Water pollution treatment apparatus and method for extracting lithium from alpha-spodumene

Abstract

The application provides a water pollution treatment equipment and a method for extracting lithium from alpha-spodumene. It relates to the field of water pollution treatment, and the water pollution treatment equipment comprises a collecting mechanism arranged on the ground, wherein the collecting mechanism comprises a collecting tank and a collecting pump, and the collecting tank is arranged on the ground. The water pollution treatment equipment provided by the application can effectively recover valuable lithium carbonate by filtering the sewage after three times of washing through a filter screen, drying the lithium carbonate precipitate on the filter screen, improving the resource utilization rate, and feeding the filtrate into the collecting tank, starting the collecting motor to stir and mix, and then feeding the sewage into a treatment tank through the collecting pump, and then adding dilute sulfuric acid into the treatment tank through a peristaltic pump to perform a neutralization reaction, so that the carbonate is converted into water and carbon dioxide, the pH is reduced, the alkaline wastewater is converted into a harmless sodium sulfate solution through the neutralization reaction, the risk of alkaline pollution of the wastewater to the environment is eliminated, the wastewater can be discharged up to the standard, and environmental pollution is avoided.

Description

Technical Field

[0001] This invention relates to the field of water pollution treatment, and more particularly to a water pollution treatment device and a method for extracting lithium from α-spodumene. Background Technology

[0002] In the process of extracting lithium from α-spodumene After sedimentation, the material is washed with deionized water, generating wastewater. Direct discharge of this wastewater can lead to water pollution, as the metal precipitates are difficult to degrade and pose a serious threat to the ecological environment and human health. Currently, mainstream wastewater treatment technologies include physical, chemical, and biological methods. Lithium, as a strategic key metal, holds an irreplaceable position in new energy, energy storage, and high-end manufacturing. Alpha-spodumene is one of the world's major sources of lithium ore, with a high theoretical lithium oxide grade, making it a primary raw material for lithium extraction from ore.

[0003] In existing water pollution treatment equipment, deionized water undergoes three washes to become wastewater during the treatment of washing wastewater. This wastewater is collected after the three washes and discharged into the treatment tank, where an acidic solution is added for neutralization. Once the wastewater meets the standards, it is discharged.

[0004] However, existing water pollution treatment equipment, when collecting wastewater from the third washing process, contains... If sedimentation is directly followed up with further processing, it will lead to material waste. Precipitation can affect subsequent processing steps.

[0005] Therefore, it is necessary to provide a water pollution treatment device and a method for extracting lithium from α-spodumene to solve the above-mentioned technical problems. Summary of the Invention

[0006] This invention provides a water pollution treatment device and a method for extracting lithium from α-spodumene, solving the problem of lithium content in washing wastewater. If sedimentation is directly followed up with further processing, it will lead to material waste. The problem of sedimentation affecting subsequent processing steps.

[0007] To solve the above-mentioned technical problems, the present invention provides a water pollution treatment device, comprising: a collection mechanism installed on the ground, the collection mechanism including: a collection tank and a collection pump, the collection tank being installed on the ground, a collection motor being fixedly installed on the top of the collection tank, the output shaft of the collection motor being fixedly connected to a collection shaft, the bottom end of the collection shaft penetrating through the top of the collection tank and extending into the interior, a collection blade being fixedly installed on the bottom end of the collection shaft, an input pipe being connected to the input end of the collection pump, one end of the input pipe penetrating through one side of the collection tank and extending into the interior, and a collection pipe being connected to the output end of the collection pump;

[0008] A funnel, which is connected to the top of the collection tank, and a filter screen is fixedly installed on the inner wall of the funnel;

[0009] A processing mechanism, which is connected to the end of the collection tube;

[0010] A dosing mechanism for adding an acidic solution into the interior of the processing unit.

[0011] Preferably, the processing mechanism includes a processing tank and a processing pump. The processing tank is connected to the end of the collection pipe and is located on the ground. A top cover is fixedly installed on the top of the processing tank, and a bottom cover is fixedly installed on the bottom of the processing tank. The processing pump is located on the ground, and the input end of the processing pump is connected to the bottom of the bottom cover through a connecting pipe. The output end of the processing pump is connected to the processing pipe.

[0012] Preferably, the dosing mechanism is fixedly installed on the top of the top cover. The dosing mechanism includes a peristaltic pump, which is fixedly installed on the top of the top cover by a bracket. The input end of the peristaltic pump is connected to a sulfuric acid tank through an extraction pipe. The sulfuric acid tank is located on the ground. The output end of the peristaltic pump is connected to a dosing pipe, and the bottom end of the dosing pipe penetrates the top of the top cover and extends into the interior of the treatment tank.

[0013] Preferably, a drive mechanism is fixedly installed on the top of the top cover. The drive mechanism includes a cylinder, which is fixedly installed on the top of the top cover. The output shaft of the cylinder passes through the top of the top cover and extends into the interior of the processing tank. A drive motor is fixedly connected to the bottom end of the cylinder output shaft. A drive shaft is fixedly connected to the output shaft of the drive motor. A mixing blade is fixedly installed on the surface of the drive shaft. A baffle is fixedly installed on the surface of the drive shaft through four support plates. The baffle is adapted to the processing tank. A baffle is fixedly installed on the top of each of the four support plates through four connecting columns. A drive ball is fixedly installed on the surface of one of the connecting columns.

[0014] Preferably, the top of the top cover is connected to an aeration mechanism, the aeration mechanism includes a return air pipe, the return air pipe is connected to the top of the top cover, the end of the return air pipe passes through the bottom of the bottom cover and extends into the interior of the treatment tank, the end of the return air pipe is connected to a distribution air pipe, and the surface of the distribution air pipe is connected to a plurality of aeration discs.

[0015] Preferably, a switch is fixedly installed on the inner wall of the treatment tank by a support column, the switch is adapted to the drive ball, the first baffle is adapted to the collection pipe, and the second baffle is adapted to the return gas pipe.

[0016] Preferably, the top of the top cover is connected to an exhaust valve, and a pH meter is fixedly installed on the inner wall of the treatment tank.

[0017] Preferably, the end of the treatment pipe is connected to a coagulation and sedimentation mechanism, which includes a coagulation tank connected to the end of the treatment pipe. The coagulation tank is located on the ground, and PAC pipes and PAM pipes are fixedly installed on the inner wall of the coagulation tank via brackets. A coagulation motor is fixedly installed on the inner wall of the coagulation tank via brackets, and the output shaft of the coagulation motor is fixedly connected to a coagulation shaft. A coagulation blade is fixedly installed at the bottom end of the coagulation shaft. A transfer pump is connected to one side of the coagulation tank via a connecting pipe. A transfer pump is installed on the ground, and the output end of the transfer pump is connected to an inclined plate sedimentation tank through a transfer pipe. The inclined plate sedimentation tank is installed on the ground by a support, and several inclined plates are fixedly installed on the inner wall of the inclined plate sedimentation tank. Three sludge discharge hoppers are connected to the bottom of the inclined plate sedimentation tank. Each of the three sludge discharge hoppers is equipped with a sludge discharge pipe. One end of each of the three sludge discharge pipes passes through the inner wall of the three sludge discharge hoppers and extends to the outside. A water-retaining weir is fixedly installed on the inner wall of the inclined plate sedimentation tank, and a drainage pipe is connected to one side of the inclined plate sedimentation tank.

[0018] A method for extracting lithium from α-spodumene includes the following steps:

[0019] S1: Take a certain amount of standard α-spodumene, add it to a spherical grinding tank, and grind it at a certain speed and according to a certain ball-to-material mass ratio for 30 minutes. Pass the powder through a 200-mesh sieve, collect the fine powder, weigh a certain amount of sodium hydroxide, and dissolve it in deionized water to prepare a solution of a certain concentration. The solution is prepared by weighing calcium oxide according to a specific mass ratio of calcium oxide to ore.

[0020] S2: First, the airtightness of the high-pressure reactor is tested. Then, according to a certain solid-liquid ratio of ore / sodium hydroxide solution, the sodium hydroxide solution, ore and calcium oxide are mixed and added to the reactor for reaction. The heating furnace is heated to 250°C at a certain heating rate. Stirring is turned on at 300 rpm and kept at this temperature for 6 hours. After naturally cooling to room temperature, the mixture is transferred to centrifuge tubes and centrifuged at 8000 rpm for 10 minutes. The supernatant is collected as the alkali-soluble filtrate and the precipitate is collected as calcium silicate residue. A certain amount of deionized water is added, and the mixture is shaken and centrifuged again at 8000 rpm for 5 minutes. The washing liquid is added to the filtrate. The pH of the washing liquid is tested to be approximately 12. If the pH is greater than 12, the washing is repeated to ensure the recovery of sodium hydroxide for reuse.

[0021] S3: Based on the filtrate The content, according to a certain A certain amount of sodium phosphate dodecahydrate was weighed out and dissolved in deionized water to prepare a solution. The filtrate was transferred to a beaker, heated to 65°C in a water bath, and stirred. The solution was then added dropwise using a peristaltic pump at a certain flow rate. After adding the solution dropwise, continue stirring for 2 hours and monitor the pH: the final reaction pH should be approximately 9. If the pH is less than 9, add more solution. Centrifuge at 8000 rpm for 10 minutes and collect. The precipitate and supernatant are recycled liquids. The supernatant contains... pH≈12, add deionized water and continue shaking and centrifuging, centrifuge at 8000 rpm for 5 minutes, the washing liquid is added to the circulating liquid, and after the circulating liquid passes the test, it is transferred to S2 for reuse;

[0022] S4: According to a certain Measure out the appropriate amount of sulfuric acid and dilute it to 50%. ,Will Transfer the precipitate to a beaker, and slowly add the diluted solution dropwise in a fume hood. Stir until no bubbles appear, then stir at room temperature for 1 hour. If incomplete dissolution occurs, heat and stir in a 40°C water bath. Filter and collect the colorless, transparent solution containing... The clear liquid was concentrated by rotary evaporation to... To reach a certain concentration;

[0023] S5: Pretreatment of the anion and cation membranes, immersing the cation membrane in 1 mol / L... In a 60°C water bath, stir for 2 hours, rinse with deionized water until pH=7, and then immerse the anion exchange membrane in a 1mol / L solution. Stir in a 60°C water bath for 2 hours, then rinse with deionized water until pH=7.

[0024] S6: Assemble the electrodialysis unit and adjust the membrane orientation: the "+" side of the cation exchange membrane should face the cathode, and the "-" side of the anion exchange membrane should face the anode. Membrane stack assembly: first assemble the anode chamber, then assemble the anion exchange membrane, then assemble the intermediate chamber for feed, then assemble the cation exchange membrane, and finally assemble the cathode chamber. The gasket thickness is 0.5 mm. Electrode solution preparation: add a certain amount of 0.1 mol / L to the anode chamber. Add deionized water to the cathode chamber and add water containing [unclear text - likely a substance or ingredient] to the intermediate chamber. The catholy solution was subjected to electrodialysis with an electric current applied, and the initial current was recorded. The catholy solution was measured every 2 hours. , Concentration, when Stop operation when the concentration is <0.1g / L;

[0025] S7: First prepare 20% The solution was transferred from the catholyte to a beaker, placed in an 80°C water bath, and magnetically stirred at 150 rpm. The mixture was then stirred according to a specific... The solution is added dropwise at a certain rate using a burette. Monitor pH: The endpoint pH ≈ 10; if pH < 10, add more. After the addition is complete, stir for 1 hour to produce a white substance. The precipitate was centrifuged at 8000 rpm for 10 minutes, and the precipitate was collected. It was washed three times with deionized water at 80°C. The washing liquid was transferred to a water pollution treatment facility for further treatment until it met discharge standards. The precipitate was transferred to a weighing bottle and dried in a vacuum drying oven at 40°C to obtain lithium carbonate. .

[0026] Preferably, in S1, the ball-to-material mass ratio is 5:1, the grinding speed is 300 rpm, and the calcium oxide / ore mass ratio is 0.2:1-0.8:1; in S2, the sodium hydroxide solution concentration is 400 g / L, the sodium hydroxide solution / ore liquid-to-solid ratio is 5-9 mL / g, and the heating furnace heating rate is 5 °C / min; in S3... The ratio is 1:3-2:3, the peristaltic pump flow rate is 1 mL / min, and the standard for the circulating solution is: when ammonium molybdate is added to the circulating solution, no yellow precipitate is formed, which proves... Excess ≤5%; a certain amount of S4 The ratio is 2:3, added drop by drop. The flow rate is 1 drop / second, concentrated Concentration reached In S5, the cation and anion membranes are Nafion N117 as the cation membrane and Selemion AMV as the anion membrane; in S6, the electrodialysis device has a membrane area of ​​10... Two pairs of films, titanium-coated ruthenium anode + 316L cathode, constant voltage of 3.5V, for 20 hours; a certain amount of S7... The ratio is 1:2 to 1.5:2, and the solution is added dropwise using a burette. The solution flow rate is 1 drop / second, and the standard for passing the washing with deionized water three times is... ≤0.1g / L.

[0027] Compared with related technologies, the water pollution treatment equipment provided by the present invention has the following beneficial effects:

[0028] This invention provides a water pollution treatment device that filters wastewater after three washings through a filter screen, recovers lithium carbonate precipitate on the screen, and dries it, effectively recovering valuable lithium carbonate and improving resource utilization. The filtrate enters a collection tank, where a collection motor is started to stir and mix it. The wastewater is then transported to a treatment tank by a collection pump, where a peristaltic pump adds dilute sulfuric acid to the treatment tank for a neutralization reaction. This converts carbonate ions into water and carbon dioxide, lowers the pH, and simultaneously converts the alkaline wastewater into a harmless sodium sulfate solution, eliminating the risk of alkaline pollution to the environment and achieving compliant discharge, thus avoiding environmental pollution. Attached Figure Description

[0029] Figure 1 A schematic diagram of a preferred embodiment of a water pollution treatment device provided by the present invention;

[0030] Figure 2 for Figure 1 The diagram shows the structure of the collection mechanism.

[0031] Figure 3 for Figure 1 The diagram shows the installation of the filter screen;

[0032] Figure 4 for Figure 1 The diagram shows the structure of the processing mechanism.

[0033] Figure 5 for Figure 1 The diagram shown is a structural schematic of the dosing mechanism.

[0034] Figure 6 A schematic diagram of the structure of a second embodiment of a water pollution treatment device;

[0035] Figure 7 for Figure 6 The diagram shows the installation of the drive mechanism;

[0036] Figure 8 for Figure 7 The diagram shows the structure of the drive mechanism.

[0037] Figure 9 for Figure 7 The diagram shown is a structural schematic of the aeration mechanism.

[0038] Figure 10 for Figure 6 The diagram shown is a structural schematic of the coagulation and sedimentation mechanism.

[0039] Figure 11 for Figure 10 Another schematic diagram of the coagulation and sedimentation mechanism shown;

[0040] Figure 12 This is a process flow diagram of a method for extracting lithium from α-spodumene.

[0041] Numbered in the diagram: 1. Collection mechanism; 101. Collection tank; 102. Collection motor; 103. Collection shaft; 104. Collection blade; 105. Collection pump; 106. Input pipe; 107. Collection pipe; 2. Funnel; 3. Filter screen; 4. Processing mechanism; 401. Processing tank; 402. Top cover; 403. Bottom cover; 404. Processing pump; 405. Processing pipe; 5. Dosing mechanism; 501. Peristaltic pump; 502. Extraction pipe; 503. Sulfuric acid tank; 504. Dosing pipe; 6. Drive mechanism; 601. Cylinder; 602. Drive motor; 603. Drive shaft; 604. Mixing blade; 605. Baffle 1 606. Connecting column; 607. Baffle II; 608. Drive ball; 609. Support plate; 7. Aeration mechanism; 701. Return air pipe; 702. Air distribution pipe; 703. Aeration disc; 8. Coagulation sedimentation mechanism; 801. Coagulation tank; 802. PAC pipe; 803. PAM pipe; 804. Coagulation motor; 805. Coagulation shaft; 806. Coagulation blade; 807. Transfer pump; 808. Transfer pipe; 809. Inclined plate sedimentation tank; 810. Inclined plate; 811. Sludge hopper; 812. Sludge pipe; 813. Weir; 814. Drainage pipe; 9. Air vent valve; 10. pH meter; 11. Switch. Detailed Implementation

[0042] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0043] First Embodiment

[0044] Please refer to the following: Figures 1-5 A water pollution treatment device includes: a collection mechanism 1 installed on the ground, the collection mechanism 1 including: a collection tank 101 and a collection pump 105. The collection tank 101 is installed on the ground, a collection motor 102 is fixedly installed on the top of the collection tank 101, the output shaft of the collection motor 102 is fixedly connected to a collection shaft 103, the bottom end of the collection shaft 103 passes through the top of the collection tank 101 and extends into the interior, a collection blade 104 is fixedly installed on the bottom end of the collection shaft 103, the input end of the collection pump 105 is connected to an input pipe 106, one end of the input pipe 106 passes through one side of the collection tank 101 and extends into the interior, and the output end of the collection pump 105 is connected to a collection pipe 107.

[0045] Funnel 2, which is connected to the top of the collection tank 101, and a filter screen 3 is fixedly installed on the inner wall of the funnel 2;

[0046] Processing mechanism 4, which is connected to the end of the collection tube 107;

[0047] The dosing mechanism 5 is used to add an acidic solution into the interior of the processing unit 4.

[0048] The processing mechanism 4 includes a processing tank 401 and a processing pump 404. The processing tank 401 is connected to the end of the collection pipe 107. The processing tank 401 is set on the ground. A top cover 402 is fixedly installed on the top of the processing tank 401, and a bottom cover 403 is fixedly installed on the bottom of the processing tank 401. The processing pump 404 is set on the ground. The input end of the processing pump 404 is connected to the bottom of the bottom cover 403 through a connecting pipe, and the output end of the processing pump 404 is connected to a processing pipe 405.

[0049] The dosing mechanism 5 is fixedly installed on the top of the top cover 402. The dosing mechanism 5 includes a peristaltic pump 501, which is fixedly installed on the top of the top cover 402 by a bracket. The input end of the peristaltic pump 501 is connected to a sulfuric acid tank 503 through an extraction pipe 502. The sulfuric acid tank 503 is located on the ground. The output end of the peristaltic pump 501 is connected to a dosing pipe 504. The bottom end of the dosing pipe 504 penetrates the top of the top cover 402 and extends into the interior of the treatment tank 401.

[0050] In actual use, the solution inside the sulfuric acid tank 503 is a dilute sulfuric acid solution; the filter screen 3 is replaced manually periodically.

[0051] The working principle of the water pollution treatment equipment provided by this invention is as follows:

[0052] First, the wastewater after three washings is recovered through funnel 2. After passing through funnel 2 and filter screen 3, the wastewater enters the collection tank 101. The precipitate is filtered above filter screen 3, recovered, and then dried to obtain lithium carbonate. .

[0053] Then, after the sewage enters the collection tank 101, the collection motor 102 is started and the collection shaft 103 drives the collection blades 104 to mix the sewage from the three washing processes in the collection tank 101. Then the collection pump 105 is started to draw out the sewage through the input pipe 106 and discharge it into the treatment tank 401 through the collection pipe 107.

[0054] Then, the peristaltic pump 501 is activated to draw dilute sulfuric acid from inside the sulfuric acid tank 503 through the extraction pipe 502, and then drips it into the treatment tank 401 through the dosing pipe 504 to carry out a neutralization reaction, lower the pH, and simultaneously... The carbonate ions in the solution are converted into water and carbon dioxide, and the neutralized wastewater is... It is an inorganic salt solution and can be discharged directly.

[0055] Finally, after the treatment is completed, the treatment pump 404 is started to extract the inorganic salt solution and discharge it through the treatment pipe 405.

[0056] Compared with related technologies, the water pollution treatment equipment provided by the present invention has the following beneficial effects:

[0057] By filtering the wastewater after three washings through filter screen 3, the lithium carbonate precipitate on filter screen 3 is recovered and dried, effectively recovering valuable lithium carbonate and improving resource utilization. The filtrate enters collection tank 101, and collection motor 102 is started to stir and mix it. Then, collection pump 105 transports the wastewater to treatment tank 401. Dilute sulfuric acid is then added to treatment tank 401 by peristaltic pump 501 to carry out a neutralization reaction, converting carbonate ions into water and carbon dioxide, lowering the pH, and converting alkaline wastewater into harmless sodium sulfate solution through the neutralization reaction. This eliminates the risk of alkaline pollution to the environment from the wastewater, achieves standard discharge, and avoids environmental pollution.

[0058] Second Embodiment

[0059] Please refer to the following: Figures 6-11 Based on the water pollution treatment device provided in the first embodiment of this application, the second embodiment of this application proposes another water pollution treatment device. The second embodiment is merely a preferred embodiment of the first embodiment, and the implementation of the second embodiment will not affect the separate implementation of the first embodiment.

[0060] Specifically, the water pollution treatment device provided in the second embodiment of this application differs in that a drive mechanism 6 is fixedly installed on the top of the top cover 402. The drive mechanism 6 includes a cylinder 601, which is fixedly installed on the top of the top cover 402. The output shaft of the cylinder 601 passes through the top of the top cover 402 and extends into the interior of the treatment tank 401. A drive motor 602 is fixedly connected to the bottom end of the output shaft of the cylinder 601. A drive shaft 603 is fixedly connected to the output shaft of the drive motor 602. A mixing blade 604 is fixedly installed on the surface of the drive shaft 603. A baffle 605 is fixedly installed on the surface of the drive shaft 603 through four support plates 609. The baffle 605 is adapted to the treatment tank 401. A baffle 607 is fixedly installed on the top of each of the four support plates 609 through four connecting columns 606. A drive ball 608 is fixedly installed on the surface of one of the connecting columns 606.

[0061] The top of the top cover 402 is connected to an aeration mechanism 7, which includes a return air pipe 701. The return air pipe 701 is connected to the top of the top cover 402, and the end of the return air pipe 701 passes through the bottom of the bottom cover 403 and extends into the interior of the treatment tank 401. The end of the return air pipe 701 is connected to a distribution air pipe 702, and the surface of the distribution air pipe 702 is connected to a plurality of aeration discs 703.

[0062] A switch 11 is fixedly installed on the inner wall of the treatment tank 401 by a support column. The switch 11 is adapted to the drive ball 608. The first baffle 605 is adapted to the collection pipe 107 and the second baffle 607 is adapted to the return gas pipe 701.

[0063] The top of the top cover 402 is connected to an exhaust valve 9, and a pH meter 10 is fixedly installed on the inner wall of the treatment tank 401.

[0064] The end of the treatment pipe 405 is connected to a coagulation and sedimentation mechanism 8, which includes a coagulation tank 801. The coagulation tank 801 is connected to the end of the treatment pipe 405 and is located on the ground. A PAC pipe 802 and a PAM pipe 803 are fixedly installed on the inner wall of the coagulation tank 801 via supports. A coagulation motor 804 is fixedly installed on the inner wall of the coagulation tank 801 via supports. The output shaft of the coagulation motor 804 is fixedly connected to a coagulation shaft 805. A coagulation blade 806 is fixedly installed at the bottom end of the coagulation shaft 805. One side of the coagulation tank 801 is connected to a transfer pump 807 via a connecting pipe. Pump 807 is installed on the ground. The output end of the transfer pump 807 is connected to an inclined plate sedimentation tank 809 through a transfer pipe 808. The inclined plate sedimentation tank 809 is installed on the ground by a bracket. Several inclined plates 810 are fixedly installed on the inner wall of the inclined plate sedimentation tank 809. Three sludge discharge hoppers 811 are connected to the bottom of the inclined plate sedimentation tank 809. Each of the three sludge discharge hoppers 811 is provided with a sludge discharge pipe 812. One end of each of the three sludge discharge pipes 812 passes through the inner wall of the three sludge discharge hoppers 811 and extends to the outside. A water-retaining weir 813 is fixedly installed on the inner wall of the inclined plate sedimentation tank 809. A drain pipe 814 is connected to one side of the inclined plate sedimentation tank 809.

[0065] In actual use, the baffle 605 is slidably installed with the processing tank 401.

[0066] The working principle of the water pollution treatment equipment provided in this embodiment is as follows:

[0067] First, after the sewage is discharged into the treatment tank 401 through the collection pipe 107, the start cylinder 601 drives the drive motor 602 to descend. At this time, the first baffle 605, which descends with the drive motor 602, blocks the outlet of the collection pipe 107. Similarly, the second baffle 607, which descends with the drive motor 602, opens the passage of the return air pipe 701. After descending, the drive ball 608 and the switch 11 are at the same horizontal height, and at the same time, the mixing blade 604 enters the depth of the sewage.

[0068] Then, the drive motor 602 is started. At this time, the drive motor 602 drives the drive shaft 603 to rotate, which in turn drives the connecting column 606 to rotate. As the drive ball 608 rotates, it continuously contacts the switch 11 and turns on the peristaltic pump 501 to add dilute sulfuric acid. At the same time, the mixing blade 604 stirs the dilute sulfuric acid and sewage simultaneously. In the early stage, the addition is slow and the stirring speed is also slow to ensure the acid is dispersed and avoid excessive local acid concentration. Carbon dioxide gas is generated at the same time. In the middle stage of the reaction, the addition speed is gradually reduced and the stirring speed is also reduced. A large number of fine bubbles of carbon dioxide gas are evenly emitted, achieving the effect of matching the drop rate of dilute sulfuric acid with the stirring speed. Finally, the addition of dilute sulfuric acid is stopped, and the cylinder 601 is driven to rise. At this time, the baffle 605 is still in the position of blocking the outlet of the collection pipe 107. Stirring continues for 15 minutes and then stops and resets.

[0069] Meanwhile, during the stirring process, baffle 2 607 opens the passage of return gas pipe 701, and baffle 1 605 blocks the outlet of collection pipe 107. Carbon dioxide gas is discharged from return gas pipe 701 and then re-enters the interior of sewage through gas distribution pipe 702 and aeration disc 703, and fully mixes the sewage with acid and alkali. The gas pressure drives the liquid circulation, realizing fully automatic stirring from bottom to top, while also preventing carbon dioxide gas from returning from collection pipe 107.

[0070] Then, the pH is monitored in real time by the pH meter 10 during the treatment process, and excess carbon dioxide gas is discharged through the exhaust valve 9 after the treatment is completed. Excess carbon dioxide gas can also be discharged in the early stage of the reaction.

[0071] Finally, the treated wastewater is discharged into the coagulation tank 801 through the treatment pipe 405. PAC is added manually through the PAC pipe 802, and the coagulation motor 804 is started to drive the coagulation blades 806 for stirring. Then PAM is added through the PAM pipe 803. During the stirring process, flocculent precipitates are generated. The transfer pump 807 is started to discharge the wastewater into the inclined plate sedimentation tank 809. The generated sludge is completely separated from the clean water. The sludge falls into the sludge discharge hopper 811, and the clean water is discharged from the weir 813 to the drain pipe 814. The sludge can be discharged manually at regular intervals by opening the sludge discharge pipe 812 for transfer and treatment.

[0072] Compared with related technologies, the water pollution treatment equipment provided in this embodiment has the following beneficial effects:

[0073] After the wastewater enters the treatment tank 401, the cylinder 601 and the drive motor 602 work together to automatically close the outlet of the collection pipe 107 and open the return gas pipe 701, ensuring the airtightness of the reaction system and preventing gas backflow. Simultaneously, the drive motor 602 drives the mixing blade 604 to stir, while the descending drive ball 608 is at the same horizontal level as the switch 11. The rotating drive ball 608 periodically touches the switch 11, achieving intermittent and slow dripping of dilute sulfuric acid. In the early stages of the reaction, low-speed stirring is combined with slow dripping to ensure uniform acid dispersion and avoid localized over-acidity and violent gas production. In the middle stages of the reaction, the dripping speed and stirring rate are gradually adjusted and continuously reduced to ensure uniform carbon dioxide escape, achieving precise coordination between acid addition and stirring. During the reaction, the return gas pipe 701 is opened by the baffle 607, and the generated carbon dioxide is reintroduced into the bottom of the sewage through the aeration disc 703. The gas pressure drives the liquid to circulate from bottom to top, achieving unpowered auxiliary stirring and enhancing the acid-base mixing effect. The neutralization process is monitored in real time by the pH meter 10, and excess gas is discharged by the exhaust valve 9 to ensure that the reaction endpoint is accurate and controllable. By adding PAC and PAM and stirring, flocculent precipitate is formed, and then the sludge and clean water are completely separated by the inclined plate sedimentation tank 809. The clean water meets the discharge standards, and the sludge is periodically discharged and transferred. This invention realizes resource recovery, automatic dripping control of dilute sulfuric acid, gas circulation enhanced mixing, and deep solid-liquid separation, which significantly improves treatment efficiency, operational stability, and environmental benefits.

[0074] A method for extracting lithium from α-spodumene includes the following steps:

[0075] S1: Take a certain amount of standard α-spodumene, add it to a spherical grinding tank, and grind it at a certain speed and according to a certain ball-to-material mass ratio for 30 minutes. Pass the powder through a 200-mesh sieve, collect the fine powder, weigh a certain amount of sodium hydroxide, and dissolve it in deionized water to prepare a solution of a certain concentration. The solution is prepared by weighing calcium oxide according to a specific mass ratio of calcium oxide to ore.

[0076] S2: First, the airtightness of the high-pressure reactor is tested. Then, according to a certain solid-liquid ratio of ore / sodium hydroxide solution, the sodium hydroxide solution, ore and calcium oxide are mixed and added to the reactor for reaction. The heating furnace is heated to 250°C at a certain heating rate. Stirring is turned on at 300 rpm and kept at this temperature for 6 hours. After naturally cooling to room temperature, the mixture is transferred to centrifuge tubes and centrifuged at 8000 rpm for 10 minutes. The supernatant is collected as the alkali-soluble filtrate and the precipitate is collected as calcium silicate residue. A certain amount of deionized water is added, and the mixture is shaken and centrifuged again at 8000 rpm for 5 minutes. The washing liquid is added to the filtrate. The pH of the washing liquid is tested to be approximately 12. If the pH is greater than 12, the washing is repeated to ensure the recovery of sodium hydroxide for reuse.

[0077] S3: Based on the filtrate The content, according to a certain A certain amount of sodium phosphate dodecahydrate was weighed out and dissolved in deionized water to prepare a solution. The filtrate was transferred to a beaker, heated to 65°C in a water bath, and stirred. The solution was then added dropwise using a peristaltic pump at a certain flow rate. After adding the solution dropwise, continue stirring for 2 hours and monitor the pH: the final reaction pH should be approximately 9. If the pH is less than 9, add more solution. Centrifuge at 8000 rpm for 10 minutes and collect. The precipitate and supernatant are recycled liquids. The supernatant contains... pH≈12, add deionized water and continue shaking and centrifuging, centrifuge at 8000 rpm for 5 minutes, the washing liquid is added to the circulating liquid, and after the circulating liquid passes the test, it is transferred to S2 for reuse;

[0078] S4: According to a certain Measure out the appropriate amount of sulfuric acid and dilute it to 50%. ,Will Transfer the precipitate to a beaker, and slowly add the diluted solution dropwise in a fume hood. Stir until no bubbles appear, then stir at room temperature for 1 hour. If incomplete dissolution occurs, heat and stir in a 40°C water bath. Filter and collect the colorless, transparent solution containing... The clear liquid was concentrated by rotary evaporation to... To reach a certain concentration;

[0079] S5: Pretreatment of the anion and cation membranes, immersing the cation membrane in 1 mol / L... In a 60°C water bath, stir for 2 hours, rinse with deionized water until pH=7, and then immerse the anion exchange membrane in a 1mol / L solution. Stir in a 60°C water bath for 2 hours, then rinse with deionized water until pH=7.

[0080] S6: Assemble the electrodialysis unit and adjust the membrane orientation: the "+" side of the cation exchange membrane should face the cathode, and the "-" side of the anion exchange membrane should face the anode. Membrane stack assembly: first assemble the anode chamber, then assemble the anion exchange membrane, then assemble the intermediate chamber for feed, then assemble the cation exchange membrane, and finally assemble the cathode chamber. The gasket thickness is 0.5 mm. Electrode solution preparation: add a certain amount of 0.1 mol / L to the anode chamber. Add deionized water to the cathode chamber and add water containing [unclear text - likely a substance or ingredient] to the intermediate chamber. The catholy solution was subjected to electrodialysis with an electric current applied, and the initial current was recorded. The catholy solution was measured every 2 hours. , Concentration, when Stop operation when the concentration is <0.1g / L;

[0081] S7: First prepare 20% The solution was transferred from the catholyte to a beaker, placed in an 80°C water bath, and magnetically stirred at 150 rpm. The mixture was then stirred according to a specific... The solution is added dropwise at a certain rate using a burette. Monitor pH: The endpoint pH ≈ 10; if pH < 10, add more. After the addition is complete, stir for 1 hour to produce a white substance. The precipitate was centrifuged at 8000 rpm for 10 minutes, and the precipitate was collected. It was washed three times with deionized water at 80°C. The washing liquid was transferred to a water pollution treatment facility for further treatment until it met discharge standards. The precipitate was transferred to a weighing bottle and dried in a vacuum drying oven at 40°C to obtain lithium carbonate. .

[0082] In S1, the ball-to-material mass ratio is 5:1, the grinding speed is 300 rpm, and the calcium oxide / ore mass ratio is 0.2:1-0.8:1; in S2, the sodium hydroxide solution concentration is 400 g / L, the sodium hydroxide solution / ore liquid-to-solid ratio is 5-9 mL / g, and the heating furnace heating rate is 5℃ / min; in S3... The ratio is 1:3-2:3, the peristaltic pump flow rate is 1 mL / min, and the standard for the circulating solution is: when ammonium molybdate is added to the circulating solution, no yellow precipitate is formed, which proves... Excess ≤5%; a certain amount of S4 The ratio is 2:3, added drop by drop. The flow rate is 1 drop / second, concentrated Concentration reached In S5, the cation and anion membranes are Nafion N117 as the cation membrane and Selemion AMV as the anion membrane; in S6, the electrodialysis device has a membrane area of ​​10... Two pairs of films, titanium-coated ruthenium anode + 316L cathode, constant voltage of 3.5V, for 20 hours; a certain amount of S7... The ratio is 1:2 to 1.5:2, and the solution is added dropwise using a burette. The solution flow rate is 1 drop / second, and the standard for passing the washing with deionized water three times is... ≤0.1g / L.

[0083] First Embodiment

[0084] Weigh 10.0g of standard α-spodumene, place it in a spherical jar, add 25.0g of grinding balls, and grind at 300rpm for 15 minutes. After grinding, stop for 5 minutes to cool, and continue grinding for another 15 minutes. Pass the sample through a 200-mesh standard sieve and vibrate it for 5 minutes. The material passing through the sieve should be ≥95%. The material remaining on the sieve should be returned to the spherical jar for re-grinding. Add 50mL of deionized water to a beaker, place it in an ice bath, and slowly add 40.0g of standard α-spodumene. After dissolving, cool to room temperature and make up to 100 mL (volume flask) to obtain a 400 g / L solution (prepare fresh for immediate use).

[0085] Check the airtightness of the autoclave and introduce air into it. The pressure was maintained at 0.5 MPa for 30 seconds without any pressure drop, indicating that the airtightness was acceptable. 10.00 g of mineral powder was then mixed with 70.0 mL of... Solution and 5.0g Mix the ingredients, add a PTFE stir bar, heat the oven to 250°C at a rate of 5°C / min, start stirring (300 rpm), and maintain the temperature for 6 hours. After naturally cooling to room temperature, transfer to a 50 mL centrifuge tube and centrifuge at 8000 rpm for 10 minutes. Collect the supernatant (alkali-soluble filtrate) and precipitate (calcium silicate residue). Add 10 mL of deionized water, shake, and continue centrifuging (8000 rpm × 5 min). Combine the washings with the filtrate. Check the pH of the washings; if it is approximately 12, repeat the washing process. Recycle.

[0086] Take 1.0 mL of filtrate and use 1% Diluted 10 times (to a final volume of 10 mL), and the result was obtained. The concentration was 7.23 g / L. 70.0 mL of the filtrate was taken and mixed at a ratio of 1.3:3. Weigh out 83.4g of sodium phosphate dodecahydrate ( Dissolve the filtrate in deionized water to prepare a solution. Transfer the filtrate to a 100 mL beaker, heat it in a water bath to 65°C and stir. Add the solution dropwise using a peristaltic pump at a flow rate of 1 mL / min. After adding the solution dropwise, continue stirring for 2 hours (monitor pH: the reaction endpoint pH≈9; if pH<9, add more solution). ,make sure (After complete precipitation), centrifuge at 8000 rpm for 10 minutes and collect. Precipitate and supernatant (circulating fluid, containing (pH≈12), add 5 mL of deionized water and continue centrifugation with shaking (8000 rpm × 5 minutes). The washing liquid is added to the circulating liquid. After the circulating liquid passes the test, it is transferred to S2 for reuse.

[0087] According to 2:3 Take 10 mL of sulfuric acid and dilute it to 50%. ,Will Transfer the precipitate to a beaker, and slowly add the diluted solution dropwise in a fume hood. (1 drop per second, to prevent splashing), stir until no bubbles remain, stir at room temperature for 1 hour (if incompletely dissolved, heat and stir in a 40°C water bath), filter and collect. The clear liquid was concentrated by rotary evaporation to... The concentration reached 40.8 g / L.

[0088] The cation exchange membrane (Nafion N117) was immersed in 1 mol / L In a 60°C water bath with stirring for 2 hours, rinse with deionized water until pH=7, and then immerse the anion exchange membrane (Selemion AMV) in 1mol / L water. In the middle stage, stir in a 60℃ water bath for 2 hours, rinse with deionized water until pH=7, install the electrodialysis apparatus, and perform electrodialysis with 3.5V DC current. Record the initial current and measure the catholyte solution every 2 hours. , Concentration, when Stop operation when the concentration is <0.1g / L, and run for 20 hours.

[0089] According to 1.1:2 Weigh out 116.6g according to the ratio. Dissolve it in 466 mL of deionized water at 80°C to prepare a 20% solution. For the solution, transfer 50 mL of catholy liquid to a beaker, incubate in an 80°C water bath with magnetic stirring (150 rpm), and add solution dropwise at a rate of 1 drop / second using a burette. Solution (monitor pH: endpoint pH≈10, if pH<10, add more) After the addition is complete, stir for 1 hour to produce a white substance. The precipitate was centrifuged at 8000 rpm for 10 minutes, the precipitate was collected, washed three times with deionized water at 80℃, the precipitate was transferred to a weighing bottle (constant weight) and dried in a vacuum drying oven at 40℃ to obtain lithium carbonate. It was then ground in an agate mortar and pestle and passed through a 100-mesh standard sieve.

[0090] Compared with related technologies, the method for extracting lithium from α-spodumene provided by the present invention has the following beneficial effects:

[0091] By adding Lithium was extracted directly from α-spodumene using an alkaline solution. With the addition of calcium oxide, the leaching residue exhibited a regular wedge shape and a smooth surface. This eliminated the sodium aluminosilicate products that originally covered the surface of spodumene, thus promoting the decomposition of α-spodumene. The lithium in the leachate was then extracted as sodium phosphate. Lithium phosphate precipitates in the form of ( ) The mother liquor obtained after lithium precipitation is reused to start the next round of autoclave leaching cycle. In ten consecutive cycles, the lithium precipitation efficiency and α-spodumene decomposition efficiency remain stable, avoiding high-temperature crystal transformation (α-spodumene to β-spodumene) and evaporation process. This method of directly recovering lithium from α-spodumene has low energy consumption.

[0092] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural or procedural transformations made based on the content of the present invention specification and drawings, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of the present invention.

Claims

1. A water pollution treatment device, characterized in that, include: A ground-based collection mechanism includes a collection tank and a collection pump. The collection tank is located on the ground, and a collection motor is fixedly installed on the top of the collection tank. The output shaft of the collection motor is fixedly connected to a collection shaft. The bottom end of the collection shaft passes through the top of the collection tank and extends into the interior. A collection blade is fixedly installed on the bottom end of the collection shaft. The input end of the collection pump is connected to an input pipe. One end of the input pipe passes through one side of the collection tank and extends into the interior. The output end of the collection pump is connected to a collection pipe. A funnel, which is connected to the top of the collection tank, and a filter screen is fixedly installed on the inner wall of the funnel; A processing mechanism, which is connected to the end of the collection tube; A dosing mechanism for adding an acidic solution into the interior of the processing unit.

2. The water pollution treatment equipment according to claim 1, characterized in that, The processing mechanism includes a processing tank and a processing pump. The processing tank is connected to the end of the collection pipe and is located on the ground. A top cover is fixedly installed on the top of the processing tank and a bottom cover is fixedly installed on the bottom of the processing tank. The processing pump is located on the ground, and the input end of the processing pump is connected to the bottom of the bottom cover through a connecting pipe. The output end of the processing pump is connected to the processing pipe.

3. The water pollution treatment equipment according to claim 2, characterized in that, The dosing mechanism is fixedly installed on the top of the cover. The dosing mechanism includes a peristaltic pump, which is fixedly installed on the top of the cover by a bracket. The input end of the peristaltic pump is connected to a sulfuric acid tank through an extraction pipe. The sulfuric acid tank is located on the ground. The output end of the peristaltic pump is connected to a dosing pipe. The bottom end of the dosing pipe passes through the top of the cover and extends into the interior of the treatment tank.

4. The water pollution treatment equipment according to claim 2, characterized in that, A drive mechanism is fixedly installed on the top of the top cover. The drive mechanism includes a cylinder, which is fixedly installed on the top of the top cover. The output shaft of the cylinder passes through the top of the top cover and extends into the interior of the processing tank. A drive motor is fixedly connected to the bottom end of the cylinder output shaft. A drive shaft is fixedly connected to the output shaft of the drive motor. A mixing blade is fixedly installed on the surface of the drive shaft. A baffle is fixedly installed on the surface of the drive shaft through four support plates. The baffle is adapted to the processing tank. A baffle is fixedly installed on the top of each of the four support plates through four connecting columns. A drive ball is fixedly installed on the surface of one of the connecting columns.

5. A water pollution treatment device according to claim 4, characterized in that, The top of the top cover is connected to an aeration mechanism, which includes a return air pipe. The return air pipe is connected to the top of the top cover, and its end extends through the bottom of the bottom cover and into the interior of the treatment tank. The end of the return air pipe is connected to a distribution air pipe, and the surface of the distribution air pipe is connected to several aeration discs.

6. A water pollution treatment device according to claim 5, characterized in that, A switch is fixedly installed on the inner wall of the treatment tank by a support column. The switch is adapted to the drive ball. The first baffle is adapted to the collection pipe and the second baffle is adapted to the return gas pipe.

7. A water pollution treatment device according to claim 2, characterized in that, An exhaust valve is connected to the top of the top cover, and a pH meter is fixedly installed on the inner wall of the treatment tank.

8. A water pollution treatment device according to claim 2, characterized in that, The end of the treatment pipe is connected to a coagulation sedimentation mechanism, which includes a coagulation tank connected to the end of the treatment pipe. The coagulation tank is located on the ground. PAC pipes and PAM pipes are fixedly installed on the inner wall of the coagulation tank via supports. A coagulation motor is fixedly installed on the inner wall of the coagulation tank via supports. The output shaft of the coagulation motor is fixedly connected to a coagulation shaft. A coagulation blade is fixedly installed at the bottom end of the coagulation shaft. A transfer pump is connected to one side of the coagulation tank via a connecting pipe. The transfer pump is located on the ground. The output end of the transfer pump is connected to an inclined plate sedimentation tank via a transfer pipe. The inclined plate sedimentation tank is located on the ground via supports. Several inclined plates are fixedly installed on the inner wall of the inclined plate sedimentation tank. Three sludge discharge hoppers are connected to the bottom of the inclined plate sedimentation tank. Each of the three sludge discharge hoppers has a sludge discharge pipe inside. One end of each of the three sludge discharge pipes passes through the inner wall of the three sludge discharge hoppers and extends to the outside. A water-retaining weir is fixedly installed on the inner wall of the inclined plate sedimentation tank. A drainage pipe is connected to one side of the inclined plate sedimentation tank.

9. A method for extracting lithium from α-spodumene, requiring the use of a water pollution treatment device as described in any one of claims 1-8, characterized in that, Includes the following steps: S1: Take a certain amount of standard α-spodumene, add it to a spherical grinding tank, and grind it at a certain speed and according to a certain ball-to-material mass ratio for 30 minutes. Pass the powder through a 200-mesh sieve, collect the fine powder, weigh a certain amount of sodium hydroxide, and dissolve it in deionized water to prepare a solution of a certain concentration. The solution is prepared by weighing calcium oxide according to a specific mass ratio of calcium oxide to ore. S2: First, the airtightness of the high-pressure reactor is tested. Then, according to a certain solid-liquid ratio of ore / sodium hydroxide solution, the sodium hydroxide solution, ore and calcium oxide are mixed and added to the reactor for reaction. The heating furnace is heated to 250°C at a certain heating rate. Stirring is turned on at 300 rpm and kept at this temperature for 6 hours. After naturally cooling to room temperature, the mixture is transferred to centrifuge tubes and centrifuged at 8000 rpm for 10 minutes. The supernatant is collected as the alkali-soluble filtrate and the precipitate is collected as calcium silicate residue. A certain amount of deionized water is added, and the mixture is shaken and centrifuged again at 8000 rpm for 5 minutes. The washing liquid is added to the filtrate. The pH of the washing liquid is tested to be approximately 12. If the pH is greater than 12, the washing is repeated to ensure the recovery of sodium hydroxide for reuse. S3: Based on the filtrate The content, according to a certain A certain amount of sodium phosphate dodecahydrate was weighed out and dissolved in deionized water to prepare a solution. The filtrate was transferred to a beaker, heated to 65°C in a water bath, and stirred. The solution was then added dropwise using a peristaltic pump at a certain flow rate. After adding the solution dropwise, continue stirring for 2 hours and monitor the pH: the final reaction pH should be approximately 9. If the pH is less than 9, add more solution. Centrifuge at 8000 rpm for 10 minutes and collect. The precipitate and supernatant are recycled liquids. The supernatant contains... pH≈12, add deionized water and continue shaking and centrifuging, centrifuge at 8000 rpm for 5 minutes, the washing liquid is added to the circulating liquid, and after the circulating liquid passes the test, it is transferred to S2 for reuse; S4: According to a certain Measure out the appropriate amount of sulfuric acid and dilute it to 50%. ,Will Transfer the precipitate to a beaker, and slowly add the diluted solution dropwise in a fume hood. Stir until no bubbles appear, then stir at room temperature for 1 hour. If incomplete dissolution occurs, heat and stir in a 40°C water bath. Filter and collect the colorless, transparent solution containing... The clear liquid was concentrated by rotary evaporation to... To reach a certain concentration; S5: Pretreatment of the anion and cation membranes, immersing the cation membrane in 1 mol / L... In a 60°C water bath, stir for 2 hours, rinse with deionized water until pH=7, and then immerse the anion exchange membrane in a 1mol / L solution. Stir in a 60°C water bath for 2 hours, then rinse with deionized water until pH=7. S6: Assemble the electrodialysis unit and adjust the membrane orientation: the "+" side of the cation exchange membrane should face the cathode, and the "-" side of the anion exchange membrane should face the anode. Membrane stack assembly: first assemble the anode chamber, then assemble the anion exchange membrane, then assemble the intermediate chamber for feed, then assemble the cation exchange membrane, and finally assemble the cathode chamber. The gasket thickness is 0.5 mm. Electrode solution preparation: add a certain amount of 0.1 mol / L to the anode chamber. Add deionized water to the cathode chamber and add water containing [unclear text - likely a substance or ingredient] to the intermediate chamber. The catholy solution was subjected to electrodialysis with an electric current applied, and the initial current was recorded. The catholy solution was measured every 2 hours. , Concentration, when Stop operation when the concentration is <0.1g / L; S7: First prepare 20% The solution was transferred from the catholyte to a beaker, placed in an 80°C water bath, and magnetically stirred at 150 rpm. The mixture was then stirred according to a specific... The solution is added dropwise at a certain rate using a burette. Monitor pH: The endpoint pH ≈ 10; if pH < 10, add more. After the addition is complete, stir for 1 hour to produce a white substance. The precipitate was centrifuged at 8000 rpm for 10 minutes, and the precipitate was collected. It was washed three times with deionized water at 80°C. The washing liquid was transferred to a water pollution treatment facility for further treatment until it met discharge standards. The precipitate was transferred to a weighing bottle and dried in a vacuum drying oven at 40°C to obtain lithium carbonate. .

10. A method for extracting lithium from α-spodumene according to claim 9, characterized in that, In S1, the ball-to-material mass ratio is 5:1, the grinding speed is 300 rpm, and the calcium oxide / ore mass ratio is 0.2:1-0.8:1; in S2, the sodium hydroxide solution concentration is 400 g / L, the sodium hydroxide solution / ore liquid-to-solid ratio is 5-9 mL / g, and the heating furnace heating rate is 5℃ / min; in S3... The ratio is 1:3-2:3, the peristaltic pump flow rate is 1 mL / min, and the standard for the circulating solution is: when ammonium molybdate is added to the circulating solution, no yellow precipitate is formed, which proves... Excess ≤5%; a certain amount of S4 The ratio is 2:3, added drop by drop. The flow rate is 1 drop / second, concentrated Concentration reached In S5, the cation and anion membranes are Nafion N117 as the cation membrane and Selemion AMV as the anion membrane; in S6, the electrodialysis device has a membrane area of ​​10... Two pairs of films, titanium-coated ruthenium anode + 316L cathode, constant voltage of 3.5V, for 20 hours; a certain amount of S7... The ratio is 1:2 to 1.5:2, and the solution is added dropwise using a burette. The solution flow rate is 1 drop / second, and the standard for passing the washing with deionized water three times is... ≤0.1g / L.

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