US3619425A

US3619425A - Counterflow liquid-granular material transfer process and apparatus

Info

Publication number: US3619425A
Application number: US9831A
Authority: US
Inventors: Claude Blain; Paul Minart; Roger Platzer; Marc Pelletier
Original assignee: Commissariat a lEnergie Atomique CEA
Current assignee: Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
Priority date: 1966-05-20
Filing date: 1970-02-09
Publication date: 1971-11-09
Anticipated expiration: 1988-11-09
Also published as: FR1515874A; US3619426A; NL6706880A; NL137123C; FR1505371A; ES340786A1; BE698314A; GB1167653A; DE1642975A1

Abstract

In the closed cycle, mobile bed, liquid-solid treatment installation disclosed herein, a given volume of the solid material is periodically displaced in the treatment chamber by a given volume of liquid under a given pressure. The solid material is advanced in the cycle through two columns which are separated from each other by at least one intermediate receiver that is located between two isolation valves through which the solid material passes without being crushed, and that receives from one of the columns a constant volume constituted of one or more batches of said given volume of solid material.

Description

United States Patent Claude Blaln Palaiseau;

Paul Minart, Grenoble; Roger Platzer, Chattlllon-Sous-Bagneux; Marc Pelletier, Grenoble, all of France Feb. 9, 1970 Division of Ser. No. 639,777,

May 19, 1967, abandoned Nov. 9, l 97 l Commissariat A LEnergie Atomique (C.E.A.)

Paris,

Societe Grenobloise DEtudes et DApplications Hydrauliques Grenoble, France July 9, 1966 France Inventors Appl. No. Filed Patented Assignees Priority COUNTERFLOW LlQUID-GRANULAR MATERIAL TRANSFER PROCESS AND APPARATUS 15 Claims, 2 Drawing Figs.

US. Cl 210/33, 210/138, 210/189, 210/195, 210/2 Int. Cl 801d 15/02, BOld 33/16 [50] Field of Search 210/33, 138,189,195, 257, 258, 262

[56] References Cited UNITED STATES PATENTS 2,693,395 1 1/1954 Berg 210/33 X 2,815,322 12/1957 Higgins 210/33 3,056,743 10/1962 Eichhorn et a1 210/33 3,272,335 9/1966 Nettel 210/262 X 3,298,950 l/l967 Mindler... 210/33 3,503,510 3/1970 Minart et a1. 210/189 Primary Examiner-Samih N. Zahama Att0rneysSylvester J. Liddy, John .1. Hart, Joe E. Daniels and Charles E. Baxley ABSTRACT: In the closed cycle, mobile bed, liquid-solid treatment installation disclosed herein, a given volume of the solid material is periodically displaced in the treatment chamber by a given volume of liquid under a given pressure. The solid material is advanced in the cycle through two columns which are separated from each other by at least one intermediate receiver that is located between two isolation valves through which the solid material passes without being crushed, and that receives from one of the columns a constant volume constituted of one or more batches of said given volume of solid material.

COUNTERFLOW LlQUID-GRANULAR MATERIAL TRANSFER PROCESS AND APPARATUS This is a division of application Ser. No. 639,777, filed May 19, 1967 and now abandoned.

This invention relates to a solid-liquid treatment installation in which a mobile bed moves in the direction of liquid flow for a few seconds at a time according to a recurrent cycle, and remains stationary with respect to the treatment column containing it during periods of reverse flow treatment. The installation may or may not be of the closed cycle type and if of such type may include more than one treatment column.

in mobile bed installations, it is nearly always necessary to know the hourly rate of volume flow and to adjust it as accurately as possible. Adjustment of the frequency of the bed movements is a simple matter with the aid of a timing device, but accurate determination and control of the volume of matter transferred at each movement is more difficult to achieve. ln the arrangements which have been proposed to date, the displacement of the material is brought about by injection of a liquid under pressure for a set time, see for example US. Pat. No. 2,815,322, dated Dec. 3, 1957. It has been found that with this method, it is not possible to obtain an amplitude of displacement that can be reproduced in time. This is why installations operating by this principle feature volume measurement tanks which are distinct from the actual treatment columns, being isolated from them and from the source of material by valves, and which are filled right up without there being a liquid layer above the material. Consequently, the filler duct from the source of material also remains full of material, so that some crushing of grains of material in the inlet valve when it closes cannot be avoided. The inlet valve has been eliminated in certain of these installations to avoid the crushing problem, but when the volumetric measurement tank empties into the column, the filler duct also does so at least partly, due to continuity, so that the exact volume which has emptied cannot be established. Experience has also shown that the use of a volumetric measurement tank for granular material is debatable in any case. It is known that the bulk volument of a given mass of granular material in a liquid depends on such different factors as grain size, roughness and shape, interstitial fluid properties and such outside factors as vibration, settling, type of wall, etc. Because of all these factors the results obtained by material volume measurement are apt to be anything but consistent over a period of time. In this connection, it might be stated that it has been found that the most important thing in a mobile bed treatment installation designed for continuous operation, is to achieve a constant rate of solid material flow. The need to keep this flow constant is more important than any ability to determine its value with the aid of a separate measurement tank, for not only is such measurement inaccurate, but the volume emptying out will not necessarily be the same as the volume of material displaced in the column while it is emptying, whether the latter be located before or after the measurement tank.

Further, in certain of the mobile bed installations, some of the operations take place in separate columns operating simultaneously, each column being described for a specific form of treatment. The solid material circulates through the installation in a closed cycle, passing through each column in turn, but in view of the specific nature of each treatment, it is necessary to isolate the individual columns from each other while providing means to allow the granular material to be transferred periodically from one to the other. At this point, it is desired to distinguish what is here termed a mobile bed installation from the type of installation in which all of the solid material is emptied out of one column after treatment and is then sent to another one for furthertreatment. Such installations are related to mobile-bed installations by the fact that each individual treatment takes place within an appropriate vessel'tank or receiver and that the solid material passes from each such vessel tank or receiver in turn to the next one, but they really operate as fixed-bed installations because there are no opposite flows of fluid and solid material in their columns to ensure a methodical transfer process.

It is known that the transfer of material in a mobile bed installation involves a certain number of problems, one of the most important of which is how to get the isolation valves or other devices to close to give a perfect seal without crushing any of the solid material. All known installations of this type characteristically have opposite flows and there is always at least one valve or cock closing against the flow of the solid material, because in order to be able to permanently isolate two successive columns in the solid material circuit, at least two valves or cocks are required in series, one of them being closed when the other is open, and vice versa, and with an intermediate receiver between them. Consequently, when such a receiver is used as a means of measuring volumes of material, some material invariably gets crushed whenever the inlet valve closes. if the measurement tank only features an emptying valve, this must also serve as an inlet valve for a further intermediate receiver, vessel or tank following the measurement tank and separated from the next column by a valve or cock closing against a flow of resin. Though one could if really necessary arrange to keep the measurement tank emptying valve open for the time required to ensure that it does not close until all the material has emptied out, the same does not apply for the intermediate receiver, which still contains some solid material when the valve between it and the next column closes.

The primary purpose of the present invention is to provide a mobile bed installation which does not have the above described disadvantages.

One of the objects of the invention is to provide an improved mobile bed treatrnent installation having a constant accurate rate of solid material flow. In accordance with the invention this object is accomplished by periodically displacing the granular material bed in a treatment column with the injection of a preset volume of liquid under a given pressure into such column.

Another object of the invention is to provide an improved mobile bed treatment installation provided with means for enabling the complete transfer of given charges of solid material from one container to another in such installation. In accordance with the invention this object is accomplished by providing in the installation intermediate such containers at least one transfer receiver having means associated therewith for isolating it from one or the other of such containers during the transfer of the solid material and thereby permanently isolating such containers from each other.

Other objects of the invention, as well as the advantages thereof, will become apparent from a perusal of the following description when read in connection with the accompanying drawings in which FIG. 1 is a diagrammatic view showing by way of example one possible form of an installation embodying the features of the invention; and

FIG. 2 is a diagram illustrating the sequence of operations in the installation of FIG. 1.

The installation shown in FIG. 1 of the drawings is of the type that may be utilized for treatment of a solution by the solid particles of a closed-circuit ion exchanger. As is shown, such an installation may comprise a large diameter fixing column generally designated 1 and an elution and washing column of smaller diameter generally designated 2. The columns 1 and 2 each basically consist of a

cylindrical body

10, 20, respectively, and a base or housing l1, 2!, respectively, surrounding the bottom portion of the

body

10, 20, respectively. The beds 10' and 20' of exchange resins filling the

columns

10, 20, respectively, are over sand beds 13, 23, respectively, having

outlet strainers

14, 24, respectively, buried in the same and connected to outlet ducts provided with valves 14a and 240, respectively.

The body 10 of the fixing column 1 is provided with a top cover 15 forming with such body an annular chamber 16 that encloses the upper portion of the cylindrical body 10. The top rim of the cylindrical body 10 functions as a circular spill for the resins from the bed 10'. Located in the chamber 16 above the body is a strainer 17 attached to the end of a liquid feed pipe 18 provided with a valve 18a adjacent to such strainer. An outlet pipe 19 provided with a valve 19a is fitted to the top of the cover so that it is in communication with the chamber 16.

The body 20 of the elution and washing column 2 has connected to its upper end a liquid outlet pipe 26 provided with a valve 260. A short distance below the entry end of the liquid outlet pipe 26 the column body 20 has connected thereto one end of a pipe 27 that runs off at an angle of 45 downwardly and provides a spill for the resins of the bed 20. The pipe 27 is provided with a valve 31 adjacently to the column body 20. Located a short distance below the entry end of the pipe 27 is a peripheral annulus or strainer 28 which is connected by a pipe provided with a valve 28a to a suitable source for the washing solution that is fed therefrom into the top of the bed 20. A little farther below the annulus 28 is a second peripheral annulus or strainer 29 that is connected to a suitable source for the eluant feed through a pipe provided with a valve 29a.

The exchange resins in the bed 20 are supplied from a storage tank 43, which discharges by gravity through a pipe 44 into the annular chamber 22 where the resins form a heap which gradually grows in height until it blocks the discharge end of the pipe 44 and thereby cuts ofi' the feed from such pipe. The discharge end of the pipe 44 is located at a given level which determines the maximum level of the heap of resins in the chamber 22 and leaves a space in the upper portion of such chamber for the fluid which is to impel the resins periodically from such chamber into the bed 20' through the annular opening between the bottom end of the body 20 and sand bed 23 in the manner described in greater detail in US. Letters Patent 3,503,510, dated Mar. 3, 1970, for Installation for Treating Liquids and Granular Solids.

The impelling liquid for delivering the resins to the bed 20' and consequently for imparting periodic forward motion to such solid material bed, is delivered tangentially into the upper portion of the annular chamber 22 through a duct or pipe 45 controlled by a valve 45a. The pipe 45 is connected to a suitable source of such liquid in a known manner. Also connected to pipe 45 at a place located between the valve 45a and such source are any suitable means, such as a liquid measuring tank, for discharging through the valve 45a when the latter is opened a given volume of impelling fluid under a given pressure. The timing for such injection of a given volume of the impelling liquid into the annular chamber 22 can be best understood, it is believed, from a consideration of FIG. 2 of the drawings. In the diagram shown in FIG. 2,-the different operations are shown on the ordinate 0V and the time periods for such operations on the abscissae OTi.

On the horizontal line designated I are plotted the treatment periods T in the column 20, which periods are separated by time periods t during which take place the aforesaid impulse operations i.e. the periods during which the measured liquid under pressure is expelled through the duct 45 and valve 45a into the annular chamber 22. The timing of these impulse operations, which are designated E, are shown on line III of FIG. 2. The points ti on line 1 indicate when the

valves

45a and 24a open and close, respectively, with relation to the treatment periods T, and the point 11 on line 1, indicates when such valves 24a and 450, open and close, respectively, with relation to such treatment periods.

It is believed that the diagram shown in FIG. 2 clearly points out that the time I selected for the impulse operations is such that this operation is carried out in its entirety before the closure of the feed valve 45a, i.e. before the beginning of a treatment in column 20. As has been previously indicated, during this injection of a preset volume of the impelling liquid under a given pressure into the annular chamber 22, a given displacement of the granular material bed in column 20 will take place. During this displacement, a certain amount of slip of the liquid takes place with respect to the grains of material. It is accordingly necessary in order to displace a given volume of the granular material, to inject a greater volume of liquid than that of the material to be displaced. It will also be appreciated that displacement of the granular material should preferably occur within a few seconds in order that the bed may progress up the column 20 as a piston with minimum loss through compaction. This it has been found can be achieved by a proper selection and control of the impelling pressure exerted on the liquid.

As will be noted in FIG. 1 of the drawings, the two columns or tanks 1 and 2 are interconnected by two resin transfer systems each of which comprises an

intermediate receiver

30 or 40 located between two valves arranged so that one valve cannot open unless the other is closed. Thus considering column 2 as the upstream tank and column 1 as the downstream tank, the material from column 2 flows to the intermediate receiver 30 which is located between the

valves

31, 32 arranged as aforesaid. Considering column 1 as the upstream tank and column 2 as the downstream tank, the material from column 1 flows to the intermediate receiver 40 which is located between the valves 41, 42 arranged as aforesaid. The intermediate receiver 30 is supplied with liquid through a liquid supply manifold 35 which is provided with a control valve 35a and which leads tangentially into the upper part of such receiver. The outlet pipe 33 from the intermediate receiver 30 leads tangentially into the upper part of the annular space 12 formed by the base 111 of column 1. The intermediate receiver 40 is connected by a pipe provided with the valve 41 to the annular chamber 16 formed at the top of column 1, and the material in such receiver discharges through a downwardly inclined pipe which is provided with the valve 42. The bottom of the intermediate receiver 40 is connected by a liquid feed pipe 46 having a control valve 460, to a source of liquid supply. The top of such receiver 40 is provided with a liquid outlet pipe 47 having a control valve 470.

The transfer system from the fixing column 1 to the foot of the elution and washing column 2 additionally includes an auxiliary tank 43 which is connected to the discharge side of the intermediate receiver 40 and which, as has been previously explained, functions as a feed hopper from which the resin flows under gravity into a pipe 44 discharging into the annular chamber 22 formed in the base of column 2.

It will be understood from what has heretofore been said that resin displacement will occur intermittently in each of the columns I. and 2. During the treatment periods which occur simultaneously, the resin beds in both columns will be stationary at the same time. In a treatment period the valves 18a and 14a of column 1 are open and the

valves

28a, 29a and 24a of column 2 are open and the fixing, elution and washing processes will all take place simultaneously. As has been previously indicated the rate of resin flow through the system is regulated in the elution and washing column 2. At a set frequency controlled by a timing device 60 which is electrically connected to and controls the aforesaid valves associated with the feed and movements of the liquids and resins throughout the system, the eluant and washing feed valves 29a and 28a, respectively, and the outlet valve 24a close,

valves

26a and 45a open, and a predetermined volume of liquid under pressure, referred to as the impulsion volume, is injected into the annular chamber 22 in the base of column 2 in the manner previously described.

Simultaneously with the aforesaid operation, an identical volume of liquid will discharge from column 2 through the pipe 26, and this impulse will depress the resin level in the annular chamber 22 and cause the bed 20' in column 2 to move upwardly as a piston for a few seconds, the resin feeding from the chamber 22 in a circumferential manner inwardly through the circular opening at the lower end of the column body 20 and into the body of the bed in a manner described more in detail in said US. Pat. No. 3,503,510. Following the upward step of bed 20', the elution and washing processes are resumed and valve 31 opens to let the resin in the upper end of said body 20 spill out through the enclosed pipe 27. When this occurs,

valves

26a and 45a are closed, and

valves

28a, 29a and 24a are open. The time between the opening and closure of valve 45a controlled by the timer 60 shall always be sufficient to enable all of the preset volume of liquid to be injected into the annular chamber 22 as has previously been pointed out in connection with the description of FIG. 2 of the drawings.

The rate of resin flow is set by selecting an appropriate combination of impulse frequency, impulse pressure and impulse volume. lnjection of a given volume of liquid under a given pressure will repeatedly cause the displacement of the same given volume of resin. As the volume of resin that is discharged through the pipe 27 at the top of column 2 after each impulse is constant, the opening rate of valve 31 can be adjusted so that it does not close until all of the given volume of resin has passed through it. The successive batches of resin which pass through the pipe 27 collect in the bottom of the intermediate receiver 30. At the same time the falling resin level in the annular chamber 22 in the base 21 of column 2 automatically starts the loaded resin flowing from hopper 43 through pipe 44 to the foot of the column until the material again heaps up to a height at which it will block off the opening to pipe 44. Hopper 43 has associated therewith a photoelectric cell resin level detector 48 which is so arranged in a control system of a type known to the art that when the level of the material in hopper 43 falls to the plane of the cell so that the cell is exposed to light, the cell triggers off the forward progression cycle of the resin bed in the fixing column 1 after valve 31 closes. When this triggering action occurs valves 14a and 18a of column 1 close, and valve 19a of such column and

valves

32 and 35a associated with the intermediate receiver 30 open. A set volume of liquid will then be injected from the manifold 35 into the receiver 30 causing the expelling of all of the resin in such receiver out through the pipe 33 and tangentially into the annular chamber 12 formed in the base 11 of column 1 where it will be distributed evenly, and at the same time, causing the resin bed 10' in column 1 to move upwardly. An equivalent volume of liquid will emerge at the head of column 1 through the manifold 19 and a part of the resin from the bed 10' will overflow the top of the column body 10 and pass into the annular chamber 16 formed by the top cover 15.

The liquid to be treated starts circulating again when the valve 19a of column 1 and the

valves

32, 35a of the intermediate receiver 30 have closed, and the valves 14a and 18a of column 1 are again opened. The liquid entering through pipe 18 is distributed over the top of the bed 10' by the strainer 17 which has numerous, upwardly directed outlet orifices so that the jets of liquid discharging from the latter will flush away the layer of resin that covered the strainer during the previous forward progression step of the bed 10'. A part of the flow of the liquid fed by the pipe 18 is bypassed or diverted through a pipe 50 provided with a control valve 50a and directed into the bottom portion of the annular chamber 16 to loosen up the resin contained in such chamber and enable it to flow through the pipe section provided with valve 41 to the intermediate receiver 40. On completion of the flow through pipe 18, valve 41 closes again and valves 46a and 47a associated with the intermediate receiver 40 open to cause a flow of liquid to rise in the tank 40 and fluidize the resin therein in order to wash out any solid impurities that may still remain from the fixing treatment in column 1. At the end of the fluidization period, valves 46a, 47a close and valve 42 opens to permit the washed resin to discharge into hopper 43 from which it will be fed into the annular chamber 22 of column 2 during a further series of impulses and until such time as the level of the resin in hopper 43 has fallen sufficiently to uncover the photoelectric cell 48 and thereby trigger off a new impulse cycle in the intermediate receiver 30 and column 1, followed by fluidization in the intermediate receiver 40.

It will be observed from the foregoing, that in the practice of the process of this invention, a given bulk volume of the resin material is made to pass from an upstream tank (2 or 1), to an intermediate receiver (30 or 40, respectively), in one or several batches, with such bulk volume remaining constant from one batch to the next and not exceeding a given maximum volume that is smaller than the intermediate tank to which it is delivered. The entire volume of material which has been fed to an intermediate receiver is then transferred to the downstream tank (1 or 2, respectively). This flow of material, first from the upstream tank to an intermediate receiver, and then from the latter to the downstream tank, can take place under gravity with the liquid and solid material flows occurring in opposite directions, and with the liquid volume corresponding to the transferred solid volume progressing upstream through the communication orifice while the solid flow progresses downwardly. On the other hand, the flow of material from an intermediate receiver to a downstream tank can also be made to take place with the liquid and solid flows both in the same direction, by injecting into the upper part of the intermediate receiver a volume of liquid at least equal to that required to entrain the entire said maximum volume of material. In the procedure herein, as demonstrated by column 1, a liquidfilled receiving space of a greater volume than said maximum volume of material is provided and maintained in the downstream tank.

In accordance witha preferred form of the invention, the volume of liquid expelling the solid material from an intermediate receiver is injected within a short space of time from a tangential injection pipe entry into such receiver, as clearly shown with respect to the intermediate receiver 30. Preferably also the intennediate receiver is made cylindrically in shape so as to ensure the most uniform vertical velocity component distribution possible for the liquid which is progressing down towards the bottom of the tank, and to facilitate complete rapid emptying of the material from the receiver or tank. The total capacity of the tank should be equivalent to more than twice and preferably nearly three times the maximum volume of material transferred in order that the rotational motion imparted to the liquid in the tank does not begin to affect its bottom until practically all of the material has been expelled.

It will also be noted from the aforesaid description, that it is within the contemplation of the invention to utilize as the liquid for entraining the material out of an intermediate tank,

either the liquid imparting motion to the bed in the upstream column, such as the intermediate tank 40 with respect to which column 1 is the upstream column, or the liquid imparting motion to the bed in the downstream column, such as the intermediate tank 30, with respect to which column 1 is the downstream column. ln the latter case, a liquid filled receiving space is provided in the downstream tank, the annular chamber 12 of column 1, the volume of which may be smaller than the maximum volume of transferred material.

It will also be observed that the installation of this invention is automatic, all operations thereof being controlled by conventional programmed systems and remote control arrangements known to those in this art. Instrumentation such as flow measurement devices and pressure recorders may also be provided as is known in the art. The operating cycles,,column base dimensions, annular chamber and auxiliary and intermediate tank capacities, and impelling fluid volumes, are all determined on the basis of their necessity to achieve the desired transfer conditions in accordance with the invention.

While we have hereinabove described and illustrated in the accompanying drawings an example of the manner in which our invention may be practiced, it will be apparent to those skilled in the art that many other forms may be utilized. Hence it is intended to include all such modifications and variations of the invention within the scope of the appended claims.

What is claimed is:

1. An installation providing a closed circuit for treating liquids and solid particles, comprising a substantially vertically disposed tubular fixing column and a substantially vertically disposed tubular elution column separate and spaced from one another, a first intermediate means located between said columns and including means for collecting solid particles discharged from said fixing column, means operable to treat such collected particles at intermittent intervals, and means for feeding intermittently to said elution column batches of such treated particles, means for impressing on each such batch of treated particles a given volume of liquid to effect intermittently a forward upward movement of a given volume of the material in said elution column, a second intermediate means located between said columns and including means for collecting the solid particles discharged from the upper end of said elution column, and means operative periodically to feed to said fixing column a batch of such collected solid particles and a given volume of liquid to effect a forward upward movement of a given volume of the material in said fixing column, means for feeding particles discharged at the upper end of said fixing column to said first intermediate collecting means, and a tubular casing enclosing the lower portion of at least one of said columns and forming with the latter a tubular chamber for holding a mass of the solid particles, and for receiving the solid particles and the liquid introduced into said at least one of said columns.

2. An installation as defined in claim 1, wherein said at least one of said columns is the elution column, and in which said treated particle feeding means feeds said treated particles into said holding chamber and said liquid impressing means rapidly injects said given volume of the liquid tangentially into such chamber above the mass of particles therein.

3. An installation as defined in claim 1, wherein said at least one of said columns is the fixing column, and in which said periodically operative feeding means feeds each batch of collected solid particles and a given volume of the liquid into such chamber above the mass of particles therein, said feeding means feeding the liquid, at least, tangentially into such chamber.

4. An installation providing a closed circuit for treating liquids and solid particles, comprising a substantially vertically disposed tubular fixing column and a substantially vertically disposed tubular elution column separate and spaced from one another, a tubular casing enclosing the lower portion of said elution column and forming with the latter a tubular chamber for holding a mass of the solid particles, means for rapidly injecting tangentially into such chamber above the mass of particles therein a given volume of liquid under a given pressure to effect a forward upward movement of a given volume of the material in such elution column, said injecting means being constructed and arranged to repeat at intermittent intervals the injection of a constant given volume of liquid under constant given pressure to effect an intermittent forward motion of given volumes of the material in said elution column, first intermediate means located between said columns for intermittently collecting batches of the solid particles discharged from said fixing column and comprising a first particle collection chamber and a second particle collection chamber both located between said tubular holding chamber and said fixing column, means operable to feed intermittently batches of particles from said fixing column to said second collection chamber and from the latter to said first collection chamber, means operable to treat the particles in said second collection chamber in the intervals between such intermittent batch feed thereof, said first collection chamber communicating with said holding chamber at a place positioned above the portion of the mass of particles remaining therein after operation of said injecting means, and constructed and arranged to feed the particles by gravity onto such mass portion, and means for controlling the discharge from such first particle collection chamber and into said holding chamber of a given volume of particles to form the mass of particles required therein prior to each operation of said injecting means, a second intermediate means located between said columns and including means for collecting the solid particles discharged from the upper end of the elution column, and means operative periodically to feed a batch of said collected solid particles and a given volume of liquid into said fixing column.

5. An installation providing a closed circuit for treating liquids and solid particles, comprising a substantially vertically disposed tubular fixing column and a substantially vertically disposed tubular elution column separate and spaced from one another, a tubular casing enclosing the lower portion of said fixing column and forming with the latter a tubular chamber for holding a mass of the solid particles, means for rapidly injecting tangentially into such chamber above the mass of particles therein a given volume of liquid under a given pressure to effect a forward upward movement of a given volume of the material in such fixing column, said injecting means being constructed and arranged to repeat at intermittent intervals the injection of a constant given volume of liquid under constant given pressure to effect an intermittent forward motion of given volumes of the material in said fixing column, and comprising a receiver tank having a solid particle entry port and a solid particle discharge port located intermediate said elution and fixing columns, means for alternately connecting the entry port of said tank to the discharge end of said elution column and the discharge port of said tank to the tubular chamber of said fixing column, first means operative intermittently to cause said elution column to discharge batches of solid particles of given volume into said connecting means and to said tank, and second means operative periodically to cause the transfer of solid particles fed to said intermediate tank to said fixing column as a liquid stream, said first operative means being constructed and arranged to cause said elution column to discharge a plurality of batches of the solid particles to said intermediate tank between each of the operations of said second operative means, said second operative means being constructed and arranged to transfer the entire volume of solid particles in said intermediate tank as a liquid stream in each operation thereof, andmeans including at least one receiver tank for collecting solid particles discharged from the upper end of said fixing column and feeding them into the lower portion of said elution column.

6. An installation for treating liquids and solid particles comprising an upstream tubularly shaped column providing a chamber for a bed of the solid particles, a downstream tubularly shaped column providing a chamber for a bed of the solid particles, a receiver tank having a solid particle entry port and a solid particle discharge port located intermediate said upstream and downstream columns, means connecting the entry port of said intermediate tank to the discharge end of said upstream column and the discharge port of said intermediate tank to the entry end of said downstream column and including means for isolating one of said intermediate tank ports when the other of its said ports is operative for the passage of solid particles therethrough, first means operative periodically to cause said upstream column to discharge a batch of solid particles of given volume into said connecting means and to said intermediate tank, and second means operative periodically to cause the transfer of solid particles fed to said intermediate tank to said downstream column, one of said upstream and downstream columns being a fixing column and the other being an elution and washing column, and each of such columns including a cylindrical tubular body, and a base portion constructed to form an annular chamber for the entry of the solid particles to be moved up inside the column, said fixing column including a top portion constructed to form an annular chamber for receiving the solid material spilling over from the top of said column and to be discharged therefrom.

7. An installation as defined in claim 6, in which said elution and washing column is the upstream column and said fixing column is the downstream column, and in which said connecting means comprises a first pipe having a valve located between said upstream column and said intermediate tank and through which the solid particles move by gravity from such column to such tank, and a second pipe having a valve between said intermediate tank and the annular chamber at the base-of said fixing column, said second pipe discharging tangentially into such annular chamber.

8. An installation as defined in claim 7, in which said first operative means includes means for rapidly injecting a given volume of liquid under a given pressure into the annular chamber at the base of said elution and washing column, and in which said second operative means includes means for injecting a given volume of liquid under a given pressure into said intermediate tank.

9. An installation as defined in claim 6, in which said fixing column is the upstream column, and said elution and washing column is the downstream column, and in which said connecting means comprises a first pipe having a valve extending from said annular chamber at the top of said fixing column to said intennediate tank. A storage hopper communicating with the annular chamber at the base of said elution and washing column, and a second pipe having a valve extending between said intermediate tank and said storage hopper.

10. An installation as defined in claim 9, including means for washing the solid particles in said intermediate tank by fluidization.

11. An installation as defined in claim 9, in which said storage hopper includes means for detecting when the level of the mass of solid particles therein falls to a given level, and means controlled by said detecting means to effect the operation of said second operative means and thereby cause an additional supply of solid particles to said storage hopper.

12. The method of treating liquids and solid particles in a closed circuit which comprises a substantially vertical tubular fixing column and a substantially vertical tubular elution column separate and spaced from one another, comprising effecting an accurate control of the volume of material passing upwardly through at least one of said columns by accumulating a mass of solid particles in a first chamber communicating with the lower portion of such one treatment column, then rapidly injecting tangentially into such chamber above such mass of solid particles a given volume of liquid under a given pressure to effect a forwardupward movement of a given volume of the material in such one column, said injection of a constant given volume of liquid under constant given pressure being repeated at intermittent intervals to effect an intermittent forward motion of such given volumes of the material in such one column, intermittently collecting batches of the solid particles discharged from the upper portion of such one column for delivery to the other column, and intermittently collecting batches of solid particles discharged from such other column for delivery to the chamber communicating with the lower portion of said one column.

13. The method defined in claim 12, in which said one column is the elution column and the collection and delivery of solid particles therefrom includes the steps of passing a plurality of batches of constant given bulk volume of solid particles from the upper portion of such elution column at periodic intervals to a second chamber for collection thereof and isolating the latter from said fixing column during the period in which such plurality of batches are moving from such elution column to such second chamber, the total volume of such batches in such period not exceeding a set maximum volume smaller than the capacity of the second chamber, and then isolating said second chamber from said elution column and transferring the entire volume of material fed to the second chamber during such period from said second chamber to the fixing column.

14. The method defined in claim 12, in which said one column is the fixing column and the collection and delivery of solid particles therefrom includes the steps of passing a bulk batch of the solid particles from said fixing column to a second chamber located between said columns and connected to but isolated from said elution column during the passage of such bulk batch thereto, treating such bulk batch of solid particles in said second chamber while isolating the latter from both said fixing and elution columns, and then feeding the solid particles treated in said second chamber in small batches of constant given bulk volume to said first chamber communicating with the lower portion of saidelution column.

15. An installation providing a closed circuit for treating liquids and solid particles, comprising a substantially vertically disposed tubular fixing column and a substantially vertically disposed tubular elution column separate and spaced from one another, a tubular casing enclosing the lower portion of at least one of said columns and forming with the latter a tubular chamber for holding a mass of the solid particles, means for rapidly injecting tangentially into such tubular chamber above the mass of particles therein a given volume of liquid under a given pressure to effect a forward upward movement of a given volume of the material in such one column, said injecting means being constructed and arranged to repeat at intermittent intervals the injection of a constant given volume of liquid under constant given pressure to effect an intermittent forward motion of given volumes of the material in said one column, a first chamber located between said columns for intermittently collecting batches of solid particles discharged from such one column for delivery to the other column, and a second chamber located between said columns for intermittently collecting batches of solid particles discharged from the other column for delivery to said tubular chamber.

Claims

2. An installation as defined in claim 1, wherein said at least one of said columns is the elution column, and in which said treated particle feeding means feeds said treated particles into said holding chamber and said liquid impressing means rapidly injects said given volume of the liquid tangentially into such chamber above the mass of particles therein.
3. An installation as defined in claim 1, wherein said at least one of said columns is the fixing column, and in which said periodically operative feeding means feeds each batch of collected solid particles and a given volume of the liquid into such chamber above the mass of particles therein, said feeding means feeding the liquid, at least, tangentially into such chamber.
4. An installation providing a closed circuit for treating liquids and solid particles, comprising a substantially vertically disposed tubular fixing column and a substantially vertically disposed tubular elution column separate and spaced from one another, a tubular casing enclosing the lower portion of said elution column and forming with the latter a tubular chamber for holding a mass of the solid particles, means for rapidly injecting tangentially into such chamber above the mass of particles therein a given volume of liquid under a given pressure to effect a forward upward movement of a given volume of the material in such elution column, said injecting means being constructed and arranged to repeat at intermittent intervals the injection of a constant given volume of liquid under constant given pressure to effect an intermittent forward motion of given volumes of the material in said elution column, first intermediate means located between said columns for intermittently collecting batches of the solid particles discharged from said fixing column and comprising a first particle collection chamber and a second particle collection chamber both located between said tubular holding chamber and said fixing column, means operable to feed intermittently batches of particles from said fixing column to said second collection chamber and from the latter to said first collection chamber, means operable to treat the particles in said second collection chamber in the intervals between such intermittent batch feed thereof, said first collection chamber communicating with said holding chamber at a place positioned above the portion of the mass of particles remaining therein after operation of said injecting means, and constructed and arranged to feed the particles by gravity onto such mass portion, and means for controlling the discharge from such first particle collection chamber and into said holding chamber of a given volume of particles to form the mass of particles required therein prior to each operation of said injecting means, a second intermediate means located between said columns and including means for collecting the solid particles discharged from the upper end of the elution column, and means operative periodically to feed a batch of said collected solid particles and a given volume of liquid into said fixing column.
5. An installation providing a closed circuit for treating liquids and solid particles, comprising a substantially vertically disposed tubular fixing column and a substantially vertically disposed tubular elution column separate and spaced from one another, a tubular casing enclosing the lower portion of said fixing column and forming with the latter a tubular chamber for holding a mass of the solid particles, means for rapidly injecting tangentially into such chamber above the mass of particles therein a given volume of liquid under a given pressure to effect a forward upward movement of a given volume of the material in such fixing column, said injecting means being constructed and arranged to repeat at intermittent intervals the injection of a constant given volume of liquid under constant given pressure to effect an intermittent forward motion of given volumes of the material in said fixing column, and comprising a receiver tank having a solid particle entry port and a solid particle discharge port located intermediate said elution and fixing columns, means for alternately connecting the entry port of said tank to the discharge end of said elution column and the discharge port of said tank to the tubular chamber of said fixing column, first means operative intermittently to cause said elution column to discharge batches of solid particles of given volume into said connecting means and to said tank, and second means operative periodically to cause the transfer of solid particles fed to said intermediate tank to said fixing column as a liquid stream, said first operative means being constructed and arranged to cause said elution column to discharge a plurality of batches of the solid particles to said intermediate tank between each of the operations of said second operative means, said second operative means being constructed and arranged to transfer the entire volume of solid particles in said intermediate tank as a liquid stream in each operation thereof, and means including at least one receiver tank for collecting solid particles discharged from the upper end of said fixing column and feeding them into the lower portion of said elution column.
6. An installation for treating liquids and solid particles comprising an upstream tubularly shaped column providing a chamber for a bed of the solid particles, a downstream tubularly shaped column providing a chamber for a bed of the solid particles, a receiver tank having a solid particle entry port and a solid particle discharge port located intermediate said upstream and downstream columns, means connecting the entry port of said intermediate tank to the discharge end of said upstream column and the discharge port of said intermediate tank to the entry end of said downstream column and including means for isolating one of said intermediate tank ports when the other of its said ports is operative for the passage of solid particles therethrough, first means operative periodically to cause said upstream column to discharge a batch of solid particles of given volume into said connecting means and to said intermediate tank, and second means operative periodically to cause the transfer of solid particles fed to said intermediate tank to said downstream column, one of said upstream and downstream columns being a fixing column and the other being an elution and washing column, and each of such columns including a cylindrical tubular body, and a base portion constructed to form an annular chamber for the entry of the solid particles to be moved up inside the column, said fixing column including a top portion constructed to form an annular chamber for receiving the solid material spilling over from the top of said column and to be discharged therefrom.
7. An installation as defined in claim 6, in which said elution and washing column is the upstream column and said fixing column is the downstream column, and in which said connecting means comprises a first pipe having a valve located between said upstReam column and said intermediate tank and through which the solid particles move by gravity from such column to such tank, and a second pipe having a valve between said intermediate tank and the annular chamber at the base of said fixing column, said second pipe discharging tangentially into such annular chamber.
8. An installation as defined in claim 7, in which said first operative means includes means for rapidly injecting a given volume of liquid under a given pressure into the annular chamber at the base of said elution and washing column, and in which said second operative means includes means for injecting a given volume of liquid under a given pressure into said intermediate tank.
9. An installation as defined in claim 6, in which said fixing column is the upstream column, and said elution and washing column is the downstream column, and in which said connecting means comprises a first pipe having a valve extending from said annular chamber at the top of said fixing column to said intermediate tank, a storage hopper communicating with the annular chamber at the base of said elution and washing column, and a second pipe having a valve extending between said intermediate tank and said storage hopper.
10. An installation as defined in claim 9, including means for washing the solid particles in said intermediate tank by fluidization.
11. An installation as defined in claim 9, in which said storage hopper includes means for detecting when the level of the mass of solid particles therein falls to a given level, and means controlled by said detecting means to effect the operation of said second operative means and thereby cause an additional supply of solid particles to said storage hopper.
12. The method of treating liquids and solid particles in a closed circuit which comprises a substantially vertical tubular fixing column and a substantially vertical tubular elution column separate and spaced from one another, comprising effecting an accurate control of the volume of material passing upwardly through at least one of said columns by accumulating a mass of solid particles in a first chamber communicating with the lower portion of such one treatment column, then rapidly injecting tangentially into such chamber above such mass of solid particles a given volume of liquid under a given pressure to effect a forward upward movement of a given volume of the material in such one column, said injection of a constant given volume of liquid under constant given pressure being repeated at intermittent intervals to effect an intermittent forward motion of such given volumes of the material in such one column, intermittently collecting batches of the solid particles discharged from the upper portion of such one column for delivery to the other column, and intermittently collecting batches of solid particles discharged from such other column for delivery to the chamber communicating with the lower portion of said one column.
13. The method defined in claim 12, in which said one column is the elution column and the collection and delivery of solid particles therefrom includes the steps of passing a plurality of batches of constant given bulk volume of solid particles from the upper portion of such elution column at periodic intervals to a second chamber for collection thereof and isolating the latter from said fixing column during the period in which such plurality of batches are moving from such elution column to such second chamber, the total volume of such batches in such period not exceeding a set maximum volume smaller than the capacity of the second chamber, and then isolating said second chamber from said elution column and transferring the entire volume of material fed to the second chamber during such period from said second chamber to the fixing column.
14. The method defined in claim 12, in which said one column is the fixing column and the collection and delivery of solid particles therefrom includes the steps of passing a bulk batch of the solid particles from said fixing column to a second chamber located between said columns and connected to but isolated from said elution column during the passage of such bulk batch thereto, treating such bulk batch of solid particles in said second chamber while isolating the latter from both said fixing and elution columns, and then feeding the solid particles treated in said second chamber in small batches of constant given bulk volume to said first chamber communicating with the lower portion of said elution column.
15. An installation providing a closed circuit for treating liquids and solid particles, comprising a substantially vertically disposed tubular fixing column and a substantially vertically disposed tubular elution column separate and spaced from one another, a tubular casing enclosing the lower portion of at least one of said columns and forming with the latter a tubular chamber for holding a mass of the solid particles, means for rapidly injecting tangentially into such tubular chamber above the mass of particles therein a given volume of liquid under a given pressure to effect a forward upward movement of a given volume of the material in such one column, said injecting means being constructed and arranged to repeat at intermittent intervals the injection of a constant given volume of liquid under constant given pressure to effect an intermittent forward motion of given volumes of the material in said one column, a first chamber located between said columns for intermittently collecting batches of solid particles discharged from such one column for delivery to the other column, and a second chamber located between said columns for intermittently collecting batches of solid particles discharged from the other column for delivery to said tubular chamber.