US2017820A - Mineral oil distillation - Google Patents

Mineral oil distillation Download PDF

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Publication number
US2017820A
US2017820A US52118A US5211825A US2017820A US 2017820 A US2017820 A US 2017820A US 52118 A US52118 A US 52118A US 5211825 A US5211825 A US 5211825A US 2017820 A US2017820 A US 2017820A
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lubricating
oil
distillation
condensate
vapors
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US52118A
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John E Schulze
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RED RIVER REFINING Co
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RED RIVER REFINING Co
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Application filed by RED RIVER REFINING Co filed Critical RED RIVER REFINING Co
Priority to US52118A priority Critical patent/US2017820A/en
Priority to GB19536/26A priority patent/GB257250A/en
Priority to AT118624D priority patent/AT118624B/de
Priority to DER68468D priority patent/DE550687C/de
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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
    • C10G7/00—Distillation of hydrocarbon oils

Definitions

  • the patented process aforesaid makes use of distillation pressures which do not exceed millimeters mercury absolute'as a maximum and which are most desirably even much lower, commonly 5 millimeters or less. Said process gives excellent resultsdn practice and at the present time is employed commercially on a large scale for the manufacture of high grade lubricating oils.
  • California and Mexican crudes generally, most 16 of which are high in sulfur and in organic acids especially.
  • Principal objects of the invention are to provide a method or process wherein the diificulties 20 heretofore encountered in utilizing this class of starting materials are overcome and production of valuable and thoroughly satisfactory high grade distillates is made possible, especially lubricating oil distillates, from low grade crudes and 25 residua of the type above discussed; also to provide apparatus for carrying out such method.
  • Other objects are in general to make it possible to obtain from such starting materials sweet and stable mineral oil distillates, whether lubricating 30 oils or not, and also irrespective of whether the distillation'be conducted under high vacuum or not. Still further objects and advantages of the invention will become apparent as the description proceeds.
  • the process of the present invention involves vaporization of the crude petroleum or other mineral oil starting material, or a large part thereof, and fractional condensation of the I resultant vapors in such manner that separation 40 of the desired condensate is effected with minimum exposure thereof to contact with the lighter vapors and gases which carry most of the deleterious compounds it is desired to exclude from said condensate, so that little or no opportunity is afforded for said condensate to absorb and become contaminated vby said compounds.
  • the desired condensate obtained in the fractional condensa- 50 tion is not allowed to cool materially below the temperature at which it is formed until after there is no further opportunity for contacting with the malodorous vapors and gases before mentioned.
  • the vaporization of the crude oil is accomplished by distillation under high vacuum of the order of magnitude characterizing the process disclosed in said Patent No. 1,448,709 before mentioned.
  • a neutralizing agent that is alkaline in nature, such as causticsoda, soda ash, lime, or other suitable basic reagent.
  • the employment of such a neutralizing agent may be in connection with an initial distillation of the starting material or in connection with a redistillation pf a crude or raw distillate obtained in an initial run.
  • FIG. 1 is a side elevation of such installation
  • Fig. 2 is a plan of same
  • Fig. 3 is a view in side elevation of an installation similar to that shown in Figs. 1 and 2 but modified to permit employment of steam in the distillation. In all the views, parts are shown broken away and in section. 1
  • l 0 represents a horizontal cylindrical still supported above a heating furnace indicated generally at H which may be constructed and fired in any suitable manner to 55., heat the still indirectly rather than by direct contact of flame with the still bottom.
  • the still Ill is especially constructed for operation under extremely high vacuum (i. e. extremely low absolute pressure) of an order of magnitude corresponding to 25 millimeters of mercury (or less) absolute pressure.
  • the still is interiorly braced as, for example, in the manner illustrated in my prior Patent No. 1,448,709, dated March 13, 1923.
  • the still is equipped with a plurality of vapor offtakes I2, in this instance ten in number, of uniform diameter, leaving the still at uniformly spaced points along the length thereof.
  • the vertical portion l2- of each of the vapor offtakes I2 is relatively very shnrtin order to minimize refluxing of distillate to the still.
  • the remainder of each of the vapor oiftakes is inclined downwardly from the vertical portion l2 toward 'the cooling coil I 3 into which each ofitake l2 leads.
  • These c 01- 'discharge into a large-diameter collecting header ing coils I3 are submerged in cooling water contained in a box or tank l4. Said cooling coils, one of which is providedfor each oiftake l2,
  • At I6 is a riser, one for each offtake l2, the risers Hi all entering a horizontal header l1.
  • two sets of vapor lines l8 and I9 extend upwardly a considerable distance above the header l1 and then bend downwardly 10 to connect with cooling coils and 2
  • the coils 20 and 2 I of which there are two in this case and which are of larger diameter than the lines l8 and I9, discharge into a collecting header 22 of still larger diameter.
  • header distillate line or deodorizer system The piping system just described, beginning with risers l6 and extending to header 22 constitute parts of what may be conveniently termed 80 the header distillate" line or deodorizer system, further reference to which will be made hereinafter.
  • the object is to get the distillation vapors out of and at least a short distance away from the still before material condensation occurs, and then to effect condensation of the desired liquid products at a. point where no refluxing of condensate to the still takes place, and under conditions such that the condensate and residual uncondensed vapors and gases are rapidly separated from each other so that absorption or solution of such vapors and gases by the condensate is practically prevented.
  • each of the vapor offtakes I2 is similarly insulated not only over portion l2, but also over its downwardly inclined portion down to the point where the riser l6 branches off. Thus there is substantially no condensation in any of the offtakes l2 until that point is reached.
  • the riser I6 is also shown insulated and the header I1 may also be insulated. But the advisability in any given instance of insulating said risers and header is determined largely by the prevailing atmospheric temperature.
  • vapor lines l8, l9 may or may not be insulated from where they leave header I! up to the point where they bend downward again, but in the present example they are uncovered and therefore air-cooled.
  • the extent to which these parts, l6l9, of the piping system are insulated may of course be adjusted as rerequire.
  • the vapors and gases in the ascending lines are on the one hand cooled sufficiently to cause nearly all vapors of desired liquid products to condense, the proportion of such vapors escaping condensation and passing over through the deodorizer system being thus minimized; while on the other hand the cooling in said ascending lines is not carried so far that the deleterious vaporous or gaseous impurities are condensed or their absorption by the useful condensate favored.
  • each offtake !2 beyond the junction of riser l6 therewith, is freely exposed to air-cooling, because in this part of the system collects the desired liquid condensate and proper cooling thereof is advantageous.
  • liquid collectng in this header is discharged through rundown line 24 to one of the run-down or receiving tanks indicated at 25, 26, 2'! and 28, there being four such receiving tanks in the battery here illustrated although of course the number may be greater or less as practical operating'conditions Said receiving tanks are connected, respectively, by valved branches 25 26 2'!- and 28, with the aforesaid line 24.
  • a look-box 29 is placed in a vertical portion of said line.
  • a look-box 32 is provided in a vertical portion of line 30, and it is also convenient to provide a sampling device 33 which is connected by valved pipe 34 with line 30, and is also provided with a valved bleeder inlet 35 and a valved draw-off pipe 36.
  • the entire distilling system is maintained under the desired degree or degrees 01 vacuum by means of a vacuum pump equipment indicated conventionally at 31, this equipment being either a single vacuum pump of suitable size or a double or triple stage pumping equipment, as may be found most desirable in any given case.
  • the intake of the vacuum pump system has a valved connection 38 to the main vacuum line 39-40 in which header-distillate receiving tank 3
  • the four main receiving tanks are connected to said line 39 by valved pipes 4!, 42, 43 and 44, for a purpose that will appear hereinafter. Said pipes extend somewhat above vacuum line 39, as indicated at 45, before entering the same, thus providing against accidental entry from said vacuum line into any of the main receiving tanks, when the valves may be open, of liquid impurities that may collect in said vacuum line.
  • the crude, sufiiciently free from moisture is charged into the still Ill up to about 80% of the cubic capacity thereof 'and the still is gradually heated up to within 10 F. or so of the temperature at which the crude has been found by preliminary test to boil initially under 5 mm. mercury absolute pressure. This temperature is usually about 350 F. with the usual run of Nevada County crude. This temperature having been attained, the distilling system is then placed under vacuum by operation of the vacuum pump system indicated at 3'! which, as already explained, may comprise as many single or multiple stage dry vacuum pumps as are found desirable to use in practice.
  • I, 42L or 43l may be opened very slightly, if necessary.
  • the cut collected in receiving tank '26 may, if
  • lubricant that can be distilled from the particular crude undergoing treatment up to the temperature where substantial decomposition or cracking begins to take place in the still.
  • this lubricant yield it is usually more convenient to divide this lubricant yield into two or more portions or cuts, and in the present instance it will be assumed that the 45 lighter portion, corresponding to light and medium motor oil, is collected in receiving tank 26 and a heavier portion, corresponding to heavy motor oil, is collected in receiver 21.
  • the distillation may be continued at an absolute pressure which has by this time been reduced usually to around 4 to 6 millimeters of mercury in the still and which may decrease gradually to as low as 1.5 to 3 millimeters toward the end of the distillation.
  • is relatively very small indeed, quite commonly amounting to as little as one-half of one per cent by volume of the crude initially charged into the still for the entire remainder of the distilr lation, and being substantially less foulthan the header distillate obtained during the gas-oil cut.
  • header-distillate This later part of the header-distillate may therefore be collected separately and re-run if desired.
  • the quantity of header-distillate obtained during the gas oil out amounts frequently to as muchas 5 per cent of the initial charge of crude. In this connection it must of course be borne in mind that this 5 per cent is largev gas oil which, in association deodorlzer lines because of the rapid rate of distillation and heavy pump pull on saidlines atthe beginning of the distillation, as above described.
  • the vac-' uum control valves are adjusted as may be necessary to maintain the before mentioned foggy appearance in the header-distillate line look-box 32, thus ensuring always a slightly lower pres-' sure in said line and in the still than in the particular receiver into. which the distillate stream may be flowing.
  • the lubricating distillate is run into tank 26 until the flash point of a test sample is about 380 F., at which stage the still temperature approximates 550 F.; but it is to be understood that the selection of thepoint at which to cut the distillate into tank 21 may be varied as plant operating conditions require.
  • the distillation is continued, running the lubricating cut into receiver 21' until tests of the distillate indicate that the point has been reached where decomposition or cracking is taking place or is about to take place in the still.
  • the approach of this point is indicated whenthe flash point of successive test samples becomes stationary instead of gradually increasing as was the case during the earlier stages of the distillation. After remaining practically stationary for some time, the flash point of test samples will be found to be gradually lowering instead of increasing, and at this point it is best practice to cut the distillate into receiving tank 28.
  • the distillation can be continued up to whatever maximum distillation temperature is found in practice to be commercially advantageous, notwithstanding the fact that the lubricating fraction thus collected in receiver 28 contains cracked products and is therefore not as high in grade as the oil collected in receivers 26 and 21.
  • the residueremaining in the still l0 after the distillation has been run as'described is asphaltic in character and may be either a hard or soft asphalt, or a flux oil, depending upon the extent to which the distillation is carried. All of these products are valuable commercially, and the particular form in which it is desirable to obtain the residue in any given instance may to a considerable extent be determined by. market conditions existing at the time.
  • the gas oil fraction collected in receiver 25 may be considered to be a finished product and disposed of as such.
  • the lubricating oil cuts in receivers 26and 21 are good lubricating oil products but still contain a small proportion of organic acidswhich should be removed in order to render the products perfectly sweet, clean, and stable. Accordingly, these cuts are most desirablyre-run in a manner to be described presently.
  • the heavy lubricating distillate contained in receiver 28 also contains organic acids but in addition is further characterized by an appreciable content of cracked products resulting from decomposition of the oil in the still at tempera-J tures above about 630 F. This heavy lubricat-' ing cut is therefore also re-run to obtain finished products.
  • the re-running of the several cuts contained in receivers 26, 21 and 28 may be-conducted in the same manner in each instance if these cuts are re-run separately. It is not essential, however, that they be separately re-run, but on the contrary the entire yield of lubricants obtained neutralizing agent having the power to react with ⁇ the organic acids and with such other impurities as may be present in such manner as to enable substantially complete elimination and separation thereof from the oil in the re-run distillae tion.
  • Various neutralizing agents may be employed for this purpose, but a caustic alkali, such as caustic soda, is effective and convenient to use and is therefore preferred. Examples of other basic reagents that may befemployed, however, are soda ash, lime, and the like.
  • caustic soda as a neutralizing agent, this may be employed in a .water solution of say30 to-40"- Baum strength. Assuming a 40 Baum solution, it is found s'uflicient to employ about a pint of the solution for each barrel of lubricating oil distillate to be re-run. The exact amount may vary somewhat depending upon the nature of the starting material. Such a proportion of the solution having been added to thecharge ofoil, the charge is then thoroughly agitated, as by blowing in air, or otherwise,'until the neutralizing agent has been uniformly distributed through the charge. The charge is then re-run in apparatus which may be of exactly the same character as that shown inFigs. 1 and 2 and hereinabove described in detail.
  • the re-run distillation may-be carried out in precisely the same manner as the first distillation except that the particular cuts of lubricating oils made may be different from or more 'numerous than those of the first distillation, it being convenient ordinarily to so determine the cuts as to obtain a. range of finished oils corresponding generally to commercial types of oils demanded by the trade.
  • oils of which identifying data are given in the foregoing table are typical of novel lubricating oils that can be produced by the process of the invention. They are all narrow-cut lubricating oils, that is, oils characterized by narrow viscosity range and narrow boiling point range, and obtained by overhead distillation, all as set forth in this applicant's prior Patent No. 1,448,709 aforesaid, but they are'sharply distinguishable from the oils disclosed in said prior patent by the fact that, for any given viscosity, the flash and fire points are, respectively, at least about 10 F. higher'and, in the case of the higher seconds at 100 F. as measured on the Saybolt universal viscosimeter. While the general color classification of this 200 viscosity product is given in the table as pale, an oil having an. N. P. A.
  • the present oils are distinguishable from the oils disclosed in the aforesaid Schulze patent by the fact that the flash and fire points are invariably considerably higher, always at least 5 F. higher, and ordinarily from 10 to 40 higher.- This superiority in fiash and fire points is the more marked the higher is the viscosity of the oils compared.
  • the dimensions and capacities of the more important'parts of one form tal cylindrical still 10 is nine feet in diameter 40 and thirty feet long, giving an approximate charging capacity ofabout 250 barrels of 42 gallons each.
  • Each of the ten offtake lines l2 has an internal diameter of ten inches, and the vertical portion I2 thereof rises to a height of 45 about eighteen inches above the still, it being desirable to have this height as small as conveniently possible.
  • Each of the cooling coils l3, into which the oiftakes l2 discharge liquid, is a three-inch pipe; and the header 15 intowhich the ten cooling coils l3 discharge is ten inches in diameter, as is also the run-down line 24 leading to the horizontal cylindrical receivers 25, 26, 21 and 28, each of which latter is in this instance seven feet in diameter by sixteen feet long.
  • Each of the ten risers I6 is six inches in diameter, and extends upward ten feet to enter the header II, which is eight inches in diameter.
  • the five deodorizer lines I 8, l9 are of four-inch pipe and extend ten feet higher.
  • , into which the lines l8, l9, discharge, are six-inch pipes; and the header 22 is ten inches in diameter as is also the line 30 leading therefrom to the small receiver 3
  • Them; vacuum line 39, 40 is ten inches in diameter .as is also the pipe 44-leading therefrom to rundown tank 28.
  • , 42 and 43 connecting tanks 25, 26 and 21 to vacuum line 39 are four inches in diameter; while the pipes 25, 26 21 and 28, which connect said tanks with rundown line 24 are six inches in diameter.
  • the vacuum-producing means be able at all times to exert a direct and free pull through the cooling coils and associated piping upon the receiving tanks; but it is also desirable that the arrangement shall be such that the pull of the vacuum-producing means upon the still can be maintained slightly greater than the pull of said means upon the receivers, thus creating a pronounced tendency for the distillate from the still to flow toward the vacuum pump by way of risers and overhead lines Iii-l8 as already described and for the purposes set forth.
  • Fig. 3 illustrates how the apparatus system may be arranged where the distillation is to be carried on with the aid of steam, most desirably superheated, introduced into the charge through valved pipe S.
  • the overhead vapor lines l8 lead to a cold condenser indicated generally at l4, there being most desirably a separate condenser coil 20 for each of the lines l8.
  • the water in condenser tank l4 should be maintained substantially cooler than that in tank Id.
  • both steam and oil vapors condense and are then discharged into header 22',from which the liquid productsare conveyed by line 30" to a receiver 3
  • While only one receiver 3
  • the vacuum line 39, M extends to the vacuum pump 31 as before described, the system as a whole being similar, except in the particulars above noted, to that illustrated in Figs. 1 and 2.
  • the manufacturing procedure involves two distillations, namely, a first distillation of a crude without the addition thereto of a neutralizing agent but with separation of a large proportion of the malodorous and other impurities as described; and a second or re-run distillation of the lubricating distillate or distillates in the same manner but with the addition of a neutralizing agent, such as caustic alkali, to the oil that is to be so re-run.
  • a neutralizing agent such as caustic alkali
  • the starting material is a crude oil containing a' rather large proportion of gas oil, say 25 to 30 per cent, such as Smackover crude for example, or where the crude contains a considerable proportion of other relatively light fractions such as gasoline, naphtha and kerosene
  • the process of the invention is also applicable to the treatment of parafllne base crudes and residua, but in treating such starting materials it is necessary to guard againstclogging of the vapor lines, cooling coils, etc. with" congealed wax. This can be readily done as by steamjacketing the apparatus parts in question and also maintaining the receiving tanks warm so that the condensates collecting therein can be removed and suitably treated for separation of contained wax by centrifuging or other appropriate method.
  • tasteless mineral oils have been known that were not water-white in color, and invariably they have been acid-treated and upon redistillation, whether at ordinary pressures or very low absolute pressures, they yield decomposition products.
  • tasteless mineral oils having appreciable color are novel products in the art.
  • the process of the invention may also be employed for production of finished lubricating oils from partially finished lubricating oils made by other processes. Furthermore even finished lubricating oils resulting from such other processes may be re-distilled in accordance with theprinciples of this invention to produce lubricating oils of much higher grade.
  • the use as starting material in the present process of such finished or partially finished oils produced by other processes is an important practical phase of the present invention.
  • the present invention makes possible the manufacture of good finished lubricating oils as direct overheaddistillates from any crude, residuum, or other heavy mineral oil material, no matter how high may be its content of sulfur, organic acids or other contaminating impurities, and that no acid treatment, filtration, or other additional finishing treatment is required to produce high grade lubricants of the best color, greatest stability and other desirable characteristics.
  • the process of producing lubricating oil distillates which comprises mixing a basic neutralizing agent with a body of mineral oil containing lubricating oil components and also lighter-and lower-boiling odor-producing components; heating said body of mineral oil to vaporizing temperature and thereby obtaining lubricating oil vapors in mixture with malodorous gases and relatively light condensable vapors, conducting the resultant hot vapors and gases into a zone wherein they are caused to pass upwardly in countercurrent contact with downwardly flowing lubricating oil condensate formed. at a higher point in said zone,
  • the process which comprises distilling a mineral oil in the presence of a basic neutralizing agent under an absolute pressure not exceeding 25 millimeters of mercury and under non-oxidizing conditions, conducting the distillation vapors upward and cooling the same under such pressure to a temperature not substantially below the vaporizing point of relatively heavy lubricating components thereof at such pressure while rapidly withdrawing uncondensed lighter vapors, and 85 still further cooling the resultant.condensate out of contact with said uncondensed vapors 3.
  • the process which comprises mixing a small proportion of a basic reagent with mineral oil compris- 4i ing lubricants associated with relatively light impurities, distilling said oil under an absolute pressure notexceeding about 25 millimeters of mercury and under non-oxidizing conditions to obtain mixed vapors therefrom while avoiding substantial refluxing to the body of mineral oil being distilled, conducting the mixed vapors rapidly into a cooling zone also maintained at an absolute pressure not exceeding about 25 millimeters of mercury and at a temperature sufiiciently low to produce a lubricating oil condensate but not much lower than the condensing temperature, whereby to prevent extensive condensation of said relatively light impurities or absorption thereof by said condensate and separately conducting uncondensed impurities and said lubricating oil condensate away from said zone under suction, the suction being maintained higher ,upon said impurities than upon said condensate.
  • the process of improving previously manufactured lubricating oils which comprises subjecting such a manufactured lubricating oil to distillation in the presence of a basic neutralizing agent at absolute pressures not exceeding 25 millimeters of mercury and most desirably substantially below 10 millimeters, and collecting directly a lubricating oil distillate of better stability than such previously manufactured oil.
  • oils as overhead distillates which comprises distilling mineral oil which contains lubricating oil components in association with odor-producing components in the presence of a basic neutralizing agent under absolute pressure not exceeding 1 25 millimeters of mercury and under non-oxidizing conditions, thereby producing a mixture of lubricating oil vapors with difficultly separable vaporous and gaseous lower-boiling malodorous contaminants, conducting the mixed distillation 15 vapors upwardly while cooling the same under such pressure sufficiently to condense desired lubricating oil components therefrom while avoiding cooling to the condensing point of the associated lower-boiling malodorous contaminants and rap- 2 idly withdrawing uncondensed vapors and gases out of contact with the resultant lubricating oil condensate, then still further cooling said condensate under such pressure out of contact with said uncondensed vapors and gases.

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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)
  • Lubricants (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
US52118A 1925-08-24 1925-08-24 Mineral oil distillation Expired - Lifetime US2017820A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US52118A US2017820A (en) 1925-08-24 1925-08-24 Mineral oil distillation
GB19536/26A GB257250A (en) 1925-08-24 1926-08-07 Improvement in mineral oil distillation
AT118624D AT118624B (de) 1925-08-24 1926-08-12 Verfahren zur Herstellung von Mineralöldestillaten unter vermindertem Druck.
DER68468D DE550687C (de) 1925-08-24 1926-08-17 Verfahren und Einrichtung zur Destillation von Mineraloelen

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US2017820A true US2017820A (en) 1935-10-15

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AT (1) AT118624B (de)
DE (1) DE550687C (de)
GB (1) GB257250A (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2476280A (en) * 1944-05-10 1949-07-19 Foster Wheeler Corp Apparatus for the distillation and fractionation of composite liquids and control means therefor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2476280A (en) * 1944-05-10 1949-07-19 Foster Wheeler Corp Apparatus for the distillation and fractionation of composite liquids and control means therefor

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GB257250A (en) 1927-09-08
DE550687C (de) 1932-05-24
AT118624B (de) 1930-07-25

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