Preparation method and device of adsorbent for adsorbing rubidium and cesium from lepidolite leaching solution

Abstract

The invention provides a method and a device for preparing an adsorbent for adsorbing rubidium and cesium from lepidolite leachate. The preparation method of the adsorbent for adsorbing rubidium and cesium from the lepidolite leachate comprises the following steps: S1, weighing straw powder, and carrying out soda boiling treatment on the straw powder; s2, filtering while hot, collecting filter residues, washing with deionized water, and drying; s3, transferring the filter residues into a high-pressure kettle, and adding deionized water for hydrothermal reaction to obtain a reaction product. According to the preparation method and device of the adsorbent for adsorbing rubidium and cesium from the lepidolite leaching solution, the adsorbent has the effects of high adsorption capacity, good selectivity and stability in the aspect of rubidium and cesium adsorption, and the material can adsorb a large number of rubidium and cesium ions due to the rich pore structure and ion exchange sites; and the enrichment capacity on low-concentration rubidium and cesium is improved.

Description

Technical Field

[0001] This invention relates to the field of radioactive pollution control technology, and in particular to a method and apparatus for preparing an adsorbent for adsorbing rubidium and cesium from lepidolite leachate. Background Technology

[0002] Rubidium and cesium are rare alkali metals with excellent optoelectronic properties, widely used in electronics, medicine, defense industry, alternative energy, and new materials. In recent years, in particular, with the rapid development of science and technology, the international market demand for rubidium and cesium has continued to increase. Therefore, the extraction, separation, and purification of rubidium and cesium have attracted great attention from researchers.

[0003] The main sources of rubidium and cesium include salt lake brines and some hard rock ores, such as cesium garnet, spodumene, and lepidolite. Lepidolite is a crucial carrier mineral for rubidium and cesium, in which rubidium and cesium substitute for potassium ions in an isomorphous manner, forming interlayer solid solutions. Mineralogical studies show that lepidolite contains 0.82%-1.58% Rb₂O and 0.02%-1.32% Cs₂O, while potassium feldspar generally contains less than 0.1% rubidium and cesium. This unique occurrence characteristic means that rubidium and cesium extraction requires overcoming the interlayer bond energy of mica, making effective separation difficult with traditional physical beneficiation methods.

[0004] Currently, the main methods for separating and extracting rubidium and cesium from salt lake brine include precipitation, extraction, and adsorption. Precipitation is unsuitable for low-concentration Rb in salt lake brine due to poor separation efficiency, low product purity, low yield, and high production costs. + Cs + Separation and extraction. Although extraction methods can rapidly separate Rb... + Cs + However, during the extraction process, some extractant and diluent will mix into the aqueous phase, which not only causes significant corrosion to the equipment but also leads to environmental pollution. Adsorption method has advantages such as high recovery rate, low pollution, and low energy consumption, and is suitable for the separation and extraction of low concentration target ions in salt lake brine.

[0005] Existing technologies for treating low-grade brine are too costly and lack economic feasibility. Rb in Tibetan salt lake brine. + Concentrations are generally < 5 mg / L. Traditional adsorbents (such as silica gel loaded with Prussian blue) have an adsorption capacity of only 4-5 mg / g, and commercial ion exchange resins have an adsorption capacity of only about 60 mg / g for radioactive Cs-137. These limitations make them unsuitable for radioactive contamination remediation due to their low adsorption capacity, leading to Rb... + Cs + It cannot be completely removed and will pollute the environment.

[0006] Therefore, it is necessary to provide a method and apparatus for preparing an adsorbent for adsorbing rubidium and cesium from lepidolite leachate to solve the above-mentioned technical problems. Summary of the Invention

[0007] This invention provides a method and apparatus for preparing an adsorbent for adsorbing rubidium and cesium from lepidolite leachate, solving the problem of the low adsorption capacity of traditional adsorbents, which leads to insufficient adsorption of rubidium and cesium. + Cs + It cannot be completely removed and will cause environmental pollution.

[0008] To solve the above-mentioned technical problems, the present invention provides a method for preparing an adsorbent for adsorbing rubidium and cesium from lepidolite leachate, comprising the following steps:

[0009] S1. Weigh the straw powder and treat it with alkali boiling.

[0010] S2. Filter while hot and collect the filter residue, wash with deionized water and dry;

[0011] S3. Transfer the filter residue to a high-pressure reactor, add deionized water to carry out a hydrothermal reaction, and obtain the reaction product.

[0012] S4. Wash the reaction product alternately with deionized water and ethanol to obtain biomass carbon wet gel.

[0013] S5. Cut the biomass carbon wet gel into small pieces, place them in a refrigerator for pre-freezing, and then transfer them to a freeze dryer to dry them to obtain porous biomass carbon dry gel.

[0014] S6. The porous biomass carbon dry gel is placed in a tube furnace and carbonized under a nitrogen atmosphere to obtain carbonized biomass carbon aerogel.

[0015] S7. Weigh out titanate and silane in a certain proportion, dissolve them in anhydrous ethanol, and stir until transparent to obtain a transparent solution;

[0016] S8. Immerse the prepared carbonized biomass carbon aerogel in a transparent solution and shake.

[0017] S9. Add KOH solutions of different concentrations and continue shaking to obtain a mixed solution;

[0018] S10. The mixture is transferred to a high-pressure reactor for hydrothermal reaction, washed and dried to obtain potassium titanate modified carbonized biomass carbon aerogel, which is the adsorbent used to adsorb rubidium and cesium from lepidolite leachate.

[0019] Preferably, the alkaline boiling treatment in S1 uses a 5% NaOH solution, heated and stirred in a water bath at 80°C for 2 hours.

[0020] Preferably, in step S2, the water is washed with deionized water until neutral and then dried at 80°C to constant weight.

[0021] Preferably, the hydrothermal reaction in S3 is carried out at a constant temperature of 180°C for 12 hours.

[0022] Preferably, in step S4, the washing is performed 3 times, and centrifugation is performed at 10,000 rpm for 5 minutes each time, until the supernatant is no longer yellow and the pH is 7.

[0023] Preferably, in step S5, the food is pre-frozen at -15°C for 12 hours and then dried in a freeze dryer at -50°C and 10Pa for 48 hours.

[0024] Preferably, in the S6 tube furnace, the temperature is increased to 800°C at a rate of 5°C / min and held for 1 hour.

[0025] Preferably, in S7, the titanate is tetrabutyl titanate, the silane is tetraethoxysilane, the molar ratio of titanate to silane in S7 is 2:1, 1:1 or 1:2, and the stirring time is 30 min.

[0026] Preferably, the oscillation time in S8 is 30 minutes.

[0027] Preferably, the concentration of KOH solution in S9 is 1, 3, 5, 7, or 10 mol / L, and the shaking time is 1 h.

[0028] Preferably, the hydrothermal reaction conditions in S10 are a temperature of 200°C and a reaction time of 24 hours.

[0029] Preferably, in step S10, the sample is washed three times with KOH solution of the corresponding concentration, then washed with deionized water until neutral, and dried at 100°C for 12 hours.

[0030] This invention also provides an adsorbent preparation apparatus for adsorbing rubidium and cesium from lepidolite leachate, applied in the method for preparing the adsorbent for adsorbing rubidium and cesium from lepidolite leachate, for preparing the adsorbent for adsorbing rubidium and cesium from lepidolite leachate, comprising: a base, a support assembly mounted on the top of the base, a water bath mounted on the support assembly, a reaction vessel mounted inside the water bath, a stirring assembly mounted on the reaction vessel for stirring during alkaline boiling treatment of the material, and a drive assembly mounted on the top of the reaction vessel. The driving component is used to drive the stirring component to rotate. A feed chute is installed on the top of the reactor, and a discharge chute is installed on the bottom of the reactor. A positioning hole is provided on the discharge chute. A sealing conversion component is installed on the base. The sealing conversion component is used to abut against the discharge chute to seal the discharge chute. A pushing component is installed at the bottom of the base. The pushing component is used to drive the sealing conversion component to rotate to achieve angle adjustment. A cleaning component is installed at the bottom of the reactor. The cleaning component is used to clean the sealing conversion component.

[0031] Preferably, the support assembly includes a support plate, a sliding rod, a fixed frame, a sliding plate, a connecting rod, a first elastic element, a first magnetic block, and a second magnetic block. The bottom of the support plate is fixed to the base. The sliding rod passes through and is slidably connected to the support plate. The fixed frame is mounted on the support plate. The sliding plate is slidably connected inside the fixed frame. One end of the connecting rod is fixed to one side of the sliding plate, and the other end is fixed to the water bath. The first elastic element is installed between the sliding plate and the side wall of the fixed frame. The first magnetic block is fixed to the sliding plate, and the second magnetic block is fixed to the side wall of the fixed frame.

[0032] Preferably, the stirring assembly includes a stirring shaft, stirring blades, and a limiting sleeve. The stirring shaft is rotatably connected to the reactor, the stirring blades are fixed to the outer surface of the stirring shaft, and the limiting sleeve is fixed to the top end of the stirring shaft.

[0033] Preferably, the drive assembly includes a mounting frame, a drive component, a sleeve shaft, a cam, a sliding shaft, a limiting block, a moving plate, a displacement block, a guide rail, and a second elastic element. The mounting frame is fixed to the reactor, the drive component is fixed to the mounting frame, the sleeve shaft is fixed to the output shaft of the drive component, the cam is fixed to the outer surface of the sleeve shaft, the sliding shaft is slidably connected to the inner surface of the sleeve shaft, the limiting block is fixed to the bottom end of the sleeve shaft, the moving plate is rotatably connected to the outer surface of the sliding shaft, the displacement block is fixed to the bottom of the moving plate, the guide rail is fixed to the reactor, the displacement block is slidably connected to the guide rail, and the second elastic element is installed between the displacement block and the guide rail.

[0034] Preferably, the sealing and conversion assembly includes a rotating shaft, a sealing plate, a filter plate, a through hole, a sliding groove, a sealing block, an abutment block, a positioning block, a groove, a third elastic element, an inclined block, a connecting plate, and a contact plate. The rotating shaft is rotatably connected to the base, the sealing plate is fixed to the outer surface of the rotating shaft, the filter plate is mounted on the sealing plate, the through hole is formed on the sealing plate, the sliding groove is disposed on the sealing plate, the sealing block is slidably connected in the sliding groove, the abutment block is fixed on the sealing block, the positioning block is fixed on the abutment block, the groove is formed on the sealing plate, the third elastic element is installed between the sidewall of the sealing block and the groove, the inclined block is fixed to the outer surface of the rotating shaft, the connecting plate is fixed to the top end of the rotating shaft, and the contact plate is fixed to the connecting plate.

[0035] Preferably, the pushing assembly includes a pushing member, a moving block, a first spur gear plate, and a first gear. The pushing member is installed at the bottom of the base, the moving block is slidably connected to the bottom of the base, the output end of the pushing member is fixedly connected to the moving block, the first spur gear plate is fixed on the moving block, and the first gear is installed on the outer surface of the rotating shaft, with the first spur gear plate meshing with the outer surface of the first gear.

[0036] Preferably, the cleaning assembly includes a connecting shaft, a second gear, a cleaning brush, and a second straight toothed plate. The connecting shaft is rotatably connected to the bottom of the reactor, the second gear is fixed to the outer surface of the connecting shaft, the cleaning brush is fixed to the bottom end of the connecting shaft, and the second straight toothed plate is fixed to the support plate. The second straight toothed plate meshes with the outer surface of the second gear.

[0037] Compared with related technologies, the method and apparatus for preparing adsorbent for adsorbing rubidium and cesium from lepidolite leachate provided by the present invention have the following advantages:

[0038] This invention provides a method and apparatus for preparing an adsorbent for adsorbing rubidium and cesium from lepidolite leachate. This invention exhibits high adsorption capacity, good selectivity, and stability in adsorbing rubidium and cesium. Its abundant pore structure and ion exchange sites enable the material to adsorb large amounts of rubidium and cesium ions, improving the enrichment capacity for low concentrations of rubidium and cesium. The special structure and chemical properties of potassium titanate give it high selectivity for rubidium and cesium ions, enabling it to preferentially adsorb rubidium and cesium in lepidolite leachate containing multiple ions, reducing interference from other ions, improving the adsorption performance of rubidium and cesium, reducing radioactive pollution, and thus improving environmental benefits. Carbonized biomass carbon aerogel has good chemical stability and mechanical strength, maintaining structural integrity in the leachate environment, and is not easily broken or dissolved, thus ensuring the stability and repeatability of the adsorption process, making it a good material for environmental remediation. It can also be reused through elution, resulting in good economic benefits. Attached Figure Description

[0039] Figure 1 This is a schematic diagram of the first embodiment of the adsorbent preparation method and apparatus for adsorbing rubidium and cesium from lepidolite leachate provided by the present invention.

[0040] Figure 2 This is a schematic diagram of the second embodiment of the adsorbent preparation method and apparatus for adsorbing rubidium and cesium from lepidolite leachate provided by the present invention.

[0041] Figure 3 for Figure 2 A schematic diagram of the back of the reactor shown;

[0042] Figure 4 for Figure 2 A schematic cross-sectional view of the reactor shown;

[0043] Figure 5 for Figure 2 The diagram shows the structural schematic of the support component.

[0044] Figure 6 for Figure 4 The diagram shows the structure of the stirring assembly.

[0045] Figure 7 for Figure 6 The enlarged schematic diagram of part A shown below;

[0046] Figure 8 for Figure 2 The diagram shows the structure of the plugging conversion assembly;

[0047] Figure 9 for Figure 8 A schematic cross-sectional view of the sealing plate shown;

[0048] Figure 10 To drive the motion state diagram of the component, where, Figure 10 (a) is the initial state diagram for driving the component. Figure 10 (b) Schematic diagram for the initial push of the component. Figure 10 (c) is a schematic diagram of the secondary drive of the component. Figure 10 (d) Schematic diagram of three pushes of the component;

[0049] Figure 11 This is a motion diagram of the sealing plate, where... Figure 11 (a) is a diagram showing the initial state of the sealing plate. Figure 11 (b) is a schematic diagram of the initial swing of the sealing plate. Figure 11 (c) is a schematic diagram of the secondary swing of the sealing plate. Figure 11 (d) is a schematic diagram of the sealing plate swinging three times.

[0050] Numbering on the map:

[0051] 1. Base;

[0052] 2. Support assembly; 21. Support plate; 22. Sliding rod; 23. Fixing frame; 24. Sliding plate; 25. Connecting rod; 26. First elastic element; 27. First magnet; 28. Second magnet.

[0053] 3. Water bath; 4. Reactor;

[0054] 5. Stirring assembly; 51. Stirring shaft; 52. Stirring blades; 53. Limiting sleeve;

[0055] 6. Drive assembly; 61. Mounting bracket; 62. Drive component; 63. Sleeve shaft; 64. Cam; 65. Sliding shaft; 66. Limiting block; 67. Moving plate; 68. Displacement block; 69. Guide rail; 610. Second elastic element.

[0056] 7. Feed chute; 8. Discharge chute; 9. Positioning hole;

[0057] 10. Blocking conversion assembly; 101. Rotating shaft; 102. Blocking plate; 103. Filter plate; 104. Through hole; 105. Slide groove; 106. Blocking block; 107. Abutting block; 108. Positioning block; 109. Groove; 1010. Third elastic element; 1011. Inclined block; 1012. Connecting plate; 1013. Contact plate;

[0058] 11. Pushing component; 111. Pushing element; 112. Moving block; 113. First spur plate; 114. First gear;

[0059] 12. Cleaning component; 121. Connecting shaft; 122. Second gear; 123. Cleaning brush; 124. Second straight tooth plate. Detailed Implementation

[0060] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0061] First Embodiment

[0062] Please refer to the following: Figure 1 This invention provides a method for preparing an adsorbent for adsorbing rubidium and cesium from lepidolite leachate, comprising the following steps:

[0063] S1. Weigh 50g of corn stalk powder that has been crushed through a 40-mesh sieve, add 500mL of 5% NaOH solution, and stir in an 80℃ water bath for 2 hours.

[0064] S2. After filtering while hot, wash with deionized water until pH=7, and dry at 80℃ to constant weight to obtain 30g of filter residue.

[0065] S3. Transfer 20g of filter residue into a 500mL autoclave, add 300mL of deionized water, seal and react at a constant temperature of 180℃ for 12 hours, then centrifuge after natural cooling.

[0066] S4. Wash with deionized water and ethanol alternately 3 times until the supernatant is colorless, to obtain about 150g of biomass carbon wet gel (BCH);

[0067] S5. Cut BCH into 1cm³ pieces, pre-freeze at -15℃ for 12 hours, then transfer to a freeze dryer (-50℃, 10Pa) and dry for 48 hours to obtain 12g of biomass carbon dry gel (BCA).

[0068] S6. Place 5g of BCA in a tube furnace, under nitrogen protection (flow rate 50mL / min), heat to 800℃ at 5℃ / min, hold for 1 hour, and cool with the furnace to obtain 4.5g of carbonized biomass carbon aerogel (CBCA).

[0069] S7. Measure 2.5 mL of TBT (0.009 mol) and 2.5 mL of TEOS (0.009 mol), dissolve them in 50 mL of anhydrous ethanol, and stir for 30 minutes until clear;

[0070] S8. Weigh 10g of CBCA and immerse it in the above solution, then shake at room temperature for 30 minutes.

[0071] S9. Add 200 mL of 5 mol / L KOH solution (40 g KOH dissolved in 200 mL of water) and continue shaking for 1 hour;

[0072] S10. Transfer to a 500mL autoclave and react at 200℃ for 24 hours. After cooling, wash three times with 5mol / L KOH solution and wash with deionized water until pH=7. Dry in an oven at 100℃ for 12 hours to obtain 11.2g of potassium titanate modified carbonized biomass carbon aerogel, which is the adsorbent used to adsorb rubidium and cesium from lepidolite leachate.

[0073] The adsorbent prepared in this invention primarily adsorbs rubidium and cesium from lepidolite leachate through a synergistic interaction of ion exchange, physical adsorption, and chemical complexation. Potassium titanate possesses a unique crystal structure containing exchangeable potassium ions. When in contact with lepidolite leachate, rubidium and cesium ions in the solution undergo ion exchange reactions with potassium ions on the surface and within potassium titanate. Due to the stronger binding affinity of rubidium and cesium ions to potassium titanate, they preferentially replace potassium ions, thus being adsorbed onto the material's surface and interior. Some functional groups or lattice structures in potassium titanate may form specific chemical bonds or complexes with rubidium and cesium ions, enhancing the adsorption selectivity and capacity for these ions. Carbonized biomass carbon aerogel has a rich porous structure and a large specific surface area, which can provide a large number of adsorption sites. Through physical actions such as van der Waals forces, it can physically adsorb rubidium and cesium ions in the leachate and adsorb them on the pore surface of the material, thereby reducing the pollution of rubidium and cesium ions to the environment. It is an environmentally friendly material for environmental remediation or restoration.

[0074] This invention uses corn stalks as biomass raw material and processes such as chemical pretreatment, hydrothermal reaction, freeze drying, and carbonization modification to prepare potassium titanate-modified carbonized biomass carbon aerogel with high porosity and excellent adsorption performance. It is used as a solvent adsorption method to extract and separate rubidium and cesium from lepidolite leachate. The raw materials are simple and readily available, turning waste into treasure, which is conducive to the implementation of environmental protection projects and improves environmental protection effects.

[0075] In one embodiment, 100 ml of lepidolite leachate was taken, and the Rb content was measured. + =50mg / L, Cs + =30 mg / L, placed in a 250 mL Erlenmeyer flask, and adjusted the pH to 7.0 with 0.1 mol / L HCl / NaOH. Add 0.2 g of potassium titanate-modified carbonized biomass aerogel, seal and shake, and take samples at 0.5 h, 1 h, 2 h, 4 h, 6 h, and 8 h respectively. After filtration, measure Rb. + / Cs + Concentration; Under the same conditions, the adsorption performance of commercial ion exchange resin (IRA-400) and zeolite was tested.

[0076] Testing showed that the potassium titanate-modified carbonized biomass aerogel exhibited improved Rb adsorption after 4 hours. + The adsorption rate is 90% for Cs + The adsorption rate was 85%. After 8 hours of adsorption, the potassium titanate-modified carbonized biomass aerogel showed a good adsorption rate for Rb. + The adsorption rate is 98% for Cs + The adsorption rate was 95%. The ion exchange resin (IRA-400) was used for 8 hours to adsorb Rb... + The adsorption rate is 75% for Cs + The adsorption rate of zeolite was 70%. After 8 hours, the zeolite showed an adsorption rate of 70% for Rb. + The adsorption rate is 60% for Cs + The adsorption rate is 56%.

[0077] Compared with related technologies, the method and apparatus for preparing adsorbent for adsorbing rubidium and cesium from lepidolite leachate provided by the present invention have the following advantages:

[0078] This invention exhibits high adsorption capacity, good selectivity, and stability in the adsorption of rubidium and cesium. Its abundant pore structure and ion exchange sites enable the material to adsorb large amounts of rubidium and cesium ions, improving its enrichment capacity for low concentrations of rubidium and cesium. The special structure and chemical properties of potassium titanate give it high selectivity for rubidium and cesium ions, enabling it to preferentially adsorb rubidium and cesium in lepidolite leachates containing multiple ions, reducing interference from other ions, improving the adsorption performance of rubidium and cesium, reducing radioactive pollution, and thus improving environmental benefits. Carbonized biomass carbon aerogel has good chemical stability and mechanical strength, maintaining structural integrity in the leachate environment, and is not easily broken or dissolved, thus ensuring the stability and repeatability of the adsorption process, making it an excellent material for environmental remediation. It can also be reused through elution, resulting in good economic benefits.

[0079] Second Embodiment

[0080] Please refer to the following: Figures 2-11The present invention also provides an adsorbent preparation apparatus for adsorbing rubidium and cesium from lepidolite leachate, applied in the method for preparing the adsorbent for adsorbing rubidium and cesium from lepidolite leachate, for preparing the adsorbent for adsorbing rubidium and cesium from lepidolite leachate, comprising: a base 1, a support assembly 2 mounted on the top of the base 1, a water bath 3 mounted on the support assembly 2, a reaction vessel 4 mounted inside the water bath 3, a stirring assembly 5 mounted on the reaction vessel 4, the stirring assembly 5 being used for stirring during the alkaline boiling treatment of the material, and a driving assembly 6 mounted on the top of the reaction vessel 4, the driving assembly 6 being used for... The stirring assembly 5 is driven to rotate. A feed trough 7 is installed on the top of the reactor 4, and a discharge trough 8 is installed on the bottom of the reactor 4. A positioning hole 9 is provided on the discharge trough 8. A sealing conversion assembly 10 is installed on the base 1. The sealing conversion assembly 10 is used to abut against the discharge trough 8 to seal the discharge trough 8. A pushing assembly 11 is installed at the bottom of the base 1. The pushing assembly 11 is used to drive the sealing conversion assembly 10 to rotate to achieve angle adjustment. A cleaning assembly 12 is installed at the bottom of the reactor 4. The cleaning assembly 12 is used to clean the sealing conversion assembly 10.

[0081] In this embodiment, a heat insulation layer is provided on the reactor 4 to keep it warm.

[0082] In this embodiment, an electric heating wire is installed inside the water bath 3 and connected to an external power source via a control switch to heat the medium inside the water bath 3. The water bath 3 is also equipped with an inlet valve and an outlet valve for changing the medium.

[0083] In this embodiment, the device is connected to an external power source via a control panel, and all electrical components within the device are powered by an external power source.

[0084] Please refer to the following: Figure 5 The support assembly 2 includes a support plate 21, a sliding rod 22, a fixed frame 23, a sliding plate 24, a connecting rod 25, a first elastic element 26, a first magnetic block 27, and a second magnetic block 28. The bottom of the support plate 21 is fixed to the base 1. The sliding rod 22 passes through and is slidably connected to the support plate 21. The fixed frame 23 is installed on the support plate 21. The sliding plate 24 is slidably connected to the inside of the fixed frame 23. One end of the connecting rod 25 is fixed to one side of the sliding plate 24, and the other end of the connecting rod 25 is fixed to the water bath 3. The first elastic element 26 is installed between the sliding plate 24 and the side wall of the fixed frame 23. The first magnetic block 27 is fixed to the sliding plate 24, and the second magnetic block 28 is fixed to the side wall of the fixed frame 23.

[0085] Preferably, there are two sliding rods 22, the sliding direction of the sliding rods 22 is horizontal, and there are two first elastic elements 26.

[0086] In this embodiment, the first elastic element 26 includes, but is not limited to, a spring, an elastic rib, and a pneumatic telescopic cylinder, and only needs to provide a rebound effect when the sliding plate 24 moves to the right.

[0087] In this embodiment, the first magnetic block 27 and the second magnetic block 28 are opposite each other with the same pole. When the first magnetic block 27 moves toward the second magnetic block 28, it can generate a repulsive force.

[0088] In this embodiment, the water bath 3 can be stably supported by two sliding rods 22, that is, the reaction vessel 4 can be supported.

[0089] In use, when the reactor 4 moves to the right, it indirectly causes the connecting rod 25 to move to the right, thereby driving the sliding plate 24 to move to the right, which in turn squeezes the first elastic element 26 and causes the first magnetic block 27 to approach the second magnetic block 28 and generate a repulsive force. The elastic force of the first elastic element 26 and the repulsive force between the first magnetic block 27 and the second magnetic block 28 facilitate the reset of the sliding plate 24, that is, facilitate the reset of the reactor 4, thus providing space for horizontal reciprocating motion.

[0090] Please refer to the following: Figure 6 The stirring assembly 5 includes a stirring shaft 51, stirring blades 52, and a limiting sleeve 53. The stirring shaft 51 is rotatably connected to the reaction vessel 4, the stirring blades 52 are fixed to the outer surface of the stirring shaft 51, and the limiting sleeve 53 is fixed to the top end of the stirring shaft 51.

[0091] In this embodiment, the limiting block 66 is adapted to the limiting sleeve 53, and the inner holes of the limiting block 66 and the limiting sleeve 53 are rectangular or other irregular shapes other than circles.

[0092] In this embodiment, there are two stirring rods 52, one located in the middle of the stirring shaft 51 and the other located at the bottom of the stirring shaft 51, which can cover the entire interior of the reactor 4 during stirring.

[0093] In the initial state, the limiting block 66 is inserted into the inside of the limiting sleeve 53.

[0094] Please refer to the following: Figure 10 (a) and Figure 11 (a) In the initial state, the sealing plate 102 seals the discharge chute 8. When in use, when the driving component 62 drives the limiting block 66 to rotate, it can drive the limiting sleeve 53 to rotate, thereby causing the stirring shaft 51 to rotate, which in turn drives the stirring blade 52 to rotate for stirring, so that the device is in the stirring state.

[0095] Please refer to the following: Figure 6 and Figure 7 The drive assembly 6 includes a mounting frame 61, a drive component 62, a sleeve shaft 63, a cam 64, a sliding shaft 65, a limiting block 66, a moving plate 67, a displacement block 68, a guide rail 69, and a second elastic element 610. The mounting frame 61 is fixed to the reactor 4, the drive component 62 is fixed to the mounting frame 61, the sleeve shaft 63 is fixed to the output shaft of the drive component 62, the cam 64 is fixed to the outer surface of the sleeve shaft 63, the sliding shaft 65 is slidably connected to the inner surface of the sleeve shaft 63, the limiting block 66 is fixed to the bottom end of the sleeve shaft 63, the moving plate 67 is rotatably connected to the outer surface of the sliding shaft 65, the displacement block 68 is fixed to the bottom of the moving plate 67, the guide rail 69 is fixed to the reactor 4, the displacement block 68 is slidably connected to the guide rail 69, and the second elastic element 610 is installed between the displacement block 68 and the guide rail 69.

[0096] In this embodiment, the driving component 62 includes, but is not limited to, an electric motor, a hydraulic motor, or a pneumatic motor, as long as it can drive the sleeve shaft 63 to rotate.

[0097] In this embodiment, the second elastic element 610 includes, but is not limited to, springs, elastic ribs, and pneumatic telescopic cylinders, and only needs to provide a rebound effect when the displacement block 68 moves upward.

[0098] In this embodiment, the sliding direction of the sliding shaft 65 is vertical, and it can extend and retract inside the sleeve shaft 63.

[0099] In one embodiment, an anti-rotation structure is provided between the sliding shaft 65 and the sleeve shaft 63. The anti-rotation structure includes an anti-rotation block and an anti-rotation groove. The anti-rotation block is fixed to the outer surface of the sliding shaft 65, and the anti-rotation groove is opened in the vertical direction on the inner surface of the sleeve shaft 63. The anti-rotation block is slidably connected inside the anti-rotation groove, which can ensure that the sliding shaft 65 can rotate with the sleeve shaft 63 while extending and retracting vertically.

[0100] In use, the rotation of the drive component 62 drives the sleeve shaft 63 to rotate, thereby causing the cam 64 to rotate, and causing the sliding shaft 65 to rotate, which in turn drives the limiting block 66 to rotate. The limiting block 66 is used to control the rotation of the stirring shaft 51. When the moving plate 67 is not squeezed by the inclined block 1011, the moving plate 67 is in its initial position. Due to gravity and the elastic force of the second elastic element 610, the limiting block 66 is placed inside the limiting sleeve 53. Thus, the rotation of the sleeve shaft 63 enables the stirring shaft 51 to rotate. When the moving plate 67 is squeezed upward by the inclined block 1011, it will drive the sliding shaft 65 to move upward, thereby causing the limiting block 66 to separate from the limiting sleeve 53. As a result, the stirring shaft 51 will not rotate, and only the cam 64 will rotate alone.

[0101] In this embodiment, the guide rail 69 provides vertical guidance for the displacement block 68, thereby ensuring that the moving plate 67 moves vertically.

[0102] When the movable plate 67 moves upward under the pressure of the inclined block 1011, it will drive the displacement block 68 to move upward and press the second elastic member 610. When the inclined block 1011 leaves the movable plate 67, the second elastic member 610 will cause the displacement block 68 to move downward, thereby driving the movable plate 67 to reset and providing a stable downward force to the movable plate 67.

[0103] Please refer to the following: Figure 8 The sealing and conversion assembly 10 includes a rotating shaft 101, a sealing plate 102, a filter plate 103, a through hole 104, a sliding groove 105, a sealing block 106, an abutment block 107, a positioning block 108, a groove 109, a third elastic element 1010, an inclined block 1011, a connecting plate 1012, and a contact plate 1013. The rotating shaft 101 is rotatably connected to the base 1. The sealing plate 102 is fixed to the outer surface of the rotating shaft 101. The filter plate 103 is mounted on the sealing plate 102. The through hole 104 is formed on the sealing plate 102. The sliding groove 105 is provided in the... On the sealing plate 102, the sealing block 106 is slidably connected in the groove 105, the abutment block 107 is fixed on the sealing block 106, the positioning block 108 is fixed on the abutment block 107, the groove 109 is formed on the sealing plate 102, the third elastic member 1010 is installed between the side wall of the sealing block 106 and the groove 109, the inclined block 1011 is fixed on the outer surface of the rotating shaft 101, the connecting plate 1012 is fixed on the top end of the rotating shaft 101, and the contact plate 1013 is fixed on the connecting plate 1012.

[0104] In this embodiment, the filter plate 103, through hole 104, and sealing block 106 are all arranged around the axis of the rotating shaft 101, and can be stably moved to the bottom of the discharge trough 8 by rotating the rotating shaft 101.

[0105] Preferably, the filter plate 103 and the sealing plate 102 are detachably connected by a snap-fit ​​or bolt.

[0106] Preferably, both the sealing plate 102 and the sealing block 106 are provided with sealing gaskets to ensure the sealing performance.

[0107] In this embodiment, the third elastic element 1010 includes, but is not limited to, a spring, an elastic rib, and a pneumatic telescopic cylinder, and only needs to provide a rebound effect when the positioning and sealing block 106 moves to the right.

[0108] In this embodiment, the positioning block 108 is adapted to the positioning hole 9.

[0109] Please refer to the following: Figure 10 (b) and Figure 11 (b) Under the stirring state, the first push of the push component 11 will drive the rotating shaft 101 to rotate, causing the sealing plate 102 to swing for the first time, and then the filter plate 103 will align with the discharge trough 8 after circumferential movement, so that the device is in the filtering state and can realize solid-liquid separation.

[0110] Please refer to the following: Figure 10 (c) and Figure 11 (c) Based on the filtration state, by pushing the component 11 again, the rotating shaft 101 will be driven to rotate further, causing the sealing plate 102 to swing twice, and then the through hole 104 will be aligned with the discharge chute 8 after circumferential movement, so that the device is in the discharge state and the filter residue can be discharged.

[0111] Please refer to the following: Figure 10 (d) and Figure 11 (d) In the discharge state, by pushing component 11 again, the rotating shaft 101 will rotate again, causing the sealing plate 102 to swing three times. This causes the sealing block 106 to move in a circular motion to the bottom of the discharge trough 8, and the contact block 107 to abut against the discharge trough 8, so that the positioning block 108 is engaged and fixed with the positioning hole 9. At this time, the inclined block 1011 will also abut against the moving plate 67, and the inclined surface will cause the moving plate 67 to move upward, driving the sliding shaft 65 to move upward, thereby driving the limiting block 66 and... When the limiting sleeve 53 separates, the connecting plate 1012 will rotate with the rotating shaft 101, causing the contact plate 1013 to rotate to the left side of the cam 64. When the cam 64 rotates, its protrusion will move to the left side and abut against the contact plate 1013 to move the reactor 4 to the right. When the protrusion of the cam 64 returns to the right side, it will work with the elastic force of the first elastic element 26 and the repulsive force between the first magnetic block 27 and the second magnetic block 28 to reset the reactor 4, thereby performing left and right reciprocating motion, so that the device is in an oscillating state.

[0112] In this embodiment, the sliding connection of the sealing block 106 ensures that the discharge trough 8 is always blocked when the reactor 4 reciprocates left and right. When the sealing block 106 moves to the bottom of the discharge trough 8 to block the discharge trough 8, the direction of the slide 105 and the moving direction of the discharge trough 8 are on the same reference plane.

[0113] In the initial state of the pushing component 11 and in the first two pushing states, the position of the contact plate 1013 after it moves will not contact the cam 64.

[0114] Please refer to it again. Figure 8The pushing assembly 11 includes a pushing member 111, a moving block 112, a first spur tooth plate 113, and a first gear 114. The pushing member 111 is installed on the bottom of the base 1, the moving block 112 is slidably connected to the bottom of the base 1, the output end of the pushing member 111 is fixedly connected to the moving block 112, the first spur tooth plate 113 is fixed on the moving block 112, and the first gear 114 is installed on the outer surface of the rotating shaft 101, and the outer surface of the first spur tooth plate 113 meshes with the outer surface of the first gear 114.

[0115] In this embodiment, the pushing component 111 includes, but is not limited to, a cylinder, a hydraulic cylinder, an electric telescopic rod, and a linear motor, which only needs to drive the moving block 112 to move linearly left and right in the horizontal direction.

[0116] In use, the pusher 111 can drive the moving block 112 to move to the left, thereby driving the first gear 114 to rotate, which in turn drives the rotating shaft 101 to rotate. When the pusher 111 retracts and drives the moving block 112 to move to the right, it can drive the first gear 114 to rotate in the opposite direction, thereby driving the rotating shaft 101 to rotate in the opposite direction and reset.

[0117] Please refer to the following: Figure 2 The cleaning assembly 12 includes a connecting shaft 121, a second gear 122, a cleaning brush 123, and a second straight toothed plate 124. The connecting shaft 121 is rotatably connected to the bottom of the reactor 4. The second gear 122 is fixed to the outer surface of the connecting shaft 121. The cleaning brush 123 is fixed to the bottom end of the connecting shaft 121. The second straight toothed plate 124 is fixed to the support plate 21 and meshes with the outer surface of the second gear 122.

[0118] In this embodiment, as the sealing plate 102 swings, the sealing block 106 moves to the bottom of the discharge trough 8 and seals it. At this time, the filter plate 103 will move to the bottom of the cleaning brush 123. Through the reciprocating motion of the reactor 4, the cleaning brush 123 can be driven to clean the filter plate 103 back and forth.

[0119] When the cleaning brush 123 reciprocates, the second gear 122 rolls on the tooth surface of the second straight tooth plate 124, thus rotating. This causes the connecting shaft 121 to rotate, driving the cleaning brush 123 to rotate. This allows the reciprocating motion to be combined with the rotation, improving the cleaning effect.

[0120] The bristles of the cleaning brush 123 are in direct contact with the surface and pore walls of the filter plate 103. Through the hardness of the bristles and the pressure during brushing, the attached filter residue is peeled off from the filter plate 103. The bristles can penetrate into the tiny pores of the filter plate 103 to remove the small blockages stuck in the pores, restore the filtration channels of the filter plate 103, and avoid the decrease in filtration efficiency due to pore blockage.

[0121] If the filter residue is tightly compacted or penetrates deep into the pores of the filter plate 103, it needs to be used in conjunction with other methods such as water washing and air blowing, or the filter plate 103 can be disassembled and replaced.

[0122] The working principle of the adsorbent preparation method and apparatus for adsorbing rubidium and cesium from lepidolite leachate provided by this invention is as follows:

[0123] Corn stalk powder and NaOH solution are added into reaction vessel 4. The stirring component 5 is rotated by the drive component 6 to make the corn stalk powder and NaOH solution react fully.

[0124] After the reaction is completed, the first push of the push component 11 causes the sealing and conversion component 10 to rotate, thereby causing the sealing plate 102 to swing for the first time, which in turn makes the filter plate 103 aligned with the discharge trough 8, thereby achieving solid-liquid separation and obtaining filter residue.

[0125] After solid-liquid separation, the sealing and conversion component 10 is rotated again by pushing component 11 a second time, which causes the sealing plate 102 to swing a second time, so that the through hole 104 is aligned with the discharge trough 8, thereby discharging the filter residue. The filter residue is then processed to obtain carbonized biomass carbon aerogel (during which the sealing plate 102 can be reset by pushing component 11 to seal the discharge trough 8, and titanate, silane and anhydrous ethanol are added to the reaction vessel 4 and stirred in the same way to form a transparent solution for later use).

[0126] By pushing component 11 three times, the sealing conversion component 10 rotates further, thereby causing the sealing plate 102 to swing three times, so that the sealing block 106 seals the discharge trough 8, and the positioning block 108 engages with the positioning hole 9, so that the contact block 107 is fixed to the discharge trough 8, thus ensuring that the sealing block 106 always seals the discharge trough 8. While the sealing conversion component 10 rotates, the inclined block 1011 lifts the moving plate 67 through the inclined surface, thereby separating the driving component 6 from the stirring component 5. At this time, the contact plate 1013 moves to the left side of the cam 64, adding the transparent solution carbonized biomass carbon aerogel into the reactor 4. Then, the driving component 6 rotates, causing the cam 64 to rotate and abut against the contact plate 1013, thereby realizing the left and right reciprocating motion of the reactor 4, thus performing the oscillation operation. After the oscillation is completed, subsequent processing is carried out to obtain the adsorbent.

[0127] Compared with related technologies, the method and apparatus for preparing adsorbent for adsorbing rubidium and cesium from lepidolite leachate provided by the present invention have the following advantages:

[0128] This invention utilizes the first push of the pushing component 11 to cause the sealing plate 102 to swing for the first time, moving the filter plate 103 to the bottom of the discharge trough 8, thereby achieving a filtering effect. The second push of the pushing component 11 causes the sealing plate 102 to swing a second time, moving the through hole 103 to contact the discharge trough 8, achieving a discharge effect. The third push of the pushing component 11 causes the sealing plate 103 to swing a third time, causing the sealing block 106 to seal and fix the discharge trough 8. At this time, the inclined block 1011 lifts the moving plate 67, separating the driving component 6 from the stirring component 5 to avoid power reduction. The contact plate 1013 moves to the left side of the cam 64, and the rotation of the cam 64 causes the reaction vessel 4 to reciprocate left and right, thus performing an oscillation operation. This invention integrates multiple functions, achieving switching between different states through the multiple extensions or contractions of the pushing component 11, enabling the device to quickly perform relevant processing steps. The operation is simple and convenient, improving the treatment efficiency of the adsorbent.

[0129] 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 method for preparing an adsorbent for adsorbing rubidium and cesium from lepidolite leachate, characterized in that, Includes the following steps: S1. Weigh the straw powder and treat it with alkali boiling. S2. Filter while hot and collect the filter residue, wash with deionized water and dry; S3. Transfer the filter residue to a high-pressure reactor, add deionized water to carry out a hydrothermal reaction, and obtain the reaction product. S4. Wash the reaction product alternately with deionized water and ethanol to obtain biomass carbon wet gel. S5. Cut the biomass carbon wet gel into small pieces, place them in a refrigerator for pre-freezing, and then transfer them to a freeze dryer to dry them to obtain porous biomass carbon dry gel. S6. The porous biomass carbon dry gel is placed in a tube furnace and carbonized under a nitrogen atmosphere to obtain carbonized biomass carbon aerogel. S7. Weigh out titanate and silane in a certain proportion, dissolve them in anhydrous ethanol, and stir until transparent to obtain a transparent solution; S8. Immerse the prepared carbonized biomass carbon aerogel in a transparent solution and shake. S9. Add KOH solutions of different concentrations and continue shaking to obtain a mixed solution; S10. The mixture is transferred to a high-pressure reactor for hydrothermal reaction, washed and dried to obtain potassium titanate modified carbonized biomass carbon aerogel, which is the adsorbent used to adsorb rubidium and cesium from lepidolite leachate.

2. The method for preparing an adsorbent for adsorbing rubidium and cesium from lepidolite leachate according to claim 1, characterized in that, The alkaline boiling treatment in S1 uses a 5% NaOH solution, heated and stirred in a water bath at 80°C for 2 hours.

3. The method for preparing an adsorbent for adsorbing rubidium and cesium from lepidolite leachate according to claim 1, characterized in that, In S7, the titanate is tetrabutyl titanate, and the silane is tetraethoxysilane. The molar ratio of titanate to silane in S7 is 2:1, 1:1, or 1:

2.

4. An apparatus for preparing an adsorbent for adsorbing rubidium and cesium from a lepidolite leachate, used in the method for preparing an adsorbent for adsorbing rubidium and cesium from a lepidolite leachate as described in any one of claims 1-3, for preparing the adsorbent for adsorbing rubidium and cesium from a lepidolite leachate, characterized in that, include: The base has a support assembly mounted on its top, a water bath mounted on the support assembly, a reaction vessel mounted inside the water bath, a stirring assembly mounted on the reaction vessel for stirring materials during alkaline boiling treatment, a drive assembly mounted on the top of the reaction vessel for driving the stirring assembly to rotate, a feed chute mounted on the top of the reaction vessel, and a discharge chute mounted on the bottom of the reaction vessel with a positioning hole, a sealing conversion assembly mounted on the base for abutting against the discharge chute to seal it, a push assembly mounted on the bottom of the base for driving the sealing conversion assembly to rotate for angle adjustment, and a cleaning assembly mounted on the bottom of the reaction vessel for cleaning the sealing conversion assembly.

5. The adsorbent preparation apparatus for adsorbing rubidium and cesium from lepidolite leachate according to claim 4, characterized in that, The support assembly includes a support plate, a sliding rod, a fixed frame, a sliding plate, a connecting rod, a first elastic element, a first magnetic block, and a second magnetic block. The bottom of the support plate is fixed to the base. The sliding rod passes through and is slidably connected to the support plate. The fixed frame is mounted on the support plate, and the sliding plate is slidably connected inside the fixed frame. One end of the connecting rod is fixed to one side of the sliding plate, and the other end is fixed to the water bath. The first elastic element is installed between the sliding plate and the side wall of the fixed frame. The first magnetic block is fixed to the sliding plate, and the second magnetic block is fixed to the side wall of the fixed frame.

6. The adsorbent preparation apparatus for adsorbing rubidium and cesium from lepidolite leachate according to claim 4, characterized in that, The stirring assembly includes a stirring shaft, stirring blades, and a limiting sleeve. The stirring shaft is rotatably connected to the reactor, the stirring blades are fixed to the outer surface of the stirring shaft, and the limiting sleeve is fixed to the top of the stirring shaft.

7. The adsorbent preparation apparatus for adsorbing rubidium and cesium from lepidolite leachate according to claim 6, characterized in that, The drive assembly includes a mounting frame, a drive component, a sleeve shaft, a cam, a sliding shaft, a limiting block, a moving plate, a displacement block, a guide rail, and a second elastic element. The mounting frame is fixed to the reactor vessel, the drive component is fixed to the mounting frame, the sleeve shaft is fixed to the output shaft of the drive component, the cam is fixed to the outer surface of the sleeve shaft, the sliding shaft is slidably connected to the inner surface of the sleeve shaft, the limiting block is fixed to the bottom end of the sleeve shaft, the moving plate is rotatably connected to the outer surface of the sliding shaft, the displacement block is fixed to the bottom of the moving plate, the guide rail is fixed to the reactor vessel, the displacement block is slidably connected to the guide rail, and the second elastic element is installed between the displacement block and the guide rail.

8. The adsorbent preparation apparatus for adsorbing rubidium and cesium from lepidolite leachate according to claim 4, characterized in that, The blocking and conversion assembly includes a rotating shaft, a blocking plate, a filter plate, a through hole, a sliding groove, a blocking block, a contact block, a positioning block, a groove, a third elastic element, an inclined block, a connecting plate, and a contact plate. The rotating shaft is rotatably connected to the base. The blocking plate is fixed to the outer surface of the rotating shaft. The filter plate is mounted on the blocking plate. The through hole is formed on the blocking plate. The sliding groove is set on the blocking plate. The blocking block is slidably connected in the sliding groove. The contact block is fixed on the blocking block. The positioning block is fixed on the contact block. The groove is formed on the blocking plate. The third elastic element is installed between the blocking block and the side wall of the groove. The inclined block is fixed to the outer surface of the rotating shaft. The connecting plate is fixed to the top end of the rotating shaft. The contact plate is fixed to the connecting plate.

9. The adsorbent preparation apparatus for adsorbing rubidium and cesium from lepidolite leachate according to claim 8, characterized in that, The pushing assembly includes a pushing member, a moving block, a first spur gear plate, and a first gear. The pushing member is installed at the bottom of the base, the moving block is slidably connected to the bottom of the base, the output end of the pushing member is fixedly connected to the moving block, the first spur gear plate is fixed on the moving block, and the first gear is installed on the outer surface of the rotating shaft. The first spur gear plate meshes with the outer surface of the first gear.

10. The adsorbent preparation apparatus for adsorbing rubidium and cesium from lepidolite leachate according to claim 5, characterized in that, The cleaning assembly includes a connecting shaft, a second gear, a cleaning brush, and a second straight toothed plate. The connecting shaft is rotatably connected to the bottom of the reactor. The second gear is fixed to the outer surface of the connecting shaft. The cleaning brush is fixed to the bottom end of the connecting shaft. The second straight toothed plate is fixed to the support plate and meshes with the outer surface of the second gear.

Images