US2762510A - Continuous percolation system - Google Patents

Continuous percolation system Download PDF

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US2762510A
US2762510A US321842A US32184252A US2762510A US 2762510 A US2762510 A US 2762510A US 321842 A US321842 A US 321842A US 32184252 A US32184252 A US 32184252A US 2762510 A US2762510 A US 2762510A
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adsorbent
adsorption column
columnar mass
mass
columnar
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Jr Harry M Gwyn
Carl D Laughlin
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Minerals & Chemicals Corp Of A
Minerals & Chemicals Corp Of America
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/02Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor with moving adsorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2215/00Separating processes involving the treatment of liquids with adsorbents
    • B01D2215/02Separating processes involving the treatment of liquids with adsorbents with moving adsorbents
    • B01D2215/021Physically moving or fluidising the adsorbent beads or particles or slurry, excluding the movement of the entire columns

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  • This invention relates to improvements in continuous countercurrent percolation systems for separationof components from a liquid organic mixture by contact of the mixture with a granular adsorbent moving downwardly through an adsorption zone in the form of a columnar mass, and it relates, more particularly, to such a system in which means are provided for continuously removing spent or partially spent adsorbent'uniformly over the entire area of the base of the columnar mass and in a manner substantially to prevent turbulence of the remaining adsorbent during movement thereof through the adsorption zone.
  • liquid organic mixtures have been separated commercially into two or more fractions through the use of solid adsorbents, both natural and artificial or synthetic, such as fullers'ea'rth, bentonite, bauxite, charcoal, silica gel, and various refined aluminas.
  • solid adsorbents both natural and artificial or synthetic, such as fullers'ea'rth, bentonite, bauxite, charcoal, silica gel, and various refined aluminas.
  • the separation may be effected whenever the mixture contains organic compounds having sufficiently diiferent adsorbabilities, and the completeness thereof depends, among other things, on relative adsorbabilities of the organic compounds to be separated.
  • highly polar organic compounds have been separated from less polar or non-polar organic compounds by selective ad sorption on various adsorbents;
  • Hydrocarbons and par ticularly petroleum stocks have been selectively separated according to chemical type, such as paraffins and naphthenes from olefins, and olefins from'aromatics.
  • known solid adsorbents have been used,'for example, to remove color bodies from hydrocarbons in the decolorization of lube oil, to remove olefins from and to desulfurize kerosine, gasoline, and diesel fuel, to degum and deasphaltize lube oil, and to separate or remove organic components from many other mixtures of organic liquids during the fractionation thereof.
  • 'It is conventional practice in commercial operations to carry out the fractionation or separation of mixtures of organic liquids into two or more fractions by the socalled percolation process.
  • the organic mixture simply is percolated or gravitated through a stationary bed of a granular adsorbent suitable for effecting the desired separation until such time as the effectiveness of the adsorbent has decreased to a level which will not permit further economical separation of the organic compounds.
  • the introduction of the charge is discontinued and the charge is diverted to another percolation unit.
  • the adsorbed fraction on the adsorbent is then removed by a suitable solvent, by heating, by burning, or by blowing with an inert gas, or by a combination of such methods.
  • the regenerated adsorbent is then reused for further treatment of the charge in another cycle of operation.
  • a non-adsorbed fraction of the'feed is removed "from the adsorption zone at a point adjacent the point "of introduction of the adsorbent.
  • the spent or partially spentadsorbent is removed from the adsorption zone at a pointadjace'nt the point of introduction of the feed.
  • the spent adsorbent is regenerated continously in associated equipment and returned to the adsorption column.
  • a bucket elevator or equivalent means, is included for removing spent or partially spent adsorbent from the base of the gravitating columnar mass.
  • the adsorbent is removed only at one'poi'nt at the base of the columnar mass.
  • the adsorbent moves more rapidly through some portions of the adsorption column than others with'result'that undesirable turbulence occurs causing a serious decrease in the efliciency of the operations;
  • some of the known systems have restrictions adjacent the lower end ofthe adsorption column which similarly interfere with uniform flow of adsorbent, likewise causing a departure from true countercurrent flow of the feed and the adsorbent and resulting in a decline" in the efficiency of the'operation.
  • one object of the present invention is to provide a novel system for operating a continuous percolation process which will obviate the aforementioned difficulties.
  • Another object of this invention is to provide a novel apparatus for operating a continuous percolation process which is so constructed and arranged that the solid adsorbent and the feed mixture pass through the adsorption column in substantially true countercurrent flow, thereby to realize a maximum efficiency of operation.
  • a further object is to'provide apparatus for operating a continuous countercurrent percolation process with maxi mum efliciency and which apparatus includes collection means for removing spent or partially spent adsorbent uniforrnly'over the entire area of the base of the columnar mass thereby to prevent substantial turbulence of the remaining adsorbent in the columnar mass during movement thereof downwardly withinthe adsorption column.
  • a still further object of the invention is to provide such apparatus in which there is included an elevating screw in contact with the base of the columnar mass of adsorbent and a plurality of collection vanes mounted on a plate and extending substantially between the outer edge of the elevating screw and the wall of the adsorption.
  • Figure 2 is a cross section taken along the line Z--2 of Figure l;
  • Figure 4 is an enlarged fragmentary view showing that a cross section taken along the line 3-3 of portion of the adsorption column adjacent the outlets for the non-adsorbed fraction, with the screens secured in the adsorption column by means of a circumferential flange;
  • Figure 5 is a fragmentary view showing the lower end of an adsorption column, including the collection vanes and elevating screw, of another embodiment of this invention.
  • Figure 6 is a fragmentary view showing the lower end of an adsorption column of still another embodiment of the invention.
  • Figure 7 is a fragmentary view showing the lower end of an adsorption column of another embodiment in which the collection vanes and the elevating screw are adapted for movement relative to one another;
  • Figure 8 is a cross section taken along the line 88 of Figure 7.
  • a system for continuous countercurrent separa- ,tion of components from a liquid organic mixture by passing the mixture through a columnar mass of granular adsorbent said system including an adsorption column adapted for continuous downward movement of the adsorbent therethrough in the form of a columnar mass, means for continuously removing spent or partially spent adsorbent uniformly over the entire area of the base of the columnar mass and in a manner to prevent substantial turbulence of the remaining adsorbent during movement of the remaining adsorbent downwardly within the adsorption column.
  • the means for continuously removing adsorbent uniformly over the entire area of the base of the columnar adsorbent mass comprises an elongated elevating tube of relatively small diameter in comparison with the diameter of the adsorption column and in axial alignment therewith, an elevating screw mounted for rotatable movement within the elevating tube and terminating at its lower end at a point below the open end of the elevating tube, a collection plate having a diameter substantially the diameter of the adsorption column mounted for rotatable movement immediately adjacent the lower endof the elevating screw in a plane normal to the axis of the elevating screw, and a plurality'of collection vanes fixedly secured to the upper face of the collection plate and extending between the elevating screw and the wall of the adsorption column in a manner such that when rotated with the plate will cause the adsorbent contacted therewith to be moved inwardly from the wall of theadsorptionl column into contact with the elevating screw and to be removed by the elevating screw from the adsorption
  • novel apparatus'of the present invention is suitable for continuous separation of any componentor components from a liquid organic mixture which are known to 4 those skilled in the art-to be capable of being separated upon percolation of the mixture through a mass of granular adsorbent in accordance with well known practices.
  • the novel apparatus may be utilized in the operation of a continuous percolation adsorption process to separate color bodies from hydrocarbons in the decolorization of lube oil, to remove olefins from and to desulfurize kerosine, gasoline, and diesel fuel, to degum and deasphaltize lube oil, and to separate hydrocarbons and particularly petroleum stock according to chemical type, such for example, as paraflins and naphthenes from olefins or olefins from aromatics.
  • any known granular percolation adsorbent may be used in the novel apparatus. For example, the.
  • apparatus suitable for the operation of a continuous percolation process employing, as the adsorbent, fullers earth clay, activated carbon, silica gel, activated alumina, magnesia, or any other known granular percolation adsorbent.
  • novel apparatus is not restricted in use to fractionation or separation operations expressly mentioned above, but the apparatus may be used to effect any separation of components from a liquid organic mixture known in the art to be possible by percolation of the mixture through a mass of granular adsorbent.
  • numeral 1 denotes generally an adsorption column, preferably having a substantially cylindrical configuration.
  • the granular adsorbent its continuously introduced from hopper 2 through tube 3 into adsorption column 1 through which it passes in the form of a columnar mass.
  • the adsorbent substantially completely fills adsorption column 1 at all times and assumes its natural angle of repose as indicated by line 4.
  • the adsorbent introduced into adsorption column 1 may comprise either fresh adsorbent or regenerated adsorbent, or a mixture thereof. Since apparatus for continuous regeneration is well known to those skilled in the art and forms no part of the present invention, such apparatus has been omitted from the drawings. It is to be recognized, however, that any suitable adsorbent regeneration equipment may be employed with the apparatus of this invention.
  • Adsorption column 1 terminates at its lower end in telescoping cylindrical section 5 which is secured as at 7 to the adsorption column wall 6 by circumferential flange 8.
  • Flange 8 may be formed integrally with wall 6 or may be sealed thereto by welding or other suitable means. It is to be noted that cylindrical section 5 extends beyond the end wall 6 and also is of a relative diameter such that an annular space is formed between section 5 and wall 6, the purpose of which will be apparent later.
  • Adsorption column 1 is closed at its lower end by end member 10 which preferably is releasably connected to section 5 by means of angle iron 11 and nut and bolt assemblies 12.
  • Feed inlet 13 preferably is comprised of two flanged sections which are secured together, as shown, by not and bolt assemblies 14, one of said flanged sections being formed integrally with end member 10. Nut and bolt assemblies 14 also function to clamp a pair of screens 15 between the abutting flanged sections of feed inlet 13 and in the path of flow of the feed mixture thereby to prevent sand, grit, and other undesirable solid particles, which might be contained in the feed, from entering the adsorption column.
  • outlets 16 are shown in Figure l as being only slightly above the mid point of the adsorption column, it is to be understood that they may be located closer to the top of the column, depending upon the height of the column.
  • screens 17 are secured to the inner wall of adsorption column 1 over outlets 16.
  • screens 17 preferably are welded or otherwise secured directly to the wall of the column.
  • the screens may be secured at either end to angle irons 18, which in turn may be removably attached by nut and bolt assemblies 19 to complementary angle irons 20 permanently afiixed to the wall of the adsorption column by welding or otherwise. With this construction, screens 17 can be readily removed for repair or replacement.
  • Figure 2 is a cross section of the apparatus taken in the plane of outlets 16 and in which is shown the relative positions of outlets 16, screens 17, annular channel 21 and nipple 23.
  • the non-adsorbed fraction passing through outlets 16 is collected in annular channel 21 formed by the wall of adsorption column 1 and channel bar 22 secured to or formed integrally with said wall, in the position shown in Figure 1. From there the non-adsorbed fraction passes through nipples 23 and thence to additional treating facilities or to storage, not shown, as desired.
  • Such means includes an elongated elevating tube 24 of relatively small diameter in comparison with the diameter of adsorption column 1, secured by welding or otherwise within the adsorption column and in axial alignment therewith, as shown.
  • a portion of elevating tube 24 extends beyond the upper end of the adsorption column and has provided therein adsorbent discharge spout 25.
  • elevating tube 24 terminates short of end member 10 in an open end 26.
  • Elevating screw 27 is mounted for rotatable movement within elevating tube 24 and its lower end rides in thrust bearing 28. The upper end of screw 27 extends through bearing 29 and is provided with gear 30 through which screw 27 may be rotated by a suitable drive mechanism, not shown.
  • Collection plate 31 having a diameter substantially the diameter of the adsorption column is keyed or otherwise secured to elevating screw 27 so that the collection plate will rotate with elevating screw 27 as a unit. It will be noted that collection plate 31 is adapted to rotate in a plane normal to the axis of the elevating screw and serves as a false bottom for adsorption column 1, supporting the columnar mass of adsorbent.
  • An upright peripheral lip 32 is formed on collection plate 31 and extends into annular space 9 between section 5 and the adsorption column wall 6, thereby to provide an adsorbent seal to prevent adsorbent from passing beyond collection plate 31.
  • a plurality of collection vanes 34 are fixedly secured to the upper face of collection plate 31 and extend substantially between the outer edge of elevating screw 27 and the adsorption column wall 6.
  • the vanes 34 are generally of an arcuate configuration and are oriented relative to screw 27 such that when the screw and collection plate 31 are rotated, adsorbent contacted by the vanes will be caused to move inwardly from the wall of adsorption column 1 into contact with the elevating screw and to be removed by the elevating screw from the adsorption column through discharge spout 25. It has been found that collection vanes 34, shaped and dis posed as shown in Figures 1 and 3, will provide satisfactory operation. It will be noted that vanes 34 taper from the outer edge to the inner edge thereof.
  • the arc of the collection vanes 34 is something more than While in Figure 3 only two vanes are shown, it is to be understood that as many as four or more may be employed, if desired.
  • the configuration of the vanes, that is the taper and the curvature may be varied provided only that when the vanes are properly rotated the adsorbent over the entire area of the base of the columnar mass is caused to be moved uniformly toward elevating screw 27.
  • adsorbent is continuously introduced into adsorption column 1 from hopper 2 through tube 3.
  • the adsorbent takes the form of a columnar mass in passing through the adsorption column and at the top of the column the adsorbent assumes its natural angle of repose such as is indicated by line 4.
  • the feed mixture is fed into adsorption column 1 through inlet 13 and after passing through the adsorbent seal flows upwardly through the columnar mass of adsorbent in countercurrent fashion.
  • the non-adsorbed traction of the mixture upon reaching the level of outlets 16, will pass therethrough into annular channel 21 and thence through nipples 23 for further treatment or storage as desired.
  • adsorption column 1 takes the form of a cylindrical tank with an integral dished head 35.
  • collection plate 31 slopes downwardly from the outer edge to the center as shown and a plurality of rollers 36 mounted by means of pedestal 37 provide additional support for the collection plate.
  • the rollers are positioned circumferentially and at spaced intervals adjacent the outer edge of plate 31.
  • roller support 37 takes the form of an annular, inverted channel formed integrally with peripheral rim 38 provided as shown on lure wall'lof'th'e adsorption embodiment the adsorbent seal is provided bydepend- Ting collar 39 rigidly aifixed to the underside of plate 31 column. Moreoverjin this and annular collar 40 provided, as shown, on the upper other manner.
  • this and annular collar 40 provided, as shown, on the upper other manner.
  • collection plate 31 is given added support by a plurality of rollers'36 mounted on annular pedestal 37 which is fixedly secured to the wall of the adsorption column.
  • Plate 31 is substantially flat and is provided with peripheral lip 32, the same as in the embodiment shown in Figure 1, which functions as one element of the adsorption seal.
  • the other element of the adsorption seal is provided by the depending leg of annular member 41 secured by bolts 42 or otherwise to L-shaped ring 43 fixedly attached in turn to the adsorption column wall, as shown.
  • the mixture fed into the adsorption column flows between the underside of plate 31 and pedestal 37, through the annular passage between the adsorption column wall and peripheral lip 32 and thence between peripheral lip 32 and the depending leg of annular member 41 into contact with the columnar mass of the adsorbent.
  • collection plate 31 and spider support 33 be made up of a plurality of sections which may be lowered into the adsorption column through a manhole 44 ( Figure l) and assembled by means of bolts or otherwise in much the same manner as the trays of a fractionation column.
  • FIG. 7 there is shown a still further embodiment of the invention.
  • This embodiment is similar to the apparatus shown in Figure 6 except that means are provided for independent rotation of collection plate 31 and elevating screw 27.
  • shank 45 of elevating screw 27 is hollow and shaft 46 extends therethrough and rests in thrust bearing 28.
  • Collection plate 31 and spider support 33 are adapted to rotate as a unit and are keyed or otherwise fixedly secured to shaft 46 whereby plate 31 and support 33 may be rotated by rotation of shaft 46.
  • the upper end of elevating screw 27 is not shown, it is to be understood that it passes through and is supported by bearing 29 ( Figure 1).
  • the upper end of shaft 46 is not shown, it is to be understood that is passes freely through gear 30 of elevating screw 27 and is adapted to be rotated by means of a drive source independent of the drive source for elevatving screw 27.
  • screw 27 is shown as a double thread screw. However, if desired, a screw having a single thread may be utilized.
  • a system for continuous countercurrent separa- I 8 tionof components from a liquidorganic mixture by percolation of the'mix'ture through a columnar mass of granular adsorbent capable of selectively adsorbing said components said system including a vertically disposed adsorption column adapted for continuous downward movement of such adsorbent therethrough in the form of a columnar mass, adsorbent inlet means adjacent the top of the adsorption column for introducing an adsorbent thereinto, feed inlet means adjacent the bottom of the adsorption column for introducing the liquid organic mixture into 'the adsorption column, and outlet means intermediate the adsorbent inlet means and the feed inlet means for continuously withdrawing a liquid nonadsorbed fraction of said mixture from the adsorption column, the combination therewith of means for continuously removing adsorbent uniformly over the entire area of the base of the columnar mass and in a manner to prevent substantial turbulence of the remaining adsorbent
  • bearing means are circumferentially disposed about the lower end of the adsorption column in a manner so as to support the outer edge of said plate.
  • a process for continuously separating components from a liquid organic mixture by means of percolation of said organic mixture through a columnar mass of granular adsorbent capable of adsorbing said components therefrom comprising the steps of continuously feeding said adsorbent to the top of a confined columnar mass thereof, continuously introducing said organic mixture adjacent the bottom of said columnar mass of adsorbent material and passing it upward thereinto, continuously withdrawing a liquid non-adsorbed fraction of said organic mixture from contact with the columnar mass of adsorbent intermediate the top and bottom of said mass, continuously urging granular adsorbent material, from the bottom strata of said columnar mass toward the bottom opening of a tubular passage, arranged to extend upwardly and concentrically through the columnar mass from a point near the bottom thereof, in a manner to avoid substantial turbulence of the remaining adsorbent material in the columnar mass, and causing adsorbent from the bottom of said columnar mass to pass upwardly through said tubular passage

Description

Sept. 11, 1956 H. M. GWYN, JR ET AL 2,762,510
CONTINUOUS PERCOLATION SYSTEM Filed Nov. 21, 1952 4 Sheets-Sheet 1 Fig.
ATTEST: INVENTORS. HARRY M. GWYN,JR. (aw BY CARL 0. LAUGHLIN ATTORN EY Sept. 11, 1956 H. M. GWYN, JR., ET AL.
commuous PERCOLATION SYSTEM 4 Sheeis-Sheet 2 Filed Nov. 21, 1952 INVENTORS. HARRY M. GWYN,JR. CARL D. LAUGHLIN A TTES T:
ATTORNEY p 11, 1956 H. M, GWYN, JR., ET AL 2,762,510
CONTINUOUS PERCOLATION SYSTEM 4 Sheets-Sheet 3 Filed Nov. 21, 1952 IIIIII III N I ////I/IIIIIIIIII/; 7
INVENTORS. HARRY M. GWYN,JR.
BY CVARL D. LAUGHLIN flmLAt 5 @M ATTORNEY Sept. 11, 1956 H. M. GWYN, JR., ET AL 2,762,510
CONTINUOUS PERCOLATION SYSTEM Filed Nov. 21, 1952 4 Sheets-Sheet 4 ATTEST; INVENTORS.
. HARRY M. GWYN JR. M 0% BY CARL o. LAUGHLFN //1M KMJ ATTORNEY United States Patent 2,762,510 CONTINUOUS PERCOLATI'ON SYSTEM Harry M. G wyn, In, Philadelphia, and Carl D. Laughlin, Drexel I-irll, Pa., assignors to Minerals & Chemicals Corporation of America, a corporation of Maryland Application November 21, 1952, Serial No. 321,842 6 Claims. (Cl. 210-425) This invention relates to improvements in continuous countercurrent percolation systems for separationof components from a liquid organic mixture by contact of the mixture with a granular adsorbent moving downwardly through an adsorption zone in the form of a columnar mass, and it relates, more particularly, to such a system in which means are provided for continuously removing spent or partially spent adsorbent'uniformly over the entire area of the base of the columnar mass and in a manner substantially to prevent turbulence of the remaining adsorbent during movement thereof through the adsorption zone. l
For many years liquid organic mixtures have been separated commercially into two or more fractions through the use of solid adsorbents, both natural and artificial or synthetic, such as fullers'ea'rth, bentonite, bauxite, charcoal, silica gel, and various refined aluminas. The separation may be effected whenever the mixture contains organic compounds having sufficiently diiferent adsorbabilities, and the completeness thereof depends, among other things, on relative adsorbabilities of the organic compounds to be separated. For example, highly polar organic compounds have been separated from less polar or non-polar organic compounds by selective ad sorption on various adsorbents; Hydrocarbons and par ticularly petroleum stocks have been selectively separated according to chemical type, such as paraffins and naphthenes from olefins, and olefins from'aromatics. More specifically, known solid adsorbents have been used,'for example, to remove color bodies from hydrocarbons in the decolorization of lube oil, to remove olefins from and to desulfurize kerosine, gasoline, and diesel fuel, to degum and deasphaltize lube oil, and to separate or remove organic components from many other mixtures of organic liquids during the fractionation thereof. 'It is conventional practice in commercial operations to carry out the fractionation or separation of mixtures of organic liquids into two or more fractions by the socalled percolation process. In that process the organic mixture simply is percolated or gravitated through a stationary bed of a granular adsorbent suitable for effecting the desired separation until such time as the effectiveness of the adsorbent has decreased to a level which will not permit further economical separation of the organic compounds. At that time, the introduction of the charge is discontinued and the charge is diverted to another percolation unit. The adsorbed fraction on the adsorbent is then removed by a suitable solvent, by heating, by burning, or by blowing with an inert gas, or by a combination of such methods. The regenerated adsorbent is then reused for further treatment of the charge in another cycle of operation.
There are several obvious disadvantages of the above described batch percolation process. In the first place, the decline in activity of the adsorbent during use over a period of time necessitates shutdown of the operation for regeneration of the adsorbent. Moreover, because of the decline in activity of the adsorbent, the composi 2. tion of the product from the adsorption zone varies during even a single cycle of operation and because of which it is necessary to properly select and'segregate the product cuts. i
Recently there have been suggested several continuous percolation processes by which liquid organic mixtures may be continually separated without shutting down the unit for the purpose of regeneration or replacement of the solid adsorbent. Such processes, for example, are disclosed in U. S. Patents Nos. 2,470,339 and 2,564,717. Broadly, thesec'ontinuous percolation processes involve introducing granular adsorbent'into' an adsorption zone and passing it therethrough in the-form of a moving column. The feed is continuously introduced into and passed through the adsorption zone in a direction opposite to the direction of passage of the adsorbent. A non-adsorbed fraction of the'feed is removed "from the adsorption zone at a point adjacent the point "of introduction of the adsorbent. Similarly, the spent or partially spentadsorbent is removed from the adsorption zone at a pointadjace'nt the point of introduction of the feed. The spent adsorbent is regenerated continously in associated equipment and returned to the adsorption column. Thus, these continuous adsorption processes involve countercurrent contact of the feed mixture with a moving column of adsorbent material. The efficiency of these processes is dependent upon maintaining true countercurrent flow of the feed and the adsorbent, and any substantial turbulence of the adsorbent in passing through the adsorption zone'will have a serious detrimental 'elfect upon 'the' operations.
In some systems heretofore proposed for operation of continuous adsorption processes, a bucket elevator, or equivalent means, is included for removing spent or partially spent adsorbent from the base of the gravitating columnar mass. The adsorbent, however, is removed only at one'poi'nt at the base of the columnar mass. As a result, the adsorbent moves more rapidly through some portions of the adsorption column than others with'result'that undesirable turbulence occurs causing a serious decrease in the efliciency of the operations; Moreover, some of the known systems have restrictions adjacent the lower end ofthe adsorption column which similarly interfere with uniform flow of adsorbent, likewise causing a departure from true countercurrent flow of the feed and the adsorbent and resulting in a decline" in the efficiency of the'operation.
Accordingly, one object of the present invention is to provide a novel system for operating a continuous percolation process which will obviate the aforementioned difficulties.
Another object of this invention is to provide a novel apparatus for operating a continuous percolation process which is so constructed and arranged that the solid adsorbent and the feed mixture pass through the adsorption column in substantially true countercurrent flow, thereby to realize a maximum efficiency of operation.
A further object is to'provide apparatus for operating a continuous countercurrent percolation process with maxi mum efliciency and which apparatus includes collection means for removing spent or partially spent adsorbent uniforrnly'over the entire area of the base of the columnar mass thereby to prevent substantial turbulence of the remaining adsorbent in the columnar mass during movement thereof downwardly withinthe adsorption column.
A still further object of the invention is to provide such apparatus in which there is included an elevating screw in contact with the base of the columnar mass of adsorbent and a plurality of collection vanes mounted on a plate and extending substantially between the outer edge of the elevating screw and the wall of the adsorption.
Figure 2 is a cross section taken along the line Z--2 of Figure l;
, F'gure 3 is Figure 1;
Figure 4 is an enlarged fragmentary view showing that a cross section taken along the line 3-3 of portion of the adsorption column adjacent the outlets for the non-adsorbed fraction, with the screens secured in the adsorption column by means of a circumferential flange;
Figure 5 is a fragmentary view showing the lower end of an adsorption column, including the collection vanes and elevating screw, of another embodiment of this invention;
Figure 6 is a fragmentary view showing the lower end of an adsorption column of still another embodiment of the invention;
Figure 7 is a fragmentary view showing the lower end of an adsorption column of another embodiment in which the collection vanes and the elevating screw are adapted for movement relative to one another; and
Figure 8 is a cross section taken along the line 88 of Figure 7.
In accordance with the present invention, there is provided, in a system for continuous countercurrent separa- ,tion of components from a liquid organic mixture by passing the mixture through a columnar mass of granular adsorbent, said system including an adsorption column adapted for continuous downward movement of the adsorbent therethrough in the form of a columnar mass, means for continuously removing spent or partially spent adsorbent uniformly over the entire area of the base of the columnar mass and in a manner to prevent substantial turbulence of the remaining adsorbent during movement of the remaining adsorbent downwardly within the adsorption column. By thus eliminating turbulence, true countercurrent flow of the granular adsorbent and the feed mixture through the adsorption column results and hence maximum operation efliciency. 7
Generally, the means for continuously removing adsorbent uniformly over the entire area of the base of the columnar adsorbent mass comprises an elongated elevating tube of relatively small diameter in comparison with the diameter of the adsorption column and in axial alignment therewith, an elevating screw mounted for rotatable movement within the elevating tube and terminating at its lower end at a point below the open end of the elevating tube, a collection plate having a diameter substantially the diameter of the adsorption column mounted for rotatable movement immediately adjacent the lower endof the elevating screw in a plane normal to the axis of the elevating screw, and a plurality'of collection vanes fixedly secured to the upper face of the collection plate and extending between the elevating screw and the wall of the adsorption column in a manner such that when rotated with the plate will cause the adsorbent contacted therewith to be moved inwardly from the wall of theadsorptionl column into contact with the elevating screw and to be removed by the elevating screw from the adsorption column, and means for rotating the elevating screw and the collection plate. The novel apparatus'of the present invention is suitable for continuous separation of any componentor components from a liquid organic mixture which are known to 4 those skilled in the art-to be capable of being separated upon percolation of the mixture through a mass of granular adsorbent in accordance with well known practices. For example, the novel apparatus may be utilized in the operation of a continuous percolation adsorption process to separate color bodies from hydrocarbons in the decolorization of lube oil, to remove olefins from and to desulfurize kerosine, gasoline, and diesel fuel, to degum and deasphaltize lube oil, and to separate hydrocarbons and particularly petroleum stock according to chemical type, such for example, as paraflins and naphthenes from olefins or olefins from aromatics. Moreover, any known granular percolation adsorbent may be used in the novel apparatus. For example, the. apparatus suitable for the operation of a continuous percolation process employing, as the adsorbent, fullers earth clay, activated carbon, silica gel, activated alumina, magnesia, or any other known granular percolation adsorbent.
It is to be understood that the novel apparatus is not restricted in use to fractionation or separation operations expressly mentioned above, but the apparatus may be used to effect any separation of components from a liquid organic mixture known in the art to be possible by percolation of the mixture through a mass of granular adsorbent.
The optimum conditions for operation of a continuous percolation process such as temperature, rates of flow of the adsorbent and the feed, type of adsorbent, and the like, are well known to those skilled in the art and form no part of this invention. Where necessary, specific conditions for any particular separation may be readily determined by calculation in accordance with established procedures which need not be discussed here.
The invention may be more readily understood by rcference to the attached drawings. Turning at this time to Figures 1 to 3, inclusive, numeral 1 denotes generally an adsorption column, preferably having a substantially cylindrical configuration. The granular adsorbent its continuously introduced from hopper 2 through tube 3 into adsorption column 1 through which it passes in the form of a columnar mass. The adsorbent substantially completely fills adsorption column 1 at all times and assumes its natural angle of repose as indicated by line 4.
It is to be understood that the adsorbent introduced into adsorption column 1 may comprise either fresh adsorbent or regenerated adsorbent, or a mixture thereof. Since apparatus for continuous regeneration is well known to those skilled in the art and forms no part of the present invention, such apparatus has been omitted from the drawings. It is to be recognized, however, that any suitable adsorbent regeneration equipment may be employed with the apparatus of this invention.
Adsorption column 1 terminates at its lower end in telescoping cylindrical section 5 which is secured as at 7 to the adsorption column wall 6 by circumferential flange 8. Flange 8 may be formed integrally with wall 6 or may be sealed thereto by welding or other suitable means. It is to be noted that cylindrical section 5 extends beyond the end wall 6 and also is of a relative diameter such that an annular space is formed between section 5 and wall 6, the purpose of which will be apparent later.
Adsorption column 1 is closed at its lower end by end member 10 which preferably is releasably connected to section 5 by means of angle iron 11 and nut and bolt assemblies 12.
The liquid organic mixture from which components are to be adsorbed is fed into adsorption column 1 from a suitable feed storage, not shown, through feed inlet 13 provided in end member 10. Feed inlet 13 preferably is comprised of two flanged sections which are secured together, as shown, by not and bolt assemblies 14, one of said flanged sections being formed integrally with end member 10. Nut and bolt assemblies 14 also function to clamp a pair of screens 15 between the abutting flanged sections of feed inlet 13 and in the path of flow of the feed mixture thereby to prevent sand, grit, and other undesirable solid particles, which might be contained in the feed, from entering the adsorption column.
In the adsorption column, the feed flows upwardly through the columnar mass of granular adsorbent which is passing downwardly in countercurrent flow. The nonadsorbed fraction passes from adsorption column 1 through one or more outlets 16. While outlets 16 are shown in Figure l as being only slightly above the mid point of the adsorption column, it is to be understood that they may be located closer to the top of the column, depending upon the height of the column.
For the purpose of substantially preventing the passage of adsorbent granules out of the column with 'the nonadsorbed fraction,'screens' 17 are secured to the inner wall of adsorption column 1 over outlets 16. In order to insure uniform flow of the columnar mass of adsorbent through the adsorption column, screens 17 preferably are welded or otherwise secured directly to the wall of the column. In the case of columns of very large diameter where relatively small restrictions 'in the column would have practically no adverse effect on the uniformity of adsorbent flow, the screens, as shown in Figure 4, may be secured at either end to angle irons 18, which in turn may be removably attached by nut and bolt assemblies 19 to complementary angle irons 20 permanently afiixed to the wall of the adsorption column by welding or otherwise. With this construction, screens 17 can be readily removed for repair or replacement. Figure 2 is a cross section of the apparatus taken in the plane of outlets 16 and in which is shown the relative positions of outlets 16, screens 17, annular channel 21 and nipple 23.
The non-adsorbed fraction passing through outlets 16 is collected in annular channel 21 formed by the wall of adsorption column 1 and channel bar 22 secured to or formed integrally with said wall, in the position shown in Figure 1. From there the non-adsorbed fraction passes through nipples 23 and thence to additional treating facilities or to storage, not shown, as desired.
As above pointed out, in accordance with this invention there is provided means for continuously removing spent adsorbent uniformly over the entire area of the base of the columnar adsorption mass in a manner to prevent turbulence of the remaining adsorbent during movement of the remaining adsorbent downwardly within the adsorption column. Such means includes an elongated elevating tube 24 of relatively small diameter in comparison with the diameter of adsorption column 1, secured by welding or otherwise within the adsorption column and in axial alignment therewith, as shown. A portion of elevating tube 24 extends beyond the upper end of the adsorption column and has provided therein adsorbent discharge spout 25. It is to be noted that elevating tube 24 terminates short of end member 10 in an open end 26. Elevating screw 27 is mounted for rotatable movement within elevating tube 24 and its lower end rides in thrust bearing 28. The upper end of screw 27 extends through bearing 29 and is provided with gear 30 through which screw 27 may be rotated by a suitable drive mechanism, not shown.
Collection plate 31 having a diameter substantially the diameter of the adsorption column is keyed or otherwise secured to elevating screw 27 so that the collection plate will rotate with elevating screw 27 as a unit. It will be noted that collection plate 31 is adapted to rotate in a plane normal to the axis of the elevating screw and serves as a false bottom for adsorption column 1, supporting the columnar mass of adsorbent. An upright peripheral lip 32 is formed on collection plate 31 and extends into annular space 9 between section 5 and the adsorption column wall 6, thereby to provide an adsorbent seal to prevent adsorbent from passing beyond collection plate 31. It will be noted that the feed mixture introduced into adsorption column 1 through inlet 13 will flow between section 5 and peripheral lip 32 and thence between peripheral lip 32 and .the adsorption column wall 6. into contact with the columnar mass of adsorbent. Such flow of the feed mixture tends to prevent the entrance of adsorbent into the adsorbent seal. Since, as above pointed out, col lection plate 31 supports the entire weight of the columnar mass of adsorbent, it is preferable to reinforce the plate by means of spider support 33. Spider support 33 may be formed integrally with collection plate 31 or may be separately formed and similarly keyed to elevating screw 27. A plurality of collection vanes 34 are fixedly secured to the upper face of collection plate 31 and extend substantially between the outer edge of elevating screw 27 and the adsorption column wall 6. The vanes 34 are generally of an arcuate configuration and are oriented relative to screw 27 such that when the screw and collection plate 31 are rotated, adsorbent contacted by the vanes will be caused to move inwardly from the wall of adsorption column 1 into contact with the elevating screw and to be removed by the elevating screw from the adsorption column through discharge spout 25. It has been found that collection vanes 34, shaped and dis posed as shown in Figures 1 and 3, will provide satisfactory operation. It will be noted that vanes 34 taper from the outer edge to the inner edge thereof. Moreover, the arc of the collection vanes 34 is something more than While in Figure 3 only two vanes are shown, it is to be understood that as many as four or more may be employed, if desired. Also, the configuration of the vanes, that is the taper and the curvature, may be varied provided only that when the vanes are properly rotated the adsorbent over the entire area of the base of the columnar mass is caused to be moved uniformly toward elevating screw 27.
In operation, adsorbent is continuously introduced into adsorption column 1 from hopper 2 through tube 3. The adsorbent takes the form of a columnar mass in passing through the adsorption column and at the top of the column the adsorbent assumes its natural angle of repose such as is indicated by line 4. Simultaneously with the introduction of the adsorbent the feed mixture is fed into adsorption column 1 through inlet 13 and after passing through the adsorbent seal flows upwardly through the columnar mass of adsorbent in countercurrent fashion. The non-adsorbed traction of the mixture, upon reaching the level of outlets 16, will pass therethrough into annular channel 21 and thence through nipples 23 for further treatment or storage as desired. At the same time, spent or partially spent adsorbent is removed uniformly over the entire area of the base of the columnar mass as a result of continual rotation in the proper direction of collection plate 31 and screw 27 as a unit. The continuous rotation is effected by means of an external drive, not shown, operatively connected with gear 30. With reference to Figure 3, screw 27 and plate 31 are rotated in a clockwise direction. As plate 31 and necessarily vanes 34 rotate, the adsorbent at the base of the columnar mass is contacted by the vanes and is caused to move uniformly toward the screw. Although there is no relative movement between screw 27 and vanes 34, it has been found that the adsorbent will be forced into the narrow passage between them and thence lifted by elevating screw 27 to the top of elevating tube 24 and discharged through chute 25. I f
Referring now to Figure 5, there is shown a second embodiment of the invention in which adsorption column 1 takes the form of a cylindrical tank with an integral dished head 35. In this embodiment of the invention, collection plate 31 slopes downwardly from the outer edge to the center as shown and a plurality of rollers 36 mounted by means of pedestal 37 provide additional support for the collection plate. The rollers are positioned circumferentially and at spaced intervals adjacent the outer edge of plate 31. Preferably roller support 37 takes the form of an annular, inverted channel formed integrally with peripheral rim 38 provided as shown on lure wall'lof'th'e adsorption embodiment the adsorbent seal is provided bydepend- Ting collar 39 rigidly aifixed to the underside of plate 31 column. Moreoverjin this and annular collar 40 provided, as shown, on the upper other manner. As in the embodiment shown in Figure 5,
collection plate 31 is given added support by a plurality of rollers'36 mounted on annular pedestal 37 which is fixedly secured to the wall of the adsorption column. Plate 31 is substantially flat and is provided with peripheral lip 32, the same as in the embodiment shown in Figure 1, which functions as one element of the adsorption seal. The other element of the adsorption seal is provided by the depending leg of annular member 41 secured by bolts 42 or otherwise to L-shaped ring 43 fixedly attached in turn to the adsorption column wall, as shown. The mixture fed into the adsorption column, it will be seen, flows between the underside of plate 31 and pedestal 37, through the annular passage between the adsorption column wall and peripheral lip 32 and thence between peripheral lip 32 and the depending leg of annular member 41 into contact with the columnar mass of the adsorbent.
In order to simplify assembly and disassembly of the apparatuses of Figures 5 and 6, it is preferred that collection plate 31 and spider support 33 be made up of a plurality of sections which may be lowered into the adsorption column through a manhole 44 (Figure l) and assembled by means of bolts or otherwise in much the same manner as the trays of a fractionation column.
While the embodiments shown in Figures 5 and 6 differ somewhat in construction from that of the apparatus shown in Figure 1, it is to be noted that the mode of operation of the latter applies equally as well to the apparatuses shown in Figures 5 and 6.
Referring at this time to Figures 7 and 8, there is shown a still further embodiment of the invention. This embodiment is similar to the apparatus shown in Figure 6 except that means are provided for independent rotation of collection plate 31 and elevating screw 27. As
shown in Figure 7, shank 45 of elevating screw 27 is hollow and shaft 46 extends therethrough and rests in thrust bearing 28. Collection plate 31 and spider support 33 are adapted to rotate as a unit and are keyed or otherwise fixedly secured to shaft 46 whereby plate 31 and support 33 may be rotated by rotation of shaft 46. While the upper end of elevating screw 27 is not shown, it is to be understood that it passes through and is supported by bearing 29 (Figure 1). Similarly, while the upper end of shaft 46 is not shown, it is to be understood that is passes freely through gear 30 of elevating screw 27 and is adapted to be rotated by means of a drive source independent of the drive source for elevatving screw 27. It will be noted that screw 27 is shown as a double thread screw. However, if desired, a screw having a single thread may be utilized.
The operation of the apparatus shown in Figures 7 and 8 is substantially the same as that of the earlier embodiments except that collection vanes 34 are reversed and screw 27 and plate 31 rotated in opposite directions. The relative movement between screw 27 and vanes 34 facilitates the uniform movement of adsorbent over the entire area of the base of the columnar mass into contact with screw 27.
We claim:
1. In a system for continuous countercurrent separa- I 8 tionof components from a liquidorganic mixture by percolation of the'mix'ture through a columnar mass of granular adsorbent capable of selectively adsorbing said components, said system including a vertically disposed adsorption column adapted for continuous downward movement of such adsorbent therethrough in the form of a columnar mass, adsorbent inlet means adjacent the top of the adsorption column for introducing an adsorbent thereinto, feed inlet means adjacent the bottom of the adsorption column for introducing the liquid organic mixture into 'the adsorption column, and outlet means intermediate the adsorbent inlet means and the feed inlet means for continuously withdrawing a liquid nonadsorbed fraction of said mixture from the adsorption column, the combination therewith of means for continuously removing adsorbent uniformly over the entire area of the base of the columnar mass and in a manner to prevent substantial turbulence of the remaining adsorbent during movement of the remaining adsorbent downwardly within the adsorption column, said means comprising an elongated elevating tube of relatively small diameter in comparison with the diameter of the adsorption column concentrically disposed within the adsorp tion column, said elevating tube terminating at its upper end at a point beyond the topof the adsorption column and having its lower end open and spaced from the bottom of the adsorption column, an elevating screw mounted for rotatable movement within the elevating tube for moving adsorbent upwardly through the elevating tube, said elevating screw terminating at its lower end at a point below the lower end of the elevating tube, an ad sorbent outlet adjacent the upper end of the elevating tube for discharging adsorbent from said elevating tube, a plate having a diameter substantially the diameter of the adsorption column and mounted for rotatable movement immediately adjacent the lower end of the elevating screw and coaxially therewith, and a plurality of vanes fixedly secured to the upper face of said plate, each vane extending substantially between the outer edge of the elevating screw and the wall of the adsorption column in a manner such that when rotated with the plate will cause adsorbent contacted therewith to be moved inwardly from the Wall of the adsorption column into contact with the elevating screw,
2. The apparatus of claim 1 wherein said elevating screw and said plate are rigidly connected together so as to be rotatable as a unit.
3. The apparatus of claim 2 wherein bearing means are circumferentially disposed about the lower end of the adsorption column in a manner so as to support the outer edge of said plate.
4. The apparatus of claim 1 wherein said elevating screw and said plate are adapted to be rotated independently of each other.
5. The apparatus of claim 1 wherein said elevating screw is provided with an axial bore extending there through and a shaft is mounted for rotatable movement within said bore and is rigidly connected with said plate whereby said elevating screw and said plate may be rotated independently of each other.
6. A process for continuously separating components from a liquid organic mixture by means of percolation of said organic mixture through a columnar mass of granular adsorbent capable of adsorbing said components therefrom, comprising the steps of continuously feeding said adsorbent to the top of a confined columnar mass thereof, continuously introducing said organic mixture adjacent the bottom of said columnar mass of adsorbent material and passing it upward thereinto, continuously withdrawing a liquid non-adsorbed fraction of said organic mixture from contact with the columnar mass of adsorbent intermediate the top and bottom of said mass, continuously urging granular adsorbent material, from the bottom strata of said columnar mass toward the bottom opening of a tubular passage, arranged to extend upwardly and concentrically through the columnar mass from a point near the bottom thereof, in a manner to avoid substantial turbulence of the remaining adsorbent material in the columnar mass, and causing adsorbent from the bottom of said columnar mass to pass upwardly through said tubular passage and out of contact with said columnar mass.
References Cited in the file of this patent UNITED STATES PATENTS 329,329 Matthiessen Oct. 27, 1885 10 Matthiessen Oct. 27, 1885 Toepfer Apr. 2, 1889 Coe Feb. 23, 1926 Force Feb. 1, 1927 Wiard Mar. 10, 1936 Bighouse Oct. 26, 1937 Bonotto Ian. 30, 1940 Green Sept. 22, 1942 Hibshman Feb. 20, 1951 FOREIGN PATENTS Australia Feb. 20, 1947

Claims (1)

  1. 6. A PROCESS FOR CONTINUOUSLY SEPARATING COMPONENTS FROM A LIQUID ORGANIC MIXTURE BY MEANS OF PERCOLATION OF SAID ORGANIC MIXTURE THROUGH A COLUMNAR MASS OF GRANULAR ADSORBENT CAPABLE OF ADSORBING SAID COMPONENTS THEREFROM, COMPRISING THE STEPS OF CONTINUOUSLY FEEDING SAID ADSORBENT TO THE TOP OF A CONFINED COLUMNAR MASS THEREOF, CONTINUOUSLY INTRODUCING SAID ORGANIC MIXTURE ADJACENT THE BOTTOM OF SAID COLUMNAR MASS OF ADSORBENT MATERIAL AND PASSING IT UPWARD THEREINTO, CONTINUOUSLY WITHDRAWING A LIQUID NON-ADSORBED FRACTION OF SAID ORGANIC MIXTURE FROM CONTACT WITH THE COLUMNAR MASS OF ADSORBENT INTERMEDIATE THE TOP AND BOTTOM OF SAID MASS, CONTINUOUSLY URGING GRANULAR ADSORBENT MATERIAL, FROM THE BOTTOM STRATA OF SAID COLUMNAR MASS TOWARD THE BOTTOM OPENING OF A TUBULAR PASSAGE, ARRANGED TO EXTEND UPWARDLY AND CONCENTRICALLY THROUGH THE COLUMNAR MASS FROM A POINT NEAR THE BOTTOM THEREOF, IN A MANNER TO AVOID SUBSTANTIAL TURBULENCE OF THE REMAINING ADSORBENT MATERIAL IN THE COLUMNAR MASS, AND CAUSING ADSORBENT FROM THE BOTTOM OF SAID COLUMNAR MASS TO PASS UPWARDLY THROUGH SAID TUBULAR PASSAGE AND OUT OF CONTACT WITH SAID COLUMNAR MASS.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2963431A (en) * 1954-06-22 1960-12-06 Metallgesellschaft Ag Process and apparatus for treating liquids with ion exchange materials
US3003641A (en) * 1958-07-25 1961-10-10 Minerals & Chem Philipp Corp Continuous percolation apparatus
WO1987001381A1 (en) * 1985-09-10 1987-03-12 Vitamins, Inc. Mass transfer extraction of liquids from solids
US4816222A (en) * 1983-09-22 1989-03-28 Fagrell Per Aake Method and apparatus for obtaining a suspension and solution
US5653815A (en) * 1994-04-08 1997-08-05 Braunschweigische Maschinenbauanstalt Ag Process for solid-liquid extraction and extraction tower for carrying out the process

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US329332A (en) * 1885-10-27 Apparatus for decolorizing sugar-liquor by upward filtration through bone-black
US329329A (en) * 1885-10-27 Bone-black filter
US400807A (en) * 1889-04-02 Apparatus for malting grain
US1574556A (en) * 1919-08-13 1926-02-23 Cycle Company Filter
US1616218A (en) * 1926-06-24 1927-02-01 John W Force Tank-cleaning device
US2033500A (en) * 1933-12-27 1936-03-10 Edward S Wiard Settled solids removing apparatus
US2096728A (en) * 1934-08-14 1937-10-26 Co Bartlett & Snow Co Apparatus for extracting oils from oleaginous materials
US2188673A (en) * 1935-08-31 1940-01-30 Extractol Process Ltd Filter for filtering liquids
US2296437A (en) * 1938-11-25 1942-09-22 Infilco Inc Water treatment and apparatus
US2542521A (en) * 1948-08-06 1951-02-20 Standard Oil Dev Co Process for segregating oxygenated hydrocarbons

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US329332A (en) * 1885-10-27 Apparatus for decolorizing sugar-liquor by upward filtration through bone-black
US329329A (en) * 1885-10-27 Bone-black filter
US400807A (en) * 1889-04-02 Apparatus for malting grain
US1574556A (en) * 1919-08-13 1926-02-23 Cycle Company Filter
US1616218A (en) * 1926-06-24 1927-02-01 John W Force Tank-cleaning device
US2033500A (en) * 1933-12-27 1936-03-10 Edward S Wiard Settled solids removing apparatus
US2096728A (en) * 1934-08-14 1937-10-26 Co Bartlett & Snow Co Apparatus for extracting oils from oleaginous materials
US2188673A (en) * 1935-08-31 1940-01-30 Extractol Process Ltd Filter for filtering liquids
US2296437A (en) * 1938-11-25 1942-09-22 Infilco Inc Water treatment and apparatus
US2542521A (en) * 1948-08-06 1951-02-20 Standard Oil Dev Co Process for segregating oxygenated hydrocarbons

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2963431A (en) * 1954-06-22 1960-12-06 Metallgesellschaft Ag Process and apparatus for treating liquids with ion exchange materials
US3003641A (en) * 1958-07-25 1961-10-10 Minerals & Chem Philipp Corp Continuous percolation apparatus
US4816222A (en) * 1983-09-22 1989-03-28 Fagrell Per Aake Method and apparatus for obtaining a suspension and solution
WO1987001381A1 (en) * 1985-09-10 1987-03-12 Vitamins, Inc. Mass transfer extraction of liquids from solids
US5653815A (en) * 1994-04-08 1997-08-05 Braunschweigische Maschinenbauanstalt Ag Process for solid-liquid extraction and extraction tower for carrying out the process

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