An automated ion exchange apparatus and automated ion exchange method

Abstract

The application relates to an automatic ion exchange device and an automatic ion exchange method, which comprise a feed bin, a controller, an exchange liquid barrel, a waste liquid tank, an ultrasonic heating tank, multiple groups of variable frequency diaphragm pumps, multiple switching valves, a filter, at least three groups of material tanks, at least three groups of liquid tanks, multiple groups of air inlet / outlet pipes, multiple groups of Y-shaped mixers, multiple groups of spiral pipe exchangers, a collection barrel and a filter screen. The application greatly improves the silver ion exchange rate under the joint action of ultrasonic waves, liquid circulation and heating through automatic control, greatly improves the silver ion exchange ratio through three times of ion exchange and three times of reuse of exchange liquid, maximizes the silver utilization rate, and improves the economic benefits.

Description

Technical Field

[0001] This invention relates to the field of radioactive gaseous effluent purification technology for nuclear facilities, specifically to an automated ion exchange device and an automated ion exchange method. Background Technology

[0002] In the event of a severe accident at a nuclear power plant, such as a core meltdown, a containment filtration and release system (FCVS) is used to filter out and depressurize radioactive materials to prevent excessively high pressure levels of radioactive vapors released into the containment vessel, which could lead to structural damage and uncontrolled release of large amounts of radioactive material. Currently, the mainstream international FCVS primarily uses silver zeolite molecular sieves as adsorbents to remove radioactive organic iodine. Furthermore, large amounts of radioactive organic iodine are also generated during spent fuel reprocessing; in these high-temperature and high-humidity environments, silver zeolite is typically used for organic iodine removal.

[0003] Silver zeolite molecular sieves are primarily loaded with silver ions through solution impregnation and ion exchange. Impregnation suffers from uneven silver ion dispersion within the molecular sieve pores, leading to stacking or pore blockage, resulting in reduced silver utilization and decreased adsorption performance. Ion exchange, on the other hand, allows for uniform silver ion dispersion across the molecular sieve framework, effectively addressing the shortcomings of solution impregnation. However, ion exchange typically suffers from slow exchange rates and low silver utilization, requiring further improvement in terms of economic efficiency and silver ion exchange ratio. This issue becomes particularly pronounced in large-scale production processes.

[0004] Furthermore, in the field of radioactive waste treatment, especially in the treatment of waste containing radioactive iodine, extremely low concentrations of radioactive iodine are usually treated by storage and decay. Large amounts of liquid containing radioactive iodine are generated during the operation of hospitals and nuclear facilities, so the treatment process requires a large storage space and a long decay time. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides an automated ion exchange device and an automated ion exchange method, which only partially solves the problems existing in the prior art.

[0006] To achieve the above objectives, the present invention provides the following technical solution: On one hand, an automated ion exchange device is proposed, comprising: a feed hopper, a controller, an exchange liquid tank, a waste liquid tank, an ultrasonic heating tank, multiple sets of variable frequency diaphragm pumps, several switching valves, a filter, at least three sets of feed tanks, at least three sets of liquid tanks, multiple sets of inlet / outlet pipes, multiple sets of Y-type mixers, multiple sets of spiral tube exchangers, a collection tank, and a filter screen; the feed hopper is connected to the first feed tank via switching valves, each set of Y-type mixers is connected to one set of feed tanks and one set of spiral tube exchangers respectively, and each set of spiral tube exchangers is arranged in the ultrasonic heating tank; each set of liquid tanks forms a closed-loop circulation circuit with the corresponding set of variable frequency diaphragm pumps and the corresponding set of spiral tube exchangers via switching valves, and the filter is connected in series between the liquid tank and the variable frequency diaphragm pump; the inlet / outlet pipes are divided into two sets, one set is installed at the upper end of each liquid tank, and the other set is installed at each feed tank. The upper part; the filter screens are respectively set at the liquid suction pipe terminals near the bottom of each material tank and the liquid suction pipe terminals at the bottom of the collection tank; the controller is electrically connected to the ultrasonic heating tank, each variable frequency diaphragm pump, and each switching valve, and is used to control the ultrasonic frequency and heating temperature of the ultrasonic heating tank, the start and stop and operating frequency of the variable frequency diaphragm pump, and the on / off state of the switching valve; the feeding bin, material tank, liquid tank, collection tank and the pipelines connecting the above components are all made of light-proof material, and the material tank, liquid tank and the pipelines arranged outside the ultrasonic heating tank are wrapped with heat insulation layer.

[0007] As a preferred technical solution, the ultrasonic frequency range of the ultrasonic heating tank is 20 to 100 kHz, including a low frequency band of 20 to 40 kHz and a mixed mid-low frequency band of 40 to 100 kHz.

[0008] As a preferred technical solution, the heating temperature range of the ultrasonic heating bath is 25–85℃.

[0009] As a preferred technical solution, the linear velocity range of the variable frequency diaphragm pump driving the exchange fluid is 0.1m / s to 3m / s.

[0010] As a preferred technical solution, the spiral tube exchanger has an internally smooth, inert tube and an adjustable tilt angle.

[0011] As a preferred technical solution, the bottom of the collection bucket has a conical structure.

[0012] As a preferred technical solution, the ultrasonic heating bath can be selected as either continuous ultrasonic mode or pulsed ultrasonic mode, with the pulse ratio of the pulsed ultrasonic mode being 1:2 to 1:4.

[0013] As a preferred technical solution, the number of material tanks, liquid tanks, Y-type mixers and spiral tube exchangers are all three sets, and the number of switching valves is 22.

[0014] On the other hand, an automated ion exchange method is provided, employing the automated ion exchange apparatus as described above, comprising the following steps: Step 1: The controller controls the opening and closing of the switching valve between the feeding bin and the first feeding trough and the feeding time through the program to feed the first feeding trough in a quantitative manner; Step 2: The controller controls the switching valve at the lower end of the first material tank, the first variable frequency diaphragm pump and the corresponding switching valve to open, so that the molecular sieve in the first material tank is mixed with the exchange liquid in the exchange liquid tank through the first Y-type mixer and enters the first spiral tube exchanger. The controller also controls the operating frequency of the first variable frequency diaphragm pump to suspend the molecular sieve in the first spiral tube exchanger. Step 3: The controller closes and opens the switching valve to form a closed loop circulation between the first liquid tank, the first variable frequency diaphragm pump and the first spiral tube exchanger. At the same time, the controller controls the ultrasonic heating tank to start the ultrasonic function and heating function, and sets the ultrasonic frequency, heating temperature and linear velocity of the exchange liquid to enable the molecular sieve to perform the first ion exchange. Step 4: After the first ion exchange is completed, the controller controls the switching valve to switch, and the molecular sieve in the first spiral tube exchanger is transferred to the second material tank through the first variable frequency diaphragm pump, and the exchange solution is recovered to the first liquid tank. Step 5: Repeat the control logic of steps 2 to 4, and through the second variable frequency diaphragm pump, the second Y-type mixer, the second spiral tube exchanger and the second liquid tank, the molecular sieve in the second material tank and the newly supplied or recovered exchange liquid in the exchange liquid tank undergo a second ion exchange, and the exchange liquid is recovered to the second liquid tank. Step 6: Continue to pass through the third variable frequency diaphragm pump, the third Y-type mixer, the third spiral tube exchanger, and the third liquid tank to allow the molecular sieve to undergo a third ion exchange, and the exchange solution can be reused three times; Step 7: The controller transfers the molecular sieve that has undergone three ion exchanges to the collection tank, and the exchange liquid after three reuses is discharged into the waste liquid tank through the switching valve. Step 8: Steps 1 to 7 above are completed automatically by the controller according to the time sequence, realizing continuous ion exchange.

[0015] As a preferred technical solution, in step 3, when the ultrasound function adopts the pulse ultrasound mode, the pulse ratio is 1:2 to 1:4.

[0016] As a preferred technical solution, in step 2, the exchange liquid is a silver nitrate solution, and in step 3, when the liquid flow rate is too low, the tilt angle of the spiral tube exchanger is adjusted to keep the molecular sieve in the ultrasonic action area.

[0017] As a preferred technical solution, step 7 further includes: washing the molecular sieve in the collection bucket with deionized water multiple times, then vacuum drying and sealing it for storage away from light.

[0018] As a preferred technical solution, in steps 5 and 6, the reuse method of the exchange solution is as follows: fresh exchange solution is used for the third ion exchange, and after the exchange, it is recycled to the second liquid tank for the second ion exchange, and after the second ion exchange, it is recycled to the first liquid tank for the first ion exchange.

[0019] Compared with the prior art, the technical solution of this application has the following beneficial effects: the present invention significantly improves the silver ion exchange rate through automatic control, under the combined action of ultrasound, liquid circulation and heating, and significantly improves the silver ion exchange ratio through three ion exchanges and three reuses of the exchange liquid, while maximizing the silver utilization rate and improving economic benefits. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of an automated ion exchange device provided by the present invention; Figure 2 This is a schematic diagram of an automated ion exchange method provided by the present invention.

[0021] The attached diagrams include the following devices and components: feed hopper (1), controller (2), exchange liquid tank (3), waste liquid tank (4), ultrasonic heating tank (5), variable frequency diaphragm pump (6-1, 6-2, 6-3), switching valve (7-1 to 7-22), filter (8-1, 8-2, 8-3), feed tank (9-1, 9-2, 9-3), liquid tank (10-1, 10-2, 10-3), inlet / outlet pipe (11-1, 11-2, 11-3, 11-4, 11-5, 11-6), Y-type mixer (12-1, 12-2, 12-3), spiral tube exchanger (13-1, 13-2, 13-3), collection tank (14), filter screen (15), etc. Detailed Implementation

[0022] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0023] Please see Figure 1This invention proposes an automated ion exchange device, comprising: a feed bin 1, a controller 2, an exchange liquid tank 3, a waste liquid tank 4, an ultrasonic heating tank 5, multiple sets of variable frequency diaphragm pumps 6-1, 6-2, 6-3, several switching valves 7-1 to 7-22, filters 8-1, 8-2, 8-3, at least three sets of feed tanks 9-1, 9-2, 9-3, at least three sets of liquid tanks 10-1, 10-2, 10-3, multiple sets of inlet / outlet pipes 11-1 to 11-6, multiple sets of Y-type mixers 12-1, 12-2, 12-3, multiple sets of spiral tube exchangers 13-1, 13-2, 13-3, a collection bin 14, and a filter screen 15; the feed bin 1 is connected to the first feed tank 9-1 via switching valve 7-1, each set of Y-type mixers is connected to one set of feed tanks and one set of spiral tube exchangers, and each set of spiral tube exchangers is arranged inside the ultrasonic heating tank 5; each The liquid tanks form a closed-loop circulation circuit with the corresponding variable frequency diaphragm pumps and the corresponding spiral tube exchangers via switching valves. Filters 8-1, 8-2, and 8-3 are connected in series between the liquid tanks and the variable frequency diaphragm pumps. The inlet / outlet pipes are divided into two groups, one group installed at the top of each liquid tank and the other group installed at the top of each material tank. Filter screens 15 are respectively installed at the liquid suction pipe terminals near the bottom of each material tank and at the liquid suction pipe terminals at the bottom of the collection tank 14. The controller 2 is electrically connected to the ultrasonic heating tank 5, each variable frequency diaphragm pump, and each switching valve to control the ultrasonic frequency and heating temperature of the ultrasonic heating tank 5, the start / stop and operating frequency of the variable frequency diaphragm pumps, and the on / off state of the switching valves. The feeding bin 1, material tanks, liquid tanks, collection tank 14, and the pipelines connecting the above components are all made of light-shielding material. The material tanks, liquid tanks, and pipelines arranged outside the ultrasonic heating tank 5 are wrapped with a heat insulation layer.

[0024] Preferably, the ultrasonic frequency range of the ultrasonic heating tank 5 is 20–100 kHz, including a low-frequency band of 20–40 kHz and a mixed mid-low frequency band of 40–100 kHz. An ultrasonic frequency of 20–40 kHz (low-frequency cavitation) or 40–100 kHz (medium-low frequency mixing) is used. The low-frequency band enhances mass transfer at the liquid-solid interface, resulting in a strong cavitation effect. The mid-low frequency cavitation effect is gentler and more uniform, and can effectively reduce adsorbent structural damage. Ultrasound helps with liquid mixing and dispersion, improving mass transfer efficiency, facilitating full contact between the silver nitrate solution and the adsorbent surface, promoting rapid ion migration, and reducing ion exchange time. Furthermore, byproducts and surface impurities are easily removed, improving exchange uniformity. The process can employ continuous ultrasound or pulsed ultrasound (e.g., 1 second operation followed by a 2-second interval, with a pulse ratio of 1:2 or 1:4 to reduce heat accumulation and structural damage). Preferably, the heating temperature range of the ultrasonic heating bath 5 is 25–85°C. Heating can increase Ag... + This improves mobility, reduces solution viscosity, and synergistically enhances ion exchange rates through ultrasonic cavitation. The relatively optimal temperature range is 40-75℃, increasing reaction rates while reducing energy consumption.

[0025] Preferably, the linear velocity range of the exchange liquid driven by the variable frequency diaphragm pump is 0.1 m / s to 3 m / s. That is, the solid-liquid contact rate: the linear velocity of the silver nitrate solution is 0.1 m / s to 3 m / s. Low flow rate helps silver ions to fully contact the adsorption medium, while high flow rate can enhance mass transfer. Preferably, a contact rate of 0.2 m / s to 1 m / s can be used.

[0026] For zeolite molecular sieves with different concentrations, silica-to-alumina ratios, and particle sizes, an optimized combination of ultrasonic frequency, heating temperature, and solid-liquid contact rate can be used to achieve the best process path for silver ion exchange. This reduces structural damage and wear to the zeolite molecular sieves, saves energy, and achieves efficient silver ion exchange within a short period of time.

[0027] Preferred, usable parameter combinations include: 60-80kHz ultrasonic frequency, 1:2 pulse time ratio, 60-75℃ temperature range, and 0.5-0.8m / s liquid velocity.

[0028] When the liquid flow rate is too low, the tilt angle of the spiral exchanger can be changed to ensure that the molecular sieve is located inside the spiral exchanger and achieves efficient ion exchange at the corresponding ultrasonic position.

[0029] Preferably, the spiral tube exchanger has an internally smooth, inert conduit and an adjustable tilt angle.

[0030] Preferably, the bottom of the collection bucket 14 has a conical structure.

[0031] Preferably, the ultrasonic heating bath 5 can be selected as either continuous ultrasonic mode or pulsed ultrasonic mode, with the pulse ratio of the pulsed ultrasonic mode being 1:2 to 1:4.

[0032] Preferably, there are three sets of material tanks, liquid tanks, Y-type mixers and spiral tube exchangers, and 22 switching valves.

[0033] Please see Figure 2 The present invention proposes an automated ion exchange method, employing the automated ion exchange device described above, comprising the following steps: Step 1: The controller 2 controls the opening and closing of the switching valve 7-1 between the feeding bin 1 and the first material trough 9-1 and the feeding duration through the program, and feeds the first material trough 9-1 in a quantitative manner; Step 2: Controller 2 controls the switching valve 7-2 at the lower end of the first material tank 9-1, the first variable frequency diaphragm pump 6-1 and the corresponding switching valves 7-5 and 7-9 to open, so that the molecular sieve in the first material tank 9-1 is mixed with the exchange liquid in the exchange liquid tank 3 through the first Y-type mixer 12-1 and enters the first spiral tube exchanger 13-1. The controller 2 also controls the operating frequency of the first variable frequency diaphragm pump 6-1 to keep the molecular sieve suspended in the first spiral tube exchanger 13-1. Step 3: Controller 2 closes switching valve 7-5 and opens switching valve 7-8, so that the first liquid tank 10-1, the first variable frequency diaphragm pump 6-1 and the first spiral tube exchanger 13-1 form a closed loop circulation. At the same time, it controls the ultrasonic heating tank 5 to start the ultrasonic function and heating function, and sets the ultrasonic frequency, heating temperature and linear velocity of the exchange liquid, so that the molecular sieve can perform the first ion exchange. Step 4: After the first ion exchange is completed, the controller 2 controls the switching valve to switch, and the molecular sieve in the first spiral tube exchanger 13-1 is transferred to the second material tank 9-2 through the first variable frequency diaphragm pump 6-1, and the exchange liquid is recovered to the first liquid tank 10-1; Step 5: Repeat the control logic of steps 2 to 4. Through the second variable frequency diaphragm pump 6-2, the second Y-type mixer 12-2, the second spiral tube exchanger 13-2 and the second liquid tank 10-2, the molecular sieve in the second material tank 9-2 and the new or recycled exchange liquid in the exchange liquid tank 3 undergo a second ion exchange. The exchange liquid is then recycled to the second liquid tank 10-2. Step 6: Continue to use the third variable frequency diaphragm pump 6-3, the third Y-type mixer 12-3, the third spiral tube exchanger 13-3 and the third liquid tank 10-3 to make the molecular sieve undergo a third ion exchange, and the exchange liquid can be reused three times; Step 7: Controller 2 controls the transfer of the molecular sieve that has completed three ion exchanges to the collection tank 14. The exchange liquid after three reuses is discharged into the waste liquid tank 4 through the switching valve 7-22. Step 8: Steps 1 to 7 above are automatically completed by controller 2 according to the time sequence to realize continuous ion exchange.

[0034] Preferably, in step 3, when the ultrasound function uses pulse ultrasound mode, the pulse ratio is 1:2 to 1:4.

[0035] Preferably, in step 2, the exchange liquid is a silver nitrate solution, and in step 3, when the liquid flow rate is too low, the tilt angle of the spiral tube exchanger is adjusted to keep the molecular sieve in the ultrasonic action area.

[0036] Preferably, after step 7, the process further includes: washing the molecular sieve in the collection bucket 14 multiple times with deionized water, then vacuum drying and sealing it for storage away from light.

[0037] Preferably, in steps 5 to 6, the reuse method of the exchange solution is as follows: fresh exchange solution is used for the third ion exchange, and after the exchange, it is recycled to the second liquid tank 10-2 for the second ion exchange, and after the second ion exchange, it is recycled to the first liquid tank 10-1 for the first ion exchange.

[0038] The specific implementation process of this invention is as follows: The controller 2 program controls the opening and closing of the valve 7-1 connecting the feeding bin 1 and the material tank 9-1, as well as the feeding duration, to quantitatively feed the material tank 9-1. The ion exchange process is as follows: The switching valve 7-2 at the lower end of the material tank 9-1 is opened, and the molecular sieve in the material tank 9-1 automatically flows out to the Y-type mixer 12-1 under gravity. Switching valves 7-5 and 7-9 are opened (the other switching valves are closed by default), and the diaphragm pump 6-1 draws the ion exchange liquid (such as a silver nitrate solution of a certain concentration) from the exchange liquid tank 3 into the Y-type mixer 12-1, carrying the molecular sieve into the flow path and into the spiral tube exchanger 13-1. The diaphragm pump, by setting a reasonable frequency (corresponding to the liquid flow rate), ensures that the gravity and buoyancy of the molecular sieve are approximately the same, causing the molecular sieve to suspend within the spiral tube exchanger. The liquid flowing out of the spiral tube exchanger enters the liquid tank 10-1. After all the molecular sieve in tank 9-1 enters the spiral exchanger, switching valve 7-2 is closed (the controller automatically controls the valve's on / off state by setting a time period equal to the required feeding duration). The controller program controls the on / off state of switching valve 7-5 and the frequency and running time of diaphragm pump 6-1 to control the volume of the initial ion exchange liquid. After the liquid feeding is complete, switching valve 7-5 is closed, and switching valve 7-8 is opened. Diaphragm pump 6-1 draws liquid from tank 10-1, keeping the molecular sieve in suspension. Simultaneously, the ultrasonic frequency and frequency combination mode of ultrasonic heating tank 5, as well as the liquid heating temperature, are set to ensure the molecular sieve rapidly completes ion exchange within the spiral exchanger at a reasonable liquid-solid contact rate, ultrasonic frequency, and liquid temperature. A particle filter 8-1 is installed in the flow path between tank 10-1 and diaphragm pump 6-1. Liquid exiting the spiral exchanger passes through the particle filter and is then circulated back into the spiral exchanger by the diaphragm pump. By setting a reasonable ion exchange duration, the exchanged ions complete the initial ion exchange within the spiral exchanger.

[0039] After the initial ion exchange in the spiral tube exchanger 13-1, the flow path is switched again (7-10 is opened, 7-9 is closed), and the frequency (liquid flow rate) of the diaphragm pump 6-1 is set. The molecular sieve in the spiral tube exchanger 13-1 is transferred into the feed tank 9-2 via a high-flow-rate carrier. Gas in the feed tank 9-2 is discharged through the inlet / outlet pipe 11-5 to maintain pressure balance in the loop. After the molecular sieve transfer is complete, the flow path is switched again (7-10 is closed, 7-11 and 7-9 are opened, other switching valves are closed by default). The diaphragm pump 6-1 is turned on to transfer the liquid in the feed tank 9-2 to the liquid tank 10-1 through a suction pipe with a filter screen located near the bottom of the feed tank. The loop connection between the feed tank 9-2 and the diaphragm pump 6-1 is disconnected (7-11 is closed). The feed tank 9-1 is refilled, and then the diaphragm pump 6-1 draws liquid from the liquid tank 10-1 to begin the first ion exchange of the next batch of molecular sieves (7-8 and 7-9 are opened to form a loop).

[0040] After the initial ion exchange of the adsorption medium (molecular sieve) is transferred to the feed tank 9-2 and the liquid transfer is complete (transferred to the liquid tank 10-1), switching valves 7-6, 7-13, and switching valve 7-3 at the lower end of feed tank 9-2 are opened. Diaphragm pump 6-2 is started and its frequency (corresponding to the liquid flow rate / flow rate) is set. Diaphragm pump 6-2 draws the exchange liquid (a silver nitrate solution of a certain concentration) from the exchange liquid tank 3 and carries the molecular sieve from feed tank 9-2 into Y-type mixer 12-2 into spiral tube exchanger 13-2. The liquid flows into liquid tank 10-2. After diaphragm pump 6-2 draws the exchange liquid to the set volume (achieved by setting the pump frequency to determine the extraction rate and extraction time), the flow path is switched (switching valve 7-6 is closed, switching valve 7-12 is opened). Similarly, the molecular sieve in spiral tube exchanger 13-2 undergoes ion exchange under ultrasonic suspension. By setting a reasonable duration using the controller, the silver nitrate liquid in liquid tank 10-2 undergoes ion exchange with the molecular sieve in spiral tube exchanger 13-2 under circulation.

[0041] After the molecular sieve in the spiral tube exchanger 13-2 completes ion exchange, the flow path is switched again (switching valve 7-13 is closed, switching valve 7-14 is opened), and the frequency (corresponding flow rate) of diaphragm pump 6-2 is set. A high flow rate is used to transfer the molecular sieve from spiral tube exchanger 13-2 into material tank 9-3. After the transfer is complete, the flow path is switched again (switching valves 7-15 and 7-13 are opened, switching valves 7-20, 7-12, and 7-14 are closed), and diaphragm pump 6-2 is turned on to transfer the liquid in material tank 9-3 into liquid tank 10-2. After the liquid transfer is complete, switching valve 7-15 is closed, disconnecting the circuit between material tank 9-3 and diaphragm pump 6-2. Simultaneously, the flow rate of diaphragm pump 6-1 is set, and a high flow rate is used to transfer the molecular sieve from spiral tube exchanger 13-1 into material tank 9-2. The liquid after secondary use is returned to liquid tank 10-1 to prepare for the third ion exchange.

[0042] As above, open switching valves 7-7, 7-17, and switching valve 7-4 at the lower end of material tank 9-3. Turn on diaphragm pump 6-3 and set its flow rate. Diaphragm pump 6-3 draws exchange liquid from exchange liquid tank 3, and the carrier slides down from material tank 9-3 onto the molecular sieve in Y-type mixer 12-3, entering spiral tube exchanger 13-3. The first batch of molecular sieves begins its third ion exchange in spiral tube exchanger 13-3. Material tank 9-1 is refilled. Simultaneously, diaphragm pump 6-1 draws liquid (third use) from liquid tank 10-1 to begin the first ion exchange of the next batch of molecular sieves, and diaphragm pump 6-2 draws liquid (second use) from liquid tank 10-2 to begin the second ion exchange with the molecular sieve in material tank 9-2. Diaphragm pump 6-1, spiral tube exchanger 13-1, and liquid tank 10-1 form a closed-loop cycle. Diaphragm pump 6-2, spiral heat exchanger 13-2, and liquid tank 10-2 form a closed loop. Diaphragm pump 6-3, spiral heat exchanger 13-3, and liquid tank 10-3 form a closed loop.

[0043] After the molecular sieve in tank 9-1 undergoes three ion exchanges successively through spiral tube exchangers 13-1, 13-2, and 13-3, it is collected into molecular sieve collection tank 14 under the high-flow-rate transport of diaphragm pump 6-3. Simultaneously, the molecular sieve that has completed its second ion exchange in spiral tube exchanger 13-2 is transferred into tank 9-3 under the high-flow-rate transport of diaphragm pump 6-2, while the molecular sieve that has completed its first ion exchange in spiral tube exchanger 13-1 is transferred into tank 9-2 under the high-flow-rate transport of diaphragm pump 6-1. The residual liquid from the three ion exchanges in tank 9-2 is transferred to liquid tank 10-1 and then discharged into waste liquid tank 4 (by opening switching valve 7-22). The first round of ion exchange is complete.

[0044] After the first round of ion exchange, the fourth batch of molecular sieves entering tank 9-1, along with the solution transferred to tank 9-3 for the second use (the solution in tank 9-3 is transferred to liquid tank 10-1 via diaphragm pump 6-1), begins the first round of ion exchange in spiral tube exchanger 13-1. The flow path switching method is as follows: open switching valves 7-21 and 7-9, close switching valves 7-15, 7-14, 7-11, 7-10, 7-8, and 7-22, and start diaphragm pump 6-1 to draw the liquid from tank 9-3 through a filter screen into liquid tank 10-1. Then, close switching valve 7-21 and open switching valves 7-8 and 7-9, allowing diaphragm pump 6-1 to draw the liquid from liquid tank 10-1, carrying it to the molecular sieve in Y-type mixer 12-1, and then transferring it to spiral exchanger 13-1. Diaphragm pump 6-1, spiral tube exchanger 13-1, and liquid tank 10-1 form a closed-loop cycle, initiating a new round of ion exchange.

[0045] The third batch of molecular sieve entering the feed tank 9-2, along with the solution transferred to the molecular sieve collection tank 14 (transferred to the liquid tank 10-2 via diaphragm pump 6-2), begins the second ion exchange in the spiral tube exchanger 13-2. The flow path switching method is as follows: Open switching valves 7-19 and 7-13, close switching valves 7-20, 7-15, 7-14, and 7-12, and start diaphragm pump 6-2 to draw the liquid from the collection tank through filter screen 16 into the liquid tank 10-2. Then, close switching valve 7-19 and open switching valves 7-12 and 7-3. Diaphragm pump 6-2 draws the liquid from the liquid tank 10-2, carrying it into the Y-type mixer 12-2, where it is transferred to the spiral exchanger 13-2. Diaphragm pump 6-2, spiral tube exchanger 13-2, and liquid tank 10-2 form a closed-loop cycle, initiating a new round of ion exchange.

[0046] After one cycle, the proportion of silver ions in the molecular sieve gradually increases and approaches its maximum after three ion exchanges. As the molecular sieve exchange process progresses, the concentration of silver ions in the subsequent liquid tank is higher than that in the previous tank. In the next cycle, the molecular sieve in tank 9-1 first exchanges with the silver ions transferred to tank 9-3 (transferred to liquid tank 10-1 via diaphragm pump 6-1), then exchanges with the silver ions transferred to collection tank 14 after being transferred to tank 9-2 (transferred to liquid tank 10-2 via diaphragm pump 6-2), and finally exchanges with the fresh silver ion solution after being transferred to tank 9-3.

[0047] In the subsequent cycle, the fresh ion exchange solution undergoes a third ion exchange with the molecular sieve that has already undergone two ion exchanges in the spiral tube exchanger 13-3. After the exchange, the liquid is transferred through collection tank 14 to liquid tank 10-2 and undergoes a second ion exchange with the molecular sieve that has undergone one ion exchange in the spiral tube exchanger 13-2. The exchange solution after secondary use is transferred through material tank 9-3 to liquid tank 10-1 and undergoes its first ion exchange with the molecular sieve that entered initially in the spiral tube exchanger 13-1. The exchange solution after three uses is transferred through material tank 9-2 to liquid tank 10-1 and then discharged to waste liquid tank 4. Through three cycles, the silver ion solution achieves maximum utilization and minimizes the silver ion concentration in the residual liquid. Through three ion exchanges, the molecular sieve not only improves the utilization rate of silver ions in the solution but also maximizes the number of silver active sites.

[0048] Through the above cycle, the new molecular sieve continuously, rapidly, and efficiently completes ion exchange under automatic control and is collected in a collection tank.

[0049] After ion exchange, the molecular sieves are washed multiple times with deionized water, then vacuum dried, sealed, and stored away from light for later use.

[0050] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. An automated ion exchange device, characterized in that, include: Feeding bin (1), controller (2), exchange liquid tank (3), waste liquid tank (4), ultrasonic heating tank (5), multiple sets of variable frequency diaphragm pumps (6-1, 6-2, 6-3), several switching valves (7-1 to 7-22), filters (8-1, 8-2, 8-3), at least three sets of material tanks (9-1, 9-2, 9-3), at least three sets of liquid tanks (10-1, 10-2, 10-3), multiple sets of inlet / outlet pipes (11-1 to 11-6), and more The system includes a set of Y-type mixers (12-1, 12-2, 12-3), multiple sets of spiral tube exchangers (13-1, 13-2, 13-3), a collection tank (14), and a filter screen (15). The feeding hopper (1) is connected to the first material tank (9-1) via a switching valve (7-1). Each set of Y-type mixers is connected to a set of material tanks and a set of spiral tube exchangers. Each set of spiral tube exchangers is arranged in the ultrasonic heating tank (5). Each set of liquid... The tank forms a closed-loop circulation circuit with the corresponding set of variable frequency diaphragm pumps and the corresponding set of spiral tube exchangers through the switching valve. The filters (8-1, 8-2, 8-3) are connected in series between the liquid tank and the variable frequency diaphragm pump. The inlet / outlet pipes are divided into two groups, one set is installed at the top of each liquid tank and the other set is installed at the top of each material tank. The filter screen (15) is respectively set at the liquid suction pipe terminal near the bottom of each material tank and the liquid suction pipe terminal at the bottom of the collection tank (14). The controller (2) is electrically connected to the ultrasonic heating tank (5), each variable frequency diaphragm pump and each switching valve, and is used to control the ultrasonic frequency and heating temperature of the ultrasonic heating tank (5), the start and stop and operating frequency of the variable frequency diaphragm pump, and the on / off state of the switching valve. The feeding bin (1), material tank, liquid tank, collection tank (14) and the pipeline connecting each component are all made of light-shielding material. The material tank, liquid tank and the pipeline arranged outside the ultrasonic heating tank (5) are wrapped with a heat insulation layer.

2. The automated ion exchange device according to claim 1, characterized in that, The ultrasonic heating tank (5) has an ultrasonic frequency range of 20 to 100 kHz, including a low frequency band of 20 to 40 kHz and a mixed mid-low frequency band of 40 to 100 kHz.

3. The automated ion exchange device according to claim 1, characterized in that, The heating temperature range of the ultrasonic heating bath (5) is 25 to 85°C.

4. The automated ion exchange device according to claim 1, characterized in that, The linear velocity range of the variable frequency diaphragm pump driving the exchange fluid is 0.1 m / s to 3 m / s.

5. The automated ion exchange apparatus according to claim 1, characterized in that, The spiral tube exchanger has an internally smooth, inert tube and its tilt angle is adjustable.

6. The automated ion exchange apparatus according to claim 1, characterized in that, The bottom of the collection bucket (14) has a conical structure.

7. The automated ion exchange apparatus according to claim 1, characterized in that, The ultrasonic heating tank (5) can be selected as either continuous ultrasonic mode or pulsed ultrasonic mode, and the pulse ratio of the pulsed ultrasonic mode is 1:2 to 1:

4.

8. The automated ion exchange apparatus according to claim 1, characterized in that, The number of material tanks, liquid tanks, Y-type mixers and spiral tube exchangers are all three sets, and the number of switching valves is 22.

9. An automated ion exchange method, characterized in that, The automated ion exchange apparatus according to any one of claims 1 to 8 comprises the following steps: Step 1: The controller (2) controls the opening and closing of the switching valve (7-1) between the feeding bin (1) and the first material trough (9-1) and the feeding duration through the program, and feeds the first material trough (9-1) in a quantitative manner; Step 2: The controller (2) controls the switching valve (7-2), the first variable frequency diaphragm pump (6-1), and the corresponding switching valves (7-5, 7-9) at the lower end of the first material tank (9-1) to open, so that the molecular sieve in the first material tank (9-1) is mixed with the exchange liquid in the exchange liquid tank (3) through the first Y-type mixer (12-1) and enters the first spiral tube exchanger (13-1), and controls the operating frequency of the first variable frequency diaphragm pump (6-1) to make the molecular sieve suspend in the first spiral tube exchanger (13-1); Step 3: The controller (2) closes the switching valve (7-5) and opens the switching valve (7-8) to make the first liquid tank (10-1), the first variable frequency diaphragm pump (6-1) and the first spiral tube exchanger (13-1) form a closed loop. At the same time, the controller controls the ultrasonic heating tank (5) to start the ultrasonic function and heating function, and sets the ultrasonic frequency, heating temperature and linear velocity of the exchange liquid to make the molecular sieve perform the first ion exchange. Step 4: After the first ion exchange is completed, the controller (2) controls the switching valve to switch and transfers the molecular sieve in the first spiral tube exchanger (13-1) to the second material tank (9-2) through the first variable frequency diaphragm pump (6-1), and the exchange liquid is recovered to the first liquid tank (10-1). Step 5: Repeat the control logic of steps 2 to 4, and use the second variable frequency diaphragm pump (6-2), the second Y-type mixer (12-2), the second spiral tube exchanger (13-2) and the second liquid tank (10-2) to make the molecular sieve in the second material tank (9-2) and the exchange liquid tank (3) perform a second ion exchange with the new supply exchange liquid or the recovered exchange liquid. The exchange liquid is then recovered to the second liquid tank (10-2). Step 6: Continue to use the third variable frequency diaphragm pump (6-3), the third Y-type mixer (12-3), the third spiral tube exchanger (13-3), and the third liquid tank (10-3) to make the molecular sieve undergo a third ion exchange, and the exchange liquid can be reused three times; Step 7: The controller (2) controls the transfer of the molecular sieve that has completed three ion exchanges to the collection tank (14), and the exchange liquid after three reuses is discharged into the waste liquid tank (4) through the switching valve (7-22). Step 8: Steps 1 to 7 above are automatically completed by the controller (2) in a time sequence to realize continuous ion exchange.

10. The automated ion exchange method according to claim 9, characterized in that, In step 3, when the ultrasound function adopts the pulse ultrasound mode, the pulse ratio is 1:2 to 1:

4.

11. The automated ion exchange method according to claim 9, characterized in that, In step 2, the exchange liquid is a silver nitrate solution. In step 3, when the liquid flow rate is too low, the tilt angle of the spiral tube exchanger is adjusted to keep the molecular sieve in the ultrasonic action area.

12. The automated ion exchange method according to claim 9, characterized in that, Step 7 is followed by: washing the molecular sieve in the collection bucket (14) with deionized water multiple times, then vacuum drying and sealing it to protect it from light.

13. The automated ion exchange method according to claim 9, characterized in that, In step 6, the reuse method of the exchange solution is as follows: fresh exchange solution is used for the third ion exchange, and after the exchange, it is recycled to the second liquid tank (10-2) for the second ion exchange, and after the second ion exchange, it is recycled to the first liquid tank (10-1) for the first ion exchange.

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