Method for extracting rubidium through flow pattern regulation and control of 3D printing microreactor

Through the flow type regulation method of 3D printing microreactors, the problems of low mass transfer efficiency and uncontrollable flow type of the traditional rubidium extraction process are solved, and efficient rubidium extraction and purification are achieved, which are suitable for the fields of catalysis, energy and electronic materials.

CN120437918APending Publication Date: 2025-08-08KUNMING UNIV OF SCI & TECH
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Patent Information

Application Number
CN202510596504.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-09
Publication Date
2025-08-08

AI Technical Summary

Technical Problem

The traditional rubidium extraction process has problems such as low mass transfer efficiency, complex multi-stage series connection, and uncontrollable flow type. The existing microreactor technology lacks a dynamic switching mechanism for laminar flow, segment plug flow, and bubble flow.

Method used

The 3D-printed micro reactor was used to design the venturi structure of the Y-shaped inlet, tapered throat and tapered outlet. The flow control was achieved by adjusting the two-phase flow rate. Combining the TBAMBP extractant and the aqueous phase with a specific pH value, five-stage series extraction was performed using the segmented flow mode.

Benefits of technology

The single-stage extraction rate was improved to 84%, the five-stage series extraction rate reached 99.34%, the unit energy consumption was reduced by 65%, the equipment volume was reduced to 0.05m3, and the product RbCl purity was ≥99.5%, which was suitable for efficient recycling of low-concentration rubidium resources.

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Abstract

The invention discloses a method for extracting rubidium through flow pattern regulation and control of a 3D printing microreactor, the microreactor adopts a Venturi structure with a Y-shaped inlet, a gradually-shrinking throat part and a gradually-expanding outlet, and the diameter of a channel is gradually shrunk to 0.6 mm from 1.6 mm and then is gradually expanded to 1.6 mm; dynamic switching of laminar flow, slug flow and multiple strings of small bubble flow is achieved by adjusting the two-phase flow velocity to be 195mu m / min to 2500mu m / min. In a slug flow mode, a TBP-kerosene organic phase and a TBAMBP extraction agent are combined, the pH value of a water phase is 10-14, the five-stage series extraction rate is larger than or equal to 99.34%, the rubidium enrichment multiple is larger than or equal to 50, and the reverse extraction rate is larger than or equal to 95%. According to the method, interface updating is enhanced through the Venturi structure, the slug flow mass transfer coefficient reaches 0.15 s <-1 >, the purity of the product RbCl is larger than or equal to 99.5%, and the method is suitable for efficient recovery of low-concentration rubidium resources and has remarkable economic value in the fields of catalysis, energy and electronic materials.
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Description

Technical Field

[0001] The present invention relates to the field of microchemical technology, and particularly to a method for regulating the flow pattern of a 3D printed microreactor to extract rubidium by extraction. Background Art

[0002] Traditional rubidium extraction processes, such as shaking extraction and stirred tanks, have the following problems:

[0003] 1. Low mass transfer efficiency: relying on molecular diffusion, the single-stage extraction rate is usually less than 60%;

[0004] 2. Complexity of multi-stage series connection: multi-stage equipment is required to be connected in series, with a large floor area and high energy consumption;

[0005] 3. Uncontrollable flow pattern: unable to regulate the interfacial area through hydrodynamics.

[0006] Although existing microreactor technologies can improve mass transfer, they have the following limitations:

[0007] 1. Single structure: fixed flow channels are difficult to adapt to different extraction systems;

[0008] 2. Insufficient flow pattern regulation: lacking a dynamic switching mechanism for laminar flow, slug flow, and bubble flow.

[0009] Therefore, providing a method that can improve the extraction efficiency, mass transfer coefficient, reduce the energy consumption ratio, and has a controllable flow pattern is an urgent problem to be solved by those skilled in the art. Summary of the Invention

[0010] In view of this, the present invention provides a method for regulating the flow pattern of a 3D printed microreactor to extract rubidium by extraction.

[0011] To solve the above technical problems, the present invention adopts the following technical solutions:

[0012] A 3D printed microreactor, comprising:

[0013] A Venturi structure with a Y-shaped inlet, a tapered throat, and a diverging outlet;

[0014] Its channel diameter tapers from 1.6 mm to 0.6 mm and then diverges to 1.6 mm;

[0015] The ratio of the throat length to the inlet diameter is 1:2, the taper angle is 15°, and the divergence angle is 10°.

[0016] Preferably, the microreactor achieves flow pattern control by adjusting the flow rates of two phases from 145 μm / min to 2500 μm / min; wherein,

[0017] The flow rate of slug flow is 149 - 1100 μm / min, 100 < Re < 500, periodic droplet generation occurs, and the interfacial renewal rate is increased;

[0018] Laminar flow rate 1195-2000μm / min, Re<100, stable two-phase interface, suitable for high viscosity systems;

[0019] Multiple strings of small bubble flow with a flow rate of >2000μm / min, Re>500, bubble dispersion to enhance mass transfer, and a specific surface area of 2000m 2 / m 3 .

[0020] Preferably, the diameter of the tapered throat is 0.6 mm;

[0021] The material of the microreactor is a light-curable resin resistant to organic solvents, specifically an acrylate or epoxy resin.

[0022] A method for extracting rubidium by flow pattern control, the method using the microreactor according to claims 1-3, in a slug flow mode, with a five-stage series extraction rate of ≥99%;

[0023] The extractant was TBAMBP, the organic phase was a TBP-kerosene system, and the volume ratios of TBP to kerosene were 1:3, 1:5, and 1:7;

[0024] The pH of the aqueous phase is 10-14, and the oil / water ratios are 1:1, 2:1, and 1:3.

[0025] Preferably, the single-stage extraction rate increases with the increase of TBP concentration. When TBP:kerosene = 1:3, 1:5, and 1:7, the single-stage extraction rates are 57%, 67%, and 75-84%, respectively.

[0026] Preferably, the aqueous phase is an alkaline solution containing rubidium, Rb + The concentration was 50-200 ppm, the pH was adjusted to 12.5±0.5 by NaOH; the TBAMBP concentration in the organic phase was 0.1-0.5 mol / L.

[0027] Preferably, the stripping solution is 0.1-0.5 mol / L HCl, the stripping phase ratio O / A=1:2, and the stripping rate is ≥95%.

[0028] Preferably, the operating temperature of the microreactor is 25-45° C., and the pressure fluctuation range is ≤5 kPa.

[0029] Preferably, the rubidium enrichment multiple after the five-stage series connection is ≥50 times; and finally the organic phase is subjected to back extraction, evaporation and crystallization to obtain the RbCl product, with a purity of ≥99.5%.

[0030] Compared with the prior art, the present invention has achieved the following technical effects:

[0031] (1) Compared with the traditional process, the single-stage extraction rate of the present invention is increased from 52% to 84%, and the five-stage series extraction rate reaches 99.34%, while the single-stage extraction rate of the traditional oscillation method is only 52%;

[0032] (2) The unit energy consumption of the present invention is reduced by 65% (4.3kW·h / kg), and the equipment volume is reduced to 0.05m 3 ;

[0033] (3) The present invention strengthens the interface renewal through the Venturi structure, and the slug flow coefficient reaches 0.15s -1 , which is three times that of laminar flow, and the purity of the product RbCl is ≥99.5%;

[0034] (4) The present invention is suitable for the efficient recovery of low-concentration rubidium resources and has significant economic value in the fields of catalysis, energy and electronic materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 This is a schematic diagram of the 3D structure of the microreactor of the present invention;

[0036] Figure 2 Microscopic images of laminar flow, slug flow, and multi-string small bubble flow patterns of the present invention;

[0037] Figure 3 Graph showing the relationship between flow rate, Reynolds number (Re), capillary number (Ca), and mass transfer coefficient (kLa) of the present invention;

[0038] Figure 4 This is the concentration decay curve of the five-stage series extraction of rubidium in the present invention. DETAILED DESCRIPTION

[0039] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0040] like Figure 1 As shown, the present invention discloses a 3D printing microreactor, comprising:

[0041] Venturi structure with Y-shaped inlet, tapered throat and gradually diverging outlet;

[0042] Among them, the diameter of the tapered throat is 0.6mm;

[0043] Its channel diameter gradually decreases from 1.6mm to 0.6mm and then gradually expands to 1.6mm;

[0044] The ratio of the throat length to the inlet diameter is 1:2, the contraction angle is 15°, and the expansion angle is 10°;

[0045] The material of the microreactor is a photo-curable resin resistant to organic solvents, specifically acrylate or epoxy resin;

[0046] The microreactor controls the flow pattern by adjusting the flow rates of the two phases from 145 μm / min to 2500 μm / min;

[0047] The slug flow rate is 149 - 1100 μm / min, 100 < Re < 500, periodic droplet generation, and the interfacial renewal rate is increased;

[0048] The laminar flow rate is 1195 - 2000 μm / min, Re < 100, the two-phase interface is stable, and it is suitable for high-viscosity systems;

[0049] The multi-string small bubble flow rate > 2000 μm / min, Re > 500, bubble dispersion enhances mass transfer, and the specific surface area reaches 2000 m 2 / m 3 .

[0050] Among them, the laminar flow, slug flow, multi-string small bubble flow pattern microscopic images of the present invention and the relationship diagrams of the flow rate and Reynolds number (Re), capillary number (Ca), and mass transfer coefficient (kLa) of the present invention are respectively as Figure 2 and Figure 3 shown.

[0051] The present invention also discloses a method for regulating the extraction of rubidium by flow pattern. Using the microreactor of claims 1 - 3, in the slug flow mode, the five-stage series extraction rate ≥ 99%;

[0052] The extractant is TBAMBP, the organic phase is a TBP-kerosene system, and the volume ratio of TBP to kerosene is 1:3, 1:5, 1:7;

[0053] The pH of the aqueous phase is 10 - 14, and the oil / water ratio is 1:1, 2:1, 1:3.

[0054] The single-stage extraction rate increases with the increase of the TBP concentration. When the corresponding TBP:kerosene = 1:3, 1:5, 1:7, the single-stage extraction rates are 57%, 67%, and 75 - 84% respectively.

[0055] The aqueous phase is an alkaline solution containing rubidium, Rb + The concentration is 50 - 200 ppm, and the pH is adjusted to 12.5 ± 0.5 by NaOH; the concentration of TBAMBP in the organic phase is 0.1 - 0.5 mol / L.

[0056] The stripping solution is 0.1 - 0.5 mol / L HCl, the stripping ratio O / A = 1:2, and the stripping rate ≥ 95%.

[0057] The operating temperature of the microreactor is 25-45°C, and the pressure fluctuation range is ≤5kPa.

[0058] After the five-stage series reaction, the rubidium enrichment multiple is ≥50 times; the organic phase is finally subjected to back extraction, evaporation and crystallization to obtain the RbCl product, with a purity of ≥99.5%.

[0059] Among them, the concentration decay curve of five-stage series extraction of rubidium is as follows Figure 4 shown.

[0060] The comparison table of single-stage extraction rate, five-stage extraction rate, unit energy consumption, and equipment volume is shown in Table 1;

[0061] Table 1:

[0062] parameter Traditional oscillation method Microreactor of the present invention Single-stage extraction rate 52% 84% Five-level extraction rate 95% 99.34% Specific energy consumption (kW·h / kg) 12.5 4.3 <![CDATA[Equipment volume (m 3 )]]> 2.0 0.05 .

[0063] Example 1: Extraction of Rubidium in Laminar Flow Mode

[0064] A 3D printed microreactor, comprising:

[0065] Venturi structure with Y-shaped inlet, tapered throat and gradually diverging outlet;

[0066] Among them, the throat diameter is 0.6mm and the total length is 50mm;

[0067] Its channel diameter gradually decreases from 1.6mm to 0.6mm and then gradually expands to 1.6mm;

[0068] The ratio of throat length to inlet diameter is 1:2, the tapering angle is 15°, and the diverging angle is 10°;

[0069] The material of the microreactor is acrylic light-curing resin;

[0070] The laminar oil phase / water phase flow rate was 1.195 mm / min, Re = 85;

[0071] A method for extracting rubidium by flow pattern control, using the microreactor of claims 1-3, in slug flow mode, with a five-stage series extraction rate of ≥99%;

[0072] The extractant was TBAMBP, the organic phase was a TBP-kerosene system, and the volume ratio of TBP to kerosene was 1:3;

[0073] The pH of the aqueous phase is 10, the oil / water ratio is 1:1,

[0074] The single-stage extraction rate increases with the increase of TBP concentration. When the TBP:kerosene ratio is 1:3, the single-stage extraction rate is 57%.

[0075] The aqueous phase is an alkaline solution containing rubidium, Rb+ The concentration was 50 ppm, and the pH was adjusted to 10.0±0.5 by NaOH; the TBAMBP concentration in the organic phase was 0.1 mol / L.

[0076] The stripping solution is 0.1-0.5 mol / L HCl, the stripping phase ratio O / A is 1:2, and the stripping rate is ≥95%.

[0077] The operating temperature of the microreactor is 25-45°C, and the pressure fluctuation range is ≤5kPa.

[0078] After the five-stage series reaction, the rubidium enrichment multiple is ≥50 times; the organic phase is finally subjected to back extraction, evaporation and crystallization to obtain the RbCl product, with a purity of ≥99.5%.

[0079] Results: Single-stage extraction rate 57%, mass transfer coefficient kLa=0.05s -1 .

[0080] Example 2: Slug Flow Mode Extraction of Rubidium

[0081] A 3D printed microreactor, comprising:

[0082] Venturi structure with Y-shaped inlet, tapered throat and gradually diverging outlet;

[0083] Among them, the throat diameter is 0.6mm and the total length is 50mm;

[0084] Its channel diameter gradually decreases from 1.6mm to 0.6mm and then gradually expands to 1.6mm;

[0085] The ratio of throat length to inlet diameter is 1:2, the tapering angle is 15°, and the diverging angle is 10°;

[0086] The material of the microreactor is acrylic light-curing resin;

[0087] Slug flow: oil phase velocity 600 μm / min, water phase velocity 400 μm / min, Re=320, droplet length 200-300 μm, frequency 15 Hz;

[0088] A method for extracting rubidium by flow pattern control, using the microreactor of claims 1-3, in slug flow mode, with a five-stage series extraction rate of ≥99%;

[0089] The extractant was TBAMBP, the organic phase was a TBP-kerosene system, and the volume ratio of TBP to kerosene was 1:5;

[0090] The pH of the aqueous phase is 12, and the oil / water ratio is 2:1.

[0091] The single-stage extraction rate increases with the increase of TBP concentration. When the TBP:kerosene ratio is 1:5, the single-stage extraction rate is 67%.

[0092] The aqueous phase is an alkaline solution containing rubidium, Rb + The concentration was 150 ppm, and the pH was adjusted to 12.0±0.5 by NaOH; the TBAMBP concentration in the organic phase was 0.3 mol / L.

[0093] The stripping solution is 0.1-0.5 mol / L HCl, the stripping phase ratio O / A is 1:2, and the stripping rate is ≥95%.

[0094] The operating temperature of the microreactor is 25-45°C, and the pressure fluctuation range is ≤5kPa.

[0095] After the five-stage series reaction, the rubidium enrichment multiple is ≥50 times; the organic phase is finally subjected to back extraction, evaporation and crystallization to obtain the RbCl product, with a purity of ≥99.5%.

[0096] Results: Single-stage extraction rate 67%, kLa=0.14s -1 .

[0097] Example 3: Extraction of rubidium using a multi-bubble flow pattern

[0098] A 3D printed microreactor, comprising:

[0099] Venturi structure with Y-shaped inlet, tapered throat and gradually diverging outlet;

[0100] Among them, the throat diameter is 0.6mm and the total length is 50mm;

[0101] Its channel diameter gradually decreases from 1.6mm to 0.6mm and then gradually expands to 1.6mm;

[0102] The ratio of throat length to inlet diameter is 1:2, the tapering angle is 15°, and the diverging angle is 10°;

[0103] The material of the microreactor is acrylic light-curing resin;

[0104] Multiple strings of small bubble flow: oil phase flow rate 2.2mm / min, water phase flow rate 1.8mm / min, Re=620, bubble diameter 50-80μm, uniform dispersion;

[0105] A method for extracting rubidium by flow pattern control, using the microreactor of claims 1-3, in slug flow mode, with a five-stage series extraction rate of ≥99%;

[0106] The extractant was TBAMBP, the organic phase was a TBP-kerosene system, and the volume ratio of TBP to kerosene was 1:7;

[0107] The pH of the aqueous phase was 14.0, and the oil / water ratio was 1:3.

[0108] The single-stage extraction rate increases with the increase of TBP concentration. When the TBP:kerosene ratio is 1:7, the single-stage extraction rate is 75%.

[0109] The aqueous phase is an alkaline solution containing rubidium, Rb + The concentration was 200 ppm, and the pH was adjusted to 14.0±0.5 by NaOH; the TBAMBP concentration in the organic phase was 0.5 mol / L.

[0110] The stripping solution is 0.1-0.5 mol / L HCl, the stripping phase ratio O / A is 1:2, and the stripping rate is ≥95%.

[0111] The operating temperature of the microreactor is 25-45°C, and the pressure fluctuation range is ≤5kPa.

[0112] After the five-stage series reaction, the rubidium enrichment multiple is ≥50 times; the organic phase is finally subjected to back extraction, evaporation and crystallization to obtain the RbCl product, with a purity of ≥99.5%.

[0113] Results: Single-stage extraction rate 75%, kLa=0.22s -1 .

[0114] Example 4: Five-stage cascade extraction

[0115] A 3D printed microreactor, comprising:

[0116] Venturi structure with Y-shaped inlet, tapered throat and gradually diverging outlet;

[0117] Among them, the throat diameter is 0.6mm and the total length is 50mm;

[0118] Its channel diameter gradually decreases from 1.6mm to 0.6mm and then gradually expands to 1.6mm;

[0119] The ratio of throat length to inlet diameter is 1:2, the tapering angle is 15°, and the diverging angle is 10°;

[0120] The material of the microreactor is acrylic light-curing resin;

[0121] Slug flow velocity 500 μm / min, Re = 280, five stages in series;

[0122] A method for extracting rubidium by flow pattern control, using the microreactor of claims 1-3, in slug flow mode, with a five-stage series extraction rate of ≥99%;

[0123] The extractant was TBAMBP, the organic phase was a TBP-kerosene system, and the volume ratio of TBP to kerosene was 1:5;

[0124] The pH of the aqueous phase is 12.5, and the oil / water ratio is 2:1.

[0125] The single-stage extraction rate increases with the increase of TBP concentration. When the TBP:kerosene ratio is 1:5, the single-stage extraction rate is 67%.

[0126] The aqueous phase was an alkaline solution containing rubidium, with an Rb+ concentration of 100 ppm and a pH adjusted to 12.5±0.5 by NaOH; the TBAMBP concentration in the organic phase was 0.2 mol / L.

[0127] The stripping solution is 0.1-0.5 mol / L HCl, the stripping phase ratio O / A is 1:2, and the stripping rate is ≥95%.

[0128] The operating temperature of the microreactor is 25-45°C, and the pressure fluctuation range is ≤5kPa.

[0129] After the five-stage series reaction, the rubidium enrichment multiple is ≥50 times; the organic phase is finally subjected to back extraction, evaporation and crystallization to obtain the RbCl product, with a purity of ≥99.5%.

[0130] Results: The total extraction rate of rubidium was 99.5%, and the residual concentration was <0.5ppm.

[0131] Example 5: TBP: kerosene = 1:3, oil / water = 1:1

[0132] A 3D printed microreactor, comprising:

[0133] Venturi structure with Y-shaped inlet, tapered throat and gradually diverging outlet;

[0134] Among them, the throat diameter is 0.6mm and the total length is 50mm;

[0135] Its channel diameter gradually decreases from 1.6mm to 0.6mm and then gradually expands to 1.6mm;

[0136] The ratio of throat length to inlet diameter is 1:2, the tapering angle is 15°, and the diverging angle is 10°;

[0137] The material of the microreactor is acrylic light-curing resin;

[0138] Slug flow 0.7 mm / min, Re = 320;

[0139] A method for extracting rubidium by flow pattern control, using the microreactor of claims 1-3, in slug flow mode, with a five-stage series extraction rate of ≥99%;

[0140] The extractant was TBAMBP, the organic phase was a TBP-kerosene system, and the volume ratio of TBP to kerosene was 1:3;

[0141] The pH of the aqueous phase was 10.5, and the oil / water ratio was 1:1.

[0142] The single-stage extraction rate increases with the increase of TBP concentration. When the TBP:kerosene ratio is 1:3, the single-stage extraction rate is 57%.

[0143] The aqueous phase is an alkaline solution containing rubidium, Rb + The concentration was 50 ppm, and the pH was adjusted to 10.5±0.5 by NaOH; the TBAMBP concentration in the organic phase was 0.1 mol / L.

[0144] The stripping solution is 0.1-0.5 mol / L HCl, the stripping phase ratio O / A is 1:2, and the stripping rate is ≥95%.

[0145] The operating temperature of the microreactor is 25-45°C, and the pressure fluctuation range is ≤5kPa.

[0146] After the five-stage series reaction, the rubidium enrichment multiple is 50 times; the organic phase is finally subjected to back extraction, evaporation and crystallization to obtain the RbCl product with a purity of ≥99.5%.

[0147] result:

[0148] The single-stage extraction rate is 57%, and the extraction rate after five-stage series connection is 99.0%;

[0149] Stripping solution Rb + The concentration is 2.5g / L and the enrichment factor is 50 times.

[0150] Example 6: TBP: kerosene = 1:5, oil / water = 2:1

[0151] A 3D printed microreactor, comprising:

[0152] Venturi structure with Y-shaped inlet, tapered throat and gradually diverging outlet;

[0153] Among them, the throat diameter is 0.6mm and the total length is 50mm;

[0154] Its channel diameter gradually decreases from 1.6mm to 0.6mm and then gradually expands to 1.6mm;

[0155] The ratio of throat length to inlet diameter is 1:2, the tapering angle is 15°, and the diverging angle is 10°;

[0156] The material of the microreactor is acrylic light-curing resin;

[0157] Multiple small bubble streams 2.4 mm / min, Re = 620;

[0158] A method for extracting rubidium by flow pattern control, using the microreactor of claims 1-3, in slug flow mode, with a five-stage series extraction rate of ≥99%;

[0159] The extractant was TBAMBP, the organic phase was a TBP-kerosene system, and the volume ratio of TBP to kerosene was 1:5;

[0160] The pH of the aqueous phase was 12.0, and the oil / water ratio was 2:1.

[0161] The single-stage extraction rate increases with the increase of TBP concentration. When the TBP:kerosene ratio is 1:5, the single-stage extraction rate is 67%.

[0162] The aqueous phase is an alkaline solution containing rubidium, Rb + The concentration was 150 ppm, and the pH was adjusted to 12.0±0.5 by NaOH; the TBAMBP concentration in the organic phase was 0.3 mol / L.

[0163] The stripping solution is 0.1-0.5 mol / L HCl, the stripping phase ratio O / A is 1:2, and the stripping rate is ≥95%.

[0164] The operating temperature of the microreactor is 25-45°C, and the pressure fluctuation range is ≤5kPa.

[0165] After the five-stage series reaction, the rubidium enrichment multiple is 50 times; the organic phase is finally subjected to back extraction, evaporation and crystallization to obtain the RbCl product with a purity of ≥99.5%.

[0166] result:

[0167] The single-stage extraction rate is 67%, and the extraction rate after five-stage series connection is 99.3%;

[0168] Stripping solution Rb + The concentration is 7.5g / L and the enrichment factor is 50 times.

[0169] Example 7: TBP: kerosene = 1:7, oil / water = 1:3

[0170] A 3D printed microreactor, comprising:

[0171] Venturi structure with Y-shaped inlet, tapered throat and gradually diverging outlet;

[0172] Among them, the throat diameter is 0.6mm and the total length is 50mm;

[0173] Its channel diameter gradually decreases from 1.6mm to 0.6mm and then gradually expands to 1.6mm;

[0174] The ratio of throat length to inlet diameter is 1:2, the tapering angle is 15°, and the diverging angle is 10°;

[0175] The material of the microreactor is acrylic light-curing resin;

[0176] Slug flow 0.74 mm / min, Re = 280;

[0177] A method for extracting rubidium by flow pattern control, using the microreactor of claims 1-3, in slug flow mode, with a five-stage series extraction rate of ≥99%;

[0178] The extractant was TBAMBP, the organic phase was a TBP-kerosene system, and the volume ratio of TBP to kerosene was 1:7;

[0179] The pH of the aqueous phase is 13.2, and the oil / water ratio is 2:1.

[0180] The single-stage extraction rate increases with the increase of TBP concentration. When the TBP:kerosene ratio is 1:7, the single-stage extraction rate is 80%.

[0181] The aqueous phase is an alkaline solution containing rubidium, Rb + The concentration was 80 ppm, and the pH was adjusted to 13.2±0.5 by NaOH; the TBAMBP concentration in the organic phase was 0.4 mol / L.

[0182] The stripping solution is 0.1-0.5 mol / L HCl, the stripping phase ratio O / A is 1:2, and the stripping rate is ≥95%.

[0183] The operating temperature of the microreactor is 25-45°C, and the pressure fluctuation range is ≤5kPa.

[0184] After the five-stage series reaction, the rubidium enrichment multiple is 50 times; the organic phase is finally subjected to back extraction, evaporation and crystallization to obtain the RbCl product with a purity of ≥99.5%.

[0185] result:

[0186] The single-stage extraction rate is 80%, and the extraction rate after five-stage series connection is 99.7%;

[0187] Stripping solution Rb + The concentration is 4.0g / L and the enrichment factor is 50 times.

[0188] The above description is merely a preferred embodiment of the present invention and does not limit the technical scope of the present invention. Therefore, any minor modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A 3D printed microreactor, characterized in that: Comprising: A Venturi structure with a Y-shaped inlet, a tapered throat, and a diverging outlet; Its channel diameter tapers from 1.6 mm to 0.6 mm and then diverges back to 1.6 mm; The ratio of the throat length to the inlet diameter is 1:2, the taper angle is 15°, and the divergence angle is 10°.

2. A 3D printing microreactor according to claim 1, characterized in that, The microreactor achieves flow pattern control by adjusting the flow rates of the two phases from 145 μm / min to 2500 μm / min; where The slug flow rate is 149 - 1100 μm / min, 100 < Re < 500, periodic droplet generation, and the interfacial renewal rate is increased; The laminar flow rate is 1195 - 2000 μm / min, Re < 100, the two-phase interface is stable, suitable for high-viscosity systems; Multiple strings of small bubble flow with a flow rate of >2000μm / min, Re>500, bubble dispersion to enhance mass transfer, and a specific surface area of 2000m 2 / m 3 .

3. A 3D printing microreactor according to claim 1, characterized in that: The diameter of the tapered throat is 0.6 mm; The material of the microreactor is a photo-curable resin resistant to organic solvents, specifically acrylate or epoxy resin.

4. A method for extracting rubidium by regulating flow pattern, characterized in that: The method uses the microreactor described in claims 1 - 3. In the slug flow mode, the five-stage tandem extraction rate is ≥99%; The extractant is TBAMBP, the organic phase is a TBP-kerosene system, and the volume ratio of TBP to kerosene is 1:3, 1:5, 1:7; The pH of the aqueous phase is 10 - 14, and the oil / water ratio is 1:1, 2:1, 1:

3.

5. The method for extracting rubidium by flow pattern control according to claim 4, characterized in that: The single-stage extraction rate increases with the increase of the TBP concentration. When TBP:kerosene = 1:3, 1:5, 1:7, the single-stage extraction rates are 57%, 67%, 75 - 84% respectively.

6. The method for extracting rubidium by flow pattern control according to claim 3, characterized in that: The aqueous phase is an alkaline solution containing rubidium, the Rb+ concentration is 50 - 200 ppm, and the pH is adjusted to 12.5 ± 0.5 with NaOH; the concentration of TBAMBP in the organic phase is 0.1 - 0.5 mol / L.

7. The method for extracting rubidium by flow pattern control according to claim 3, characterized in that: The stripping solution is 0.1 - 0.5 mol / L HCl, the stripping phase ratio O / A = 1:2, and the stripping rate is ≥95%.

8. The method for extracting rubidium by flow pattern control according to claim 3, characterized in that: The operating temperature of the microreactor is 25 - 45°C, and the pressure fluctuation range is ≤5 kPa.

9. The method for extracting rubidium by flow pattern control according to claims 4-8, characterized in that: After five-stage tandem, the rubidium enrichment multiple is ≥50 times; the final organic phase is stripped, evaporated, and crystallized to obtain RbCl product, and its purity is ≥99.5%.