Rubidium extraction device

Abstract

The invention provides a rubidium extraction device, which comprises: an extraction section, which comprises a plurality of first high-speed centrifugal extractors connected in series, and a water phase raffinate is introduced into the last-stage first high-speed centrifugal extractor; the water-phase raffinate is water-phase raffinate obtained after cesium is removed from leached frozen clear liquid of lepidolite, and the water-phase raffinate is alkaline and comprises rubidium, sodium, potassium and lithium ions; in the extraction section, t-BAMBP is diluted by adopting ESCAID 110, the concentration of the extraction agent is 0.4-0.6 mol / L of t-BAMBP, and in the extraction section, the concentration of OH <-> in the liquid to be extracted is controlled to be 0.6 mol / L; the washing section comprises a plurality of second high-speed centrifugal extractors which are connected in series; and the reverse extraction section comprises a plurality of third high-speed centrifugal extractors which are connected in series. According to the rubidium extraction device provided by the invention, t-BAMBP is diluted through ESCAID 110, and a high-speed centrifugal extractor is combined, so that the stages of extraction, washing and reverse extraction can be greatly reduced, the cost is reduced, and the reaction time is shortened.

Description

Technical Field

[0001] This application relates to the technical field of cesium separation, and particularly to an extraction device for rubidium. Background Art

[0002] Due to its unique properties, rubidium plays an important role in many high-tech fields such as aerospace, atomic energy, biology, and energy. Its application development has attracted more and more attention, and the extraction, separation, and industrial production of rubidium have also become a research hotspot. Rubidium is usually contained in other minerals and often coexists with various metal elements such as lithium and potassium. Lepidolite contains abundant elements such as lithium, potassium, rubidium, and cesium. When lepidolite is treated with sulfuric acid, a mixed by-product containing rubidium, cesium, and potassium can be obtained. For example, CN110550646A "A Preparation Method of Cesium Sulfate and Rubidium Sulfate" discloses that specific ratios of t-BAMBP and No. 260 solvent oil and t-BAMBP and n-hexane are successively used as extraction solutions, which can better separate rubidium, cesium, and potassium in the solution; high-purity cesium sulfate and rubidium sulfate are obtained. Another example is CN106929693A "A Method for Extracting and Separating Cesium, Rubidium, and Potassium", which discloses that the alkalinity of the solution containing rubidium, cesium, and potassium is adjusted to 0.8 - 1.0 mol / L in one step; the adjusted solution enters the extraction and separation process of cesium and rubidium, and the extractant is 0.5 - 1.5 mol / L t-BAMBP and No. 260 solvent oil; the saturated organic phase carrying cesium is washed with deionized water to wash away rubidium in the organic phase; after washing rubidium, the organic phase is subjected to back-extraction to obtain a back-extract solution of cesium, realizing the separation of cesium and rubidium; the raffinate solution for extracting cesium is subjected to extraction and separation of rubidium and potassium, and after extraction of rubidium, washing of potassium, and back-extraction operations, a back-extract solution of rubidium is obtained, realizing the separation of rubidium and potassium. However, these separation and extraction methods are relatively complex and require more than ten stages of extraction, washing, and back-extraction, greatly increasing the time and cost. Summary of the Invention

[0003] The object of the present invention is to solve the above problems and provide an extraction device for rubidium.

[0004] The technical solution of this application is realized as follows: The present invention provides an extraction device for rubidium, comprising: Extraction section, which includes a plurality of first high-speed centrifugal extractors connected in series. Each first high-speed centrifugal extractor includes a first extraction inlet and a second extraction inlet provided at one end, and a first extraction outlet and a second extraction outlet provided at the other end; and the first extraction inlet is communicated with the first extraction outlet, and the second extraction inlet is communicated with the second extraction outlet; between two adjacent first high-speed centrifugal extractors, the second extraction outlet of the upper-stage first high-speed centrifugal extractor is communicated with the second extraction inlet of the lower-stage first high-speed centrifugal extractor through a pipeline, and the first extraction inlet of the upper-stage first high-speed centrifugal extractor is communicated with the first extraction outlet of the lower-stage first high-speed centrifugal extractor through a pipeline; and an extractant is introduced into the second extraction inlet of the first-stage first high-speed centrifugal extractor through a pipeline, and an aqueous phase raffinate is introduced into the first extraction inlet of the last-stage first high-speed centrifugal extractor; the aqueous phase raffinate is the aqueous phase raffinate after cesium removal from the leaching and freezing clear liquid of lepidolite, the aqueous phase raffinate is alkaline, and includes rubidium, sodium, potassium and lithium ions; the extractant is ESCAID 110 diluted with t-BAMBP, and the concentration of the extractant is 0.4-0.6 mol / L of t-BAMBP. During the extraction section, control the concentration of OH - in the liquid to be extracted to be 0.6 mol / L; Washing section, which includes a plurality of second high-speed centrifugal extractors connected in series. Each second high-speed centrifugal extractor includes a first washing inlet and a second washing inlet provided at one end, and a first washing outlet and a second washing outlet provided at the other end, and the first washing inlet is communicated with the first washing outlet, and the second washing inlet is communicated with the second washing outlet; between two adjacent second high-speed centrifugal extractors, the second washing outlet of the upper-stage second high-speed centrifugal extractor is communicated with the second washing inlet of the lower-stage second high-speed centrifugal extractor through a pipeline, and the first washing inlet of the upper-stage second high-speed centrifugal extractor is communicated with the first washing outlet of the lower-stage second high-speed centrifugal extractor through a pipeline; and the second washing inlet of the first-stage second high-speed centrifugal extractor is communicated with the second extraction outlet of the last-stage first high-speed centrifugal extractor through a pipeline, and first washing sulfuric acid is introduced into the first washing inlet of the last-stage second high-speed centrifugal extractor, and the first washing post-liquid flows out from the first washing outlet of the first-stage second high-speed centrifugal extractor; The stripping section includes a plurality of third high-speed centrifugal extractors connected in series. Each third high-speed centrifugal extractor includes a first stripping inlet and a second stripping inlet provided at one end, and a first stripping outlet and a second stripping outlet provided at the other end. The first stripping inlet is communicated with the first stripping outlet, and the second stripping inlet is communicated with the second stripping outlet. Between two adjacent third high-speed centrifugal extractors, the second stripping outlet of the upper-level third high-speed centrifugal extractor is communicated with the second stripping inlet of the lower-level third high-speed centrifugal extractor through a pipeline, and the first stripping inlet of the upper-level third high-speed centrifugal extractor is communicated with the first stripping outlet of the lower-level third high-speed centrifugal extractor through a pipeline. And the second stripping inlet of the first-level third high-speed centrifugal extractor is communicated with the second washing outlet of the last-level second high-speed centrifugal extractor through a pipeline. Second stripping sulfuric acid is introduced into the first stripping inlet of the last-level third high-speed centrifugal extractor, stripped liquid flows out from the first stripping outlet of the first-level third high-speed centrifugal extractor, and the second stripping outlet of the last-level third high-speed centrifugal extractor is communicated with the second extraction inlet of the first-level first high-speed centrifugal extractor to form a cycle of the extraction liquid.

[0005] As a further improvement, during the extraction section, control the concentration of OH - in the liquid to be extracted to be 0.6 mol / L.

[0006] As a further improvement, during the extraction section, control the O / A ratio to be 5.3 - 5.6:1.

[0007] As a further improvement, the extraction section includes 3 - 5 first high-speed centrifugal extractors connected in series; the washing section includes 4 - 6 second high-speed centrifugal extractors connected in series; the stripping section includes 2 - 4 third high-speed centrifugal extractors connected in series.

[0008] As a further improvement, the extraction section includes 4 first high-speed centrifugal extractors connected in series; the washing section includes 5 second high-speed centrifugal extractors connected in series; the stripping section includes 3 third high-speed centrifugal extractors connected in series. As a further improvement, the concentration of the first washing sulfuric acid is 0.02 mol / L - 0.03 mol / L.

[0009] As a further improvement, during the washing section, control the O / A ratio to be 7.3 - 7.7:1.

[0010] As a further improvement, the concentration of the second stripping sulfuric acid is 0.20 mol / L - 0.21 mol / L.

[0011] As a further improvement, during the stripping section, control the O / A ratio to be 19 - 21:1.

[0012] The advantages or beneficial effects in the above technical solutions at least include: For the rubidium extraction device provided by the present invention, ESCAID 110 is used to dilute t-BAMBP, and combined with a high-speed centrifugal extractor, thereby significantly reducing the number of extraction, washing, and stripping stages, reducing costs and reaction time. Further, by reducing the number of extraction stages, the present invention can significantly reduce equipment investment and operating costs, while reducing the consumption of chemicals and the generation of waste liquid, thereby reducing the overall production cost. In addition, by precisely controlling the extractant concentration, O / A ratio, and process parameters of each stage, the present invention can effectively improve the extraction rate and purity of rubidium, reduce the co-extraction of impurities, and ensure the high purity of the final product. And using ESCAID 110 as a diluent has lower toxicity and higher safety compared to traditional solvents such as sulfonated kerosene, is more environmentally friendly, and is more friendly to the environment. At the same time, by optimizing the process flow, the generation of waste liquid is reduced, and environmental pollution is reduced. Finally, through the design of the stripping section, the extraction liquid can be recycled, improving the utilization rate of resources, reducing the waste of extractant, and further reducing the production cost. Brief Description of the Drawings

[0013] The drawings illustrate exemplary embodiments of the present application in embodiments of the present invention and, together with the description thereof, are used to explain the principles of the present application. These drawings are included to provide a further understanding of the present application and are included in this specification and form a part of this specification.

[0014] Figure 1 Shows a schematic diagram of the cesium extraction device provided by an embodiment of the present invention.

[0015] Figure 2 Shows a schematic diagram of the rubidium extraction device provided by an embodiment of the present invention. Detailed Description of the Embodiments

[0016] Embodiments of the present application will be described in more detail below with reference to the drawings. Although some embodiments of the present application are shown in the drawings, it should be understood that the present application can be implemented in various forms and should not be construed as limited to the embodiments set forth herein. On the contrary, these embodiments are provided to more thoroughly and completely understand the present application. It should be understood that the drawings and embodiments of the present application are only for exemplary purposes and are not used to limit the protection scope of the present application.

[0017] It should be noted that, without conflict, the embodiments in the present application and the features in the embodiments can be combined with each other. The present application will be described in detail below with reference to the drawings and in combination with the embodiments.

[0018] The names of the messages or information exchanged between multiple devices in the embodiments of this application are for illustrative purposes only and are not used to limit the scope of these messages or information.

[0019] Referring to Figure 1 , an embodiment of the present invention provides an extraction device for cesium, comprising: An extraction section 10, which includes a plurality of first high-speed centrifugal extractors 11 connected in series. Each first high-speed centrifugal extractor 11 includes a first extraction inlet 110 and a second extraction inlet 112 provided at one end, and a first extraction outlet 111 and a second extraction outlet 113 provided at the other end. The first extraction inlet 110 is communicated with the first extraction outlet 111, and the second extraction inlet 112 is communicated with the second extraction outlet 113. Between two adjacent first high-speed centrifugal extractors 11, the second extraction outlet 113 of the upper-stage first high-speed centrifugal extractor 11 is communicated with the second extraction inlet 112 of the lower-stage first high-speed centrifugal extractor 11 through a pipeline, and the first extraction inlet 110 of the upper-stage first high-speed centrifugal extractor 11 is communicated with the first extraction outlet 111 of the lower-stage first high-speed centrifugal extractor 11 through a pipeline. And an extractant is introduced into the second extraction inlet 112 of the first-stage first high-speed centrifugal extractor 11 through a pipeline, and a liquid to be extracted 12 is introduced into the first extraction inlet 110 of the last-stage first high-speed centrifugal extractor 11, and an aqueous-phase raffinate 13 flows out from the first extraction outlet 111 of the first-stage first high-speed centrifugal extractor 11.

[0020] A washing section 20, which includes a plurality of second high-speed centrifugal extractors 21 connected in series. Each second high-speed centrifugal extractor 21 includes a first washing inlet 210 and a second washing inlet 212 provided at one end, and a first washing outlet 211 and a second washing outlet 213 provided at the other end. The first washing inlet 210 is communicated with the first washing outlet 211, and the second washing inlet 212 is communicated with the second washing outlet 213. Between two adjacent second high-speed centrifugal extractors 21, the second washing outlet 213 of the upper-stage second high-speed centrifugal extractor 21 is communicated with the second washing inlet 212 of the lower-stage second high-speed centrifugal extractor 21 through a pipeline, and the first washing inlet 210 of the upper-stage second high-speed centrifugal extractor 21 is communicated with the first washing outlet 211 of the lower-stage second high-speed centrifugal extractor 21 through a pipeline. And the second washing inlet 212 of the first-stage second high-speed centrifugal extractor 21 is communicated with the second extraction outlet 113 of the last-stage first high-speed centrifugal extractor 11 through a pipeline, and first washing sulfuric acid 22 is introduced into the first washing inlet 210 of the last-stage second high-speed centrifugal extractor 21, and a first post-washing liquid 23 flows out from the first washing outlet 211 of the first-stage second high-speed centrifugal extractor 21, and the first post-washing liquid 23 is an aqueous phase.

[0021] The stripping section 30 includes a plurality of third high-speed centrifugal extractors 31 connected in series. Each third high-speed centrifugal extractor 31 includes a first stripping inlet 310 and a second stripping inlet 312 provided at one end, and a first stripping outlet 311 and a second stripping outlet 313 provided at the other end. The first stripping inlet 310 is communicated with the first stripping outlet 311, and the second stripping inlet 312 is communicated with the second stripping outlet 313. Between two adjacent third high-speed centrifugal extractors 31, the second stripping outlet 313 of the upper-level third high-speed centrifugal extractor 31 is communicated with the second stripping inlet 312 of the lower-level third high-speed centrifugal extractor 31 through a pipeline, and the first stripping inlet 310 of the upper-level third high-speed centrifugal extractor 31 is communicated with the first stripping outlet 311 of the lower-level third high-speed centrifugal extractor 31 through a pipeline. And the second stripping inlet 312 of the first-level third high-speed centrifugal extractor 31 is communicated with the second washing outlet 213 of the last-level second high-speed centrifugal extractor 21 through a pipeline. The second stripping sulfuric acid 32 is introduced into the first stripping inlet 310 of the last-level third high-speed centrifugal extractor 31, the stripped solution 33 flows out from the first stripping outlet 311 of the first-level third high-speed centrifugal extractor 31, and the second stripping outlet 313 of the last-level third high-speed centrifugal extractor 31 is communicated with the second extraction inlet 112 of the first-level first high-speed centrifugal extractor 11 to form a cycle of the extraction solution.

[0022] In one embodiment, the solution to be extracted 12 is the frozen clear liquid obtained by leaching lepidolite, and its main element contents are shown in Table 1: Table 1 Element composition of the frozen clear liquid (g / L)

[0023] In one embodiment, the extractant uses ESCAID 110 to dilute t-BAMBP, and the concentration of t-BAMBP is 0.4 - 0.6 mol / L. The present invention creatively uses ESCAID 110 to dilute t-BAMBP, thereby greatly reducing the extraction, washing and stripping stages and improving the extraction efficiency.

[0024] Under alkaline conditions, the H on the phenol hydroxyl group of t-BAMBP in the extractant is easily replaced by metal ions to form phenolate, and the extraction sequence of this system is cesium > rubidium > potassium > sodium. For 0.4 - 0.6 mol / L of t-BAMBP, when supplemented with 0.4 mol / L of OH - , the saturated loading amount of cesium can reach 5.5 g / L. Therefore, in this embodiment, preferably, the solution to be extracted 12 includes 0.4 mol / L of OH - .

[0025] Preferably, the extraction section 10 includes 3 to 5 first high-speed centrifugal extractors 11 connected in series. In one embodiment, the extraction section 10 includes 4 first high-speed centrifugal extractors 11 connected in series. Therefore, the extractant is introduced through a pipeline into the second extraction inlet 112 of the first high-speed centrifugal extractor 11 at the first stage, and the liquid to be extracted 12 is introduced into the first extraction inlet 110 of the first high-speed centrifugal extractor 11 at the fourth stage. The aqueous phase raffinate 13 flows out from the first extraction outlet 111 of the first high-speed centrifugal extractor 11 at the first stage, and the cesium-loaded organic phase flows out from the second extraction outlet 113 of the first high-speed centrifugal extractor 11 at the fourth stage and enters the scrubbing section 20.

[0026] More preferably, in order to obtain the best extraction effect, preferably, the feeding ratio of the extractant to the liquid to be extracted 12 needs to be strictly controlled. The effects of O / A being 1:1, 1:1.2, 1:1.5, 1:1.8, 1:2 in the extraction section 10 on the Cs extraction effect are shown. The results are shown in Table 2.

[0027] Table 2 Effects of different O / A on Cs extraction effect

[0028] It can be seen from the data that in the cesium extraction stage, the extraction rates of Cs and Rb decrease with the increase of the aqueous phase flow rate. When the aqueous phase flow rate ratio is above 1.8, the co-extraction rate of Rb can be controlled within 5%, which is beneficial for the scrubbing section to elute Rb completely. Comparing the data of O / A being 1:1 and 1:1.5, it is recommended to select O / A of 1:1.8 - 2.0 for extraction, reducing the dosage of the organic extractant. At the same time, the Cs extraction rate can be increased by increasing the number of extraction stages. That is, preferably, the O / A ratio in the extraction section 10 is 1:1.8 - 2.0. In one embodiment, the O / A ratio in the extraction section 10 is about 1:1.8, that is, the volume ratio of the extractant to the liquid to be extracted 12 is about 1:1.8.

[0029] In one embodiment, after detection and analysis, the element content of the aqueous phase raffinate 13 is shown in Table 3: Table 3 Element composition of cesium extraction raffinate (g / L)

[0030] It can be seen from Table 3 that the cesium ions in the aqueous phase raffinate 13 are significantly reduced, while other metals have no significant change.

[0031] Preferably, the washing section 20 includes 4 to 7 second high-speed centrifugal extractors 21 connected in series. In one embodiment, the washing section 20 includes 5 second high-speed centrifugal extractors 21 connected in series. Therefore, the second washing inlet 212 of the second high-speed centrifugal extractor 21 at the first stage is connected to the second extraction outlet 113 of the first high-speed centrifugal extractor 11 at the fourth stage through a pipeline. The first washing sulfuric acid 22 is introduced into the first washing inlet 210 of the second high-speed centrifugal extractor 21 at the fifth stage, and the first post-washing liquid 23 flows out from the first washing outlet 211 of the second high-speed centrifugal extractor 21 at the first stage.

[0032] To obtain the best extraction effect, preferably, in the washing section 20, the feeding ratio of the first washing sulfuric acid 22 to the cesium-loaded organic phase needs to be strictly controlled. Preferably, the O / A ratio in the washing section 20 is 2 to 3:1. In one embodiment, the O / A ratio in the washing section 20 is about 2.5:1, that is, the volume ratio of the cesium-loaded organic phase to the first washing sulfuric acid 22 is about 2.5:1, so that impurity ions can be fully washed away. Further, the first washing sulfuric acid 22 also needs to be strictly controlled. Preferably, the concentration of the first washing sulfuric acid 22 is 0.02 mol / L to 0.03 mol / L. In one embodiment, the concentration of the first washing sulfuric acid 22 is about 0.025 mol / L.

[0033] Preferably, the stripping section 30 includes 2 to 4 third high-speed centrifugal extractors 31 connected in series. In one embodiment, the stripping section 30 includes 3 third high-speed centrifugal extractors 31 connected in series. Therefore, the second stripping inlet 312 of the third high-speed centrifugal extractor 31 at the first stage is connected to the second washing outlet 213 of the second high-speed centrifugal extractor 21 at the fifth stage through a pipeline, so that the washed cesium-loaded organic phase flowing out from the second washing outlet 213 of the second high-speed centrifugal extractor 21 at the fifth stage flows into the third high-speed centrifugal extractor 31 at the first stage. The second stripping sulfuric acid 32 is introduced into the first stripping inlet 310 of the third high-speed centrifugal extractor 31 at the third stage, and the stripped liquid 33 flows out from the first stripping outlet 311 of the third high-speed centrifugal extractor 31 at the first stage. The second stripping outlet 313 of the third high-speed centrifugal extractor 31 at the third stage is connected to the second extraction inlet 112 of the first high-speed centrifugal extractor 11 at the first stage to form a cycle of the extraction liquid.

[0034] To achieve the best stripping effect, preferably, in the stripping section 30, the feeding ratio of the second stripping sulfuric acid 32 to the cesium-loaded organic phase after washing needs to be strictly controlled. Preferably, the O / A ratio in the stripping section 30 is 14-16:1. In one embodiment, the O / A ratio in the stripping section 30 is about 15:1, that is, the volume ratio of the cesium-loaded organic phase after washing to the second stripping sulfuric acid 32 is about 15:1, so that sufficient stripping can be achieved. Further, the second stripping sulfuric acid 32 also needs to be strictly controlled. Preferably, the concentration of the second stripping sulfuric acid 32 is 0.16 mol / L - 0.17 mol / L. In one embodiment, the concentration of the second stripping sulfuric acid 32 is about 0.164 mol / L. Further, after the stripped solution 33 is precisely filtered and then evaporated and crystallized, cesium sulfate crystals can be obtained, and its purity can reach more than 99.9%.

[0035] Please refer to Figure 2 As shown, as a further improvement, in order to further process the aqueous raffinate 13 to obtain rubidium sulfate, the present invention further uses the above equipment to extract rubidium. Specifically, the embodiment of the present invention provides an extraction device for rubidium, including: An extraction section 10, which includes a plurality of first high-speed centrifugal extractors 11 connected in series. Among them, each first high-speed centrifugal extractor 11 includes a first extraction inlet 110 and a second extraction inlet 112 provided at one end, and a first extraction outlet 111 and a second extraction outlet 113 provided at the other end, and the first extraction inlet 110 is communicated with the first extraction outlet 111, and the second extraction inlet 112 is communicated with the second extraction outlet 113; between two adjacent first high-speed centrifugal extractors 11, the second extraction outlet 113 of the upper-stage first high-speed centrifugal extractor 11 is communicated with the second extraction inlet 112 of the lower-stage first high-speed centrifugal extractor 11 through a pipeline, and the first extraction inlet 110 of the upper-stage first high-speed centrifugal extractor 11 is communicated with the first extraction outlet 111 of the lower-stage first high-speed centrifugal extractor 11 through a pipeline; and an extractant is introduced into the second extraction inlet 112 of the first-stage first high-speed centrifugal extractor 11 through a pipeline, and the aqueous raffinate 13 is introduced into the first extraction inlet 110 of the last-stage first high-speed centrifugal extractor 11, and the second aqueous raffinate 14 flows out from the first extraction outlet 111 of the first-stage first high-speed centrifugal extractor 11. The second aqueous raffinate 14 can be used for the extraction of other metal ions.

[0036] The washing section 20 includes a plurality of second high-speed centrifugal extractors 21 connected in series. Each second high-speed centrifugal extractor 21 includes a first washing inlet 210 and a second washing inlet 212 provided at one end, and a first washing outlet 211 and a second washing outlet 213 provided at the other end. The first washing inlet 210 is communicated with the first washing outlet 211, and the second washing inlet 212 is communicated with the second washing outlet 213. Between two adjacent second high-speed centrifugal extractors 21, the second washing outlet 213 of the upper-stage second high-speed centrifugal extractor 21 is communicated with the second washing inlet 212 of the lower-stage second high-speed centrifugal extractor 21 through a pipeline, and the first washing inlet 210 of the upper-stage second high-speed centrifugal extractor 21 is communicated with the first washing outlet 211 of the lower-stage second high-speed centrifugal extractor 21 through a pipeline. And the second washing inlet 212 of the first-stage second high-speed centrifugal extractor 21 is communicated with the second extraction outlet 113 of the last-stage first high-speed centrifugal extractor 11 through a pipeline. The first washing sulfuric acid 22 is introduced into the first washing inlet 210 of the last-stage second high-speed centrifugal extractor 21, and the second washing post-liquid 24 flows out from the first washing outlet 211 of the first-stage second high-speed centrifugal extractor 21.

[0037] The stripping section 30 includes a plurality of third high-speed centrifugal extractors 31 connected in series. Each third high-speed centrifugal extractor 31 includes a first stripping inlet 310 and a second stripping inlet 312 provided at one end, and a first stripping outlet 311 and a second stripping outlet 313 provided at the other end. The first stripping inlet 310 is communicated with the first stripping outlet 311, and the second stripping inlet 312 is communicated with the second stripping outlet 313. Between two adjacent third high-speed centrifugal extractors 31, the second stripping outlet 313 of the upper-stage third high-speed centrifugal extractor 31 is communicated with the second stripping inlet 312 of the lower-stage third high-speed centrifugal extractor 31 through a pipeline, and the first stripping inlet 310 of the upper-stage third high-speed centrifugal extractor 31 is communicated with the first stripping outlet 311 of the lower-stage third high-speed centrifugal extractor 31 through a pipeline. And the second stripping inlet 312 of the first-stage third high-speed centrifugal extractor 31 is communicated with the second washing outlet 213 of the last-stage second high-speed centrifugal extractor 21 through a pipeline. The third stripping sulfuric acid 34 is introduced into the first stripping inlet 310 of the last-stage third high-speed centrifugal extractor 31, and the second stripping post-liquid 35 flows out from the first stripping outlet 311 of the first-stage third high-speed centrifugal extractor 31. The second stripping outlet 313 of the last-stage third high-speed centrifugal extractor 31 is communicated with the second extraction inlet 112 of the first-stage first high-speed centrifugal extractor 11 to form a circulation of the extraction liquid.

[0038] In one embodiment, the aqueous raffinate 13 is the aqueous raffinate after extracting cesium from the frozen clear liquid obtained by leaching lepidolite, and its main element contents are shown in Table 3.

[0039] In one embodiment, the extractant uses ESCAID 110 to dilute t-BAMBP, and the concentration of t-BAMBP is 0.4 - 0.6 mol / L. The present invention creatively uses ESCAID 110 to dilute t-BAMBP, thereby greatly reducing the extraction, washing, and stripping stages and improving the extraction efficiency.

[0040] Under alkaline conditions, the H on the phenolic hydroxyl group of t-BAMBP in the extractant is easily replaced by metal ions to form phenolate, and the extraction sequence of this system is cesium > rubidium > potassium > sodium. When 0.6 mol / L of OH is added to 0.4 - 0.6 mol / L of t-BAMBP, - the saturated loading capacity of rubidium can reach 4.1 g / L. Therefore, in this embodiment, preferably, the to-be-extracted liquid 12 includes 0.6 mol / L of OH. - .

[0041] Preferably, the extraction section 10 includes 3 - 5 first high-speed centrifugal extractors 11 connected in series. In one embodiment, the extraction section 10 includes 4 first high-speed centrifugal extractors 11 connected in series. Therefore, the extractant is introduced through a pipeline into the second extraction inlet 112 of the first high-speed centrifugal extractor 11 at the first stage, while the aqueous raffinate 13 is introduced into the first extraction inlet 110 of the first high-speed centrifugal extractor 11 at the fourth stage. The second aqueous raffinate 14 flows out from the first extraction outlet 111 of the first high-speed centrifugal extractor 11 at the first stage, and the rubidium-loaded organic phase flows out from the second extraction outlet 113 of the first high-speed centrifugal extractor 11 at the fourth stage and enters the washing section 20.

[0042] More preferably, in order to obtain the best extraction effect, preferably, the feeding ratio of the extractant to the aqueous raffinate 13 needs to be strictly controlled, and the influence of O / A being 5.3:1, 5.4:1, 5.5:1, 5.6:1, 5.7:1 in the extraction section 10 on the extraction effect of Rb is used. The results are shown in Table 4.

[0043] Table 4 Influence of different O / A on the extraction effect of Rb

[0044] As can be seen from the data, during the rubidium extraction stage, the Rb extraction rate decreases as the aqueous phase flow rate increases. When the aqueous phase flow rate ratio is above 5.4, the Rb extraction rate (%) can reach over 99%. Preferably, in the extraction section 10, the O / A ratio is 5.3 - 5.6:1. In one embodiment, the O / A ratio in the extraction section 10 is about 5.4:1, that is, the volume ratio of the extractant to the aqueous phase raffinate 13 is about 5.4:1.

[0045] Preferably, the washing section 20 includes 4 - 7 second high - speed centrifugal extractors 21 connected in series. In one embodiment, the washing section 20 includes 5 second high - speed centrifugal extractors 21 connected in series. Therefore, the second washing inlet 212 of the second high - speed centrifugal extractor 21 at the first stage is connected to the second extraction outlet 113 of the first high - speed centrifugal extractor 11 at the fourth stage through a pipeline. And the first washing sulfuric acid 22 is introduced into the first washing inlet 210 of the second high - speed centrifugal extractor 21 at the fifth stage, and the second washed solution 24 flows out from the first washing outlet 211 of the second high - speed centrifugal extractor 21 at the first stage.

[0046] To obtain the best extraction effect, preferably, in the washing section 20, the feeding ratio of the first washing sulfuric acid 22 to the rubidium - loaded organic phase needs to be strictly controlled. Preferably, in the washing section 20, the O / A ratio is 7.3 - 7.7:1. In one embodiment, the O / A ratio in the washing section 20 is about 7.5:1, that is, the volume ratio of the rubidium - loaded organic phase to the first washing sulfuric acid 22 is about 7.5:1, so that impurity ions can be washed away sufficiently. Further, the first washing sulfuric acid 22 also needs to be strictly controlled. Preferably, the concentration of the first washing sulfuric acid 22 is 0.02 mol / L - 0.03 mol / L. In one embodiment, the concentration of the first washing sulfuric acid 22 is about 0.025 mol / L.

[0047] Preferably, the stripping section 30 includes 2 to 4 third high-speed centrifugal extractors 31 connected in series. In one embodiment, the stripping section 30 includes 3 third high-speed centrifugal extractors 31 connected in series. Therefore, the second stripping inlet 312 of the third high-speed centrifugal extractor 31 at the first stage is connected to the second washing outlet 213 of the second high-speed centrifugal extractor 21 at the fifth stage through a pipeline, so that the washed rubidium-loaded organic phase flowing out from the second washing outlet 213 of the second high-speed centrifugal extractor 21 at the fifth stage flows into the third high-speed centrifugal extractor 31 at the first stage. And third stripping sulfuric acid 34 is introduced into the first stripping inlet 310 of the third high-speed centrifugal extractor 31 at the third stage, and the second stripped solution 35 flows out from the first stripping outlet 311 of the third high-speed centrifugal extractor 31 at the first stage. The second stripping outlet 313 of the third high-speed centrifugal extractor 31 at the third stage is connected to the second extraction inlet 112 of the first high-speed centrifugal extractor 11 at the first stage to form a circulation of the extraction solution.

[0048] To obtain the best stripping effect, preferably, in the stripping section 30, the feeding ratio of the second stripping sulfuric acid 32 to the washed rubidium-loaded organic phase needs to be strictly controlled. Preferably, the O / A ratio in the stripping section 30 is 19 to 21:1. In one embodiment, the O / A ratio in the stripping section 30 is about 20:1, that is, the volume ratio of the washed rubidium-loaded organic phase to the third stripping sulfuric acid 34 is about 20:1, so that sufficient stripping can be achieved. Further, the third stripping sulfuric acid 34 also needs to be strictly controlled. Preferably, the concentration of the third stripping sulfuric acid 34 is 0.20 mol / L to 0.21 mol / L. In one embodiment, the concentration of the third stripping sulfuric acid 34 is about 0.206 mol / L. Further, after the second stripped solution 35 is precisely filtered and then evaporated and crystallized, rubidium sulfate crystals can be obtained, and their purity can reach more than 99%.

[0049] Those skilled in the art should understand that the above embodiments are only for clearly explaining the present application, rather than limiting the scope of the present application. For those skilled in the art, other changes or variations can be made on the basis of the above disclosure, and these changes or variations are still within the scope of the present application.

Claims

1. An extraction device for rubidium, characterized in that, Comprising: An extraction section, which includes a plurality of first high-speed centrifugal extractors connected in series. Each first high-speed centrifugal extractor includes a first extraction inlet and a second extraction inlet provided at one end, and a first extraction outlet and a second extraction outlet provided at the other end; and the first extraction inlet is communicated with the first extraction outlet, and the second extraction inlet is communicated with the second extraction outlet; between two adjacent first high-speed centrifugal extractors, the second extraction outlet of the upper-stage first high-speed centrifugal extractor is communicated with the second extraction inlet of the lower-stage first high-speed centrifugal extractor through a pipeline, and the first extraction inlet of the upper-stage first high-speed centrifugal extractor is communicated with the first extraction outlet of the lower-stage first high-speed centrifugal extractor through a pipeline; and an extractant is introduced into the second extraction inlet of the first-stage first high-speed centrifugal extractor through a pipeline, and an aqueous phase raffinate is introduced into the first extraction inlet of the last-stage first high-speed centrifugal extractor; the aqueous phase raffinate is the aqueous phase raffinate after cesium removal from the leaching and freezing clear liquid of lepidolite, the aqueous phase raffinate is alkaline, and includes rubidium, sodium, potassium and lithium ions; the extractant is prepared by diluting t-BAMBP with ESCAID110, and the concentration of the extractant is 0.4 - 0.6 mol / L of t-BAMBP; during the extraction section, the O / A ratio is controlled to be 5.3 - 5.6:1; A washing section, which includes a plurality of second high-speed centrifugal extractors connected in series. Each second high-speed centrifugal extractor includes a first washing inlet and a second washing inlet provided at one end, and a first washing outlet and a second washing outlet provided at the other end, and the first washing inlet is communicated with the first washing outlet, and the second washing inlet is communicated with the second washing outlet; between two adjacent second high-speed centrifugal extractors, the second washing outlet of the upper-stage second high-speed centrifugal extractor is communicated with the second washing inlet of the lower-stage second high-speed centrifugal extractor through a pipeline, and the first washing inlet of the upper-stage second high-speed centrifugal extractor is communicated with the first washing outlet of the lower-stage second high-speed centrifugal extractor through a pipeline; and the second washing inlet of the first-stage second high-speed centrifugal extractor is communicated with the second extraction outlet of the last-stage first high-speed centrifugal extractor through a pipeline, and first washing sulfuric acid is introduced into the first washing inlet of the last-stage second high-speed centrifugal extractor, and a first washed solution flows out from the first washing outlet of the first-stage second high-speed centrifugal extractor; The stripping section includes a plurality of third high-speed centrifugal extractors connected in series. Each third high-speed centrifugal extractor includes a first stripping inlet and a second stripping inlet provided at one end, and a first stripping outlet and a second stripping outlet provided at the other end. The first stripping inlet is communicated with the first stripping outlet, and the second stripping inlet is communicated with the second stripping outlet. Between two adjacent third high-speed centrifugal extractors, the second stripping outlet of the upper-level third high-speed centrifugal extractor is communicated with the second stripping inlet of the lower-level third high-speed centrifugal extractor through a pipeline, and the first stripping inlet of the upper-level third high-speed centrifugal extractor is communicated with the first stripping outlet of the lower-level third high-speed centrifugal extractor through a pipeline. And the second stripping inlet of the first-level third high-speed centrifugal extractor is communicated with the second washing outlet of the last-level second high-speed centrifugal extractor through a pipeline. Second stripping sulfuric acid is introduced into the first stripping inlet of the last-level third high-speed centrifugal extractor, stripped liquid flows out from the first stripping outlet of the first-level third high-speed centrifugal extractor, and the second stripping outlet of the last-level third high-speed centrifugal extractor is communicated with the second extraction inlet of the first-level first high-speed centrifugal extractor to form a cycle of the extraction liquid.

2. The rubidium extraction device according to claim 1, wherein: In the extraction section, control the concentration of OH in the solution to be extracted - to be 0.6 mol / L.

3. The rubidium extraction device according to claim 2, characterized in that: The extraction section includes 3 to 5 first high-speed centrifugal extractors connected in series; the washing section includes 4 to 6 second high-speed centrifugal extractors connected in series; the stripping section includes 2 to 4 third high-speed centrifugal extractors connected in series.

4. The rubidium extraction device according to claim 3, characterized in that: The extraction section includes 4 first high-speed centrifugal extractors connected in series; the washing section includes 5 second high-speed centrifugal extractors connected in series; the stripping section includes 3 third high-speed centrifugal extractors connected in series.

5. The rubidium extraction device according to claim 1, characterized in that: The concentration of the first washing sulfuric acid is 0.02 mol / L to 0.03 mol / L.

6. The rubidium extraction device according to claim 1, wherein: During the washing section, the O / A ratio is controlled to be 7.3 to 7.7:

1.

7. The rubidium extraction device according to claim 1, characterized in that: The concentration of the second stripping sulfuric acid is 0.20 mol / L to 0.21 mol / L.

8. The rubidium extraction device according to claim 1, wherein: During the stripping section, the O / A ratio is controlled to be 19 to 21:1.

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