or the re-refining of suc materials.

The present patent application is a continuation in part of my copendingpatent application,

. Serial No. 241,960, filed November 23, 1938.

More specifically my invention relates to the treatment of oils such as mineral oils of a lubrieating nature or of an insulating nature, and mineral waxes, etc., all of which are subject to more or less deterioration when exposed to air, moisture, metals or other agents which cause contamination such as oxidation, polymerization, etc. as well as contamination by solid materials in suspension.

In the case of lubricating oils, for example, it has been found that although the most modern methods are used in the refining of these oils for lubricating purposes yet certain undesirable properties remain in should be removed. It is known also that in use, lubricating oils are subject to contamination by water, free and in solution, metallic particles,

dust and other solids and air both free and dissolved. It has been discovered, also, that varying shock loads detrimentally afiect. such oils. Under such trying conditions many materials such lubricants xwhich carbon in suspension and precipitated; carbon is also precipitated on the terminals and oil gases and hydrogen are produced as well as some un.- saturates. V The effect of this israpid oil deterioration from the arc, carbonization of the oil, decreased rupture capacity, explosion hazard v and possible failure of the breaker. In the case of electric transformers, water, gas in solution, organic fluids and volatiles, organic acids, sludges, resinous bodies and compounds, tars, pitches and oxyasphaltic compounds are produced due to the heat from operation of the transformer. This, of course, lowers the insulation value of the oil, prevents proper heat dissipation, induces gas pocket formation, creates explosion hazards and volatile corrosion, promotes power factor losses and possible failure of the equipment. I might say that in the case of oil-insulated electric cables the high electric stresses due to operation "of the cable causes deterioration of the insulating oil in much the same fashion as in the case of transformers, the effect of which may be failure of the cable due to ionization, wax formation, a decrease in resistivity and an increase in the power factor. In the case of mineral waxes I have found that the products of oxidation together with free water and dissolved gases producediscoloration are produced in the oil which deleteriously affect the same so far as itsuse as a lubricant is concerned.

Without attempting to exhaust the subject, I might say that these contaminants produce sludges due to excessive heating, free and amorphous carbon, stable and unstable emulsions, polymerization products, soluble and insoluble resins and gums, acids, metallic soap, asphaltic sludges; free acids, dissolved gases and free water as well as addition agents are present in the oil. The oil also becomes discolored 'So far as a lubricating oilis concerned, the presence of these various materials inthe oil causes excessive bearing wear, over-heated bearings, increases internal oil friction, reduces the film strength, etc.

Insulating oils are subjected to contamination and deterioration as the result of contact of the heated hydrocarbon with air or certain other of the mineral wax and in many cases liberates unsaturated compounds and forms insoluble resins, gums, soaps and various types of sludge impurities. the type of mineral wax.

The present inventionprovides a process for the removal of the impurities or contaminants above referred to.

My process, it is to be-noted, may be continuous or intermittent.

Broadly speaking, myimproved process is directed to the treatment of the oils and waxes above referred to wherein I agitate a mixture of the oil or wax to be treated and an adsorbent material while the mixture is at an elevated tem-v perature and under vacuum. After this treatment the mixture is filtered.

More specifically, in practicing my invention a the material to be treated is introduced into a heating and mixing chamber which is hermetically sealed and connected to any .suitable commercial type fractional condenser. A suitable adsorbent material, such as bone char, carbon black, fullers earth, etc., is added to the charging stock in the heating and mixing chamber. The amount of adsorbent material employed so far as maximum amount is concerned is not These vary slightly in degree with to the mixing and heating chamber.

thermal decomposition or deterioration, the heat-' critical'except. perhaps for economical reasons.

For example, I may add from one-half per cent to twelve per cent, or even as high as forty per cent in special cases, by weight of the oil or wax being treated or processed. In addition to the adsorbent material I prefer to add water and in some cases superheated steam as a flushing agent and an alkali such as, potassium hydroxide or calcium hydroxide or the like to bring about saponification of any' residual acid which is present and which is prgbably due to oxidation of the oil or wax due to contact of the heated material with air. I have found that this residual acid is not readily adsorbable by the adsorbent material of the mixture. The addition of the potassium hydroxide saponifies this acid as above mentioned so that the same may be readily removed.

The amount of water and alkali added may be varied within a wide range. For example, I

\ may saythat theamount of water or steam added may also be accomplished during treatment and while in the presence of adsorbent materials which may or may not have some definite action as catalysts.

For example, in the treatment of certain mineral waxes I am able to produce a pure white wax which may be used in the manufacture of artificial honeycombs from which all traces of odor are removed. In the case of electrical insulating oils the high vacuum accelerates the removal of the free water of solution as well as all gases with which the oil may be saturated and which woulddeleteriously affect the electrical and physical characteristics of this class of oil.

may-vary between one-quarter of a pound and.

After' this treatment of the material in the heating and mixing chamber I pass the material through a filter in a closed filter chamber. .Various forms of filter materials maybe employed.

.For' example, I paper, glass cloth, glass wool or metallic screens, any or allof which may be pro,- tected with a'diatomaceous filter aid, so as to secure the maximum degree of clarity of the ma "terial being treated. The material may be driven pump or a turbine impellor while the mixture is being raised to an elevated temperature in a range suflicient to drive off the water and the low boiling point volatile impurities. The temperature range extends up to a value in the neighborhood of the flash point of the oil or wax in its finally treated state and includes an elevated temperature below the flash point of the finally H treated oil or wax and preferably embraces a range 'of approximately 50 to 150 degrees F. below the flash point of the finally treated oil or wax. It will beappreciated, of course, that at such a temperature the water, light ends and volatile oxidation products will be driven off and flow into the condenser which, as above noted, is connected.

Because of ing of the mixture at a temperature substantially I beyond thefiash point of the finally treated oil or wax causes a material reduction in the yield of the oil or wax being treated. At temperatures below the flash point of the finally treated oil or wax, the yield is good, but as the temperature substantially exceeds the flash point of the finally treated oil or wax, the yield rapidly-decreases, rendering the process uneconomical.

The mixture is maintained at this elevated temperature and subjected to agitation for from fifteen minutes to an hour, for example.

As above mentioned. I prefer to employ a vacuum on the heating and mixing chamber, although good results are obtained without the employment of a vacuum. If a vacuum isemployed I prefer a high vacuum from twenty-eight to thirty inches of mercury as referred to a thirty inch barometer at 'sea level. The purpose ofutilizinga vacuum is to increase' the rate of distillation at a lower temperature of. oils which are quitesensitive to cosity.

1 The above remarks apply also .to the treatment of mineral waxes. Fr 1 H-ydr'ogenization of the liquids being treated the action of heat,.especia'lly those. of a low vispumped through the filter ordrawn through.

It will be understood thatin the filtering op.- eration the adsorbent materialwith it adsorbed impurities such, as resins,,; inetallicsoaps, heavy residual acids, .polymer'products. mechanical impurities, etc are removed The treated material. W.-- tion suitable for. use or service.

- a' cleancondi- .It win. beseen-ffrom "all of the foregoing that the present-invention provides a process for the treatment pf oils-and waxes, whereby contam-- inants in 'these' materials which deleteriously feet the same are removed, the process being adapted for use in connection "with the refining-1" of such oils and waxes as well as to, the re-re'-, r fining of the sameafter they have beenin'servicaf r The specification and the claims are directedito .a .process for removing impuritiesfrornqa con taminated or used mineral substance :of th'e class" consisting of mineral oils andjmineral fwaxes.

The term contaminatedfias' ii sedxherein means an oil or wax which isuniitlfor-aspecific purpose. Itis to be understoodggo'fcourse,'that changes may be made in.- theprocedures above, described without departing from;; the"spirit and scope of my invention.

I claim as my invention:

1.- Theprocess for removing impurities froma contaminated or used mineral substance of the class consisting of, mineral oils and mineral waxes.

which process comprises mechanically mixing and agitating the contaminated or used mineral substance'and a' solid adsorbent material in a sealed containerv to adsorb the high boiling point impurities, heating the mixture of the mineral substance being treated and the solidadsorbent material in the sealed container under vacuum at a temperature in the'range of approximately 50 to degrees F. below the flash point of the finally treated mineral substance to drive off the water and the low boiling point volatile impurities, and

separating the adsorbent material with its adsorbent impurities fromthe'rnineral substancebeing treated to recoverthelatter.

2. The process for removing impurities from a contaminated or used mineral oil, which'pr'ocess I comprises mechanically mixing and agitating the contaminated-caused oil and a solid adsorbent materialin-asealed container to adsorb the high boiling ,point impurities, heating the mixture of the" oil'being treated and the solid adsorbent marterial the sealed container under vacuum at a Tli 50 to 150 degrees F. below theflashzpoint of the i the latter.

v to recover the latter.

, eral substance being treated and the solid ad;

v vacuum at a temperature below the flash point 1 comprises mechanicallymixing and agitating the contaminated or used oil anda solid adsorbent treated oil to drive off the'water and the low boi-lmaterial in a sealed container to adsorb the high ing point volatile impurities, and separatingthe boiling po nt impuri s, heating he mixture of adsorbent material with its adsorbed impurities 5 the Oil being treated and thz solid adsorbent mafrom the oil being treated to recover the latter. rial in t e sea ed con ainerunder. vacuum a a 3. The process for removingimpuritiesefrom a mp r ure elow the h p n f h n l y contaminated or used mineral wax. which-process treated Oil drive Off the Water a e low comprises mechanically mixing and agitating the boiling Point Volatile impurities, and Separating temperaturein the range of: approximatelytfl to 150 degrees F. below the flash point of the finally contaminated or used wax, and a solid adsorbent the adsorbent material with its adsorbed impuri? ties from the oil being treated to recover the material in a sealed container-to adsorb the high latter,

boiling point impurities, heating the mixture of the wax being treated and, the solid adsorbent material in the sealed container: ,under vacuum contaminated or usedimiheraliwax, w i p ess at a temperature in the range. of approximately comprises mechanicallym n n agitating the contaminated or used wax. 'and'a solid adsorbent material in a sealed containerto adsorb the high finally treated wax to drive-01f thew'ateriand the v boiling point impurities, heating the mixture of.

low boiling point volatile i'mpurities, and separating the adsorbent materialwith itsdads'orbedimpurities from the wax being 4. Theeprocess for remo n Purities froma contaminated or used mne oil,l,whichg"'process comprises mechanically m in nd agitatin'g the contaminated or used/o 1a olid'jiadsorbent ma p es. m the W "terial, an alkali, and ari e. eous medium of the v classeconsisting of water and steamfinfa sealed T p c s f0 container to adsorb the gh boiling point im- I a a purities, heating thejfm -xturecort e oii beingpr se m amca ly e si s t e treated, the adsorbentfmaterial; the alkali and centaminetedior iised as i ads n ia -i the aqueous medium i'n'fthe sealed container. un-r teriel; an l i -d antique-011$ l l t class consisting or. water and steam in a-sealed der vacuum at a temperature infthe range of ap-g v v t H proximately to 150 degrees F..be1ow the flash o iner to adso b t i h b ns point mypurities, heating themixture ofi the oil being point of the finally treatedjoil. to drive of! the v i water and the low boiling pointivolatil'eil'npuri 35- t e d-th adsorbent mat ial. t e alkaliand ties, and separating theadsorbent material with the 11111180115 di imt l n r- 3 1 its adsorbed impuritiesfro'm the oil being treated a m e -J-a temperature; below the ifl 1 point-of vtheflnistlly treated ;;oil in drive off the 5. The process forfremoving impurities from a class consisting of mineral oils and mineral waxes, which process comprises mechanically mixing and agitating the contaminated or used" mineralsubstance, a solid adsorbent material I I r and an aqueous medium of the class consisting 1 5 1 e i t 0f i h e and mineral Wa of water and steam, in a sealed' container to ad- .wh c r c s wm ises m c a cal y i sorb the high boiling point impurities,, heating r insn l',ieei h is the contaminated or "used-m nthe mixture of the mineralsubstance beingtreah 'i' t he. o id. adsorbent materi and an ed, the solid adsorbent material and theagu'eous medium in the sealed container under vacuum a ed to recover the latte'r.

water and the low boiling point volatile imp ties, and separating the a orben'tmaterial" its adsorbed impurities ;fr'om the rni' f stance being treated toirec'oyerj 6'. The process fori-emoving' contaminated or usedmin class consisting of' inine'ra I waxes, which process comprises mec'hanically 1 mixing and agitating thecon'tamihated or used mineral substance and=a solid adsorbent material in a sealed container: to adsorb the high boiling in point impurities, heating the mixture of-the min- 05 and ag tating the coir subs'tance', a solid has) and an aqueou's'm n a sealed container to adsorb separating-theladsorbent mat rial with its adsorbed impurities-1mm the mineral substance beingtreated to'grecover the latter.

. 1 1 The procession re sorbent material in the sealed container under I J of the finally treated mineral substance to drive- 7 the high "be h with its adsorbed impurities from themineral substance being treated to recover the latter.

7. The process for removingimpurities from a ous'mediumlin' the sealed container under vacuum at altemperature in the range of 50 to,150

'degree's F; below the flash pointof the finely contaminated or used mineral oil,which; process treated oil to drive oil the water and the low 8. The process for removing impurities from a the wax being treated and the so1id;adsorbent: t t recover 20 material in the sealed container under vacuum .at a temperature'below the flash point of the finally treated wax to drive- 01i the water -and'the purities, and separat moving impuritiesfrom :a I contaminated or used'mineralcil, which process water and the jlow' boiling point volatile impuri-' contaminated or used mineral substance of the 40 T a epa th adsbrbent er l; h:

,1 its adsorbentiimpurities-from the oilflbeing treat f.

. (10. Theyprocess for removinginipuritiesffrom, a contaminated or used i'mineral substance of the-1 in the sealed container-under vacuum at a tem-f per-ature j below: the hash point [of the finally treatedinineral substance to driveeoff the water moviiigimpurities from a H I v h g point impurities, heating'the off the water and the low boiling point volatile) mixture;oif',the;mineral substance being treated,

, impurities, and separating the adsorbent material theyaq bgm mat i l, t lk and t boiling point volatile impurities, and separating the adsorbent material with its adsorbed impurities tromthe mineral substance being treated to recover the latter.

12. The process for removing impurities from a contaminated or used mineral substance 01 the class consisting of mineral oils and mineral waxes, which process comprises mechanically mixing and agitating the contaminated or used mineral substance, a solid adsorbent material, an alkali, and an aqueous medium or the class consisting of water and steam in a sealed container to adsorb the high boiling point impurities, heating the mixture of the mineral substance being treated, the adsorbent material, the alkali and the aqueous medium in the sealed container under vacuum at a temperature below the flash point of the finely treated oil to drive off the water and the low boiling point volatile impurities, and separating the: adsorbent material with its adsorbed impurities from the mineral substance being treated to recover the latter.

13. The process for removing impurities from a.

, contaminated or used mineral wax, which process comprises mechanically mixing and agitating the contaminated or used wax, a solid adsorbent material. an alkali, and an aqueous mediums! the class consisting of water and steam in a sealed container to adsorb the high boiling. point -,im-

purities, heating the mixture of .the wax being treated, the adsorbent material, the alkali'and the aqueous medium in the sealed container un-' der vacuum at a temperature in the range of approximately 50 to 150 degrees F. below the flash point of the finally treated wax to drive of! the water and the low boiling' point volatile impurities, and separating the adsorbent material with its adsorbed impurities from the wax being treated to recover the latter.

14. The process for removing impurities from a contaminated or used mineral wax, which process comprises mechanically mixing and agitating the contaminated or used wax, a solid adsorbent material, an alkali, and an aqueous medium or the class consisting of water and steam in a sealed container ,to adsorb the high boiling point impurities, heating the mixture of the wax being treated, the-adsorbent material, the alkali and the aqueous inedium in the sealed container under vacuum' at a temperature below the flash point of the finally treated waxto drive off the water and the low boiling point volatile impurities, and separating the adsorbent material with its adsorbed impurities from the wax beingtreated to recover the latter.

RUSSELL P. DUNMIRE.

Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US2585895 *Mar 17, 1950Feb 12, 1952Sun Oil CoWax refining
US3265609 *Jul 27, 1962Aug 9, 1966Sun Oil CoWax refining
US4846962 *Feb 12, 1987Jul 11, 1989Exxon Research And Engineering CompanyFurfural, phenol or methylpyrrolidone solvent extraction
US5098556 *Jun 14, 1990Mar 24, 1992Lyondell Petrochemical CompanyTreatment of off-specification white mineral oil made by two stage hydrogenation
Classifications
U.S. Classification208/26, 208/284, 208/299, 208/27, 210/664
International ClassificationC10G25/00, C10G25/06, C10M175/00
Cooperative ClassificationC10G25/06, C10M175/00
European ClassificationC10M175/00, C10G25/06