A method for extracting and separating tantalum and niobium

Abstract

The application provides a method for extracting and separating tantalum and niobium, and relates to the technical field of tailing treatment.The method comprises the following steps: step A1, a proper amount of oxalic acid is weighed and dissolved in deionized water, and after dissolving, the oxalic acid solution with a certain concentration is prepared by transferring into a volumetric flask; step A2, a certain amount of tantalum standard solution and niobium standard solution are respectively taken and added into the prepared oxalic acid solution; step A3, hydrochloric acid solution is added to adjust PH; step A4, a proper amount of DOAP is weighed and added into chloroform, and after being fully stirred and dissolved, the DOAP chloroform solution is prepared; step A5, the water phase and the organic phase are respectively measured by using a pipette, and are added into a separatory funnel according to a certain volume ratio; and step A6, the separatory funnel is placed in a constant-temperature oscillator to oscillate, so that the two phases are fully contacted. The scheme finally realizes the process of simplifying the extraction and separation of tantalum and niobium, reduces the cost, and improves the recovery rate.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of tailings treatment, and particularly relates to a method for extracting and separating tantalum and niobium. BACKGROUND

[0002] With the continuous development of science and technology, the demand for rare metals such as tantalum and niobium is increasing. Efficient and green extraction and separation of tantalum and niobium is of great significance to guarantee national strategic resource security and promote the development of high-tech industries. At the same time, developing new extraction and separation technologies can reduce environmental pollution and achieve sustainable use of resources, which meets the requirements of sustainable social and economic development. Tantalum (Ta) and niobium (Nb) are refractory rare metals with high melting point (tantalum melting point 2996℃, niobium melting point 2468℃), high boiling point, high hardness, strong corrosion resistance and other characteristics. They are often coexisting in nature due to their similar chemical properties. Their similar outer electron structures make their behaviors similar in many chemical reactions, which also brings great challenges to separation and purification.

[0003] The prior art has low comprehensive utilization rate in the tailings treatment process. The tailings contain valuable metals such as tantalum, niobium, lithium and non-metallic resources such as feldspar and quartz, but the recovery target is single and secondary emissions are common. The flotation process has limitations. Fine-grained tantalum and niobium flotation needs to rely on high-priced collectors, and the removal effect of iron impurities is limited, which affects the quality of subsequent products.

[0004] In the existing extraction method, comprehensive environmental protection, economy and resource utilization rate are considered. It is urgent to optimize the current reaction parameters to improve the leaching rate. New extractants are developed to develop high selectivity and low toxicity extractants to meet the market demand for simplifying the process and reducing the cost of extracting and separating tantalum and niobium.

[0005] Therefore, it is necessary to provide a method for extracting and separating tantalum and niobium to solve the above technical problems. SUMMARY

[0006] The present application provides a method for extracting and separating tantalum and niobium, which solves the problem of optimizing the process and cost of extracting and separating tantalum and niobium in the related art.

[0007] To solve the above technical problems, the method for extracting and separating tantalum and niobium provided by the present application comprises the following steps:

[0008] Step A1, a certain amount of oxalic acid is weighed and dissolved in deionized water, and then transferred to a volumetric flask to prepare an oxalic acid solution with a certain concentration;

[0009] Step A2, a certain amount of tantalum standard solution and niobium standard solution are respectively taken and added to the prepared oxalic acid solution;

[0010] Step A3, adjust PH by adding hydrochloric acid solution;

[0011] Step A4, weigh a proper amount of DOAP, add into chloroform, stir well to dissolve, prepare DOAP chloroform solution;

[0012] Step A5, use pipette to measure water phase and organic phase respectively, add into separatory funnel according to certain volume ratio;

[0013] Step A6, put separatory funnel into constant temperature shaker, shake to make two phases contact well;

[0014] Step A7, after shaking, take out separatory funnel, centrifuge to separate organic phase and water phase, collect into clean conical flask respectively;

[0015] Step A8, take separated organic phase, add equal volume of nitric acid as stripping agent, put into separatory funnel;

[0016] Step A9, shake to transfer tantalum from organic phase to water phase, after centrifugation, collect water phase containing tantalum;

[0017] Step A10, add equal volume of mixed solution of nitric acid and oxalic acid as stripping agent to residual organic phase;

[0018] Step A11, after shaking and centrifugation, collect water phase containing niobium.

[0019] Preferably, the water phase is oxalic acid metal solution, and the organic phase is DOAP chloroform solution.

[0020] Preferably, the concentration of oxalic acid solution in step A1 is 0.1-1.0 M.

[0021] Preferably, the concentration of tantalum and niobium in the oxalic acid solution in step A2 is 100-500 mg / L.

[0022] Preferably, the PH in step A3 is 1.0-3.0.

[0023] Preferably, the concentration of DOAP chloroform solution in step A4 is 0.1-0.5 M.

[0024] Preferably, the volume ratio in step A5 is 1:1-3:1.

[0025] Preferably, the shaking time in step A6 is 10-30 min, and the constant temperature is 24-26℃.

[0026] Preferably, the DOAP is di-n-octylamino propanol, and its preparation method is as follows:

[0027] Step B1: Add dioctylamine and solvent to a three-necked flask and stir to dissolve;

[0028] Step B2: Slowly add the catalyst and continue stirring until completely dissolved;

[0029] Step B3: Install the constant pressure dropping funnel, condenser and thermometer, and ensure the device is sealed;

[0030] Step B4: Raise the oil bath temperature to a certain temperature and maintain the reaction system at a constant temperature;

[0031] Step B5: Slowly add propylene oxide dropwise through a constant pressure dropping funnel;

[0032] Step B6: After the addition is complete, continue stirring the reaction until there is no obvious exothermic phenomenon.

[0033] Step B7: After the reaction solution has cooled to room temperature, slowly add 1 M HCl to adjust the pH.

[0034] Step B8: Transfer the solution to a separatory funnel and add the extractant to extract the product;

[0035] Step B9: Combine the organic phases, add a desiccant, and filter to remove the desiccant;

[0036] Step B10: Place the organic phase in a vacuum distillation apparatus and remove the extractant under normal pressure;

[0037] Step B11: Adjust the vacuum level, raise the temperature, and collect the distillate to obtain di-n-octylaminopropanol.

[0038] Preferably, the constant temperature oscillator in step A6 includes a constant temperature chamber and an oscillation device, wherein the oscillation device is integrated and installed in the constant temperature area of ​​the constant temperature chamber.

[0039] Compared with related technologies, the method for extracting and separating tantalum and niobium provided by the present invention has the following beneficial effects:

[0040] During the extraction process, these complexes transfer from the aqueous phase to the organic phase, thereby separating niobium and tantalum from the metal oxalate solution. By adjusting conditions such as the acidity and DOAP concentration of the aqueous phase, the selectivity and efficiency of the extraction can be improved. Subsequently, a back-extraction agent can be used to transfer niobium and tantalum back from the organic phase to the aqueous phase, achieving further separation and enrichment.

[0041] The protonated DOAP cation complexes with the oxalate ion to form a hydrophobic ion pair, which is then transferred to the organic phase (chloroform) by extraction. The long alkyl chain (dioctyl) of DOAP enhances its hydrophobicity, and the propanol group provides additional coordination sites, improving its complexation ability with niobium and tantalum.

[0042] Ultimately, this will simplify the extraction and separation process of tantalum and niobium, reduce costs, and improve recovery rates. Attached Figure Description

[0043] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the structures shown in these drawings without creative effort.

[0044] Figure 1 A flowchart of a method for extracting and separating tantalum and niobium provided by the present invention;

[0045] Figure 2 A flowchart of the method for preparing di-n-octylaminopropanol provided by the present invention;

[0046] Figure 3 A three-dimensional diagram of the constant temperature oscillator provided by the present invention;

[0047] Figure 4 for Figure 3 A schematic cross-sectional view of the support cover connection section shown.

[0048] Figure 5 for Figure 4 The top view of the connecting slider section shown;

[0049] Figure 6 for Figure 3 A schematic diagram of the structure of section AA shown;

[0050] Figure 7 for Figure 6 The enlarged schematic diagram of part A shown below;

[0051] Figure 8 for Figure 6 The enlarged schematic diagram of section B is shown below;

[0052] Figure 9 for Figure 4 The diagram shows the structure of the lifting plate in the unlocked state.

[0053] Figure 10 The schematic diagram of the unlocking principle of the constant temperature oscillator provided by the present invention, wherein, Figure 10 (a) in the diagram is a structural schematic of the lifting plate in the assembled connection state. Figure 10 (b) is a structural diagram of the lifting plate state switching process. Figure 10 (c) in the diagram is a schematic diagram of the lifting plate in the separated and replaceable state;

[0054] Figure 11 for Figure 6 The braking principle of the locking plate shown is as follows: Figure 11 (a) in the middle is Figure 10 A schematic diagram of the locking plate in state (a) is shown. Figure 11 (b) in the middle is Figure 10 A schematic diagram of the locking plate in state (b) is shown. Figure 11 (c) in the middle is Figure 10 A schematic diagram of the locking plate in state (c) is shown.

[0055] Figure 12 A three-dimensional diagram of a preferred embodiment of the isothermal oscillator provided by the present invention.

[0056] Explanation of icon numbers:

[0057] 1. Vibration mechanism; 11. Drive housing; 12. Vibration frame; 13. Support cover; 131. Limiting slide rail; 132. Elastic support component;

[0058] 2. Mounting mechanism; 21. Connecting slider; 20. Mounting cavity; 201. Limiting groove;

[0059] 3. Assembly mechanism; 31. Fixing plate; 32. First telescopic component; 33. Lifting plate; 34. Drive shaft; 35. Drive frame; 350. Drive inclined hole;

[0060] 4. Venting mechanism; 41. Venting component; 411. Venting hole; 412. Sliding cavity; 413. Switch plate; 414. Second telescopic component; 415. Transmission rod; 42. Connecting hose; 43. Connecting rubber plug; 44. Pressure sensor;

[0061] 5. Locking mechanism; 51. Third telescopic component; 52. Synchronization plate; 53. Locking plate;

[0062] 100. Separatory funnel bottle.

[0063] The realization of the objective, functional features and advantages of the present invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation

[0064] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0065] This invention provides a method for extracting and separating tantalum and niobium.

[0066] Please see Figure 1 In one embodiment of the present invention, the method for extracting and separating tantalum and niobium includes the following steps:

[0067] Step A1: Weigh an appropriate amount of oxalic acid and dissolve it in deionized water. After dissolving, transfer the solution to a volumetric flask to prepare an oxalic acid solution of a certain concentration.

[0068] Step A2: Take a certain amount of tantalum standard solution and niobium standard solution respectively and add them to the oxalic acid solution prepared above;

[0069] Step A3: Add hydrochloric acid solution to adjust the pH;

[0070] Step A4: Weigh an appropriate amount of DOAP, add it to chloroform, stir thoroughly to dissolve, and prepare a DOAP chloroform solution;

[0071] Step A5: Use a pipette to measure the aqueous phase and organic phase separately, and add them to the separatory funnel according to a certain volume ratio;

[0072] Step A6: Place the separatory funnel in a constant temperature shaker and shake it to ensure that the two phases are in full contact;

[0073] Step A7: After shaking, remove the separatory funnel, centrifuge to separate the organic phase and the aqueous phase, and collect them separately into clean conical flasks.

[0074] Step A8: Take the separated organic phase, add an equal volume of nitric acid as a back-extraction agent, and place it in a separatory funnel;

[0075] Step A9: Shake to transfer tantalum from the organic phase to the aqueous phase, centrifuge to separate the layers, and collect the aqueous phase containing tantalum;

[0076] Step A10: Add an equal volume of a mixed solution of nitric acid and oxalic acid as a back-extraction agent to the remaining organic phase;

[0077] Step A11: After oscillation and centrifugation to separate the layers, collect the aqueous phase containing niobium.

[0078] The aqueous phase is a metal oxalate solution, and the organic phase is a DOAP chloroform solution.

[0079] The concentration of the oxalic acid solution in step A1 is 0.1-1.0 M.

[0080] The concentrations of tantalum and niobium in the oxalic acid solution in step A2 are 100-500 mg / L.

[0081] In step A3, the pH is 1.0-3.0.

[0082] In step A4, the concentration of the DOAP chloroform solution is 0.1-0.5M.

[0083] The volume ratio in step A5 is 1:1 to 3:1.

[0084] In step A6, the oscillation time is 10-30 minutes and the constant temperature is 24-26℃.

[0085] In step A7, the centrifugation speed is 4000 rpm and the centrifugation time is 5-10 min.

[0086] The concentration of nitric acid in step A8 is 2-6M.

[0087] In step A9, the concentration of nitric acid is 1-3M and the concentration of oxalic acid is 0.1-1.0M.

[0088] In this embodiment, the contents of tantalum and niobium in the aqueous phase before extraction, after extraction, and after back-extraction were determined using ICP-MS or ICP-OES, and the extraction rate was calculated. Each experiment was performed in parallel (at least three times), and the average value was taken as the result to reduce experimental error. The extraction rate varies depending on the extraction conditions; the extraction rate of tantalum can reach 96%-99%, and the extraction rate of niobium can reach 94%-98%.

[0089] In this scheme, the amino and hydroxyl groups in the DOAP molecule can form stable complexes with niobium and tantalum ions in oxalic acid solution. During the extraction process, these complexes are transferred from the aqueous phase to the organic phase, thereby achieving the separation of niobium and tantalum from the oxalic acid metal solution. By adjusting conditions such as the acidity of the aqueous phase and the concentration of DOAP, the selectivity and efficiency of the extraction can be improved. Subsequently, a back-extraction agent can be used to transfer niobium and tantalum back from the organic phase to the aqueous phase, achieving further separation and enrichment.

[0090] In this extraction process, oxalic acid acts as a strong complexing agent, forming stable anionic complexes with niobium and tantalum, inhibiting the hydrolysis of metal ions and increasing their solubility in the aqueous phase. Furthermore, under acidic conditions, the amino group (-NH2) in the DOAP molecule is protonated to generate an ammonium cation, enhancing its electrostatic interaction with the oxalate metal complex anion. The protonated DOAP cation complexes with the oxalate ion to form a hydrophobic ion pair, which is transferred to the organic phase (chloroform) through extraction. The long alkyl chain (dioctyl) of DOAP enhances its hydrophobicity, and the propanol group provides additional coordination sites, improving its complexing ability with niobium and tantalum.

[0091] The method features high extraction efficiency and selectivity. Under optimized conditions (pH 1.0-3.0, DOAP concentration 0.3M, ratio 1:2), tantalum extraction rate can reach 96%-99%, and niobium extraction rate 94%-98%. It is environmentally friendly, avoiding the use of hydrofluoric acid (HF) and reducing the risk of fluoride pollution. The low-toxicity solvent chloroform is used as the extractant, which is less toxic than solvents such as benzene, and can be recycled through distillation. Parameters (such as pH, DOAP concentration, and ratio) can be optimized through single-factor and orthogonal experiments to adapt to different raw material compositions. The conditions are adjustable and support multi-stage extraction. It is suitable for low-grade raw materials (such as tantalum and niobium ore tailings) and has resistance to interference from impurities (such as Fe³⁺ and Al³⁺) in complex systems.

[0092] In this embodiment, as Figure 2 As shown, the DOAP is di-n-octylaminopropanol, and its preparation method is as follows:

[0093] Step B1: Add dioctylamine and solvent to a three-necked flask and stir to dissolve;

[0094] Step B2: Slowly add the catalyst and continue stirring until completely dissolved;

[0095] Step B3: Install the constant pressure dropping funnel, condenser and thermometer, and ensure the device is sealed;

[0096] Step B4: Raise the oil bath temperature to a certain temperature and maintain the reaction system at a constant temperature;

[0097] Step B5: Slowly add propylene oxide dropwise through a constant pressure dropping funnel;

[0098] Step B6: After the addition is complete, continue stirring the reaction until there is no obvious exothermic phenomenon.

[0099] Step B7: After the reaction solution has cooled to room temperature, slowly add 1 M HCl to adjust the pH.

[0100] Step B8: Transfer the solution to a separatory funnel and add the extractant to extract the product;

[0101] Step B9: Combine the organic phases, add a desiccant, and filter to remove the desiccant;

[0102] Step B10: Place the organic phase in a vacuum distillation apparatus and remove the extractant under normal pressure;

[0103] Step B11: Adjust the vacuum level, raise the temperature, and collect the distillate to obtain di-n-octylaminopropanol.

[0104] Example 1:

[0105] A method for preparing di-n-octylaminopropanol (DOAP) involves adding 12.5 g of di-n-octylamine and 50 mL of anhydrous ethanol to a 250 mL three-necked flask, stirring magnetically until completely dissolved, then slowly adding 0.2 g of sodium hydroxide, continuing stirring for 10 minutes until dissolved. A constant-pressure dropping funnel, condenser, and thermometer are installed, ensuring the apparatus is sealed. The oil bath temperature is raised to 45°C, and the system is maintained at a constant temperature. 4.44 g of propylene oxide is slowly added dropwise through the constant-pressure dropping funnel (approximately over 30 minutes), controlling the temperature not to exceed 50°C. After the addition is complete, the reaction is maintained at 45°C with stirring for 3.5 hours. After the reaction solution cools to room temperature, 1 M hydrochloric acid is added dropwise to adjust the pH to 7.0. The solution is transferred to a separatory funnel, 50 mL of dichloromethane is added, the mixture is shaken for 2 minutes, and then allowed to stand for phase separation. This extraction is repeated twice, and the organic phases are combined. Add 5 g of anhydrous magnesium sulfate to the organic phase, shake for 10 minutes, let stand for 2 hours, filter, and transfer the dried organic phase to a distillation flask. First, remove dichloromethane at atmospheric pressure (approximately 40°C). Adjust the vacuum pump to a vacuum level of 5 mmHg, slowly raise the temperature to 140°C, and collect the distillate (DOAP).

[0106] Weigh 49.6 g of oxalic acid, dissolve it in deionized water, and transfer it to a 500 mL volumetric flask. Make up to volume to obtain a 0.8 M oxalic acid solution. Pipette 20 mL of niobium standard solution and 20 mL of tantalum standard solution separately, and add them to the oxalic acid solution to make the concentration of niobium and tantalum both 400 mg / L. Adjust the pH of the solution to 1.8 with 1 M hydrochloric acid. Weigh 11.25 g of DOAP, dissolve it in chloroform, and transfer it to a 250 mL volumetric flask. Make up to volume to obtain a 0.3 M DOAP chloroform solution. Add 40 mL of metal oxalic acid solution (aqueous phase) and 40 mL of DOAP chloroform solution (organic phase) to a 100 mL separatory funnel. Place the separatory funnel in a constant temperature shaker and shake at 28°C for 25 minutes. After shaking, remove the separatory funnel and centrifuge it at 4000 rpm for 5 minutes to separate the two phases into organic and aqueous phases, which are then collected in clean conical flasks.

[0107] Take 40 mL of the extracted organic phase, add 40 mL of 5 M nitric acid as a back-extraction agent, place it in a 100 mL separatory funnel, and shake for 25 minutes to transfer tantalum from the organic phase to the aqueous phase. After centrifugation and separation, collect the aqueous phase containing tantalum. Add 40 mL of a mixed solution of 2.5 M nitric acid and 0.25 M oxalic acid as a back-extraction agent to the remaining organic phase, shake for 25 minutes, centrifuge and separate the layers, and collect the aqueous phase containing niobium.

[0108] The aqueous phases containing tantalum and niobium were analyzed. The concentration of tantalum in the tantalum-containing aqueous phase was 10.6 mg / L, and the extraction rate of tantalum was 97.35%. The concentration of niobium in the niobium-containing aqueous phase was 17.72 mg / L, and the extraction rate of niobium was 95.57%.

[0109] Example 2:

[0110] The preparation steps were the same as in Example 1. During extraction, 40 mL of metal oxalate solution (aqueous phase) and 80 mL of DOAP chloroform solution (organic phase) were added to a 250 mL separatory funnel. The funnel was placed in a constant-temperature shaker and shaken at 28°C for 25 minutes. After shaking, the funnel was removed and centrifuged at 4000 rpm for 5 minutes to separate the two phases, separating the organic and aqueous phases, which were then collected separately in clean Erlenmeyer flasks. The back-extraction procedure was the same as in Example 1.

[0111] The aqueous phases containing tantalum and niobium were analyzed. The concentration of tantalum in the tantalum-containing aqueous phase was 5.32 mg / L, and the extraction rate of tantalum was 98.67%. The concentration of niobium in the niobium-containing aqueous phase was 14.6 mg / L, and the extraction rate of niobium was 96.35%.

[0112] The constant temperature oscillator described in step A6 includes a constant temperature chamber and an oscillation device, wherein the oscillation device is integrated and installed in the constant temperature area of ​​the constant temperature chamber.

[0113] In practical use, existing funnel oscillation equipment only supports funnels of a specific size. When it is necessary to oscillate funnels larger than the current size, it is necessary to purchase a complete set of equipment of the corresponding size. This makes it inconvenient to replace the sample rack without changing the main structure of the oscillation unit.

[0114] To address the aforementioned technical problems, this application also provides an oscillation device to solve the problem of inconvenience in replacing the sample holder without changing the main oscillation structure.

[0115] Please refer to the following: Figures 3 to 5 The oscillation device includes:

[0116] Vibration mechanism 1, the vibration mechanism 1 includes a drive housing 11, a vibration frame 12 and a support cover 13, the vibration frame 12 is installed on the vibration part of the drive housing 11, the vibration frame 12 has a T-shaped structure, the support cover 13 is installed on the drive housing 11, a limiting slide rail 131 is fixed on the support cover 13, and an elastic support member 132 is fixed inside the limiting slide rail 131;

[0117] The mounting mechanism 2 is inserted into the limiting slide rail 131 and slidably connected via a connecting slider 21, the bottom of which abuts against the top of the elastic support member 132.

[0118] Assembly mechanism 3 includes a fixed plate 31, a first telescopic member 32 and a lifting plate 33. The fixed plate 31 is fixedly mounted on the mounting mechanism 2, the fixed part of the first telescopic member 32 is fixedly mounted on the mounting mechanism 2, and the lifting plate 33 is fixedly mounted on the telescopic part of the first telescopic member 32.

[0119] When the lifting plate 33 and the fixing plate 31 are clamped on the vibration frame 12, and the connecting slider 21 is inserted into the range of the limiting slide rail 131, the vibration frame 12 is used to synchronously drive the installation mechanism 2 to vibrate up and down as a whole.

[0120] In this embodiment, the first telescopic member 32 is any one of an electric telescopic rod, a telescopic cylinder, or a hydraulic telescopic cylinder, used to directly drive the lifting plate 33 to adjust its height, so as to facilitate the assembly or replacement of the mounting mechanism 2 on the vibration frame 12.

[0121] The drive housing 11 adopts the existing drive structure of the funnel oscillator, which is used to drive the up-and-down reciprocating oscillation adjustment of the vibration frame 12, providing a power source for the oscillation processing of the separating funnel; the drive housing 11 is integrated with a control panel for starting and stopping the equipment and adjusting the oscillation amplitude.

[0122] In this embodiment, the mounting mechanism 2 is integrated with a rotatable and adjustable sample rack, which is used to assemble and lock the separatory funnel 100 to maintain the stability of the separatory funnel 100 after installation and use.

[0123] In this embodiment, the lifting plate 33 has two usage states:

[0124] like Figure 4 As shown, in the assembled connection state, the fixing plate 31 and the lifting plate 33 are clamped and fixed on the vibration frame 12. The entire mounting mechanism 2 can vibrate up and down synchronously with the vibration frame 12, providing oscillation processing for the separating funnel.

[0125] like Figure 9 As shown, in the separation and replacement state, the lifting plate 33 moves down and separates from the vibration frame 12, and the fixing plate 31 separates from the vibration frame 12 under the elastic support of the elastic support member 132. The continuous movement of the vibration frame 12 does not affect the dismantling of the installation mechanism 2, which facilitates the overall dismantling and replacement of the installation mechanism 2.

[0126] The principle of disassembly and replacement of the entire installation mechanism 2 is as follows:

[0127] When the installation mechanism 2 needs to be disassembled and replaced during continuous oscillation, the first telescopic member 32 is activated. The first telescopic member 32 drives the lifting plate 33 to move downward. After the lifting plate 33 moves downward, it is out of the vibration range of the vibration frame 12. The elastic support member 132 supports the connecting slider 21 upward under the action of elastic support. The connecting slider 21 synchronously drives the entire installation mechanism 2 and the fixing plate 31 to move upward. After the fixing plate 31 moves upward, it is out of the vibration range of the vibration frame 12.

[0128] When the lifting plate 33 is lowered to its fully retracted state, a disassembly gap is reserved between the lifting plate 33 and the vibration range of the vibration frame 12. During disassembly, the mounting mechanism 2 is pulled upwards as a whole, and the mounting mechanism 2 drives the connecting slider 21 to move upwards and out of the range of the limiting slide rail 131. During this period, the lifting plate 33 will not enter the vibration range of the vibration frame 12. Then, the mounting mechanism 2 is pulled horizontally out of the connection range of the vibration frame 12, realizing the quick disassembly of the mounting mechanism 2 as a whole. After disassembly, the mounting mechanism 2 that needs to be replaced can be reinstalled.

[0129] Ultimately, this allows for the quick and easy removal and replacement of the mounting mechanism 2 regardless of whether the vibration frame 12 is in operation, enabling the replacement and use of mounting mechanisms 2 of different specifications on the same vibration mechanism 1, thereby improving the adaptability of the equipment.

[0130] Please refer to the following: Figure 6 and Figure 8 An installation cavity 20 is formed between the installation mechanism 2 and the fixing plate 31. The oscillation device also includes a locking mechanism 5, which includes a third telescopic member 51, a synchronization plate 52, and a locking plate 53. The two ends of the third telescopic member 51 are fixedly connected to the installation mechanism 2 and the synchronization plate 52. The synchronization plate 52 is slidably installed on the installation mechanism 2 and is located within the range of the installation cavity 20. One end of the locking plate 53 is fixed on the synchronization plate 52, and the other end of the locking plate 53 passes through the connecting slider 21 and faces the surface of the limiting slide rail 131.

[0131] In this embodiment, when the locking plate 53 is separated from the limiting slide rail 131, the connecting slider 21 can slide stably between the limiting slide rail 131;

[0132] When the locking plate 53 abuts against the limiting slide rail 131, the connecting slider 21 and the limiting slide rail 131 are damped and decelerated to prevent inertial oscillation during the dismantling of the installation mechanism 2.

[0133] When the lifting plate 33 switches from the assembled connection state to the separated replacement state, the third telescopic component 51 is activated. The third telescopic component 51 drives the synchronous plate 52 to retract. The synchronous plate 52 drives the locking plate 53 to retract and abut against the surface of the limiting slide rail 131. This provides damping braking when the installation mechanism 2 is replaced during the continuous oscillation of the vibration frame 12, effectively preventing the installation mechanism 2 from being affected by inertia and thus affecting the disassembly and replacement during equipment operation.

[0134] After the lifting plate 33 is fully adjusted to the separation and replacement state, the third telescopic member 51 is activated again. The third telescopic member 51 drives the synchronous plate 52 to extend, and the synchronous plate 52 drives the locking plate 53 to extend and separate from the limiting slide rail 131, so as to provide stable removal support after the installation mechanism 2 is stable.

[0135] In a preferred embodiment, the locking plate 53 can also be elastically connected to the synchronization plate 52 via an independent elastic telescopic tube to facilitate elastic braking between the locking plate 53 and the limiting slide rail 131.

[0136] Please refer to the following: Figure 4 and Figure 7 The oscillation device further includes a venting mechanism 4, which includes a venting component 41, a connecting hose 42, and a connecting plug 43. The bottom of the venting component 41 is fixed to the top of the mounting mechanism 2. The venting component 41 is provided with vertically intersecting venting holes 411 and sliding cavities 412. The connecting hose 42 connects the input end of the venting hole 411 and the top of the connecting plug 43. A second telescopic component 414 is installed on the venting component 41. A switch plate 413 is fixed to the telescopic part of the second telescopic component 414. The switch plate 413 is slidably installed within the range of the sliding cavity 412. A switch hole is provided on the switch plate 413.

[0137] When the switch plate 413 retracts, the vent 411 closes; when the switch plate 413 extends, the vent 411 opens.

[0138] In this embodiment, the connecting rubber stopper 43, the connecting hose 42, and the venting device 41 are interconnected. When the connecting rubber stopper 43 is connected to the separating funnel bottle 100, it can provide a rapid venting function.

[0139] During the shaking process, the separatory funnel 100 needs to be manually stopped and the inside of the separatory funnel needs to be vented in stages to ensure the stability and safety of the shaking process.

[0140] In this embodiment, a pressure sensor 44 is integrated on the venting component 41. The sensing probe of the pressure sensor 44 is connected to the venting port 411. When the switch plate 413 is closed, it can monitor the air pressure within the range of the connecting hose 42 and the venting port 411 in real time. A pipe is provided at the output end of the venting port 411 for stable venting.

[0141] In this embodiment, after the connecting rubber stopper 43 is inserted into the port of the separating funnel bottle 100, the switch valve of the port is adjusted to a half-open state. This ensures the connection between the separating funnel bottle 100 and the connecting hose 42, and reduces splashing when the solution is shaken.

[0142] Automatic deflation principle:

[0143] When it is necessary to release the vent in stages during the oscillation process of the separating funnel bottle 100, the first telescopic member 32 controls the lifting plate 33 to move away from the vibration range of the vibrating frame 12, and the fixing plate 31 moves away from the vibration range of the vibrating frame 12 under the support of the elastic support member 132. The third telescopic member 51 controls the locking plate 53 to abut against the limiting slide rail 131, so that the mounting mechanism 2 and the separating funnel bottle 100 are removed from the vibration state and remain stable. While maintaining stability, the second telescopic member 414 is activated. The second telescopic member 414 drives the switch plate 413 to move upward. During the upward movement of the switch plate 413, the switch hole and the vent hole 411 are interconnected, realizing automatic venting of the separating funnel bottle 100 after stabilization.

[0144] After the venting is completed, the second telescopic member 414 drives the switch plate 413 to move down. The switch plate 413 causes the switch hole to be misaligned with the vent hole 411, thereby closing the vent hole 411 and providing sealing support for the continued oscillation of the separatory funnel bottle 100.

[0145] Furthermore, the top of the venting component 41 is provided with a placement groove, and the connecting rubber plug 43 can be inserted into the placement groove and stored when not in use.

[0146] In an optional embodiment of this example, the second telescopic member 414 is an electric telescopic rod used to directly drive the switching adjustment of the switch plate 413.

[0147] In another optional implementation of this embodiment, please refer to the following: Figure 6 and Figure 7 The second telescopic member 414 is a connecting rod structure, and the bottom of the second telescopic member 414 penetrates through the mounting mechanism 2 and is inserted into the range of the mounting cavity 20;

[0148] A transmission frame 35 is fixedly mounted on the top of the synchronization plate 52, and the two ends of a transmission rod 415 are respectively hinged to the bottom of the second telescopic member 414 and the top of the transmission frame 35.

[0149] During the process of the synchronization plate 52 driving the locking plate 53 to abut against the limiting slide rail 131, the synchronization plate 52 drives the transmission frame 35 to move synchronously. The transmission frame 35 pushes the second telescopic member 414 upward through the transmission rod 415. The second telescopic member 414 drives the switch plate 413 upward, realizing the adaptive opening of the switch plate 413. Finally, while the locking plate 53 abuts against the limiting slide rail 131 for braking, the switch plate 413 is opened synchronously to release air.

[0150] In an optional embodiment of this example, the third telescopic member 51 is an electric telescopic rod used to directly drive the movement and adjustment of the synchronization plate 52.

[0151] In another optional implementation of this embodiment, please refer to the following: Figure 6 and Figure 7 The third telescopic component 51 is a spring telescopic tube, and the third telescopic component 51 elastically connects the mounting mechanism 2 and the synchronization plate 52;

[0152] The mounting mechanism 2 has a limiting groove 201. One end of the lifting plate 33 passes through the limiting groove 201 and is slidably connected to the mounting mechanism 2. The lifting plate 33 and the transmission frame 35 are staggered. The transmission frame 35 has a transmission inclined hole 350. A transmission shaft 34 is inserted into the transmission inclined hole 350 and is fixedly connected to the lifting plate 33. The transmission shaft 34 is connected to the transmission frame 35 through the transmission inclined hole 350.

[0153] In this embodiment, the transmission inclined hole 350 has a V-shaped structure. While the lifting plate 33 is adjusted up and down, the lifting plate 33 can synchronously drive the transmission shaft 34 to rise and fall. The transmission shaft 34 drives the transmission frame 35 to move and adjust synchronously through the transmission inclined hole 350. The lifting power of the lifting plate 33 can be used to realize the braking of the locking plate 53 and the adaptive switching adjustment of the switch plate 413.

[0154] In this embodiment, the lifting plate 33 includes three working modes:

[0155] like Figure 10 (a) and Figure 11In (a) of the oscillation mode, the lifting plate 33 and the fixing plate 31 are clamped on the vibration frame 12, the switch plate 413 is closed, and the locking plate 53 is separated from the limiting slide rail 131, which facilitates the oscillation treatment of the separatory funnel bottle 100 after installation.

[0156] like Figure 10 (b) and Figure 11 In (b) of the above, in the venting mode, the lifting plate 33 and the fixing plate 31 are removed from the vibration range of the vibrating frame 12, the switch plate 413 is opened, and the locking plate 53 abuts against the limiting slide rail 131 to brake, so as to automatically vent the separatory funnel bottle 100 after it leaves the oscillation state. After venting, it can be restored to the oscillation mode. In this state, the separatory funnel bottle 100 can also be replaced.

[0157] like Figure 10 (c) and Figure 11 In (c), the replacement mode is such that while the lifting plate 33 and the fixing plate 31 are removed from the vibration range of the vibration frame 12, there is also a reserved space for upward removal and replacement. The switch plate 413 is closed, and the locking plate 53 is separated from the limiting slide rail 131, so as to facilitate the replacement of the installation mechanism 2 of different specifications and meet the requirement of quick replacement of the installation mechanism 2 without stopping the machine.

[0158] Synchronous adjustment principle:

[0159] like Figure 10 (a) to Figure 10 In (b), when it is necessary to vent or replace the separatory funnel bottle 100, the first telescopic component 32 is activated. The first telescopic component 32 drives the lifting plate 33 to move down, and the lifting plate 33 drives the transmission shaft 34 to move down. The transmission shaft 34 first drives the transmission frame 35 to move to the right through the transmission inclined hole 350, so that the lifting plate 33 switches from the oscillation mode to the venting mode. Synchronous braking and adaptive venting are achieved at the same time as the lifting plate 33 opens.

[0160] like Figure 10 (b) to Figure 10 In (c), when the installation mechanism 2 needs to be replaced, the first telescopic member 32 is activated again. The first telescopic member 32 drives the lifting plate 33 to continue to move downward. The lifting plate 33 drives the transmission shaft 34 to move downward. The transmission shaft 34 drives the transmission frame 35 to move to the left through the transmission inclined hole 350, so that the lifting plate 33 changes mode when switching from the venting mode. The brake is unlocked at the same time as the lifting plate 33 opens, so that the installation mechanism 2 can be used for different specifications to meet the needs of different specifications of dispensing funnel bottles 100.

[0161] Ultimately, when the lifting plate 33 switches from the oscillation mode to the venting mode, the braking of the mounting mechanism 2 and the automatic opening of the switch plate 413 are simultaneously achieved; when the lifting plate 33 is adjusted from the venting mode to the replacement mode, the braking of the mounting mechanism 2 is simultaneously released. Regardless of whether the vibrating frame 12 is in working condition, the rapid replacement of the mounting mechanism 2 can be met, so as to maintain the continuous operation of the vibrating frame 12 while meeting the needs of venting and replacing the separating funnel bottle 100 and replacing the mounting mechanism 2.

[0162] In the preferred embodiment of this invention, please refer to... Figure 12 There are four installation mechanisms 2 arranged around the assembly range of the vibration frame 12; the number of installation mechanisms 2, assembly mechanisms 3, venting mechanisms 4 and locking mechanisms 5 are equal and arranged in a one-to-one correspondence.

[0163] The installation mechanism 2, equipped with four workstations, satisfies the oscillation processing requirements of four separating funnel bottles 100; meets the requirements for automatic venting; allows for the replacement / installation of separating funnel bottles 100 without shutting down the machine; and allows for the quick replacement of any of the installation mechanisms 2. This improves the efficiency of the oscillation processing.

[0164] The working principle of the oscillation device provided in this embodiment is as follows:

[0165] like Figure 4 , Figure 10 (a) and Figure 11 As shown in (a), it can be defined that in the initial state, the lifting plate 33 is in the oscillation mode, and the vibration frame 12 is used to drive the installation mechanism 2 and the liquid separation funnel bottle 100 in the installation state to vibrate up and down, so as to facilitate the oscillation treatment of the internal stored solution.

[0166] Please refer to the following: Figure 10 (a) to Figure 10 (b) and Figure 11 (a) to Figure 11 In (b), when the vibrating frame 12 is in working condition and it is necessary to vent the inside of the separating funnel bottle 100, the first telescopic member 32 is activated. The first telescopic member 32 drives the lifting plate 33 to move down and out of the vibration range of the vibrating frame 12. At the same time as the lifting plate 33 moves down, the elastic support member 132 provides downward elastic support to the connecting slider 21 under the action of elastic support, so that the entire mounting mechanism 2 and the fixing plate 31 are slightly raised, so that the fixing plate 31 also moves out of the vibration range of the vibrating frame 12.

[0167] During the process of both the fixed plate 31 and the lifting plate 33 being removed from the vibration range of the vibration frame 12, the lifting plate 33 drives the transmission shaft 34 to move downward. The transmission shaft 34 first drives the transmission frame 35 to move to the right through the transmission inclined hole 350. The transmission frame 35 then drives the locking plate 53 to move to the right through the synchronous plate 52 and abuts against the limiting slide rail 131, thereby achieving the stability of the installation mechanism 2 after it is removed from the vibration.

[0168] When the transmission frame 35 moves, the transmission rod 415 pushes the second telescopic member 414 to move upward. The second telescopic member 414 drives the switch plate 413 to move upward. When the switch plate 413 moves upward, the switch hole gradually connects with the vent hole 411, and the gas in the separating funnel bottle 100 is released quickly.

[0169] Please refer to the following: Figure 10 (b) to Figure 10 (c) and Figure 11 (b) to Figure 11 In (c), when the entire installation mechanism 2 needs to be replaced, the first telescopic component 32 is activated again. The first telescopic component 32 drives the lifting plate 33 to move down. The lifting plate 33 moves down and provides space for the replacement of the installation mechanism 2.

[0170] As the lifting plate 33 moves downward, the lifting plate 33 drives the transmission shaft 34 to continue moving downward. The transmission shaft 34 drives the transmission frame 35 to move to the left through the transmission inclined hole 350. The transmission frame 35 drives the locking plate 53 to move to the left, so that the locking plate 53 and the limiting slide rail 131 are released from the braking state, providing support for the overall removal and replacement of the installation mechanism 2.

[0171] When the transmission frame 35 moves to the left, the transmission rod 415 synchronously pulls the second telescopic member 414 downward. The second telescopic member 414 drives the switch plate 413 downward and blocks the range of the vent hole 411, thereby realizing the automatic closing of the vent hole 411.

[0172] like Figure 9 , Figure 10 (c) and Figure 11 As shown in (c), the lifting plate 33 is in the replacement mode, the vibration frame 12 can continue to maintain the vibration state, the installation mechanism 2 can be pulled upward first, so that the connecting slider 21 is removed from the range of the limiting slide rail 131, and then the installation mechanism 2 is pulled horizontally away from the installation range of the vibration frame 12.

[0173] Ultimately, this allows for convenient and rapid replacement of the entire installation mechanism 2, while also enabling simultaneous automatic venting of the separating funnel bottle 100 and stable braking during venting.

[0174] The above description is only a preferred embodiment of the present invention and does not limit the patent scope of the present invention. All equivalent structural transformations made under the concept of the present invention using the contents of the present invention specification and drawings, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.

Claims

1. A method for extracting and separating tantalum and niobium, characterized in that, Includes the following steps: Step A1: Weigh an appropriate amount of oxalic acid and dissolve it in deionized water. After dissolving, transfer the solution to a volumetric flask to prepare an oxalic acid solution of a certain concentration. Step A2: Take a certain amount of tantalum standard solution and niobium standard solution respectively and add them to the oxalic acid solution prepared above; Step A3: Add hydrochloric acid solution to adjust the pH; Step A4: Weigh an appropriate amount of DOAP, add it to chloroform, stir thoroughly to dissolve, and prepare a DOAP chloroform solution; Step A5: Use a pipette to measure the aqueous phase and organic phase separately, and add them to the separatory funnel according to a certain volume ratio; Step A6: Place the separatory funnel in a constant temperature shaker and shake it to ensure that the two phases are in full contact; Step A7: After shaking, remove the separatory funnel, centrifuge to separate the organic phase and the aqueous phase, and collect them separately into clean conical flasks. Step A8: Take the separated organic phase, add an equal volume of nitric acid as a back-extraction agent, and place it in a separatory funnel; Step A9: Shake to transfer tantalum from the organic phase to the aqueous phase, centrifuge to separate the layers, and collect the aqueous phase containing tantalum; Step A10: Add an equal volume of a mixed solution of nitric acid and oxalic acid as a back-extraction agent to the remaining organic phase; Step A11: After oscillation and centrifugation to separate the layers, collect the aqueous phase containing niobium; The concentration of the oxalic acid solution in step A1 is 0.1-1.0 M; The concentrations of tantalum and niobium in the oxalic acid solution in step A2 are 100-500 mg / L; In step A3, the pH is 1.0-3.0; In step A4, the concentration of the DOAP chloroform solution is 0.1-0.5M; The volume ratio in step A5 is 1:1-3:1; In step A6, the oscillation time is 10-30 minutes and the constant temperature is 24-26℃.

2. The method for extracting and separating tantalum and niobium according to claim 1, characterized in that, The aqueous phase is a metal oxalate solution, and the organic phase is a DOAP chloroform solution.

3. The method for extracting and separating tantalum and niobium according to claim 2, characterized in that, The DOAP is di-n-octylaminopropanol, and its preparation method is as follows: Step B1: Add dioctylamine and solvent to a three-necked flask and stir to dissolve; Step B2: Slowly add the catalyst and continue stirring until completely dissolved; Step B3: Install the constant pressure dropping funnel, condenser and thermometer, and ensure the device is sealed; Step B4: Raise the oil bath temperature to a certain temperature and maintain the reaction system at a constant temperature; Step B5: Slowly add propylene oxide dropwise through a constant pressure dropping funnel; Step B6: After the addition is complete, continue stirring the reaction until there is no obvious exothermic phenomenon. Step B7: After the reaction solution has cooled to room temperature, slowly add 1 M HCl to adjust the pH. Step B8: Transfer the solution to a separatory funnel and add the extractant to extract the product; Step B9: Combine the organic phases, add a desiccant, and filter to remove the desiccant; Step B10: Place the organic phase in a vacuum distillation apparatus and remove the extractant under normal pressure; Step B11: Adjust the vacuum level, raise the temperature, and collect the distillate to obtain di-n-octylaminopropanol.

4. The method for extracting and separating tantalum and niobium according to claim 3, characterized in that, The constant temperature oscillator described in step A6 includes a constant temperature chamber and an oscillation device, wherein the oscillation device is integrated and installed in the constant temperature area of ​​the constant temperature chamber.

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