DE2263912A1 - CONTINUOUS ION EXCHANGE PROCESS AND DEVICE FOR IT - Google Patents

Description

Patent attorney Dipl.-Phys. Gerhard Lied I 8 Munich 22 Steinsdorfstr. 21-22 Tel. 29 84

B 5917

Robert Ramptοη Porter
1415 Federal Way, Salt Lake City, United States of America

Rossinn Uranium Limited

13th Floor, Unicorn House, 70 Marsha / Street, Johannesburg, Transvaal, Republic of South Africa

Continuous ion exchange process and Vorricht clothes

this .

The present invention relates to a continuous ion exchange process and an apparatus therefor. One of the-

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like method and apparatus are used, for example, in the Extraction of mineral components from a solution that contains such components, e.g. from an Auslaur », - IfJ dissolving or removing unwanted minerals that are dissolved in a liquid, e.g. in hydration of hard water by removing calcium ions from it.

The treatment of solutions by exchanging clay is currently being used to a large extent both for the extraction of minerals as well as used to soften water. Conventional systems often require pressure vessels as ion exchange containers in which the solution through a fixed bed of clay exchange material, e.g. mineral zeolite, or synthetic ion exchange resin, is pressed. A disadvantage of the fixed bed system is that the solution must be clarified before it is introduced into the pressure tank because solids in the solution tend to clog the bed of ion exchange material. In the usual Systems require an interruption in the flow of solution to allow periodic regeneration of the ion exchange material. Continuous systems have already been proposed however, they were very expensive to manufacture and difficult to operate because of the ion exchange material continuously or at intervals from the adsorption columns had to be removed ^ in order to either carry out a further exchange of ions with a continuously flowing pipe.

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lead or for the purpose of leaching and regeneration.

The method according to the invention for extracting ions from a liquid solution is characterized in that the solution is successively introduced into and through each clay exchange container a series of two or more vessels, each containing an adsorption column of ion exchange material, the loaded adsorption column removed from the first container of the series, then the removed adsorption column by the relatively The little loaded adsorption column from the second container of the series is replaced while the solution is continuously flows and the same for each subsequent container of the The adsorption column carries out the series in the order in which it is carried out Replaced from the last container of the holiday by practically unloaded ion exchange material, continuously the treated one Solution is drawn off from the last container of the series and continuously circulates during the treatment period repeated.

The solution treated in this way flows from the last container in the series for use, for example in the case of softened water, or for waste or reuse in the case of an empty Lc ¹ solution from which a rich mineral has been extracted by the ion exchange material.

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_BATH

-k-

The adsorption column in the first container in the series can be removed in a discontinuous manner. This can include removing the entire column at once or, more preferably, removing the ion exchange material is continuously withdrawn, e.g. during a certain period of time with the help of an air lift. Then the adsorption column from the second container in the series to the first container in a similar manner, and so on one after the other from container to container as it switches in series if the following containers are present in the particular series under consideration. Regardless of it like that Removal or transport of the adsorption columns is carried out, an adsorption column becomes practically complete removed or transported from its ion exchange container before it is replaced by the subsequent adsorption column. The last adsorption column in the series is replaced with fresh or regenerated ion exchange material, usually the latter by eluted material from the first adsorption column.

The sequence is performed continuously in cycles during any given operating period of the method. Everyone Circulation is preferably automatic in timed sequences under the control of suitable instruments carried out, e.g. with the help of an automatic. Sequence valve

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tils, through which compressed air is alternately supplied to air lifts that are connected to the Tonenaausduschbeh'1.1tern.

Both anionic .ils can also be used in the adsorption columns cationic material used. In this case it will accomplished removal from the first container with a double air lift. The bottom of one is exactly above the interface of the two materials in the column and the bottom of the other at the base of the column.

The elution of the ion exchange material from the first column for circulation through the system as regenerated material is preferably carried out in one or more} .luier \ n ^ ^>i.h'M tsrn, which may or may not take place in a residence kettle. The introduction of regenerated ion exchange material into the last ion exchange vessel in the series from the elution vessel or vessels can be accomplished by pumping from one to the other in the form of a slurry. The pump is started and stopped manually as required. On the other hand, it can also be under the automatic control of suitable timing devices which are correlated in their operation with the automatic sequence valve which controls the operation of the air lifts. In order to avoid equilibrium errors in the systems, which arise from the fact that it is difficult to transport the ionic

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309828 / 08A7

austau3Chmateria] s of a Rehalter /.urn another of the Sv ^

precisely set, it is a possible, but significant feature of the invention that an excess of the ion exchange material is present either in the first Tonenaustaur.chbeh / JLter of the 'series or in the retention container, if one is present, or in both such containers, ur.d that the riuierun ^ sbehälter or the containers are conventional Festbettionenaustausch- container. These precautions in the system establish Z <Mhlunp, s or monitoring devices by which the amount of ion exchange material in any given approach from such
Material sent to the last ion exchange tank in the series can be kept constant. In this context, it will be desirable to use a visual level indicator on the residence tank , if the control is manual
or a level control instrumentation, if the control is carried out automatically.

The invention is illustrated by the following drawings
The method and the device are explained in more detail for this purpose.

Figure 1 is a vertical axial section view of a
Ion exchange tank containing an adsorption column,
which can expand upwards. Such containers are
typical of the type of ion exchange container used for the
Invention methods can be used.

OFUGJNAL INSPECTED

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«.7 -

Figure 2 is a horizontal section along line 2-2 of Figure 1.

Figure 3 is a top view.

Figure H is a schematic showing a complete ion exchange treatment system zeip, t, which is on a series of ion exchange vessels is constructed. The successive figures are indicated. A preferred one is included Arrangement of the elution and elution control apparatus. The figure is in the state where the adsorption column . «From the first ion exchange container in the elution container is to be eluted. The adsorption column from the second ion exchange tank in the series has replaced the

What au «de» «r ^ th ion exchange tank to the elution tank was transported.

FIG. 5 is a view corresponding to that of FIG. 1, however in fragments and shows a moment when both anionic as well as cationic exchange material is used. In this arrangement, each ion exchange container 10 is the Systems, which is shown in Figure U, open at the top and is about an inlet pipe 11, see Figure 1, with the solution to be treated delivers. This inlet pipe is connected via a coupling 12 connected to a distribution head 13, the branches 13a

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which are equipped with downwardly directed lens spray nozzles 13b, the flow of the solution n ^e f! ^en let the bottom 10a of the container flow out.

The solution injected in this way rises vigorously through an adsorption column IU of a suitable ion exchange material, e.g. a synthetic resin that is capable of exchanging ions with ions to swap out of the solution to be removed. The adsorption column is not blocked off at the top. She is free to move upwards under the influence of the ascending solution im Expand container. The height of the container is sufficiently greater than the height of the adsorption column so that essentially only a clear solution at the top of the container overflows into a duct 15, from where it flows through a pipe 16 by gravity flows to the bottom of the next container in the series. Tube 16 is like tube 11 with the coupling piece 1? of such connected to the next boiler and serves as an inflow pipe to deliver the solution.

The solution flows continuously from a source into the first ion exchange tank of the series and then alternately into and from subsequent ion exchange containers of the series, a total of S of such containers being in series, as shown in FIG. 4 and as indicated by the appended numbers 1-5. The completely treated solution becomes continuous withdrawn through the flue pipe 17 for use,

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e.g. in the case of softened water or for reuse or to waste in cases of Lftsun [* en, the dissolved Contains ions of usable metals, e.g. uranium. A trap 18 for the ion exchange material accidentally is carried along by the outflowing solution, if desired in the flue pipe 1? built-in"

In the present system, the ion exchange material _t loaded with ions extracted from the flowing solution is periodically removed from the adsorption column IM from the first (No. 1) ion extraction container of the series with the aid of an air lift 19, which has its inlet 19a at the bottom of the column immediately above the bottom 10 a C. ~, z Kf-ii Lc. This air lift extends to the top of a residence container 20 which forms part of the elution devices. In a similar manner, alternately less loaded ion exchange material is removed from the adsorption columns of the subsequent ion exchange containers with the aid of corresponding air lifts 21 and transported to the next following ion exchange containers through the open tops of the same.

Although at once each adsorption column of the ion exchange tank be able to be removed and transported, be it manually or mechanically, e.g. through the use of suitable Baskets in the cauldrons that hold the corresponding pillars and

309828/084 7 BAD-OWGiNM.

Suitable mechanisms for lifting and trapping such baskets will include the use of air lifts to progressively move the ion exchange material over each one Adsorption column preferred. As it is shown here, can Air for such air lifts in succession from suitable sources Via dit corresponding inlet pipes 22 and under the control of an automatic sequence valve 23 are fed. Each ion exchange vessel 10 is preferably provided with a central immersion pipe 2 * * through which the ion exchange material is conveyed Help of the air lifts is supplied to the overflowing Lflsunc to avoid.

The elution devices of the present case include a single elution container 25 in the form of a fixed bed ion exchange container which can be of conventional construction and which is adapted to receive the loaded ion exchange material from the residence container 20 by controlling the valve 26. The elution vessel 25 has the usual device 27 for the inflow of the eluate, 28 for the inflow of wash water and material transporting water, 29 for the outflow of the eluate, 30 for the outflow of the wash water and 31 for the discharge, as well as 32 for the river of the regenerated ion exchange material in the open head of the last ion exchange container in the series. Separate time counting devices in the usual design are provided for οie elution devices, as shown in Figure ** .

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Ee is a feature of the present invention, that the monitoring of the system and that the maintenance of the file weight with regard to the amount of ion exchange material in each adsorption column in the elution devices is achieved in which an excess of ion exchange material 33, see Figure 4, in the retention tank 20 or if such a retention tank is not available in the system, it is provided in the first ion exchange tank of the system in order to compensate for any deficiency in the adsorption column that was transported .

If the elution devices are operated manually , as already mentioned, a visual level indicator is provided on the holding tank. If, on the other hand, work is carried out automatically, then a stand control instrumentation is available.

The system can be used for the use of both cationic and anionic ion exchange materials in the corresponding adsorption columns IH. The cationic material 3 * occupies approximately half of the adsorption column 14 in the ion exchange container 10, as is shown in FIG. 5, while the anionic material 35 occupies approximately the upper half of these adsorption columns. The usual air lift 19 normally ends at the foot of the column. An additional air lift 36 is provided at the boundary layer

ORKaINAL INSPECTED

ends between the cationic and anionic material in the column.

30902 8/08

Claims (1)

-43- Claims DaP 1) A process for the extraction of ions from a liquid solution, characterized in that _t is continuously the solution successively into and through Ionenau jam se hbehri It it a series of two or more containers leitet-, each initially includes a Adsorptionssaule of ion exchange material, loaded adsorption column removed from the first container of the series, then the removed adsorption column replaced by the relatively lightly loaded adsorption column from the leading container of the series, while the solution flows continuously, the same for each of the subsequent containers of the series alternately carries out the Adsorpiionsschu '. a of the last container in the series is replaced by essentially unloaded ion exchange material, the treated solution is continuously withdrawn from the last container in the series and the cycle is continuously repeated while the process is being carried out. 2) The method according to claim 1, characterized in that the loaded adsorption column is brought from the first container to elute in an elution container with a fixed bed and the resulting _; passes essentially uncharged ion exchange material into the last ion exchange vessel in the series. 2263312 3) Method according to claim 1 or 2, characterized in that that the loaded adsorption column is removed from the first container first in a retention tank and then in the Elution container » U) Method according to claim 3, characterized in that one starts with ion exchange material in the adsorption column, slide transported out of the ar3tan ion exchange container becomes ,, in the Verwail container by excess material that is in iatztaren, compensates. i) Method according to the continuing claims, characterized thereby, that there is any lack of ion exchange material in the Adacrptionasäule, which zuπ from the second container arst-sn container is transported in the arstsn container with überüasijjaa material that contained int the second container is, auaglaicht. 6) Process according to the preceding claims 2 to 5, thereby being able to use the resultant, essentially ionic acid material in the last ion exchange d ^ s » Sari * at the same time during the removal of the unb * lad * non Adaiw ^ isionaaauls from de * t aritar. Ion exchange path *. * - copy BATH 7) Method according to the preceding claims, characterized in that the Fatfernung and the transport of the Adsorptionssäulan from the containers is carried out by progressively removing the ion exchange material from the foot of the corresponding columns through a guide upwards that extends upwards through the column extends ₅ whereby air under pressure is introduced into the lower part of such a guide. 8) Method according to the preceding claims, characterized in that the adsorption column made of ion exchange material is kept free in each of the ion exchange containers and flows through the solution ₃ dia upwards through this , is expanded to oban . 9) Device for the continuous extraction of ions from a liquid solution, characterized by a series of ion exchange containers, each initially containing an adsorption column of ion exchange material, an inlet at the bottom of the adsorption column of the first container of the series for the continuous introduction of the to be treated Solution, an outlet at the top of the adsorption column of the last container in the series for the continuous withdrawal of the treated solution, a flow guide for each container of the 3-sria, the last one extending from the head of the COPY Adsorption column extends from this container to the foot of the adnorptive column of the next container in the series, so that the solution is continuously forwarded. TuH. which can flow one adsorption column to the top of this Sc ¹ JuIe and then '/.urr foot of the next following adsorption column, devices in connection with the first container of the series for removing the adsorption column therefrom, devices in connection with each of the following containers in the series for the transport of the adsorption column of this container to the next container of the series, devices for the replacement of the adsorption column of the last container of the series with essentially unloaded ion exchange material and devices for the operation of the removal devices, the transport devices and the replacement devices, 10) The method according to claim 9, characterized by additional 'devices for eluting the loaded adsorption column, which was removed from the first container of the series and for introducing the eluted ion exchange material therefrom into the last container in the series to replace the adsorption column that was removed from it. 11) The method according to claim 10, that the Eluierun ^ svorrichtungen consist of at least one ion exchange container with a fixed bed and that the adsorption column of the first ion COPY S917 226397? exchange container of the series an '"' excess of ton exchange material to measure material and the system to monitor in the elution devices, 12) device ^ / according to claims 10 or ll ^ e characterizes by elution devices consisting of at least one Ion exchange tanks with a fixed bed consist of a retention tank, which is suitable to be supplied to any ion exchange container and by an excess of ion exchange material in the holding tank to measure the material and monitor the system. 13) Device according to claims 9 to 12, characterized in that daft the ion exchange material in the corresponding adsorption columns both from anion material and from Cation material and the devices for removing the adsorption column from the first container of the device series for the selective and separate removal of both the anion material and the cation material. 14) Device according to claim 13, characterized in that the devices for selective and separate removal both the anion material as well as the cation material contain relevant air lifts, the entrance to a of which exactly above the size; £ r> depends on the two materials BADOFSiGfNAL 2/6391? is located in the p. and the entrance to the other of which lies exactly above the container foot, 15) Device according to claims 9 to 14, characterized in that daft the devices for operating the removal devices, the transport devices and the Substitute devices are capable of sequentially timed the various specified devices To operate sequences so that when a container of ion exchange material is empty that proportionately little loaded ion exchange material from the next container in the series of containers transported to this and essentially unloaded ion exchange material finally into the last empty container of the series of Containers is introduced. 16) Device according to claims 9 to 15, characterized in that daft the devices for operating the distance, Transport and replacement devices are suitable, the removal and transport devices successively in timed sequences and the replacement devices to operate at the same time as the removal devices. 17) Device according to claims 9 to 15, characterized _{59l7 BATHROOM} ORIGINAL 3 0 9 8 2 R / J 3 \ Ί -I'd- ' indicates that the devices for removing the adsorption columns from the first container of the series and the devices for transporting the adsorption columns from column to column are air lifts. 1 8 The apparatus of claim 17, characterized in that the means for operating the distance-, the transport and the L'rsatzvorrichtungen an automatic sequence valve for controlling the Preßluftflußes include the air lifts, 19) A method for the extraction of ions from a liquid solution, which is characterized in that it contains in wesent union what has been described with reference to the drawings , 20) Device for the continuous extraction of ions from a liquid solution, characterized in that it contains essentially what has been described with reference to the drawings ., 21) Product of the method or the device according to the preceding claims. 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