US845456A - Separating low-boiling products from the burning-oil distillate of petroleum to raise the fire test thereof. - Google Patents

Separating low-boiling products from the burning-oil distillate of petroleum to raise the fire test thereof. Download PDF

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US845456A
US845456A US2664800A US1900026648A US845456A US 845456 A US845456 A US 845456A US 2664800 A US2664800 A US 2664800A US 1900026648 A US1900026648 A US 1900026648A US 845456 A US845456 A US 845456A
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distillate
oil
steam
test
water
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Herman Frasch
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Standard Oil Co
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G7/00Distillation of hydrocarbon oils

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  • This invention relates to the separation from the burning-oil distillate of petroleum of those portions which on account of their volatility (or low boiling-points) are liable to form ex losive mixtures with air at, comparative y speaking, low temperatures, or,
  • the present invention relates to the separation of the more volatile constituents from tlip whole or any desired fraction of such disti ate.
  • the low-test burning-oil distillate is subjected to free steam, with or without being exposed at the same time to the dry heat of 'closed coils, and the resulting vapors are water with which the said stream of distillate is mingled being the water of condensation from nearly the whole (or at least from the chief portion) of the injected steam.
  • the low-test distillate this latter need be kept at a steam heat only for a short time, (under two hourssteaming for a few minutes, not over fifteen, having, in fact, given excellent results,) so that the alteration in color can be reduced to a minimum, and, in fact, becomes hardly perceptible, (if perceptible at all.)
  • the volume of distillate is limited relatively to the volume of steam admitted thereinto, (such limitation being itself a special feature of invention but it follows from this concentration of the energy of the steam on so small a volume of distillate that the resulting vapors contain much more burning oil than those given off from the very much larger volume of distillate subjected to steam in the procedure indicated above.
  • Thepreliminary heating of the low-test distillate is important in order that it may not condense the low boiling products. Practically a temperature of about 170 Fahrenheit will be suitable for raising the distillate to 150 Fahrenheit'fire test and can be obtained by recovery of heat from the high-test distillate hot from the steaming operation; but a less or even a greater degree of preliminary heating can be resorted to.
  • the presence of the considerable volume of hot water is also important in equalizing the heat, by reason of With less expenditure of time and heat than by the current procedure indicated above.
  • distillate In subjecting the distillate to the free steam they may be brought together in any ordinary or suitable way, even in the same manner in' which said distillate and the oilvapors are brought into contact with each other; but it is an advantage and special improvement -to admit the free steam into a further advantage (and special improvement) to divide said traveling body into a success1on of two, three, or more communlcatmg pools and to make said pools diminish in dept-h, so that the removal of the last portions of the low-boiling products takes place from a shallower layer than that (or those) from which the earlier portions are removed and that consequently there is less danger of retaining low-boiling products in the distillate.
  • Figure 1 is a diagram in elevation of apparatus suitable for carrying the invention into effect.
  • Fig. 2 is an elevation, partly broken away and partly in vertical section, of a portion of the heatexchanger belonging to said apparatus.
  • Fig. 3 is a vertical section, partly broken away, of
  • Fig. 4 is a plan of a portion of the heat-exchanger.
  • Fig. 5 is a vertical section, partly in elevation and artly broken away, of the horizontal still, distilling and rectifying column, and rectifier belonging to said apparatus.
  • Fig. 5 is .a detail view illustrating a feature of said horizontal still.
  • Fig. 6 is a transverse section of the horizontal still and
  • Fig. 7 is a detail view showing two water-discharge pipes for this still, either of which pipes can be used.
  • the a paratus as a whole consists, as shown, 0 a distilling and rectifying column A, having a supply-pipe 2 opening into its upper part, arectifying-column B discharging its products of condensation into the upper' part of said column A, a horizontal stlll C, which receives the liquids from said column A and is provided with closed steamcoils 3 and perforated steam-coils 4 and also with a draw-oil 5'for the water, and a heatexchanger D connected withthe outlet from still C by the pipe 6, drainage-tank G, pipe 6*, pump E, and pipe 6, and with the upper part of the column A by said pipe 2.
  • the rectifying-column B is shown provided with a jacket 9, having pipes 10 and 11 for introducing and carrying off a cooling liquid. It may be water or any other cooling liquid.
  • a special jacket is not es-. sential to the rectifying action, since it sutlices for this that the vapors are repeatedly brought in contact with returning condensate from higher parts of the rectifyingcolumn. s
  • At 12 is an additional supply-pipe entering the upper part of the'rectifying-column B for discharging distillate thereinto when desired. It can be usefully employed, for example, in filling the apparatus with high-test distillate in starting, or it can be used to introduce low-test distillate then or during the operation, the distillate in either case being preliminarily heated or not as the case may be.
  • the vapor-outlet 13 from this rectifier B can be connected with an ordinary condenser (not shown) or with other appliance or appliances which have heretofore been connected with the vapor-outlets of stills, and will therefore suggest themselves.
  • the columns A and B are divided, as shown, into a number of chambers by horizontal partitions 14, which are perforated and provided each with a pipe 15 and bell 16 and overflow-pipes 17.
  • the vapors rising through the pipes 15 are by the bells 16 brought repeatedly into contact with liquid, which forms a layer on each partition above the edge of the bell and flows from chamber to chamber through the pipes 17
  • This is a common structure of column in arts which employ rectifying, distilling, or absorbing columns. It forms no part of the invention and can be replaced by any known or suitable arrangement for bringing vapors and liquids repeatedly into contact with each other as they pass through the apparatus. Numerous arrangements ofthis description areknown in various chemical industries.
  • dams or partitions 18 to divide the traveling body of liquid into a succession of pools, which communicate by overflowing one into the other. This separation into pools aids" in keeping the different parts of the body of liquid, which have been subjected to difier-- ent degrees of steaming, better separated from one another.
  • each dam except the last is provided at the bottom with an opening 19, (see Fig. 5;) but other arrangements could be provided for its conveyance, if preferred.
  • the draw-off 5 which is provided, as shown, with a swinging arm 20, that can be turned to raise or lower its open outer end, and so determine the de that which the layer of water under the distillate shall stand.
  • the closed coil is supplied from the main with exhaust-steam from engines used to supply power at the works or from other sources (or it may be with live steamor both live and exhaust steam) and discharges into the drain-pipe 22.
  • the perforated coil is supplied from the main 23 with live steam, (or it may be with "exhaust-steam or with both live and exhaust steam.)
  • perforated coil is to be understood any appropriate device for introducing free steam into the distillate. As shown, these coils consist of a number of straight pipes. They are perforated on the under side with holes,
  • The-heat-exchanger D consists, as shown,
  • Each element (see Figs. 2 and 3) resembles a tubular boiler or condenser in that it consists of a number of tubes 24 between the partition-plates 25 of a shell 26.
  • the shell is thus divide d into two compartments or chambers by the partitions and the tubes, and the compartments are connected by the ipes 27 and 28 into two series, so that the hig.
  • ..-test distillate starting at one end of one series may pass over one surface of the tubes, (outside or inside, as-the case may be, but inside, as shown,) while the low-test distillate starting at the other end of the other series passes over the other surface of said tubes, (outside, as shown.)
  • Other known or suitable forms of heat-exchangers can be used instead.
  • the body of oil in the still C is limited relatively to the volume of steamadmitted through the perforated coils, so that all the low-boiling products are removed in a short internal diameter at such places as to form compartments or poolseach nine and a half feet in length, it is recommended to use pipe for coils as follows, namely: in the first compartment or pool, two hundred andthirtyeight feet of one-inch wrought-iron unperforated pipe for the closed coils and firtyfour feet or Wroughtiron perforated pipe for the open coils in the second compartment or -2o pool, two hundred and four feet of one-inch unperforated pipe andthirty-six-feet of oneinch perforated pipe; in the third compartment or pool, one hundred and fiftythree feet of one-inch unperforated pipe and twentyseven feet of one-inch perforated pipe, and, in the last compartment, one hundred and nineteen feet of one-inch unperforated pipe and eighteen feetpf one-inch perforated
  • the temperatures in columns A and B are such as to effect the condensation therein of the chief part of the steam let into the perforated coils ofstill C.
  • the temperature in the still C is about that of water-vapor under the barometric pressure inside of the stillpressure in the still is not reduced below that of the outside atmosphere.
  • the horizontally-traveling body of oil in the stillC being divided into a succession of communicating pools by the dams 18 the different parts are kept separate, and the dams being of diminishing height the pools are of diminishing depth so that the free to it, about 212 Fahrenheitwhen' the steam has less oil to pass upthrough-a condition which is believed to conduct to the efficiency of its action.
  • the oil in the still C it is also an advantage and special improvement to decrease the volume of free steam per cubic foot of oillas the latter ap I proaches the outlet 6 because, for onereason, the content of low-boilingproducts being less, it is not considered desirable to evaporate so large a proportion of the oil as in the earlier portion of the steaming opera tion, when the proportion ofsuch products is greater.
  • the length of perforated steam- 7 coil is' greatest in the pool next the column A and decreases in order, being least inthe pool next the outlet 6", and this decrease is in greater ratio than the decrease in the cubical contents of the pools, due toitheir diminishing depth toward said outlet.
  • volume of, free steam decreases also, as shown, with reference to the s uare foot of exposed upper surface of the iquid being steamed, and this. is considered advantageous, as modifying the evaporation in a desirable manner.”
  • the low-test distillate could be heated prelimiand rectifying column A otherwise than by means of the high-test distillate but in this, case the economical advantage of imparting the heat of the outgoing high-test distillate to the incoming low-test distillate would be lost, and the ability most perfectly to secure this economy is an important advantage atdistillation of the present invention for the periodical Working of current practice.
  • the liquid to be distilled of any suitable kind can be introduced at the place or places described for the low-test distillate, the
  • the outgoing residual liquid and the incoming liquid to be distilled can be passed through a heat-exchanger in opposite directions, as described above, for the outgoing high-test distillate and the incoming low-test distillate;
  • theformer being the residual liquidfrom the therefore, in any of the hereinafter-Written claims the expression raising the fire test of burning-oil distillate occurs,such claim is intended to include only the special distillation in which said low-boiling products are removed from the said burning-oil distillate.
  • the expression liquid to be distilled includes, first, said burning-oil distillate; second, other petroleum or hydrocarbon oil, especially but not exclusively an oil con.-
  • any other appropriate liquid especially, but not exclusively, such a liquid as contains substances with boiling-points below that of water.
  • the improvement consisting in causlng a body of the liquid to be distilled'to travel horizontally and to diminish in depth as it approaches the outlet therefor, and delivering free steam at intervals below the surface of said body'in such manner that the volume of so-delivered steam per cubic foot of liquid is lessened as said liquid approaches the outlet therefor, substantially as described.
  • the continuous process which is characterized by the partial evaporation of the said oil at about the boi ingpoint of water by contact of free steam therewith, and the repeated contact of the evolved vapors with the specified petroleum or hydro carbon oil of a temperature below the boilingpoint of water and not lower than about Fahrenheit below tht? same mingled with returning condensate of hot oil and the hot water from the chief part of said free steam, substantially as described.

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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)

Description

No.845,456. PATENTED FEB. 26, 1907, H. FRASGH;
S EPARATING LOW BOILING PRODUCTS FROMTHE BURNING OIL' DISTILLATE OF PETROLEUM TO RAISE THE FIRE TEST THEREOF.
APPLICATION FILED AUG. 11, 1900. 2 sums-sum 1.
PATENTED FEB. 26, 1907. H; FRASGH. DUGTS FROM THE BURNING OIL DISTILLATE 'SEP'ARATING LOW BOILING PRO OF PETROLEUM TO RAISE THE FIRE TEST THEREOF.
APPLICATION FILED AUG. 11, 1900.
new/hm /104? 2 SHEETS-SHEET 2.
Witneoau UNITED STATES PATENT OFFICE- HERMAN FRASCH, OF NEW YORK, N. Y., ASSIGN OR TO STANDARD OIL COM- PANY, OF BAYONNE, NEW JERSEY, A CORPORATION OF NEW JERSEY.
SEPA RATING LOW-BOILING PRODUCTS'FROM THE BURNING-OIL DISTILLATE 0F PETROLEUM TO RAISE 'THE FIRE TEST THEREOF.
Specification of Letters Patent.
Patented Feb. 26,1907.
Application filed August 11. 1900. Serial No. 26,648.
citizen of the United States, residing at the city of New York, borough of Manhattan, county of New York, in the State of New York, have invented certain new and useful Improvements in Separating Low-Boiling Products from the Burning-Oil Distillate of Petroleum to Raise the Fire Test Thereof; and I do hereby declare the following to be a full, clear, and exact description of the invention.
This invention relates to the separation from the burning-oil distillate of petroleum of those portions which on account of their volatility (or low boiling-points) are liable to form ex losive mixtures with air at, comparative y speaking, low temperatures, or,
in other words, it relates to raising the fire test of burning-oil distillate.
In the fractionation of the crude petroleum by distillation the operation can be so conducted as to give burning-oil distillate having as it comes from the end of the condenser the fire test desired; but in so proceeding, prior to the recovery of this hightest distillate, there would be received a product too light to be burned in a lamp and too heavy for use as naphtha, (benzin,) yet containing desirable portions of burning oil and naphtha. It has been the practice, therefore, to commence the collection of distillate for burning oil while yet the more volatile constituents of the crude oil are coming over, and to resort to a supplementary distillation to remove these constituents, or, in other words, to raise the fire test of the burning-oil distillate. The particular points at which the collection of this distillate shall be gin and end and in what manner the distillation is to be conducted are determined by the judgment of the manufacturer, according to the character of the products which he is making and other considerations, and he may of course collect the said distillate in fractions, one or more of which would be of the proper fire test as the same came from the, condenser and these could be mixed with the remainder of low fire test after this has been deprived of its more volatile constituents but in practice all the distillate for the particular grade of burning oil being and subjected to the operation for raising the fire test.
The present invention relates to the separation of the more volatile constituents from tlip whole or any desired fraction of such disti ate.
tion by fire heat in order to raise the fire test; but while this was effective in this regard in using fire under the still the boilingso high that a polymerization set in with an accompanying coloring of the distillate, which made the subsequent treatment with acid very difficult. In fact, some oils subjected to such supplementary fire-distillation could not be made white at all. To remove this difficulty, the supplementary distillation for fire test was effected by steam, the distillate of low test being brought into contact with free steam. Various processes and apparatus have been roposed at various times for such steam-stil ing; but the current procedure prior to my present invention was as follows: The low-test distillate was placed in a large still, having a capacity in large refineries of from two thousand five hundred to four thousand barrels, and provided with steam-coils, some of them closed so as to raise the temperature by dry heat and others perforated to allow free steam to enter the oil. The still was also provided with a small the still was filled, the steam was let on at first into the closed coils and then into the perforated coils also and the heating and steaming were continued until the distillate was brought to the proper fire test, which, in the case of the large stills above mentioned, would take about two days. Then the distillate had to be cooled down preparatorv for treatment with acid, the still was refilled, and its contents heated and steamed as before. During the steam-stilling the steam would carry over more or less'of the burning oil, which would be recovered by the rectifying-column and returned to the. still. This procedure is objectionable as well because I the prolonged subjection-of the distillate to l the temperature of the steam makes the At first resort was had'to a partial distilla rectifying-column, through which the vapors passed on their way to the condenser. When,
manufactured is collected or mixed together point of the more volatile constituents was i ICO color somewhat darker and the distillate harder to treat with acid, as also because a great deal of time is lost and heat wasted.
In accordance with the present invention the low-test burning-oil distillate is subjected to free steam, with or without being exposed at the same time to the dry heat of 'closed coils, and the resulting vapors are water with which the said stream of distillate is mingled being the water of condensation from nearly the whole (or at least from the chief portion) of the injected steam. The
water which returns along with the stream of distillate is separated by settling and decantation within the still or in an outside receptacle. By this process in order effectively to drive off the low-boiling products, which may constitute twenty per cent., more or less, of
the low-test distillate, this latter need be kept at a steam heat only for a short time, (under two hourssteaming for a few minutes, not over fifteen, having, in fact, given excellent results,) so that the alteration in color can be reduced to a minimum, and, in fact, becomes hardly perceptible, (if perceptible at all.) Thus to shorten the time of steaming the volume of distillate is limited relatively to the volume of steam admitted thereinto, (such limitation being itself a special feature of invention but it follows from this concentration of the energy of the steam on so small a volume of distillate that the resulting vapors contain much more burning oil than those given off from the very much larger volume of distillate subjected to steam in the procedure indicated above. By bringing these vapors repeatedly into contact with the stream of preliminarilyheated low-test distillate mingled with hot water there takes place a fractional condensation which causes most (if not all) of the burning oil to become condensed and united in said stream of distillate, while allowing the more volatile constituents (low-boiling products) to pass away and, if necessary or desired, the vapors can be subjected to further cooling, with the object of collecting any remaining portions fit for burning oil or of separating the vapors into various grades of naphtha.
Thepreliminary heating of the low-test distillate is important in order that it may not condense the low boiling products. Practically a temperature of about 170 Fahrenheit will be suitable for raising the distillate to 150 Fahrenheit'fire test and can be obtained by recovery of heat from the high-test distillate hot from the steaming operation; but a less or even a greater degree of preliminary heating can be resorted to. There are advantages in having the low-test distillate heated to about or above the fire test desired, preliminarily to bringing it in contact with the vapors, and such heating is regarded as a special feature of invention; but the use of a materially-lower degree is not excluded altogether. The presence of the considerable volume of hot water is also important in equalizing the heat, by reason of With less expenditure of time and heat than by the current procedure indicated above.
In subjecting the distillate to the free steam they may be brought together in any ordinary or suitable way, even in the same manner in' which said distillate and the oilvapors are brought into contact with each other; but it is an advantage and special improvement -to admit the free steam into a further advantage (and special improvement) to divide said traveling body into a success1on of two, three, or more communlcatmg pools and to make said pools diminish in dept-h, so that the removal of the last portions of the low-boiling products takes place from a shallower layer than that (or those) from which the earlier portions are removed and that consequently there is less danger of retaining low-boiling products in the distillate. So far as I am aware it is new to steam low-test burning-oil distillate in this way i1- respective of what may be done with the resulting vapors, and such steaming is therefore included as an essential element in some, although. not in all, of my claims. Moreover, I believe it to'be new to raise the fire-test of burning-oil distillate by subjecting the latter to free steam and bringing the resulting vapors into repeated contact with a stream of distillate mirrgled wit-h hot water, even if the said distillate consist only or substantially of the products of the fractional condensation of said vapors. In such case the supply of low-test distillate, where it would not exert I preliminary heating, since it would become heated by the steam; but, nevertheless, it
fire-test of burning-oil distillate; but the same involves also processes of more general applicationthat 1s to say, to the distillatlon of oily liquids, especially those containing petroleum-naphtha along with heavier liq uids for the removal of the naphtha therefrom, and still more broadly to the distillation of liquids in general. As these more general processes are illustrated by the special processes above described for raising the fire-test of burning-oil distillate, it will suflice to refer to the'hereinafter-written claims for pointing them out.
In the accompanying drawings, which form part of this specification, Figure 1 is a diagram in elevation of apparatus suitable for carrying the invention into effect. Fig. 2 is an elevation, partly broken away and partly in vertical section, of a portion of the heatexchanger belonging to said apparatus. Fig. 3 is a vertical section, partly broken away, of
one of the elements of said exchanger, the
section being in a plane transverse to that of Fig. 2. Fig. 4 is a plan of a portion of the heat-exchanger. Fig. 5 is a vertical section, partly in elevation and artly broken away, of the horizontal still, distilling and rectifying column, and rectifier belonging to said apparatus. Fig. 5 is .a detail view illustrating a feature of said horizontal still. Fig. 6 is a transverse section of the horizontal still and Fig. 7 is a detail view showing two water-discharge pipes for this still, either of which pipes can be used.
The a paratus as a whole consists, as shown, 0 a distilling and rectifying column A, having a supply-pipe 2 opening into its upper part, arectifying-column B discharging its products of condensation into the upper' part of said column A, a horizontal stlll C, which receives the liquids from said column A and is provided with closed steamcoils 3 and perforated steam-coils 4 and also with a draw-oil 5'for the water, and a heatexchanger D connected withthe outlet from still C by the pipe 6, drainage-tank G, pipe 6*, pump E, and pipe 6, and with the upper part of the column A by said pipe 2. The
' heat-exchanger is rovided with an outlet 7 through the heat-exchanger. The pumps E l.
for the high-test distillate and an inlet 8 for the low-test distillate,-whose fire test is to' be raised in the column A and still C and which is preliminarily heated in the heat-exchanger D by taking up the heat from the high-test distillate, and so cooling the latter on its way and F move the high-test and the low-test distillate, respectively, in opposite directions through the heat-exchanger. '1 he small pipe 6 is for equalizing the pressures in the still C and tank G.
The rectifying-column B is shown provided with a jacket 9, having pipes 10 and 11 for introducing and carrying off a cooling liquid. It may be water or any other cooling liquid. A special jacket, however, is not es-. sential to the rectifying action, since it sutlices for this that the vapors are repeatedly brought in contact with returning condensate from higher parts of the rectifyingcolumn. s
At 12 is an additional supply-pipe entering the upper part of the'rectifying-column B for discharging distillate thereinto when desired. It can be usefully employed, for example, in filling the apparatus with high-test distillate in starting, or it can be used to introduce low-test distillate then or during the operation, the distillate in either case being preliminarily heated or not as the case may be. The vapor-outlet 13 from this rectifier B can be connected with an ordinary condenser (not shown) or with other appliance or appliances which have heretofore been connected with the vapor-outlets of stills, and will therefore suggest themselves. v The columns A and B are divided, as shown, into a number of chambers by horizontal partitions 14, which are perforated and provided each with a pipe 15 and bell 16 and overflow-pipes 17. The vapors rising through the pipes 15 are by the bells 16 brought repeatedly into contact with liquid, which forms a layer on each partition above the edge of the bell and flows from chamber to chamber through the pipes 17 This is a common structure of column in arts which employ rectifying, distilling, or absorbing columns. It forms no part of the invention and can be replaced by any known or suitable arrangement for bringing vapors and liquids repeatedly into contact with each other as they pass through the apparatus. Numerous arrangements ofthis description areknown in various chemical industries.
The still 0, as shown, holds a body of liq uid which travels (or flows) horizontally at an appropriate speed through the same, being supplied at one end by the stream from the column A through the lowermost pipes 17 (or by any other suitable connection, if preferred) and discharging in a stream at the other through the pipe 6. At intervals are dams or partitions 18 to divide the traveling body of liquid into a succession of pools, which communicate by overflowing one into the other. This separation into pools aids" in keeping the different parts of the body of liquid, which have been subjected to difier-- ent degrees of steaming, better separated from one another. By making the dams or ICO partitions 18 diminish in height toward the outlet 6* the further advantage, as above explained, is secured of having the horizontallytraveling body of liquid diminish in depth as it approaches said outlet 6'.
The water which is delivered with the oil from the column A settles to the bottom of.
the still C and if not otherwise disposed of would fill the pools to the tops of the dams 18. To allow it to pass from one pool to the next, each dam (except the last) is provided at the bottom with an opening 19, (see Fig. 5;) but other arrangements could be provided for its conveyance, if preferred. From the pool next the outlet 6 the water can be discharged by the draw-off 5, which is provided, as shown, with a swinging arm 20, that can be turned to raise or lower its open outer end, and so determine the de that which the layer of water under the distillate shall stand.
In each compartment of the still C, except the small one drained by outlet 6", are a closed steam-coil 3 and a perforated coil 4.
The closed coil is supplied from the main with exhaust-steam from engines used to supply power at the works or from other sources (or it may be with live steamor both live and exhaust steam) and discharges into the drain-pipe 22. The perforated coil is supplied from the main 23 with live steam, (or it may be with "exhaust-steam or with both live and exhaust steam.) By perforated coil is to be understood any appropriate device for introducing free steam into the distillate. As shown, these coils consist of a number of straight pipes. They are perforated on the under side with holes,
which may be an eighth "of an inch in diameter and one foot apart, so as finely to divide the entering steam.
The-heat-exchanger D consists, as shown,
of a number of connected elements, as many of these being used as may be judged useful to transfer the heat from the outgoing hightest to the entering low-test distillate, say
ten, such as shown for the apparatus represented, although for lack of space only nine are indicated. Each element (see Figs. 2 and 3) resembles a tubular boiler or condenser in that it consists of a number of tubes 24 between the partition-plates 25 of a shell 26. The shell is thus divide d into two compartments or chambers by the partitions and the tubes, and the compartments are connected by the ipes 27 and 28 into two series, so that the hig. ..-test distillate starting at one end of one series may pass over one surface of the tubes, (outside or inside, as-the case may be, but inside, as shown,) while the low-test distillate starting at the other end of the other series passes over the other surface of said tubes, (outside, as shown.) Other known or suitable forms of heat-exchangers can be used instead.
In raising the fire test of burning-oil distillate with this apparatus the stream of lowtest distillate passes over the heat-conducting walls of the heat-exchanger Dto wit, the walls of the tubes 24 in the several elements, as shownin the opposite direction to the stream of high-test distillate from the still 0, so that in cooling the latter distillate the former is heated preliminarily to its intro duction into the distilling and rectifying column A, say to 170 Fahrenheit, or more or less, according to circumstances, but most advantageously above the fire test to be secured in the distillate. The preliminarily-heated distillate fed into the upper part of the column A descends through the same and supplies the body of distillate in the still 0. This being supplied at one end by a stream and discharging at the other end in a stream travels after the manner of a river and is subjected to free steam from the perforated coils 4 at intervals in its travel, while at the same time it is heated by the dry heat of the closed coils3. This dry heat'is not so important as the free steam and can. beomitted, if preferred; The vapors resulting from the action of the free steam (aided by the dry heat of coils 3, if this be used) pass up through the column A and are repeatedly brought in contact with the stream of preliminarily-heated distillate until they pass into and through the rectifying-column B, and so on to the condenser or condensers (not shown) or other apparatus. As the vapors rise the chief part, or, in fact, nearly all of the steam from the perforated coils 4, is condensed, and mingling with the stream of preliminarily-heated distillate forms part of the stream with which the later rising vapor's are continually brought into contact. The oil condensed from the vapors also mingles with the stream, and as it descends is reevaporated more or less, so that there are repeated condensations and revaporations, whereby the oil-vapors from the still C are rectified and a naphtha suitably free from products fit for burning ing distillate in the column A. The vapors are subjected to a further rectification in the column B.
The body of oil in the still C is limited relatively to the volume of steamadmitted through the perforated coils, so that all the low-boiling products are removed in a short internal diameter at such places as to form compartments or poolseach nine and a half feet in length, it is recommended to use pipe for coils as follows, namely: in the first compartment or pool, two hundred andthirtyeight feet of one-inch wrought-iron unperforated pipe for the closed coils and firtyfour feet or Wroughtiron perforated pipe for the open coils in the second compartment or -2o pool, two hundred and four feet of one-inch unperforated pipe andthirty-six-feet of oneinch perforated pipe; in the third compartment or pool, one hundred and fiftythree feet of one-inch unperforated pipe and twentyseven feet of one-inch perforated pipe, and, in the last compartment, one hundred and nineteen feet of one-inch unperforated pipe and eighteen feetpf one-inch perforated pipe.- The perforations may be one-eighth- 0 inch diameter, twelveinches between centers, and may be located on-the under side of the pipes. The closed coils would best be supplied with exhaust, the open coils withlive steam[ The supply of low-test distillate is so regulated that enough to fill the oil-spaces of column A and still 0 will be introduced by pipe 2 every fifteen minutes, more or less.
The supply of free steam-is regulated to give oil of the desired fire test, and the tempera- 4 ture of the liquid in the acket 9 is sufficiently below the boiling-point of Water to prevent the passage of burning-oil hydrocarbons through the column B.
In'raising its fire test about twenty per cent. of the low-test distillate may ordinarily, according to my experience, be separated as low-boiling products, but of course the percentage may vary. Thus if the composition of the low-test distillate should 5 vary, either from difference in the crude oil or in the process of distillation, the removal of a greater or a less percentage of such products might be'necessary in order to have burning oil of the same fire test; but a vari- 5 5 ation may also result from a variation in the manufacturers-wishes with respect to the grade of burning oil to be obtained. For some grades a lower fire test suffices than for others, andthe manufacturer naturally deioosires to retain in' the burning oil the lowest boiling products which would be consistent with the desired fire test. The temperature of the liquid in the jacket 9 would consequently be adjusted to-prevent these latter productsfrom passing over with those whose presence the burning oil would prevent it Irom having the desired fire test.
The temperatures in columns A and B are such as to effect the condensation therein of the chief part of the steam let into the perforated coils ofstill C. The temperature in the still C is about that of water-vapor under the barometric pressure inside of the stillpressure in the still is not reduced below that of the outside atmosphere. 1
The horizontally-traveling body of oil in the stillC being divided into a succession of communicating pools by the dams 18 the different parts are kept separate, and the dams being of diminishing height the pools are of diminishing depth so that the free to it, about 212 Fahrenheitwhen' the steam has less oil to pass upthrough-a condition which is believed to conduce to the efficiency of its action. In steaming the oil in the still C it is also an advantage and special improvement to decrease the volume of free steam per cubic foot of oillas the latter ap I proaches the outlet 6 because, for onereason, the content of low-boilingproducts being less, it is not considered desirable to evaporate so large a proportion of the oil as in the earlier portion of the steaming opera tion, when the proportion ofsuch products is greater.
As shown, the length of perforated steam- 7 coil is' greatest in the pool next the column A and decreases in order, being least inthe pool next the outlet 6", and this decrease is in greater ratio than the decrease in the cubical contents of the pools, due toitheir diminishing depth toward said outlet. volume of, free steam decreases also, as shown, with reference to the s uare foot of exposed upper surface of the iquid being steamed, and this. is considered advantageous, as modifying the evaporation in a desirable manner."
As said above, the chief part of the free steam admitted under the surface ofthe horizontally-traveling body of oil in still 0 is condensed in columns A and B and is thus along with the oil from said columns, consist ing in part of fresh distillate from the pipe 2 and in part of oil which has been evaporated in still 0 and column A and recondensed in columns A and B. In still C the water settles to the bottom and passes through the openings 19 at the bottoms of dams lS into the com artment or pool, from which it is The returned to still C in the form of hot water,
decante by the draw-off 5. It could, of I course, be withdrawn with the oil by allowing'it to pass the last dam 18, for which purposerthe pipe 20, having its open lower end near the'bottom of the still and its open up per end inserted through the dam near the top, may be providedl .By swinging the pipeQO so that its 'lower end 1s brought nearer to or fartherfrom the bottom of the still the depth of the water in the latter can I I tending the substitution of the continuous f is subjected to-free steam in the column A, and
steam (in closed or perforated coils, or both) narily to its introduction into the distilling be regulated.
It will of course be understood that the low-test distillate could be heated prelimiand rectifying column A otherwise than by means of the high-test distillate but in this, case the economical advantage of imparting the heat of the outgoing high-test distillate to the incoming low-test distillate would be lost, and the ability most perfectly to secure this economy is an important advantage atdistillation of the present invention for the periodical Working of current practice. .Furtherfthe distillate introduced by pipe 2 is thereby in part evaporated, and such subjection and evaporation are not necessarily dependent upon the use of the still C; but the capacity of an apparatus of a iven size for effective removal or the low-boi ing products would be much less if dependence were bad solely upon evaporation in column A than it is when use is made of a special steaming appliance, (like the still C.) i
The subjection of the vapors rising in column A to the returning stream of condensed oil mingled with hot water from the chief portion of the free steam is not dependent upon the said stream containing also the lowtest distillate, but it is advantageous to have it-contain the same, and if it is'desired to ob-' tain such advantage the low-test distillate should, as shown, he introduced at so high a point on the column A as in its descent to have a material influence on the rising vapors.
For using the present invention for distillati'on other than the separation of the lowboiling products ofburning-oil distillate from etroleum to raise the fire test of said distilate and for which said invention may be ap plicable, the skill ofthe Workers in such other distillation will sufiice in the light of the foregoing description. It is not intended to assert, however, that said invention is superior to the current practice in all sorts of distillat1on only it is intended to secure matters of my invention, hereinbefore described, which may be new and useful as well otherwise, as in the special distillation for raising the fire test of burning-oil distillate for such other uses as the same may severally be applicable.
The liquid to be distilled of any suitable kind can be introduced at the place or places described for the low-test distillate, the
can be used at the temperatures and of the volume considered most suitable, and the outgoing residual liquid and the incoming liquid to be distilled can be passed through a heat-exchanger in opposite directions, as described above, for the outgoing high-test distillate and the incoming low-test distillate;
theformer being the residual liquidfrom the therefore, in any of the hereinafter-Written claims the expression raising the fire test of burning-oil distillate occurs,such claim is intended to include only the special distillation in which said low-boiling products are removed from the said burning-oil distillate. In other claims more general expressions are used. Thus the expression liquid to be distilled includes, first, said burning-oil distillate; second, other petroleum or hydrocarbon oil, especially but not exclusively an oil con.-
taining hydrocarbons with boiling-points below that of water, while consisting mainly of higher boiling products; third, any other appropriate liquid, especially, but not exclusively, such a liquid as contains substances with boiling-points below that of water.
The boiling-point of water in the hereinafter-written claims refers to its boiling-point under the barometric pressure in the still.
This is intended to be practically that of the I outside atmosphere,'but it is not essential that it should be so.
I claim as my invention or discovery' 1. The burning-o distillate, consisting in partially evaporating the low-test distillate by contact of free steam therewith at about the boiling fpoirit of water, cooling the resulting mixture of oil and-water vapors gradually until the heavier oil-vapors and the chief part of the water-'va or are ultimately condensed and so separate from the vapors of the low-boiling products which pass over, bringing the said mixture of oiland Water'vaporsduring said process of raising the fire test of 1 cooling thereof into'repeated contact with the returning condensate of hot Water and hot oil and also@with a strea'm of'low-test distillate preliminarily heated to atemperature below the boiling-point of water and not lower than about 60 Fahrenheit below the same, and separating the.oil and water of condensation from each other, substantially as described.
2. The process of raising thefire test of burning-oil distillate, consisting in partially evaporating the low-test distillate by contact of free steam therewith at about the boiling-point of water, cooling the resulting mixture of oil and waten vapors gradually until the heavier oil-vapors and the chief part of the water-vapor are ultimately condensed and so separated from the vapors of the lowboiling (products which pass over, bringing the sa1 of such: oil at about the boiling-point of water mixture of 011 and water vapors free steam in suflicient volume to drive off during said cooling thereof into repeated the low-boiling products in a short time, .to
contact with the returning condensate of hot water and hot oil, and separating the oil and water of condensation from each other, substantially as described.
3. The rocess of raising the fire test of burning-oil distillate, consisting in partially evaporating the low-test distillate by contact therewith at about the boiling- )oint of water of free steam in sufficient volume to drive off the low-boiling products in a short time, to wit, under two hours, cooling the resulting mixture of oil and water vapors gradually until the heavier oil-vapors and the chief part of the water-vapor are ultimately condensed and so separated from the vapors of the low-boiling products which pass over, bringing the said mixture of oil and water vapors during said coolingt'hereof into repeated contact with thereturning condensate of hot water and hot oil and also with a stream of low-test distillate, and separating the oil and water of condensation from each other, substantially as described.
4. The rocess of raising the fire test of burning-oi distillate, consisting in partially evaporating the low-test distillate by contact therewith at about the boilingoint of water of free steam in suflicient vo ume to drive off the low-boiling products in a short time, to wit, under two hours, cooling the resulting mixture of oil and water vapors hydrocarbon oil containing hydrocarbons with boiling-points below that of water while consisting mainly of higher boiling products, consisting in admitting free steam at intervals below the surface of a horizontallytraveling body of such oil at about the boiling-point of water, cooling the resulting mixture of oil and water vapors until the heavier oil-vapors and the chief part of the watervapor are .conndensed and so separated from the vapors of the lowboiling products which pass over, and separating the oil and water of condensation from each other, substantially as described.
6. The process of distilling petroleum or hydrocarbon oil containing hydrocarbons with boiling-points below that of water while consisting mainldy of higher boiling products,
consisting in a mitting at intervals below the surface-0f a horizontally-traveling body wit, under two hours, cooling theresulting mixture of oil and water vapors until the heavier oil-vapors and the chief part of the water-vapor are condensed and so separated from the vapors of the low-boiling products which pass over, andseparating'the oil and Water of condensation from each other, substantially as described. i
7. In the distillation of provement consisting in delivering free steam at intervals below the surfaceof a horizontally-traveling body of the liquid to be distilled in such manner that the volume of sodelivered steam per cubic foot of liquid is lessened as the said liquid approaches the outlet therefor, substantially as described.
8. In the distillation of liquids, the improvement consisting in causlng a body of the liquid to be distilled'to travel horizontally and to diminish in depth as it approaches the outlet therefor, and delivering free steam at intervals below the surface of said body'in such manner that the volume of so-delivered steam per cubic foot of liquid is lessened as said liquid approaches the outlet therefor, substantially as described.
9: In the distillation of liquids, the improvement consisting in causing a body of the liquid to be distilled to travel horizonliquids, ,the im tally and to diminish in depth as it approaches'the outlet therefor, and delivermg free steam at intervals below the surface of said body in such manner that the volume of so-delivered steam per square foot of exposed upper surface of said liquid is lessened assaid liquid approaches the outlet therefor, substantially as described.
10. The process of distillation,, consisting in delivering free steam at intervals below the surface of a horizontally-traveling body of the liquid to be distilled in such manner that the volume of so-delivered steam per cubic foot of liquid is lessened as the said liquid approaches the outlet therefor, and cooling the resulting mixture of vapors so as to condense a portion ofthem while allowing another portion to pass over, substantially as described.
, 11. The process of distlllation, conslstmg IIS in causing a body. of the liquid to be distilled of liquid is lessened as said liquid approaches the outlet therefor, and cooling the resulting mixture of vapors so asto-condense a portion of them while allowing another portion to-pass over, substantially as described.
12. -The process of distillation, consisting in causing a body of the liquid to be distilled to travel horizontally and to diminish in as it approaches the outlet therefor, delivering free steam at intervals below the surface of said body in such manner that the volume of so-delivered steam per square foot of exposed u pcr surface of said liquid is lessened as said iquid approaches the outlet therefor, and cooling the resulting mixture of vapors so as to condense a portion of them while allowing another portion to pass over, substantially as described.
1 13. For separating low-boiling products from petroleum or' hydrocarbon oil which contains hydrocarbons with boiling-points below that of water While consisting mainly of higher boiling products, the continuous process which consists in partially evaporating said oil by contact of free steam therewith, gradually cooling the evolved vapors, bringing the body of said vapors into repeated contact with returning condensate, and adjusting the vapor-cooling to such extent below the boiling-point of water and the free-steam admission to such amount in excess of what passes over with the hydrocarbons that the hydrocarbons passing over are mainly those .with boiling-points below that of water and that the returning condensate is composed of the hot water from the chief part of said free steam as well as of the hot oil of condensation, substantially as described.
'14. For separating low-boiling products from petroleum or hydrocarbon oil which contains hydrocarbons with boiling points below' that of water while consisting mainly of higher boiling products, the continuous process which consists n partially evaporating said oil by contact of free steam there- .with, gradually cooling the evolved vapors,
bringing the body of said vapors int-o repeated contact with a stream of said oil preiminarily heated by exchange of temperature with the oil from which the low-boiling products have been separated and mingled with returning condensate, and adjusting the, vapor-cooling to such extent below the boiling-point of water and the free-steam admission to such amount in excess of what passes over with the hydrocarbons that the hydrocarbons passing over are mainly those with depth I boiling-points below that of water and that the returning condensate is composed of the hot water from the chief part of said free steam as well as of the hot oil of condensation, substantially as described.
15. For separating low-boiling products from petroleum or hydrocarbon oil which contains hydrocarbons with boi'ing-points below that of water while consisting mainly of higher boi'ing products, the continuous process which consists in partially evaporating said oil by contact of free steam therewith, gradually cooling the evolved vapors, bringing the body of said vapors into repeated contact with returning condensate, adiusting the vapor cooling to such extent below the boiling-point of water and the freesteam admission to such amount in excess of what passes over with the hydrocarbons that the hydrocarbons passing over are mainly those with boiling-points below that of water and thatthe returning condensate is composed of the hot water from the chief part of said free steam as well as of the hot oil of condensation, and continuously separatin the oil and water from each other by settling and decantation, substantially as described.
16. For separating low-boiling products from petroleum or hydrocarbon oil containing hydrocarbons with boiling-points below that of water while consisting mainly of higher boiling products, the continuous process, which is characterized by the partial evaporation of the said oil at about the boi ingpoint of water by contact of free steam therewith, and the repeated contact of the evolved vapors with the specified petroleum or hydro carbon oil of a temperature below the boilingpoint of water and not lower than about Fahrenheit below tht? same mingled with returning condensate of hot oil and the hot water from the chief part of said free steam, substantially as described.
In testimony whereof I a'flix my signature in presence of two Witnesses.
HERMAN FRASCH VVitnesses WM. H. ERWIN, W. B. HENRY.
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