LIQUID-LIQUID EXTRACTION DEVICE
20240269580 ยท 2024-08-15
Assignee
Inventors
- Junya OHNO (Tokyo, JP)
- Hideki ISHIZAWA (Tokyo, JP)
- Tomokiyo TAKEYAMA (Tokyo, JP)
- Akiyoshi ODA (Tokyo, JP)
- Hiroaki Takahashi (Tokyo, JP)
- Kouji NAKASHIMA (Tokyo, JP)
- Tadashi NOUMI (Tokyo, JP)
- Tomoya Fujita (Tokyo, JP)
- Mitsuhiro IWAFUNE (Tokyo, JP)
- Takao Suzuki (Tokyo, JP)
Cpc classification
B01D11/0465
PERFORMING OPERATIONS; TRANSPORTING
International classification
Abstract
A multi-tower liquid-liquid extraction apparatus having two or more extraction towers arranged in parallel. Each tower has a heavy-liquid supplying port at the top and a heavy-liquid discharging port at the bottom. Additionally, each tower has a light-liquid supplying port at the bottom and a light-liquid discharging port at the top. The heavy-liquid channels of the extraction towers are connected in series. Furthermore, at least two of the extraction towers are connected to respective diaphragm chambers through their respective piping. These diaphragm chambers have a closed space, part of the wall of which is formed by a diaphragm whose volume is changed by an operating drive section. The piping between each extraction tower and its respective diaphragm chamber is equipped with a pressure-regulating chamber and an on/off valve to regulate the internal pressure.
Claims
1. A multi-tower liquid-liquid extraction apparatus comprising a plurality of extraction towers, n (n being an integer of 2 or more) extraction towers being arranged in parallel; each extraction tower comprising a heavy liquid supply portion on the top side of the tower and a heavy liquid discharge portion on the bottom side of the tower, and, comprising a light liquid supply portion on the bottom side of the tower and a light liquid discharge portion on the top side of the tower; (a) the heavy liquid discharge portion of the first extraction tower of the n extraction towers being connected via piping to the heavy liquid supply portion of the second extraction tower, the heavy liquid discharge portion of the second extraction tower being connected via piping to the heavy liquid supply portion of the third extraction tower, the heavy liquid discharge portion of the (n?1).sup.th extraction tower being connected via piping to the heavy liquid supply portion of the n.sup.th extraction tower, and in this way, heavy liquid channels of the n extraction towers being connected in series, and/or; (b) the light liquid discharge portion of the n.sup.th extraction tower of the n extraction towers being connected to the light liquid supply portion of the (n?1).sup.th extraction tower via piping, the light liquid discharge portion of the (n?1).sup.th extraction tower being connected to the light liquid supply portion of the (n?2).sup.th extraction tower via piping, the light liquid discharge portion of the second extraction tower being connected to the light liquid supply portion of the first extraction tower via piping, and in this way light liquid channels of the n extraction towers being connected in series, and; at least two of these n respective extraction towers being connected to respective diaphragm chambers by respective piping, said diaphragm chambers having a closed space with a portion of its walls formed by a diaphragm, thereby volume of the closed space being changed by operation of a drive section; the piping between each extraction tower and its respective diaphragm chamber being equipped with a pressure-regulating chamber and an on/off valve to adjust the internal pressure.
2. The liquid-liquid extraction apparatus according to claim 1, wherein a modified diaphragm pump is used as the diaphragm chambers, the modified diaphragm pump being formed by removing, from a diaphragm pump driven by electricity or compressed air with two chamber sections in which diaphragms forming walls of each chamber are operated alternately, check valves at inlet and outlet of each chamber, and blocking the outlet for one chamber section and the inlet for the other chamber section by a bulkhead, thereby providing only one liquid flow path to each chamber section, and each chamber section being equipped with a nozzle for degassing, and the piping from the two extraction towers are connected to the improved diaphragm pump, respectively.
3. The liquid-liquid extraction apparatus according to claim 1, wherein the n extraction towers are two extraction towers.
4. The liquid-liquid extraction apparatus according to claim 1, wherein the amplitude of the extraction apparatus is adjustable from the pressure difference between the pressure at any position in the tower and the pressure in the pressure-regulating chamber, which is derived from the average density of the liquid and the height of the liquid level within each extraction tower.
5. The liquid-liquid extraction apparatus according to claim 1, wherein pulsation of said extraction apparatus is carried out in a manner that only one of the towers is pulsated by adjusting the pressure in the pressure adjustment chamber and the on/off valve.
6. The liquid-liquid extraction apparatus according to claim 1, wherein the pulsation of said extraction apparatus is varied in amplitude according to the respective extraction tower by individually adjusting the pressure in the pressure-regulating chamber.
7. The liquid-liquid extraction apparatus according to claim 1, wherein each of said extraction towers has a gas-liquid interface at the top of the tower and is connected to each other through a pressure equalization pipe at the top of the column, and the pressure in the tower is uniform.
8. A liquid-liquid extraction apparatus according to claim 1, wherein the n extraction towers are three or more extraction towers, and the adjacent extraction towers are each with three or more towers, or any two or more towers, connected through piping to the modified diaphragm pump.
Description
BRIEF DESCRIPTION OF THE DRAWING
[0036]
[0037]
MODES FOR CARRYING OUT THE INVENTION
[0038] The invention is described in more detail below according to the embodiments.
[0039]
[0040] The liquid-liquid extraction apparatus of the present invention is a multi-tower liquid-liquid extraction apparatus having a plurality of extraction towers, where n (n is an integer of 2 or more) extraction towers are arranged in parallel.
[0041] In the embodiment shown in
[0042] Because multiple extraction towers are arranged in parallel, even if it is necessary to increase the contact efficiency and residence time between liquids, the height can be lower than that of a single extraction column, making it easy to install in existing facilities.
[0043] In the liquid-liquid extraction apparatus of the present invention, each extraction tower has a heavy liquid supply portion on the top side of the tower and a heavy liquid discharge portion on the bottom side of the tower, and in addition, a light liquid supply portion on the bottom side of the tower and a light liquid discharge portion on the top side of the tower. In the embodiment shown in
[0044] In the liquid-liquid extraction apparatus of the present invention, in order to function as a multi-tower, it is necessary to fulfill: [0045] (a) the heavy liquid discharge portion of the first extraction tower of the n extraction towers is connected via piping to the heavy liquid supply portion of the second extraction tower, the heavy liquid discharge portion of the second extraction tower is connected via piping to the heavy liquid supply portion of the third extraction tower, . . . the heavy liquid discharge portion of the (n?1).sup.th extraction tower is connected via piping to the heavy liquid supply portion of the n.sup.th extraction tower, and in this way, heavy liquid channels of the n extraction towers are connected in series, and/or; [0046] (b) the light liquid discharge portion of the n.sup.th extraction tower of the n extraction towers is connected to the light liquid supply portion of the (n?1).sup.th extraction tower via piping, the light liquid discharge portion of the (n?1).sup.th extraction tower is connected to the light liquid supply portion of the (n?2).sup.th extraction tower via piping, . . . the light liquid discharge portion of the second extraction tower is connected to the light liquid supply portion of the first extraction tower via piping, and in this way the light liquid channels of the n extraction towers are connected in series.
[0047] In the embodiment shown in
[0050] In the embodiment shown in
[0051] In
[0052] Further, in the liquid-liquid extraction apparatus of the present invention, in the aspect of employing one or more towers for positive extraction for component separation, and for back-extraction for separation of extracted substances from an extractant, respectively, the number of extraction towers (n) of said conditions (a) and (b) is set to a value less than that total number (N) with respect to the total number (N) of extraction towers of the liquid-liquid extraction apparatus as a whole, in order to satisfy the heavy-liquid channels and/or the light-liquid channels in the serial connection configuration.
[0053] Moreover, in the liquid-liquid extraction apparatus of the present invention, at least two of these n respective extraction towers 10, 20 are connected via respective piping 42, 52 to respective diaphragm chambers 44, 54 having a closed space with a portion of the walls formed by a diaphragm. The volume of the closed space can be changed by the operation of a drive section.
[0054] The piping 42, 52 between each of the extraction towers 10, 20 and the respective diaphragm chambers 44, 54 is provided with pressure-regulating chambers 46, 56 and on/off valves 48, 58 that can adjust the internal pressure.
[0055] Thus, in one embodiment of the liquid-liquid extraction apparatus of the present invention, the pulsation of said extraction apparatus can pulsate only one of the towers by adjusting the pressure in the pressure-regulating chambers 46 and 56 and the on/off valves 48 and 58, respectively. Alternatively, the pulsation can be applied to each of the extraction towers 10, 20 individually, by adjusting the pressure in the pressure-regulating chambers 46, 56 separately.
[0056] Therefore, in the liquid-liquid extraction apparatus of the present invention, for example, in a system where the difference in specific gravity between light and heavy liquids is small and the liquids tend to mix, the amplitude can be reduced to suppress the flooding phenomenon in which the liquid droplets do not fall or rise. In a system where the difference in specific gravity between light and heavy liquids is large, the amplitude can be increased and the frequency can be increased to suppress the droplets from moving too fast. Thus the scope of the applicable system is wider.
[0057] In addition, in the liquid-liquid extraction apparatus of the present invention, for example, in a system in which the mass transfer rate is large in the first tower 10 is large, the liquid flow rate of the first tower is large compared to that of the second tower 20, and therefore, from the viewpoint of preventing the flooding, it is possible to carry out a correspondence in which the amplitudes of the first and second towers are varied, or in which the amplitude of the first tower only is stopped.
[0058] It should be noted that in the embodiment shown in
[0059] In the liquid-liquid extraction apparatus of the present invention, the diaphragm chambers 44 and 54 that provide pulsation to each of the extraction columns 10 and 20 are not particularly limited as long as they have a closed space whose walls are partially formed by diaphragms and whose volume can be changed by operating a drive unit, as described above, to provide pulsation to each of the extraction towers 10 and 20. The multiple diaphragm chambers 44 and 54 may be independent of each other. In the liquid-liquid extraction system, since the diaphragm chambers as pulsators are installed outside of the extraction columns 10 and 20, maintenance is easy, and since there are no operating parts inside the extraction columns, such as Karr columns and RDCs, it is easy to cope with a malfunction in the event of a malfunction.
[0060] In one preferred embodiment of the liquid-liquid extraction apparatus, as shown in
[0061] As the above-described modified diaphragm pump 60 as the pulsator connected to the two towers used in the preferred embodiment of the liquid-liquid extraction apparatus of the present invention, since the liquids do not mix between the two diaphragm chambers 44 and 54 inside thereof, it is possible to use one or more towers to perform the positive extraction for the separation of the components, and other one or more towers to the back-extraction for the separation of the extracted substances from the extractant, respectively.
[0062] In one embodiment shown in
[0063] In the embodiment in which one diaphragm pump is connected to three or more extraction towers by branching one or both of the two piping 42 and 52 that are connected to the diaphragm pump 60, the pressure-regulating chambers as the chambers 46 and 56 provided in the middle of the piping as shown in
[0064] In the liquid-liquid extraction apparatus of the present invention, multiple piping and valves can be installed by branching off from the diaphragm pump 60 as the pulsator in advance to apply pulsation to the extraction towers. Depending on the system, the position at which the pulsation is applied can be selected arbitrarily by operating the valves, and the amplitude of each pulsation can be controlled as desired.
[0065] In one embodiment of the liquid-liquid extraction apparatus of the present invention shown in
[0066] Furthermore, in one embodiment of the liquid-liquid extraction apparatus of the present invention shown in
Example
[0067] Hereinafter, the present invention is more specifically described based on examples.
[0068]
[0069] In
[0070] A heavy liquid was made up of 20% formic acid as the component to be extracted, 15% inorganic salt as the other component dissolved, and the rest was aqueous medium, while a mixed light liquid was prepared with tributyl phosphate (TBP) as the extractant and n-decane as the diluting solvent of the extractant in the mass ratio (TBP:decane=) 3:1. The density of the heavy liquid was 1190 kg/m.sup.3 and the light liquid was 900 kg/m.sup.3.
[0071] To make the heavy liquid a dispersed phase, shower nozzles 14 and 24 having a nozzle aperture of 1.5 mm in diameter and a number of holes of 10 were used to supply heavy liquid to each of the towers 10 and 20.
[0072] To make the mixture of extractant and diluting solvent a light liquid (continuous phase), nozzles 15 and 25 for liquid supply were provided in the cavity at the bottom of the tower, and the mixture was fed from there and drained from overflow nozzles 16 and 26 at the top of the towers, the outlet of the continuous phase.
[0073] For continuous countercurrent liquid-liquid extraction using two towers, heavy liquid as a dispersed phase was supplied from the first tower (left tower in the
Comparative Example 1: No Pulsation
[0074] The extraction process was performed without running the diaphragm pump. The holdings were pre-loaded into the tower, and data were measured as a steady state when the feed rate of light and heavy liquids reached five times the volume of the column.
[0075] The flow rate of the light liquid was twice the flow rate of the heavy liquid in terms of the mass ratio. As a result, the following composition was obtained.
TABLE-US-00001 TABLE 1 extraction Formic agent + Moisture acid salt diluent compo- compo- compo- compo- Capacity sition sition sition sition kg/h Pre-processed 0 0 0 1.000 200 light liquid Pre-processed 0.65 0.2 0.15 0 100 heavy liquids Post-processed 0.025 0.082 0 0.893 224 light liquids Post-processed 0.781 0.022 0.197 0 76 Heavy Liquid
[0076] The formic acid recovery from the heavy liquid under this condition was 91.8%.
Example 1: With Pulsation Only in the Second Tower
[0077] First, gas was removed from the gas release line of the diaphragm while supplying liquid from the tower into the diaphragm to fill the diaphragm pump 30 with liquid. Then, pulsation was applied to the second tower 20 only. The volume pushed by the diaphragm was 80 ml, and the porosity of the packed bed was 98%. The liquid level moved about 5 cm per beat (amplitude). The frequency was set to 30 Hz, and the other conditions were the same as those of the no-pulsation.
[0078] As a result, the following composition was obtained.
TABLE-US-00002 TABLE 2 extraction Formic agent + Moisture acid salt diluent compo- compo- compo- compo- Capacity sition sition sition sition kg/h Pre-processed 0 0 0 1.000 200 light liquid Pre-processed 0.65 0.2 0.15 0 100 heavy liquids Post-processed 0.025 0.089 0 0.886 225 light liquids Post-processed 0.792 0.008 0.2 0 75 Heavy Liquid
Example 2: First Tower with Pulsation, Same Pulsation Conditions as in Example 1
[0079] Pulsation was also applied to the first tower as well. Other than this, an experiment was conducted under the same conditions as in Example 1. As a result, it was difficult for the heavy liquid to drop to the bottom of the first tower which was the dispersed phase, and a phenomenon of stagnation in the tower (flooding) occurred. This phenomenon was detected by the pressure in the tower. Since the first tower has a supply port for the heavy liquid phase and a supply port from the light liquid phase discharge port of the second tower, the amount of formic acid was increased, and as a result, the flow rate of the liquid to be processed was increased as compared with the second tower, and it was difficult for the heavy liquid as the dispersed phase to drip down due to the effect of pulsation, and the flooding occurred as a result.
Example 3: Pulsation in Both Towers, the Amplitude of the Pulsation Changed to Half
[0080] A damper was used and operated with the amplitude of the conditions in Example 2 set to half (2.5 cm) for both towers, while adjusting the pressure in the damper by the amount of compressed air introduced, and operation was performed. As a result, the following composition was obtained.
TABLE-US-00003 TABLE 3 extraction Formic agent + Moisture acid salt diluent compo- compo- compo- compo- Capacity sition sition sition sition kg/h Pre-processed 0 0 0 1.000 200 light liquid Pre-processed 0.65 0.2 0.15 0 100 heavy liquids Post-processed 0.025 0.088 0 0.887 226 light liquids Post-processed 0.797 0.001 0.202 0 74 Heavy Liquid
[0081] The concentration of formic acid in the post-processed heavy liquid decreased to 0.001 in terms of the mass fraction. Formic acid recovery was 99.6.
DESCRIPTION OF SYMBOLS
[0082] 10, 20: Extraction tower [0083] 12, 22: Packing bed [0084] 14, 24: Shower nozzle [0085] 15, 25: Nozzle [0086] 16, 26: Overflow nozzle [0087] 17, 27: Drain [0088] 44, 54: Diaphragm chamber [0089] 60: Diaphragm pump [0090] 64A, 64B: Bulkhead [0091] 66A, 66B: Gas release nozzle