U-shaped tubular extraction equipment and use method thereof

Abstract

The invention relates to U-shaped pipe type extraction equipment and a use method thereof. The U-shaped pipe type extraction equipment comprises a U-shaped pipeline, a stirring device and a separating device, the U-shaped pipeline comprises a first vertical section, a transverse section and a second vertical section which are connected in sequence; the U-shaped pipeline further comprises an extraction raw material inlet formed in the first vertical section; the stirring device is positioned on the transverse section of the U-shaped pipeline; the separation device is positioned above the U-shaped pipeline, and the lower part of the separation device is respectively communicated with the tops of the first vertical section and the second vertical section; the separation device comprises a light phase discharge port and a heavy phase discharge port, and the light phase discharge port and the heavy phase discharge port are formed in the side part of the separation device. The separation device is arranged above the U-shaped pipeline, so that the whole equipment forms a circulating pipe type structure, the standing time of mixed liquid can be controlled, the single-stage extraction efficiency is improved, meanwhile, the occupied area of the equipment is greatly reduced, and industrial amplification is facilitated.

Description

Technical Field

[0001] The present invention relates to the field of extraction technology, in particular to a liquid-liquid extraction device, and specifically to a U-shaped tube extraction device and a use method thereof. Background Art

[0002] Liquid-liquid extraction is a separation technology widely used in chemical, metallurgical, pharmaceutical and environmental protection fields, with many advantages such as high separation efficiency and high selectivity. Extraction equipment mainly includes mixing and settling tanks, extraction towers, tubular extraction equipment, centrifugal extraction equipment, liquid membrane extraction equipment, ultrasonic extraction equipment, etc. Different extraction equipment is suitable for different process requirements and material characteristics. Choosing the right equipment is crucial to improving extraction efficiency and reducing costs.

[0003] The mixing and settling tank has unique advantages in terms of equipment simplicity, operational flexibility, and anti-clogging ability, but its mass transfer efficiency and solvent utilization rate are not high, so it is more suitable for crude extraction of raw liquid and small-scale production scenarios. The extraction tower adopts countercurrent extraction, which has high mass transfer efficiency, but axial backmixing is prone to occur during operation. In addition, the flow of materials in the tower depends on the density difference of the materials and the packing structure, and the increase in processing capacity is limited. In comparison, the centrifugal extractor has a higher volumetric efficiency and mass transfer speed, but its drum is prone to clogging and has poor processing capacity for solid-containing materials. However, advanced extraction technologies such as liquid membrane extraction equipment and ultrasonic extraction equipment can only be well applied in laboratories due to their high technical barriers and difficulty in amplification. It is still difficult to achieve large-scale industrial application.

[0004] Tubular extraction devices are usually composed of one or more connected tubes. The extraction process is achieved through the rapid flow of liquid. The contact efficiency between the solvent and the extract is high, the extraction speed is fast, and the parameters such as flow rate, temperature and pressure are easy to control, which is convenient for optimizing the extraction and separation process. It is particularly suitable for research and development work in laboratory environments. At the same time, it can handle materials with high solid content. However, its limitations in large-scale industrial applications still need to be further improved and overcome.

[0005] CN213492120U discloses a new type of tubular extractor with good sealing effect and timely sewage discharge, which changes the traditional box-type mixing and settling tank into a pipeline type, enhances the sealing performance of the equipment, and solves the leakage and volatilization problems in the extraction process of volatile organic phase. However, it is still a mixing and settling tank equipment in essence.

[0006] CN103254262A discloses a method for extracting androstenedione using a pipeline continuous ultrasonic extraction technology, which strengthens the liquid-liquid two-phase dispersion mixing in the pipeline by an ultrasonic method, reduces the amount of solvent used in the extraction process, and reduces energy consumption. However, since the extraction process in the tubular structure is a liquid-liquid downstream extraction, in order to increase the extraction efficiency, the required pipeline length is very long and the floor space is large. In addition, the mixed liquid after extraction still needs to be separated by a disc centrifuge, and the process is more complicated.

[0007] In summary, it is necessary to develop a tubular extraction equipment that can reduce the footprint while improving the extraction efficiency and optimizing the extraction process. Summary of the invention

[0008] In order to solve the above technical problems, the present invention uses a U-shaped pipe for extraction and arranges a separation device above the U-shaped pipe, so that the entire equipment forms a circulating tubular structure, which can improve the extraction efficiency while reducing the occupied area.

[0009] To achieve this object, the present invention adopts the following technical solutions:

[0010] In a first aspect, the present invention provides a U-shaped tube type extraction device, the U-shaped tube type extraction device comprising a U-shaped pipeline, a stirring device and a separation device;

[0011] The U-shaped pipeline comprises a first vertical section, a transverse section and a second vertical section connected in sequence; the U-shaped pipeline also comprises an extraction raw material inlet arranged in the first vertical section;

[0012] The stirring device is located in the transverse section of the U-shaped pipe;

[0013] The separation device is located above the U-shaped pipe, and the lower part of the separation device is communicated with the top of the first vertical section and the top of the second vertical section respectively;

[0014] The separation device comprises a light phase discharge port and a heavy phase discharge port, wherein the light phase discharge port and the heavy phase discharge port are arranged at a side of the separation device.

[0015] The U-shaped tube extraction equipment of the present invention better realizes the integrated structure of the mixed extraction U-shaped pipeline and the separation device. The present invention can make full use of the advantages of the U-shaped pipeline, such as fast fluid flow rate and high turbulence intensity, to improve the extraction mass transfer rate; at the same time, the stirring device is arranged in the transverse section of the U-shaped pipeline to shear the mixed liquid to promote the breakup of droplets, reduce the size of droplets, increase the contact area of ​​the liquid-liquid two-phase, thereby improving the extraction efficiency; the stirring device also provides power for the transportation and circulation of the mixed liquid; the mixed liquid can be quickly extracted in the U-shaped pipeline, and the light phase and the heavy phase can be quickly separated in the separation device; by controlling the inlet flow rate and outlet flow rate of the mixed liquid, the single-stage extraction efficiency of the equipment can be quantitatively controlled. The U-shaped tube extraction equipment has a fast extraction speed, a large processing capacity, can process high-solid content materials, has stable operation, good controllability, small footprint, is easy to operate continuously, and is easy to industrially scale up. It can process large-flow, high-solid content liquid-liquid two-phase extraction processes and has broad application prospects.

[0016] The U-shaped tube extraction equipment provided by the present invention can be used alone, or at least two sets of equipment can be used in series or in parallel. Those skilled in the art can make a selection according to the specific process.

[0017] As a preferred technical solution of the present invention, the U-shaped pipe further includes a mixer inside; wherein the stirring device and the mixer are sequentially arranged along the material flow direction.

[0018] Preferably, the mixer is arranged in the second vertical section.

[0019] The mixer provided in the second vertical section of the present invention can further mix the mixed liquid in the U-shaped pipe, so that the mixed liquid can still be fully mixed during the upward flow, thereby preventing liquid stratification and improving the extraction and separation effect.

[0020] Preferably, the mixer comprises a static mixer.

[0021] Preferably, the static mixer comprises a spoiler.

[0022] Preferably, the shape of the spoiler comprises a spiral fin.

[0023] Preferably, the stirring device comprises an axial flow pump.

[0024] Preferably, the axial flow pump comprises an impeller and a central shaft.

[0025] Preferably, the impeller is connected to the central axis, and geometric centers of the impeller and the central axis overlap.

[0026] Preferably, blades are arranged in the circumferential direction of the impeller.

[0027] Preferably, the blades comprise push-down blades.

[0028] As a preferred technical solution of the present invention, the ratio of the outermost dimension of the blade of the stirring device to the diameter of the U-shaped pipe is (0.5-0.95):1, for example, it can be 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1 or 0.95:1, but is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0029] The present invention limits the ratio of the outermost dimension of the blade of the stirring device to the diameter of the U-shaped pipe, which can further promote the shearing of the mixed liquid by the stirring device, so as to promote the breakup of droplets, reduce the size of droplets, increase the contact area between the liquid and liquid phases, and thus improve the extraction efficiency. If the ratio of the outermost dimension of the blade to the diameter of the U-shaped pipe is less than 0.5, the contact area between the blade and the mixed liquid is too small, and the shearing and conveying capacity is insufficient, which easily leads to a slow liquid circulation flow rate and a large droplet size; if the ratio of the outermost dimension of the blade to the diameter of the U-shaped pipe is greater than 0.95, when the impeller rotates rapidly, the deformation of the central axis will cause friction between the blade and the pipe, which is not conducive to the stable operation of the equipment.

[0030] Preferably, the downward pressure angle of the downward pressure blade is 15-75°, for example, it can be 15°, 25°, 35°, 45°, 55°, 65° or 75°, but is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0031] Preferably, the rotation speed range of the impeller is 100-1500 rpm, for example, it can be 100 rpm, 300 rpm, 500 rpm, 1000 rpm or 1500 rpm, but it is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0032] Preferably, the ratio of the length of the impeller of the stirring device in the U-shaped pipe to the diameter of the U-shaped pipe is (0.5-2):1, for example, it can be 0.5:1, 0.7:1, 1:1, 1.5:1 or 2:1, but is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0033] The present invention limits the ratio of the length of the impeller of the stirring device in the U-shaped pipe to the diameter of the U-shaped pipe, thereby further increasing the contact area between the liquid-liquid two phases, improving the extraction efficiency, and providing power for the circulation of the mixed liquid; if the ratio of the length of the impeller in the U-shaped pipe to the diameter of the U-shaped pipe is less than 0.5, the thrust of the stirring device will be insufficient, the flow rate of the mixed liquid will be reduced, the particles in the mixed liquid will be settled, and the extraction efficiency will be finally reduced; if the ratio of the length of the impeller in the U-shaped pipe to the diameter of the U-shaped pipe is greater than 2.0, the friction loss will be increased, the stirring efficiency will be reduced, the cavitation risk will be increased, and it will be not conducive to the stable operation of the equipment.

[0034] Preferably, the structure of the separation device includes a horizontal cylinder and / or a horizontal cuboid.

[0035] As a preferred technical solution of the present invention, the internal cavity of the separation device includes a clarification chamber and a mixing chamber from top to bottom.

[0036] Preferably, a transverse baffle is provided between the mixing chamber and the clarifying chamber, and the transverse baffle isolates the clarifying chamber and the mixing chamber into two independent spaces.

[0037] The present invention arranges the clarification chamber above the mixing chamber, which can reduce the floor space compared to the horizontal series arrangement of the mixing chamber and the clarification chamber. At the same time, since the clarification chamber is located at the upper part of the separation device, the clarification area can be made into a thin layer phase separation, which can greatly reduce the volume of the clarification chamber. The present invention adopts the gravity separation principle, so that the extracted light phase and heavy phase liquid can be naturally stratified in the clarification chamber, which is convenient for the subsequent two-phase separation.

[0038] Preferably, the spatial volume ratio of the mixing chamber to the clarifying chamber is 1:(1-20), for example, it can be 1:1, 1:5, 1:10, 1:15 or 1:20, but it is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0039] As a preferred technical solution of the present invention, the mixing chamber and the clarifying chamber are connected by an outer tube, and the outer tube is connected to a material outlet arranged on the mixing chamber and a material inlet arranged on the clarifying chamber; the material inlet and the material outlet are respectively arranged on the sides of the clarifying chamber and the mixing chamber.

[0040] The mixing chamber and the clarifying chamber of the present invention are connected by an outer tube, and the mixed liquid flows from the material outlet on the mixing chamber through the outer tube into the clarifying chamber. Compared with opening a channel on the transverse baffle to allow the mixed liquid to enter the clarifying chamber from the mixing chamber, the use of an outer tube to connect the mixing chamber and the clarifying chamber can set a solenoid valve on the outer tube, and the residence time of the mixed liquid in the U-shaped tube is controlled by adjusting the valve opening, and the flow rate of the mixed liquid entering the clarifying chamber is controlled, thereby controlling the single-stage extraction efficiency of the equipment and optimizing the extraction effect.

[0041] Preferably, the material outlet is arranged at a side of the mixing chamber close to the second vertical section.

[0042] Preferably, the diameter of the U-shaped pipe is 30-500 mm, for example, 30 mm, 100 mm, 200 mm, 300 mm, 400 mm or 500 mm, but is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0043] Preferably, the diameter of the horizontal cylinder is 30-2000 mm, for example, 30 mm, 100 mm, 500 mm, 1000 mm or 2000 mm, but is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0044] Preferably, the height of the horizontal cuboid is 30-2000 mm, for example, 30 mm, 100 mm, 500 mm, 1000 mm or 2000 mm, but is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0045] As a preferred technical solution of the present invention, an overflow phase separation weir and a vertical partition are arranged inside the clarification chamber.

[0046] The overflow phase-separation weir inside the clarification chamber of the present invention is used to adjust the heavy phase liquid level and the light phase liquid level; the entrainment phenomenon between the light phase and the heavy phase can be reduced; its vertical partition can suppress fluid turbulence, prolong the residence time of the mixed liquid in the clarification chamber, promote the sedimentation of the heavy phase, and improve the extraction and separation effect.

[0047] Preferably, the overflow phase separation weir is arranged on the side of the clarification chamber close to the first vertical section; and two adjacent vertical partitions are staggered.

[0048] Preferably, the number of the vertical partitions is 1-10, for example, 1, 2, 4, 6, 8 or 10, but is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0049] As a preferred technical solution of the present invention, the heavy phase discharge port and the light phase discharge port are arranged on the side of the clarification chamber, and the heavy phase discharge port is arranged below the light phase discharge port.

[0050] Preferably, the heavy phase discharge port and the light phase discharge port are arranged on a side of the clarification chamber away from a material inlet.

[0051] The present invention arranges the light phase discharge port and the heavy phase discharge port of the clarification chamber at the side of the clarification chamber away from the material inlet, that is, at the side close to the first vertical section, which can effectively alleviate the stratification of the liquid-liquid two phases in the clarification chamber and improve the extraction efficiency.

[0052] Preferably, a sleeve is arranged outside the U-shaped pipe.

[0053] Preferably, the material of the U-shaped pipe includes any one of stainless steel, polytetrafluoroethylene, fiberglass, polypropylene, polyvinyl chloride, Hastelloy or titanium alloy, or a combination of at least two of them, wherein typical but non-limiting combinations include: a combination of stainless steel and polytetrafluoroethylene, a combination of stainless steel and fiberglass, a combination of polytetrafluoroethylene and polypropylene, a combination of stainless steel and titanium alloy, a combination of stainless steel, fiberglass and titanium alloy, a combination of stainless steel, fiberglass and Hastelloy, a combination of polytetrafluoroethylene, polypropylene and polyvinyl chloride, a combination of stainless steel, fiberglass, Hastelloy and titanium alloy, a combination of stainless steel, polytetrafluoroethylene, polypropylene and polyvinyl chloride, a combination of stainless steel, polytetrafluoroethylene, fiberglass, Hastelloy and titanium alloy, a combination of stainless steel, polytetrafluoroethylene, polypropylene, polyvinyl chloride and titanium alloy, a combination of stainless steel, polytetrafluoroethylene, fiberglass, polypropylene, polyvinyl chloride and titanium alloy, a combination of stainless steel, polytetrafluoroethylene, fiberglass, polypropylene, polyvinyl chloride and titanium alloy, a combination of stainless steel, polytetrafluoroethylene, fiberglass, polypropylene, Hastelloy and titanium alloy, a combination of stainless steel, polytetrafluoroethylene, fiberglass, polypropylene, polyvinyl chloride, Hastelloy and titanium alloy.

[0054] The specific material selection of the U-shaped pipe in the present invention needs to comprehensively consider factors such as medium corrosiveness, operating temperature, operating pressure, economy and processing performance.

[0055] Preferably, the ratio of the length to the diameter of the U-shaped pipe is (10-100):1, for example, it can be 10:1, 20:1, 40:1, 60:1, 80:1 or 100:1, but is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0056] Preferably, the first vertical segment, the transverse segment and the second vertical segment are connected via an arc-shaped corner.

[0057] Preferably, the U-shaped tube extraction equipment further comprises a heavy phase storage device and a light phase storage device.

[0058] Preferably, a first pipeline and a third pipeline are sequentially arranged between the light phase storage device and the extraction raw material inlet along the material flow direction.

[0059] Preferably, a second pipeline and a third pipeline are sequentially arranged between the heavy phase storage device and the extraction raw material inlet along the material flow direction.

[0060] Preferably, the U-shaped tube extraction equipment further comprises an automatic control system.

[0061] Preferably, the automatic control system includes a temperature sensor, a pressure sensor, a liquid level sensor, a flow sensor and a solenoid valve.

[0062] Preferably, the temperature sensor is disposed between the stirring device and the mixer.

[0063] Preferably, the automatic control system comprises two of the pressure sensors.

[0064] Preferably, the two pressure sensors are both arranged in the first vertical section of the U-shaped pipe.

[0065] Preferably, the two pressure sensors are respectively arranged above and below the extraction raw material inlet.

[0066] Preferably, the automatic control system comprises three liquid level sensors.

[0067] Preferably, the three liquid level sensors are respectively arranged in the clarification chamber, the heavy phase storage device and the light phase storage device.

[0068] Preferably, the automatic control system comprises three flow sensors.

[0069] Preferably, the automatic control system includes three solenoid valves.

[0070] Preferably, the solenoid valve and the flow sensor are sequentially arranged on the first pipeline, the second pipeline and the outer pipe along the material flow direction.

[0071] Preferably, the ratio of the distance between the extraction raw material inlet and the bottom of the first vertical section to the length of the first vertical section is (1 / 9-2 / 3):1, for example, it can be 1 / 9:1, 2 / 9:1, 1 / 3:1, 4 / 9:1, 5 / 9:1 or 2 / 3:1, but is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0072] In a second aspect, the present invention provides a method for using the U-shaped tube extraction equipment according to the first aspect, the method comprising: passing a heavy phase raw material liquid and a light phase extraction solvent into the extraction raw material inlet of the U-shaped pipe, and turning on the stirring device to allow the materials to flow through the stirring device and the separation device in sequence to perform liquid-liquid extraction and separation.

[0073] The heavy phase raw material liquid and the light phase extraction solvent are introduced into the extraction raw material inlet of the U-shaped pipe, and the stirring device is turned on to shear the mixed liquid of the heavy phase raw material liquid and the light phase extraction solvent to promote the breakup of droplets. At the same time, the stirring device can provide power for the circulation of the mixed liquid in the U-shaped pipe and for the mixed liquid to enter the subsequent separation device. After the mixed liquid enters the separation device, liquid-liquid separation is performed. The U-shaped tube extraction equipment provided by the present invention has the advantages of simple use method, easy operation, and easy industrial scale-up.

[0074] As a preferred technical solution of the present invention, the method of use further comprises: between the stirring device and the separation device, using a mixer to perform a second mixing of the heavy phase raw material liquid and the light phase extraction solvent.

[0075] The present invention uses a mixer between the stirring device and the separation device to perform a second mixing of the heavy phase raw material liquid and the light phase extraction solvent, which can further mix the mixed liquid and prevent the mixed liquid from stratifying and droplet aggregation during the upward flow process.

[0076] As a preferred technical solution of the present invention, when the material flows through the separation device, the first part of the material enters the clarification chamber of the separation device for separation, and the second part of the material continues to enter the U-shaped pipe through the mixing chamber of the separation device for circulation and mixing.

[0077] The present invention can control the residence time of the material in the clarification chamber by controlling the flow rate of the material entering the clarification chamber, so as to promote the sedimentation of the heavy phase and improve the extraction and separation effect. At the same time, the first part of the material enters the clarification chamber for separation, so as to remove the target component in time and avoid its accumulation in the mixed liquid. The second part of the material continues to circulate and mix in the U-shaped pipe to maintain the contact between the two phases, ensure that the unextracted components can be fully contacted, and finally optimize the separation effect.

[0078] Preferably, the method of use comprises the following steps:

[0079] (1) Premixing the light phase extraction solvent and the heavy phase raw material liquid, and then inputting them into the extraction raw material inlet on the U-shaped pipe;

[0080] (2) turning on the stirring device to mix and transport the heavy phase raw material liquid and the light phase extraction solvent;

[0081] (3) After being mixed by the stirring device, the heavy phase raw material liquid and the light phase extraction solvent flow through the mixer for a second mixing;

[0082] (4) After the second mixing in the mixer, the first part of the material in the U-shaped pipe enters the clarification chamber of the separation device for separation, and the light phase liquid and heavy phase liquid separated in the clarification chamber are discharged through the light phase discharge port and the heavy phase discharge port respectively, and the second part of the material continues to enter the U-shaped pipe through the mixing chamber of the separation device for circulation mixing.

[0083] Preferably, the delivery flow rates of the heavy phase raw liquid and the light phase extraction solvent are independently 0.001-10 m 3 / h, for example, it can be 0.001m 3 / h、0.01m 3 / h、0.1m 3 / h、1m 3 / h、5m 3 / h or 10m 3 / h, but is not limited to the listed values, and other values ​​not listed within the above numerical range are also applicable.

[0084] Preferably, the volume ratio of the first part of the material entering the clarification chamber to the material in the U-shaped pipe is (0.1-0.8):1, for example, it can be 0.1:1, 0.2:1, 0.4:1, 0.6:1 or 0.8:1, but is not limited to the listed values, and other unlisted values ​​within the above numerical range are also applicable.

[0085] The present invention limits the volume ratio of the first part of the material entering the clarification chamber to the material in the U-shaped pipe to (0.1-0.8):1, so as to control the residence time of the material in the clarification chamber to promote the heavy phase sedimentation and improve the extraction and separation effect. If the volume ratio of the first part of the material entering the clarification chamber to the material in the U-shaped pipe is less than 0.1:1, the space in the clarification chamber cannot be fully utilized, which will reduce the processing capacity of the equipment; if the volume ratio of the first part of the material entering the clarification chamber to the material in the U-shaped pipe is greater than 0.8:1, the residence time of the mixed liquid in the U-shaped pipe is too short, and the target extraction substance in the raw material liquid is difficult to achieve effective extraction. In addition, it will also cause the liquid entering the clarification chamber to be unable to be fully stratified, which will reduce the extraction efficiency.

[0086] Compared with the prior art, the present invention has at least the following beneficial effects:

[0087] (1) The U-shaped tube extraction equipment provided by the present invention combines a U-shaped pipe and a separation device so that the entire equipment forms a circulating tube structure. The flow velocity and turbulence intensity of the fluid in the pipe are very high, which is conducive to improving the extraction rate; the circulating tube structure can make the mixed liquid circulate and be extracted in the pipe. By controlling the inlet and outlet flow rates of the mixed liquid, the residence time of the mixed liquid can be controlled, the single-stage extraction efficiency can be improved, and the maximum utilization of resource recovery can be achieved;

[0088] (2) At the same time, unlike the traditional tubular extraction device which needs to be connected to an external liquid separation device, the U-shaped tubular extraction device provided by the present invention sets the separation device above the U-shaped pipe, which greatly reduces the footprint of the equipment. The U-shaped tubular extraction device provided by the present invention has better controllability and is easier to industrially scale up on the basis of ensuring stable operation of the equipment.

[0089] (3) Furthermore, the U-shaped tube extraction equipment provided by the present invention can process materials with high solid content and has the advantages of simple use and easy operation. BRIEF DESCRIPTION OF THE DRAWINGS

[0090] Figure 1 It is a schematic diagram of the structure of the U-shaped tube extraction equipment provided in Example 1 of the present invention.

[0091] Figure 2 This is a front view of the overall structure of the static mixer provided in Example 1 of the present invention.

[0092] Figure 3 The present invention Figure 2 A cross-sectional view of the static mixer taken along AA.

[0093] Figure 4 It is a schematic diagram of the structure of the rotating parts of the axial flow pump provided in Example 1 of the present invention.

[0094] Figure 5 It is a schematic diagram of the structure of the axial flow pump blade provided in Example 1 of the present invention.

[0095] Figure 6 It is a schematic diagram of the structure of the U-shaped tube extraction equipment provided in Example 4 of the present invention.

[0096] Figure 7 It is a schematic diagram of the structure of the U-shaped tube extraction equipment provided in Example 5 of the present invention.

[0097] Figure 8 It is a schematic diagram of the structure of the U-shaped tube extraction equipment provided in Example 6 of the present invention.

[0098] Fig. 9 It is a schematic diagram of the structure of the U-shaped tube extraction equipment provided in Example 7 of the present invention.

[0099] Fig.10 It is a structural schematic diagram of the U-shaped tube extraction equipment provided in Comparative Example 1 of the present invention.

[0100] Fig.11 It is a schematic diagram of the structure of the packed tower extraction equipment provided in Comparative Example 2 of the present invention.

[0101] Fig.12This is a water phase content diagram obtained by performing CFD simulation on the extraction process provided in Application Example 1 of the present invention.

[0102] Fig.13 This is a water phase content diagram obtained by performing CFD simulation on the extraction process provided in Application Example 5 of the present invention.

[0103] Fig.14 The CFD simulation of the extraction process provided in Application Example 4 of the present invention is performed to obtain the Hf in the aqueous phase. 4+ Ion content graph.

[0104] Fig.15 The CFD simulation of the extraction process provided in Application Example 4 of the present invention is performed to obtain the Hf 4+ Ion content graph.

[0105] Fig.16 It is a schematic diagram showing the variation of the single-stage extraction efficiency with the processing amount of the extraction solvent / raw material liquid in the present invention.

[0106] Among them, 1-U-shaped pipeline; 101-first vertical section; 102-lateral section; 103-second vertical section; 2-axial flow pump; 3-separation device; 4-light phase storage device; 5-heavy phase storage device; 6-clarification chamber; 7-mixing chamber; 8-vertical partition; 9-overflow phase separation weir; 10-light phase discharge port; 11-heavy phase discharge port; 12-lateral baffle; 13-static mixer; 14-flow sensor; 1401-first flow sensor; 1402-second flow sensor; 1403-third flow sensor; 15-solenoid valve; 1501-first solenoid valve; 1502-second solenoid valve; 1503-third solenoid valve; 16-temperature degree sensor; 17-liquid level sensor; 1701-first liquid level sensor; 1702-second liquid level sensor; 1703-third liquid level sensor; 18-pressure sensor; 1801-first pressure sensor; 1802-second pressure sensor; 19-extraction raw material inlet, 20-material outlet; 21-material inlet; 22-outer pipe; 23-heat exchange sleeve; 24-blades; 25-impeller; 26-central axis; 27-first pipeline; 28-second pipeline; 29-third pipeline; 30-channel; 31-vertical baffle; 32-light phase inlet; 33-heavy phase inlet; 34-light phase outlet; 35-heavy phase outlet; 36-Raschig ring. DETAILED DESCRIPTION

[0107] The technical solution of the present invention is further described below in conjunction with the accompanying drawings and through specific implementation methods. However, the following examples are only simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention shall be subject to the claims.

[0108] Example 1

[0109] This embodiment provides a U-shaped tube extraction device, such as Figure 1 As shown, the U-shaped tube extraction equipment includes a U-shaped pipeline 1, a stirring device, a static mixer 13, a separation device 3, a light phase storage device 4 and a heavy phase storage device 5.

[0110] Among them, the material of the U-shaped pipe 1 is stainless steel, its diameter is 40mm and the total length is 1200mm, that is, the ratio of the length to the diameter of the U-shaped pipe 1 is 30:1, and the U-shaped pipe 1 includes a first vertical section 101, a transverse section 102 and a second vertical section 103 connected in sequence, and the first vertical section 101, the transverse section 102 and the second vertical section 103 are connected by an arc corner, and an extraction raw material inlet 19 is provided on the first vertical section 101, and the ratio of the distance between the extraction raw material inlet 19 and the bottom of the first vertical section 101 to the length of the first vertical section 101 is 2 / 3:1, and a heat exchange sleeve 23 is provided outside the U-shaped pipe 1.

[0111] The stirring device is an axial flow pump 2, which is located in the transverse section 102 of the U-shaped pipeline 1. The structural diagram of the rotating part of the axial flow pump 2 is as shown in FIG. Figure 4 As shown, the axial flow pump 2 includes an impeller 25 and a central shaft 26 whose geometric centers overlap and are connected to each other. Four downward pressure blades 24 with a downward pressure angle of 50° are arranged in the circumferential direction of the impeller. The structural schematic diagram of the blade 24 is shown in FIG. Figure 5 As shown, the ratio of the length of the impeller 25 in the U-shaped pipe 1 to the diameter of the U-shaped pipe 1 is 1:1, and the ratio of the outermost dimension of the blade 24 to the diameter of the U-shaped pipe 1 is 0.7:1.

[0112] The U-shaped tube extraction device connects a static mixer 13 with a spoiler inside to the second vertical section 103 of the U-shaped pipe 1 through a flange, wherein the specific structure of the static mixer 13 is as follows: Figure 2 and Figure 3 As shown, the static mixer includes a cylindrical pipe made of stainless steel and a spoiler in the shape of a spiral fin.

[0113] The separation device 3 is located above the U-shaped pipe 1 , and the lower portion of the separation device 3 is communicated with the top of the first vertical section 101 and the top of the second vertical section 103 , respectively.

[0114] The separation device 3 is an internal cavity container, and its structure is a horizontal rectangular structure with a length, width and height of 400 mm, 50 mm and 400 mm respectively. Its internal cavity includes a clarification chamber 6 and a mixing chamber 7 from top to bottom. The two chambers are separated by a transverse baffle 12, so that the spatial volume ratio of the clarification chamber 6 and the mixing chamber 7 is 3:1, and the material outlet 20 of the mixing chamber and the material inlet 21 of the clarification chamber are connected by an outer tube 22. The material inlet 21 and the material outlet 20 are respectively arranged on the sides of the clarification chamber 6 and the mixing chamber 7, and the material outlet 20 is arranged on the side of the mixing chamber 7 close to the second vertical section 103.

[0115] Six vertical partitions 8 and an overflow phase-separating weir 9 close to the first vertical section 101 are arranged inside the clarification chamber 6, and two adjacent vertical partitions 8 are staggered; the clarification chamber includes a light phase discharge port 10 and a heavy phase discharge port 11, wherein the light phase discharge port 10 and the heavy phase discharge port 11 are arranged on the side away from the clarification chamber material inlet 21 and close to the first vertical section 101, and the heavy phase discharge port 11 is arranged at the lower part of the light phase discharge port 10.

[0116] The light phase storage device 4 is connected to the extraction raw material inlet 19 via a first pipeline 27 and a third pipeline 29 connected in sequence, and the heavy phase storage device 5 is connected to the extraction raw material inlet 19 via a second pipeline 28 and a third pipeline 29 connected in sequence.

[0117] The U-tube extraction equipment also includes a flow sensor 14, a solenoid valve 15, a temperature sensor 16, a liquid level sensor 17 and a pressure sensor 18, wherein a first solenoid valve 1501 and a first flow sensor 1401 are sequentially arranged on the first pipeline along the material flow direction, a second solenoid valve 1502 and a second flow sensor 1402 are sequentially arranged on the second pipeline, a third solenoid valve 1503 and a third flow sensor 1403 are sequentially arranged on the outer tube, the temperature sensor 16 is arranged between the axial flow pump 2 and the static mixer 13, a first liquid level sensor 1701, a second liquid level sensor 1702 and a third liquid level sensor 1703 are respectively arranged in the light phase storage device 4, the heavy phase storage device 5 and the clarification chamber 6, and a first pressure sensor 1801 and a second pressure sensor 1802 are respectively arranged above and below the extraction raw material inlet 19.

[0118] Example 2

[0119] This embodiment provides a U-shaped tube extraction device, which includes a U-shaped pipeline 1, a stirring device, a static mixer 13, a separation device 3, a light phase storage device 4 and a heavy phase storage device 5.

[0120] Among them, the material of the U-shaped pipe 1 is titanium alloy, its diameter is 500mm and the total length is 5000mm, that is, the ratio of the length to the diameter of the U-shaped pipe 1 is 10:1, and the U-shaped pipe 1 includes a first vertical section 101, a transverse section 102 and a second vertical section 103 connected in sequence, and the first vertical section 101, the transverse section 102 and the second vertical section 103 are connected by an arc corner, and an extraction raw material inlet 19 is arranged on the first vertical section 101, and the ratio of the distance between the extraction raw material inlet 19 and the bottom of the first vertical section 101 to the length of the first vertical section 101 is 1 / 9:1, and a heat exchange sleeve 23 is arranged outside the U-shaped pipe 1.

[0121] The stirring device is an axial flow pump 2, which is located in the transverse section 102 of the U-shaped pipe 1. The axial flow pump 2 includes an impeller 25 and a central axis 26 whose geometric centers overlap and are interconnected. Four downward pressure blades 24 with a downward pressure angle of 15° are arranged in the circumferential direction of the impeller. The ratio of the length of the impeller 25 in the U-shaped pipe 1 to the diameter of the U-shaped pipe 1 is 0.5:1, and the ratio of the outermost dimension of the blade 24 to the diameter of the U-shaped pipe 1 is 0.95:1.

[0122] The U-shaped tube extraction device connects a static mixer 13 with a spoiler inside to the second vertical section 103 of the U-shaped pipe 1 through a flange.

[0123] The separation device 3 is located above the U-shaped pipe 1 , and the lower portion of the separation device 3 is communicated with the top of the first vertical section 101 and the top of the second vertical section 103 , respectively.

[0124] The separation device 3 is an internal cavity container, and its structure is a horizontal rectangular structure with a length, width and height of 2000mm, 300mm and 2000mm respectively. Its internal cavity includes a clarification chamber 6 and a mixing chamber 7 from top to bottom. The two chambers are separated by a transverse baffle 12, so that the spatial volume ratio of the clarification chamber 6 and the mixing chamber 7 is 1:1, and the material outlet 20 of the mixing chamber and the material inlet 21 of the clarification chamber are connected by an outer tube 22. The material inlet 21 and the material outlet 20 are respectively arranged on the sides of the clarification chamber 6 and the mixing chamber 7, and the material outlet 20 is arranged on the side of the mixing chamber 7 close to the second vertical section 103.

[0125] The clarification chamber 6 is provided with 10 vertical partitions 8 and an overflow phase separation weir 9 close to the first vertical section, and two adjacent vertical partitions 8 are staggered; the clarification chamber includes a light phase discharge port 10 and a heavy phase discharge port 11, wherein the light phase discharge port 10 and the heavy phase discharge port 11 are arranged on the side away from the clarification chamber material inlet 21 and close to the first vertical section 101, and the heavy phase discharge port 11 is arranged at the lower part of the light phase discharge port 10.

[0126] The light phase storage device 4 is connected to the extraction raw material inlet 19 via a first pipeline 27 and a third pipeline 29 connected in sequence, and the heavy phase storage device 5 is connected to the extraction raw material inlet 19 via a second pipeline 28 and a third pipeline 29 connected in sequence.

[0127] The U-tube extraction equipment also includes a flow sensor 14, a solenoid valve 15, a temperature sensor 16, a liquid level sensor 17 and a pressure sensor 18, wherein a first solenoid valve 1501 and a first flow sensor 1401 are sequentially arranged on the first pipeline along the material flow direction, a second solenoid valve 1502 and a second flow sensor 1402 are sequentially arranged on the second pipeline, a third solenoid valve 1503 and a third flow sensor 1403 are sequentially arranged on the outer tube, the temperature sensor 16 is arranged between the axial flow pump 2 and the static mixer 13, a first liquid level sensor 1701, a second liquid level sensor 1702 and a third liquid level sensor 1703 are respectively arranged in the light phase storage device 4, the heavy phase storage device 5 and the clarification chamber 6, and a first pressure sensor 1801 and a second pressure sensor 1802 are respectively arranged above and below the extraction raw material inlet 19.

[0128] Example 3

[0129] This embodiment provides a U-shaped tube extraction device, which includes a U-shaped pipeline 1, a stirring device, a static mixer 13, a separation device 3, a light phase storage device 4 and a heavy phase storage device 5.

[0130] Among them, the material of the U-shaped pipe 1 is polytetrafluoroethylene (PTFE-BP), its diameter is 30mm and the total length is 3000mm, that is, the ratio of the length to the diameter of the U-shaped pipe 1 is 100:1, and the U-shaped pipe 1 includes a first vertical section 101, a transverse section 102 and a second vertical section 103 connected in sequence, and the first vertical section 101, the transverse section 102 and the second vertical section 103 are connected through an arc corner, and an extraction raw material inlet 19 is provided on the first vertical section 101, and the ratio of the distance between the extraction raw material inlet 19 and the bottom of the first vertical section 101 to the length of the first vertical section 101 is 2 / 9:1, and a heat exchange sleeve 23 is provided outside the U-shaped pipe 1.

[0131] The stirring device is an axial flow pump 2, which is located in the transverse section 102 of the U-shaped pipe 1. The axial flow pump 2 includes an impeller 25 and a central axis 26 whose geometric centers overlap and are interconnected. Four downward pressure blades 24 with a downward pressure angle of 75° are arranged in the circumferential direction of the impeller. The ratio of the length of the impeller 25 in the U-shaped pipe 1 to the diameter of the U-shaped pipe 1 is 2:1, and the ratio of the outermost dimension of the blade 24 to the diameter of the U-shaped pipe 1 is 0.5:1.

[0132] The U-shaped tube extraction device connects a static mixer 13 with a spoiler inside to the second vertical section 103 of the U-shaped pipe 1 through a flange.

[0133] The separation device 3 is located above the U-shaped pipe 1 , and the lower portion of the separation device 3 is communicated with the top of the first vertical section 101 and the top of the second vertical section 103 , respectively.

[0134] The separation device 3 is an internal cavity container, and its structure is a horizontal cylindrical structure with a diameter of 300 mm and a length of 1000 mm. Its internal cavity includes a clarification chamber 6 and a mixing chamber 7 from top to bottom. The two chambers are separated by a transverse baffle 12, so that the spatial volume ratio of the clarification chamber 6 and the mixing chamber 7 is 20:1, and the material outlet 20 of the mixing chamber and the material inlet 21 of the clarification chamber are connected by an outer tube 22. The material inlet 21 and the material outlet 20 are respectively arranged on the sides of the clarification chamber 6 and the mixing chamber 7, and the material outlet 20 is arranged on the side of the mixing chamber 7 close to the second vertical section 103.

[0135] A vertical partition 8 and an overflow phase-separating weir 9 close to the first vertical section are arranged inside the clarification chamber 6, and two adjacent vertical partitions 8 are staggered; the clarification chamber includes a light phase discharge port 10 and a heavy phase discharge port 11, wherein the light phase discharge port 10 and the heavy phase discharge port 11 are arranged on the side away from the clarification chamber material inlet 21 and close to the first vertical section 101, and the heavy phase discharge port 11 is arranged at the lower part of the light phase discharge port 10.

[0136] The light phase storage device 4 is connected to the extraction raw material inlet 19 via a first pipeline 27 and a third pipeline 29 connected in sequence, and the heavy phase storage device 5 is connected to the extraction raw material inlet 19 via a second pipeline 28 and a third pipeline 29 connected in sequence.

[0137] The U-tube extraction equipment also includes a flow sensor 14, a solenoid valve 15, a temperature sensor 16, a liquid level sensor 17 and a pressure sensor 18, wherein a first solenoid valve 1501 and a first flow sensor 1401 are sequentially arranged on the first pipeline along the material flow direction, a second solenoid valve 1502 and a second flow sensor 1402 are sequentially arranged on the second pipeline, a third solenoid valve 1503 and a third flow sensor 1403 are sequentially arranged on the outer tube, the temperature sensor 16 is arranged between the axial flow pump 2 and the static mixer 13, a first liquid level sensor 1701, a second liquid level sensor 1702 and a third liquid level sensor 1703 are respectively arranged in the light phase storage device 4, the heavy phase storage device 5 and the clarification chamber 6, and a first pressure sensor 1801 and a second pressure sensor 1802 are respectively arranged above and below the extraction raw material inlet 19.

[0138] Example 4

[0139] This embodiment provides a U-shaped tubular extraction device, which is the same as Embodiment 1 except that no static mixer 13 is provided on the second vertical section 103 .

[0140] The U-shaped tube extraction device described in this embodiment is as follows Figure 6 shown.

[0141] Example 5

[0142] The present embodiment provides a U-shaped tubular extraction device, which differs from the embodiment 1 only in that, except that the material inlet 21 and the material outlet 20 are respectively arranged on the sides of the clarification chamber 6 and the mixing chamber 7, and the material outlet 20 is arranged on the side of the mixing chamber 7 close to the second vertical section 101, the light phase discharge outlet 10 and the heavy phase discharge outlet 11 are arranged on the side close to the second vertical section 103, and the material is kept in the clarification chamber to flow through the vertical partition 8 and the overflow phase separation weir 9 in sequence, and the third liquid level sensor 1703 is arranged between the vertical partition 8 and the overflow phase separation weir 9, the rest is the same as the embodiment 1.

[0143] The U-shaped tube extraction device described in this embodiment is as follows Figure 7 shown.

[0144] Example 6

[0145] This embodiment provides a U-shaped tube extraction device, which is different from the first embodiment only in that, in addition to connecting the material outlet 20 of the mixing chamber and the material inlet 21 of the clarification chamber through the outer tube 22, a channel 30 is opened on the transverse baffle between the mixing chamber 7 and the clarification chamber 6 of the separation device, and the channel is close to the second vertical section 103, so that the mixed liquid enters the clarification chamber 6 through the channel 30, and the rest is the same as the first embodiment.

[0146] This embodiment cannot control the ratio of the mixed liquid entering the clarification chamber to the mixed liquid in the mixing chamber. Figure 8 shown.

[0147] Example 7

[0148] This embodiment provides a U-shaped tubular extraction device, which is different from Example 1 only in that the mixing chamber 7 and the clarifying chamber 6 of the separation device are adjusted from being arranged in parallel vertically to being arranged in parallel horizontally, and the mixing chamber 7 and the clarifying chamber 6 are arranged in sequence along the material flow direction, and the mixing chamber 7 and the clarifying chamber 6 are separated by a vertical baffle 31 accordingly, and the rest are the same as Example 1.

[0149] The U-shaped tube extraction device described in this embodiment is as follows Fig. 9 shown.

[0150] Example 8

[0151] This embodiment provides a U-shaped tube extraction device, which is different from Example 1 only in that, except that the ratio of the outermost dimension of the blade 24 of the axial flow pump 2 to the diameter of the U-shaped pipe 1 is adjusted to 0.2:1, the rest is the same as Example 1.

[0152] Example 9

[0153] This embodiment provides a U-shaped tube extraction device, which is different from Example 1 only in that, except that the ratio of the outermost dimension of the blade 24 of the axial flow pump 2 to the diameter of the U-shaped pipe 1 is adjusted to 0.98:1, the rest is the same as Example 1.

[0154] Example 10

[0155] This embodiment provides a U-shaped tube extraction device, which is different from Example 1 only in that, except that the ratio of the length of the impeller 25 of the axial flow pump 2 in the U-shaped pipe 1 to the diameter of the U-shaped pipe 1 is adjusted to 0.3:1, the rest is the same as Example 1.

[0156] Embodiment 11

[0157] This embodiment provides a U-shaped tube extraction device, which is different from Example 1 only in that, except that the ratio of the length of the impeller 25 of the axial flow pump 2 in the U-shaped pipe 1 to the diameter of the U-shaped pipe 1 is adjusted to 3:1, the rest is the same as Example 1.

[0158] Comparative Example 1

[0159] This comparative example provides a U-shaped tube extraction device, which is the same as Example 1 except that the axial flow pump 2 is located in the first vertical section 101 of the U-shaped pipe 1 and the axial flow pump 2 is placed vertically.

[0160] The U-shaped tube extraction equipment described in this comparative example is as follows Fig.10 shown.

[0161] Comparative Example 2

[0162] This comparative example provides a packed tower extraction device, the diameter of the packed tower extraction device is 30mm, the effective height of the extraction section is 1500mm, and the effective extraction volume is ensured to be the same as that of the U-shaped tube extraction device. The packing adopts Raschig ring 36, the diameter of the Raschig ring is 10mm, the thickness is 2.5mm, and the height is 2.5mm. The light phase liquid enters from the light phase inlet 32 ​​below the extraction tower, and the heavy phase liquid enters from the heavy phase inlet 33 above the extraction tower. The two phases of liquid countercurrently complete the extraction process, and the light phase liquid after the extraction is completed is discharged from the light phase outlet 34, and the heavy phase liquid after the extraction is completed is discharged from the heavy phase outlet 35.

[0163] The packed tower extraction equipment described in this comparative example is as follows Fig.11 shown.

[0164] Application Example 1

[0165] This application example provides a method for using the U-shaped tube extraction device described in Example 1, and the method includes:

[0166] (1) Set the flow rate to 0.22m 3 / h extraction solvent and flow rate is 0.22m 3 / h raw material liquid is pre-mixed and then input into the extraction raw material inlet on the U-shaped pipe;

[0167] (2) turning on the axial flow pump so that the speed of the axial flow pump impeller is 600 rpm to mix and transport the raw material liquid and the extraction solvent;

[0168] (3) After being mixed by the axial flow pump, the raw material liquid and the extraction solvent flow through a static mixer for a second mixing;

[0169] (4) After the second mixing in the static mixer, 30% of the material in the U-shaped pipe enters the clarification chamber of the separation device for separation. The light phase liquid and heavy phase liquid separated in the clarification chamber are discharged through the light phase discharge port and the heavy phase discharge port respectively. 70% of the material continues to enter the U-shaped pipe through the mixing chamber of the separation device for circulation mixing.

[0170] The U-shaped tube extraction equipment described in Example 1 was used to extract Hf 4+ The extraction process of the solution was simulated by CFD, and the water phase content diagram was obtained as shown in Fig.12 As shown, from Fig.12 It can be seen that when the water content is 100%, it is red, and when the organic content is 100%, it is blue. Fig.12 The color distribution is relatively uniform, indicating that the liquid-liquid contact is good during the extraction process.

[0171] Application Example 2

[0172] This application example provides a method for using the U-shaped tube extraction device described in Example 2, and the method includes:

[0173] (1) Set the flow rate to 10m 3 / h extraction solvent and flow rate 10m 3 / h raw material liquid is pre-mixed and then input into the extraction raw material inlet on the U-shaped pipe;

[0174] (2) turning on the axial flow pump so that the speed of the axial flow pump impeller is 1500 rpm to mix and transport the raw material liquid and the extraction solvent;

[0175] (3) After being mixed by the axial flow pump, the raw material liquid and the extraction solvent flow through a static mixer for a second mixing;

[0176] (4) After the second mixing in the static mixer, 10% of the material in the U-shaped pipe enters the clarification chamber of the separation device for separation. The light phase liquid and heavy phase liquid separated in the clarification chamber are discharged through the light phase discharge port and the heavy phase discharge port respectively. 90% of the material continues to enter the U-shaped pipe through the mixing chamber of the separation device for circulation mixing.

[0177] Application Example 3

[0178] This application example provides a method for using the U-shaped tube extraction device described in Example 3, and the method includes:

[0179] (1) Set the flow rate to 0.1m 3 / h extraction solvent and flow rate is 0.1m 3 / h raw material liquid is pre-mixed and then input into the extraction raw material inlet on the U-shaped pipe;

[0180] (2) turning on the axial flow pump so that the speed of the axial flow pump impeller is 100 rpm to mix and transport the raw material liquid and the extraction solvent;

[0181] (3) After being mixed by the axial flow pump, the raw material liquid and the extraction solvent flow through a static mixer for a second mixing;

[0182] (4) After the second mixing in the static mixer, 80% of the material in the U-shaped pipe enters the clarification chamber of the separation device for separation. The light phase liquid and heavy phase liquid separated in the clarification chamber are discharged through the light phase discharge port and the heavy phase discharge port respectively. 20% of the material continues to enter the U-shaped pipe through the mixing chamber of the separation device for circulation mixing.

[0183] Application Example 4

[0184] This application example provides a method for using the U-tube extraction device described in Example 4. The method is the same as Application Example 1 except that the U-tube extraction device provided in Example 4 is used and the second mixing of the static mixer is not performed after the axial flow pump mixing and transportation.

[0185] The U-shaped tube extraction apparatus described in Example 4 was used to extract Hf 4+ The extraction process of the solution was simulated by CFD, and the Hf 4+ Ion content diagram and Hf in organic phase 4+ The ion content diagrams are as follows Fig.14 and Fig.15 As shown, from Fig.14 It can be seen that Hf 4+When the ion content is 2.49g / kg, it is red. 4+ As the ion content decreases, the color gradually changes to blue, and the feed port is red, which means that the Hf 4+ The ion content is the highest. Along the material flow direction, the blue color gradually deepens, that is, along the material flow, the extraction efficiency gradually increases. Similarly, from Fig.15 It can be seen that Hf 4+ When the ion content is 0g / kg, it is blue. 4+ As the ion content increases, the color gradually changes to yellow, and the feed port is blue, which means that the Hf 4+ The ion content is 0g / kg, and the yellow color gradually deepens along the material flow direction, that is, the extraction efficiency gradually increases along the material flow rate.

[0186] At the same time, in order to better verify the effect of the processing volume on the extraction effect, based on Application Example 4, the processing volume was adjusted to 0.0022m 3 / h, 0.022m 3 / h、0.11m 3 / h and 0.44m 3 / h, and tested its single-stage extraction efficiency. The results are as follows Fig.16 As shown, from Fig.16 It can be seen that with the increase of processing volume, the single-stage extraction efficiency gradually decreases.

[0187] Application Example 5

[0188] This application example provides a method for using the U-shaped tube extraction device described in Example 5. In addition to using the U-shaped tube extraction device provided in Example 5, the method is the same as Application Example 1 except that step (4) is adjusted as follows: after the second mixing in the static mixer, the material flows through the mixing chamber of the separation device, 30% of the material enters the clarification chamber of the separation device for separation, and the light phase liquid and heavy phase liquid separated in the clarification chamber are discharged through the light phase discharge port and the heavy phase discharge port respectively, and 70% of the material continues to enter the U-shaped pipe for circulation mixing.

[0189] The U-shaped tube extraction apparatus described in Example 5 was used to extract Hf 4+ The extraction process of the solution was simulated by CFD, and the water phase content diagram was obtained as shown in Fig.13 As shown, from Fig.13 It can be seen that when the water content is 100%, it is red, and when the organic content is 100%, it is blue. Fig.13 The blue distribution in the dotted box is more concentrated, indicating that the organic phase is aggregated there and the contact between the liquid and liquid phases is poor, which will eventually lead to a decrease in the extraction efficiency.

[0190] Application Example 6

[0191] This application example provides a method for using the U-shaped tube extraction device described in Example 6. In addition to using the U-shaped tube extraction device provided in Example 6, the method is the same as Application Example 1 except that step (4) is adjusted as follows: after the second mixing in the static mixer, part of the material in the U-shaped tube enters the clarification chamber of the separation device for separation, and the light phase liquid and heavy phase liquid separated in the clarification chamber are discharged through the light phase discharge port and the heavy phase discharge port respectively, and the remaining material continues to enter the U-shaped tube through the mixing chamber of the separation device for circulation mixing.

[0192] Application Example 7

[0193] This application example provides a method for using the U-shaped tube extraction device described in Example 7. The method is the same as Application Example 1 except that the U-shaped tube extraction device provided in Example 7 is used and step (4) is adjusted as follows: after the second mixing in the static mixer, the materials in the U-shaped tube sequentially enter the mixing chamber and the clarifying chamber of the separation device and are separated in the clarifying chamber. The light phase liquid and the heavy phase liquid separated in the clarifying chamber are discharged through the light phase discharge port and the heavy phase discharge port, respectively.

[0194] Application Example 8

[0195] This application example provides a method for using the U-shaped tube extraction device described in Example 8, and the method for using is the same as that in Application Example 1.

[0196] Application Example 9

[0197] This application example provides a method for using the U-shaped tube extraction device described in Example 9, and the method of use is the same as that of Application Example 1.

[0198] Application Example 10

[0199] This application example provides a method for using the U-shaped tube extraction device described in Example 10, and the method for using is the same as that of Application Example 1.

[0200] Application Example 11

[0201] This application example provides a method for using the U-shaped tube extraction device described in Example 11, and the method for using is the same as that in Application Example 1.

[0202] Comparative application example 1

[0203] This comparative application example provides a method for using the U-shaped tube extraction device described in Comparative Example 1, and the method for using is the same as that in Application Example 1.

[0204] Comparative Application Example 2

[0205] This comparative application example provides a method for using the packed tower extraction device described in Comparative Example 2, and the method comprises:

[0206] (1) Set the flow rate to 0.0022m 3 / h extraction solvent and flow rate is 0.0022m 3 / h raw material liquid is added into the packed tower extraction equipment through the light phase inlet and the heavy phase inlet respectively;

[0207] (2) Under the action of density difference, the raw material liquid flows downward and contacts the upward-flowing extraction solvent in countercurrent. The extraction solvent is dispersed into small droplets under the action of the filler, and the two-phase contact realizes extraction;

[0208] (3) After the extraction is completed, the light phase liquid is layered at the top of the packed tower extraction equipment and discharged from the light phase outlet; the heavy phase liquid is layered at the bottom of the packed tower extraction equipment and discharged from the heavy phase outlet.

[0209] The methods described in the above application examples 1-11 and comparative application examples 1-2 are used to extract Hf 4+ The extraction process of the solution was simulated by CFD. The extraction system was MIBK-HSCN system. 4+ The ion concentration is 2.49 g / kg. During the simulation, the concentration of ions in the heavy phase liquid and the light phase liquid at the outlet is detected. After the ion concentration is stable, according to the formula Calculate the extraction efficiency, where C 萃原水相 is the concentration of hafnium in the raw material liquid before extraction, in g / kg, C 萃余水相 is the concentration of hafnium in the liquid discharged from the heavy phase outlet after extraction, in g / kg. The test results are shown in Table 1.

[0210] Table 1

[0211]

[0212] The test results show that:

[0213] (1) It can be seen from Application Examples 1 to 3 that the present invention combines a U-shaped pipe and a separation device to form a circulating tubular structure for the entire device, and controls the residence time of the mixed liquid by controlling the inlet and outlet flow rates of the mixed liquid, thereby improving the single-stage extraction efficiency and processing capacity, so that the single-stage extraction efficiency reaches more than 57.6%. At the same time, the separation device is arranged above the U-shaped pipe, which greatly reduces the footprint of the equipment, facilitates industrial scale-up, and is suitable for industrial extraction processes of large-flow, high-solid content liquid-liquid two-phase systems.

[0214] (2) It can be seen from Application Example 1 and Application Example 4 that the U-shaped tube extraction device used in Application Example 1 is provided with a static mixer 13 on the second vertical section 103, and its single-stage extraction efficiency is 60.5%; while the U-shaped tube extraction device used in Application Example 4 is not provided with a static mixer 13 on the second vertical section 103, and its single-stage extraction efficiency is only 52.8%. This shows that the mixer provided in the second vertical section of the present invention can further mix the mixed liquid in the U-shaped pipe, so that the mixed liquid can still be fully mixed during the upward flow process, thereby preventing liquid stratification and improving the extraction efficiency.

[0215] (3) Through application examples 1 and 5, combined with Fig.12 and Fig.13 It can be seen that the light phase discharge port and the heavy phase discharge port in the U-shaped tube extraction equipment used in Application Example 1 are arranged on the side away from the material inlet 21 of the clarification chamber and close to the first vertical section 101, and its single-stage extraction efficiency is 60.5%; while the light phase discharge port 10 and the heavy phase discharge port 11 in the U-shaped tube extraction equipment used in Application Example 5 are arranged on the side close to the second vertical section 103, and its single-stage extraction efficiency is 48.4%. This shows that the present invention can effectively alleviate the stratification of the liquid-liquid two phases in the clarification chamber and improve the extraction efficiency by arranging the light phase discharge port and the heavy phase outlet of the clarification chamber on the side close to the first vertical tube.

[0216] (4) It can be seen from Application Example 1 and Application Example 6 that in the U-shaped tube extraction device used in Application Example 1, the material outlet 20 of the mixing chamber and the material inlet 21 of the clarifying chamber are connected by the outer tube 22, and its single-stage extraction efficiency is 60.5%; while in the U-shaped tube extraction device used in Application Example 6, a channel 30 is opened on the transverse baffle between the mixing chamber 7 and the clarifying chamber 6 of the separation device, and the channel is close to the second vertical section 103, so that the mixed liquid enters the clarifying chamber 6 through the channel 30, and its single-stage extraction efficiency is 46.0%. This shows that the present invention connects the mixing chamber and the clarifying chamber through an outer tube, which can better control the residence time of the material in the U-shaped pipe and improve the extraction efficiency.

[0217] (5) It can be seen from Application Examples 1 and 7 that the clarification chamber 6 in the separation device of the U-shaped tube extraction device used in Application Example 1 is arranged above the mixing chamber 7, the two chambers are separated by a transverse baffle 12, and the material outlet 20 of the mixing chamber and the material inlet 21 of the clarification chamber are connected by an outer tube 22, and the single-stage extraction efficiency is 60.5%; while the mixing chamber 7 and the clarification chamber 6 of the separation device of the U-shaped tube extraction device used in Example 7 are arranged side by side along the material flow direction, and the mixing chamber 7 and the clarification chamber 6 are connected by a vertical baffle 12. The single-stage extraction efficiency is 45.7%, which shows that the present invention can reduce the floor space by arranging the clarification chamber above the mixing chamber, that is, arranging them in parallel from top to bottom, compared with the left-right parallel arrangement of the mixing chamber and the clarification chamber. At the same time, since the clarification chamber is located at the upper part of the separation device, the clarification area can be made into a thin layer phase separation, which can greatly reduce the volume of the clarification chamber. The present invention adopts the principle of gravity separation, so that the light phase and the heavy phase liquid of the extraction can be naturally separated in the clarification chamber, which is convenient for the subsequent two-phase separation to improve the single-stage extraction efficiency.

[0218] (6) It can be seen from Application Example 1 and Application Examples 8-9 that the ratio of the outermost dimension of the blade 24 in the U-shaped tube extraction device used in Application Example 1 to the diameter of the U-shaped pipe 1 is 0.7:1, and its single-stage extraction efficiency is 60.5%; while the ratio of the outermost dimension of the blade 24 in the U-shaped tube extraction device used in Application Example 8 to the diameter of the U-shaped pipe 1 is 0.2:1, and its single-stage extraction efficiency is 54.5%; the ratio of the outermost dimension of the blade 24 in the U-shaped tube extraction device used in Application Example 9 to the diameter of the U-shaped pipe 1 is 0.98:1, and its single-stage extraction efficiency is 55.2%. This shows that the present invention can further promote the shearing of the mixed liquid by the stirring device by limiting the ratio of the outermost dimension of the blade of the stirring device to the diameter of the U-shaped pipe, so as to promote the breakup of droplets, reduce the size of droplets, increase the contact area between the liquid and liquid phases, and thus improve the extraction efficiency.

[0219] (7) It can be seen from Application Example 1 and Application Examples 10-11 that the ratio of the length of the impeller 25 of the axial flow pump 2 in the U-shaped pipe 1 to the diameter of the U-shaped pipe 1 in Application Example 1 is 1:1, and its single-stage extraction efficiency is 60.5%; while the ratio of the length of the impeller 25 of the axial flow pump 2 in the U-shaped pipe 1 to the diameter of the U-shaped pipe 1 in Application Example 10 is 0.3:1, and its single-stage extraction efficiency is 55.9%; the ratio of the length of the impeller 25 of the axial flow pump 2 in the U-shaped pipe 1 to the diameter of the U-shaped pipe 1 in Application Example 10 is 3:1, and its single-stage extraction efficiency is 54.4%. This shows that the present invention can further increase the contact area between the liquid-liquid two phases and improve the extraction efficiency by limiting the ratio of the length of the impeller of the stirring device in the U-shaped pipe to the diameter of the U-shaped pipe, while providing power for the circulation of the mixed liquid.

[0220] (8) It can be seen from Application Example 1 and Comparative Application Example 1 that the present invention can shear the mixed material by arranging the axial flow pump in the lower lateral section of the U-shaped pipe to promote the breakup of droplets, reduce the size of droplets, increase the contact area between the liquid and liquid phases, and thus improve the extraction efficiency.

[0221] (9) It can be seen from Application Example 1 and Comparative Application Example 2 that the present invention combines a U-shaped pipe and a separation device to form a circulating tubular structure for the entire device, thereby improving the single-stage extraction efficiency and processing capacity. Under the same equipment extraction volume conditions, the U-shaped tubular extraction device of the present invention has a higher extraction efficiency. At the same time, since the liquid-liquid two-phase flow in the packed tower extraction device is driven only by the density difference, its processing capacity is relatively low. The processing capacity of the U-shaped tubular extraction device of the present invention can reach about 100 times the processing capacity of the packed tower extraction device.

[0222] In summary, the present invention combines a U-shaped pipe and a separation device so that the entire device forms a circulating tubular structure, and controls the residence time of the mixed liquid by controlling the inlet and outlet flow rates of the mixed liquid, thereby improving the single-stage extraction efficiency and processing capacity. At the same time, the separation device is arranged above the U-shaped pipe, which greatly reduces the footprint of the equipment, facilitates industrial scale-up, and is suitable for industrial extraction processes of large-flow, high-solid content liquid-liquid two-phase systems.

[0223] The applicant declares that the above is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention shall fall within the protection scope and disclosure scope of the present invention.

Claims

1. A U-shaped tube extraction device, characterized in that: The U-shaped tube extraction equipment comprises a U-shaped pipeline, a stirring device and a separation device; The U-shaped pipeline comprises a first vertical section, a transverse section and a second vertical section connected in sequence; the U-shaped pipeline also comprises an extraction raw material inlet arranged in the first vertical section; The stirring device is located in the transverse section of the U-shaped pipe; The separation device is located above the U-shaped pipe, and the lower part of the separation device is communicated with the top of the first vertical section and the top of the second vertical section respectively; The separation device comprises a light phase discharge port and a heavy phase discharge port, wherein the light phase discharge port and the heavy phase discharge port are arranged at a side of the separation device.

2. The U-shaped tube extraction equipment according to claim 1, characterized in that: The U-shaped pipe also includes a mixer inside; wherein the stirring device and the mixer are sequentially arranged along the material flow direction; The mixer is disposed in the second vertical section; The mixer comprises a static mixer.

3. The U-shaped tube extraction equipment according to claim 1, characterized in that: The ratio of the outermost dimension of the blade of the stirring device to the diameter of the U-shaped pipe is (0.5-0.95):1; And / or, the ratio of the length of the impeller of the stirring device in the U-shaped pipe to the diameter of the U-shaped pipe is (0.5-2):

1.

4. The U-shaped tube extraction device according to any one of claims 1 to 3, characterized in that: The internal cavity of the separation device includes a clarification chamber and a mixing chamber from top to bottom; A transverse baffle is provided between the mixing chamber and the clarifying chamber, and the transverse baffle separates the clarifying chamber and the mixing chamber into two independent spaces.

5. The U-shaped tube extraction equipment according to claim 4, characterized in that: The mixing chamber and the clarifying chamber are connected through an outer tube, and the outer tube is connected to a material outlet arranged on the mixing chamber and a material inlet arranged on the clarifying chamber; the material inlet and the material outlet are respectively arranged at the sides of the clarifying chamber and the mixing chamber; The material outlet is arranged at a side of the mixing chamber close to the second vertical section.

6. The U-shaped tube extraction equipment according to claim 4, characterized in that: An overflow phase separation weir and a vertical partition are arranged inside the clarification chamber; Wherein, the overflow phase separation weir is arranged on the side of the clarification chamber close to the first vertical section; and two adjacent vertical partitions are staggered.

7. The U-shaped tube extraction equipment according to claim 4, characterized in that: The heavy phase discharge port and the light phase discharge port are arranged on the side of the clarification chamber, and the heavy phase discharge port is arranged below the light phase discharge port; The heavy phase discharge port and the light phase discharge port are arranged at the side of the clarification chamber away from the material inlet.

8. A method for using the U-shaped tube extraction device according to any one of claims 1 to 7, characterized in that: The method of use comprises: introducing heavy phase raw material liquid and light phase extraction solvent into the extraction raw material inlet of the U-shaped pipe, and starting the stirring device to make the materials flow through the stirring device and the separation device in sequence to perform liquid-liquid extraction and separation.

9. The method of use according to claim 8, characterized in that: The method of use further comprises: using a mixer between the stirring device and the separation device to perform a second mixing on the heavy phase raw material liquid and the light phase extraction solvent.

10. The method of use according to claim 8 or 9, characterized in that: When the material flows through the separation device, the first part of the material enters the clarification chamber of the separation device for separation, and the second part of the material passes through the mixing chamber of the separation device and continues to enter the U-shaped pipe for circulation and mixing.

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