A U-tube type extraction device and its usage method

Abstract

The present invention relates to a U-shaped tube extraction device and a method for using the same. The U-shaped tube extraction device comprises a U-shaped pipe, a stirring device and a separation device; the U-shaped pipe comprises a first vertical section, a transverse section and a second vertical section which are connected in sequence; the U-shaped pipe further comprises an extraction raw material inlet arranged on 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 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 arranged on the side part of the separation device. In the present invention, the separation device is arranged above the U-shaped pipe, so that the whole device forms a circulating tube structure, the residence time of the mixed liquid can be controlled, the single-stage extraction efficiency is improved, and at the same time, the floor area of the device is greatly reduced, which is easy for industrial scale-up.

Description

Technical Field

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

[0002] Liquid-liquid extraction is a separation technology widely used in the fields of chemical engineering, metallurgy, pharmaceuticals, environmental protection, etc., and has many advantages such as high separation efficiency and high selectivity. Extraction devices mainly include mixer-settlers, extraction towers, tube type extraction devices, centrifugal extraction devices, liquid membrane extraction devices, ultrasonic extraction devices, etc. Different extraction devices are suitable for different process requirements and material characteristics, and selecting the appropriate device is crucial for improving extraction efficiency and reducing costs.

[0003] Mixer-settlers have unique advantages in terms of equipment simplicity, operation flexibility, anti-blocking ability, etc., but their mass transfer efficiency and solvent utilization rate are not high. Therefore, they are more suitable for rough extraction of raw liquid and small-scale production scenarios. The extraction tower adopts countercurrent extraction with high mass transfer efficiency, but axial backmixing is likely to occur during the operation process. In addition, the flow of materials in the tower depends on the density difference of materials and the packing structure, and the processing capacity improvement is limited. In comparison, the centrifugal extractor has a high volumetric efficiency and mass transfer speed, but its drum is easily blocked and its processing capacity for solid-containing materials is poor. Advanced extraction technologies such as liquid membrane extraction devices and ultrasonic extraction devices are only able to achieve good applications in the laboratory due to disadvantages such as high technical barriers and difficulty in scaling up, and it is still relatively difficult to achieve large-scale industrial applications.

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

[0005] CN213492120U discloses a novel tube type extractor with good sealing effect and capable of discharging sewage in time, which changes the traditional box type mixer-settler 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 phases. However, it still essentially belongs to the mixer-settler equipment.

[0006] CN103254262A discloses a method for extracting androstenedione by using a pipeline type continuous ultrasonic extraction technology. By strengthening the liquid-liquid two-phase dispersion and mixing in the pipeline through ultrasonic method, the solvent consumption in the extraction process is reduced, and the energy consumption is lowered. However, since the extraction process in the tubular structure is a liquid-liquid co-current extraction, in order to increase the extraction efficiency, a very long pipeline length is required, and the floor area is very large. In addition, the mixed liquid after extraction still needs to be separated by a disc centrifuge, and the process is more complex.

[0007] In summary, it is necessary to develop a tubular extraction device that can reduce the floor area while improving the extraction efficiency and optimizing the extraction process. Summary of the Invention

[0008] To solve the above technical problems, the present invention uses a U-shaped pipeline for extraction, and a separation device is arranged above the U-shaped pipeline, so that the whole device forms a circulating tubular structure, which can reduce the floor area while improving the extraction efficiency.

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

[0010] In the first aspect, the present invention provides a U-shaped tubular extraction device, which includes a U-shaped pipeline, a stirring device and a separation device;

[0011] The U-shaped pipeline includes a first vertical section, a horizontal section and a second vertical section connected in sequence; the U-shaped pipeline further includes an extraction raw material inlet arranged on the first vertical section;

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

[0013] The separation device is located 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;

[0014] The separation device includes 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 on the side of the separation device.

[0015] The U-shaped tube extraction equipment of the present invention preferably realizes the integrated structure of the mixing and extraction U-shaped pipe and the separation device. The present invention can make full use of the advantages of the U-shaped pipe, such as fast fluid flow rate and high turbulence intensity, to improve the extraction mass transfer rate. At the same time, a stirring device is arranged in the horizontal section of the U-shaped pipe to shear the mixed liquid, so as to promote the breakup of liquid droplets, reduce the size of liquid droplets, increase the contact area between the liquid-liquid two phases, and thus improve 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 pipe, 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 the advantages of fast extraction speed, large processing capacity, ability to handle materials with high solid content, stable operation, good controllability, small floor area, easy continuous operation, and easy industrial scale-up. It can handle the liquid-liquid two-phase extraction process with large flow rate and high solid content, 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 set up in series or in parallel. Those skilled in the art can choose according to the specific process.

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

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

[0019] The present invention arranges a mixer in the second vertical section to 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, preventing liquid stratification, and improving the extraction and separation effect.

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

[0021] Preferably, the static mixer includes a flow disturbing member.

[0022] Preferably, the shape of the flow disturbing member includes spiral fins.

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

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

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

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

[0027] Preferably, the blades include downward pressing 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 it is not limited to the listed values. Other unlisted values within the above numerical range are equally applicable.

[0029] By limiting the ratio of the outermost dimension of the blade of the stirring device to the diameter of the U-shaped pipe, the present invention can further promote the shearing of the mixing liquid by the stirring device, so as to promote the fragmentation of liquid droplets, reduce the size of liquid droplets, increase the contact area between the liquid-liquid two 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 mixing liquid is too small, and the shearing and conveying capabilities are insufficient, which easily leads to a slow liquid circulation flow rate and large liquid 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 shaft will cause friction between the blade and the pipe, which is not conducive to the stable operation of the equipment.

[0030] Preferably, the pressing angle of the pressing-type blade is 15-75°. For example, it can be 15°, 25°, 35°, 45°, 55°, 65° or 75°, but it is not limited to the listed values. Other unlisted values within the above numerical range are equally 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. Other unlisted values within the above numerical range are equally 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 it is not limited to the listed values. Other unlisted values within the above numerical range are equally applicable.

[0033] 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, the present invention can further increase the contact area between the liquid-liquid two phases, improve the extraction efficiency, and at the same time provide 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, it will lead to insufficient thrust of the stirring device, a decrease in the flow rate of the mixed liquid, causing the particles in the mixed liquid to settle, and ultimately reducing the extraction efficiency. 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, it will increase the frictional loss, decrease the stirring efficiency, and increase the cavitation risk, which is 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 sequentially includes a clarification chamber and a mixing chamber from top to bottom.

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

[0037] The present invention arranges the clarification chamber above the mixing chamber. Compared with the horizontal series arrangement of the mixing chamber and the clarification chamber, it can reduce the floor area. At the same time, since the clarification chamber is located in the upper part of the separation device, it can make the clarification area form a thin-layer phase separation, which can greatly reduce the volume of the clarification chamber. The present invention adopts the principle of gravity separation, enabling the extraction light phase and heavy phase liquids to naturally stratify in the clarification chamber, facilitating the subsequent two-phase separation.

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

[0039] As a preferred technical solution of the present invention, the mixing chamber and the clarification chamber are connected by an outer pipe, and the outer pipe is connected to the material outlet provided on the mixing chamber and the material inlet provided on the clarification chamber; the material inlet and the material outlet are respectively arranged on the side parts of the clarification chamber and the mixing chamber.

[0040] The mixing chamber and the clarification chamber of the present invention are connected by an outer pipe, and the mixed liquid flows from the material outlet on the mixing chamber through the outer pipe into the clarification chamber. Compared with opening a hole in the horizontal baffle to allow the mixed liquid to enter the clarification chamber from the mixing chamber, using an outer pipe to connect the mixing chamber and the clarification chamber can set a solenoid valve on the outer pipe, control the residence time of the mixed liquid in the U-shaped pipe by adjusting the valve opening, control the flow rate of the mixed liquid entering the clarification chamber, 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 portion 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, it can be 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 value range are equally applicable.

[0043] Preferably, the diameter of the horizontal cylinder is 30 - 2000 mm, for example, it can be 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 value range are equally applicable.

[0044] Preferably, the height of the horizontal cuboid is 30 - 2000 mm, for example, it can be 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 value range are equally 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; it can reduce the entrainment phenomenon between the light phase and the heavy phase; its vertical partition can inhibit fluid turbulence, extend 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 at a side portion of the clarification chamber close to the first vertical section; two adjacent vertical partitions are distributed staggeredly.

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

[0049] As a preferred technical solution of the present invention, the heavy phase discharge port and the light phase discharge port are arranged at a side portion 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 at a side portion of the clarification chamber far from the material inlet.

[0051] By arranging the light-phase discharge port and the heavy-phase discharge port of the clarification chamber on the side of the clarification chamber away from the material inlet, that is, on the side close to the first vertical section, the present invention can effectively alleviate the liquid-liquid two-phase stratification 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 or a combination of at least two of stainless steel, polytetrafluoroethylene, fiberglass, polypropylene, polyvinyl chloride, Hastelloy, or titanium alloy. 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, Hastelloy, and titanium alloy, a combination of stainless steel, polytetrafluoroethylene, fiberglass, polypropylene, polyvinyl chloride, Hastelloy, and titanium alloy.

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

[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. Other unlisted values within the above numerical range are also applicable.

[0056] Preferably, the first vertical section, the horizontal section, and the second vertical section are connected by an arc-shaped corner.

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

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

[0059] Preferably, a second pipe and a third pipe 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 includes 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 arranged between the stirring device and the mixer.

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

[0064] Preferably, both of the pressure sensors are 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 includes three of the 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 includes three of the flow sensors.

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

[0070] Preferably, the solenoid valve and the flow sensor are successively arranged on the first pipe, the second pipe, 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. Other unlisted values within the above numerical range are equally 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 for using includes: feeding 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 enable the material to flow through the stirring device and the separation device in sequence for liquid-liquid extraction and separation.

[0073] Feed the heavy-phase raw material liquid and the light-phase extraction solvent into the extraction raw material inlet of the U-shaped pipe, and turn on the stirring device to shear the mixture of the heavy-phase raw material liquid and the light-phase extraction solvent, promoting the breakup of droplets. At the same time, the stirring device can provide power for the circulating flow of the mixture in the U-shaped pipe and the entry of the mixture into the subsequent separation device. After the mixture enters the separation device, liquid-liquid separation is carried out. The U-shaped tube extraction equipment provided by the present invention has the advantages of simple use method, easy operation, and being easy to scale up industrially.

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

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

[0076] As a preferred technical solution of the present invention, when the material flows through the separation device, wherein, a first part of the material enters the clarification chamber of the separation device for separation, and a second part of the material continues to enter the U-shaped pipe through the mixing chamber of the separation device for circulating 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 to promote the sedimentation of the heavy phase and improve the extraction separation effect. At the same time, the first part of the material entering the clarification chamber for separation can timely remove the target component to avoid its accumulation in the mixture, and the second part of the material continuing to circulate and mix in the U-shaped pipe can maintain the two-phase contact to ensure that the unextracted components can fully contact, ultimately optimizing the separation effect.

[0078] Preferably, the usage method includes the following steps:

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

[0080] (2) Turn 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] 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. The light-phase liquid and the 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 circulating mixing.

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

[0085] By limiting 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, the present invention can control the residence time of the material in the clarification chamber to promote heavy-phase sedimentation and improve the extraction 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, and the processing capacity of the equipment will be reduced; 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 it is difficult to effectively extract the target extraction substance in the raw material liquid. In addition, it will also cause the liquid entering the clarification chamber to not fully stratify, reducing 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 the U-shaped pipe and the separation device, making the whole equipment form a circulating tube structure. The fluid flow velocity and turbulence intensity in the pipe are very large, which is beneficial 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, improving the single-stage extraction efficiency and realizing the maximum utilization of resource recovery;

[0088] (2) Meanwhile, different from the traditional tubular extraction device that requires an external liquid separation device, the U-shaped tubular extraction equipment provided by the present invention sets the separation device above the U-shaped pipe, greatly reducing the floor area of the equipment. On the basis of ensuring the stable operation of the equipment, the U-shaped tubular extraction equipment provided by the present invention has better controllability and is easier to scale up industrially.

[0089] (3) Further, the U-shaped tubular extraction equipment provided by the present invention can handle materials with a high solid content and has the advantages of simple usage method and easy operation. BRIEF DESCRIPTION OF THE DRAWINGS

[0090] Figure 1 is a schematic structural diagram of the U-shaped tubular extraction equipment provided in Embodiment 1 of the present invention.

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

[0092] Figure 3 is the present invention Figure 2 a sectional view of the static mixer in the present invention taken along A-A.

[0093] Figure 4 is a schematic structural diagram of the rotating part of the axial flow pump provided in Embodiment 1 of the present invention.

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

[0095] Figure 6 is a schematic structural diagram of the U-shaped tubular extraction equipment provided in Embodiment 4 of the present invention.

[0096] Figure 7 is a schematic structural diagram of the U-shaped tubular extraction equipment provided in Embodiment 5 of the present invention.

[0097] Figure 8 is a schematic structural diagram of the U-shaped tubular extraction equipment provided in Embodiment 6 of the present invention.

[0098] Figure 9 is a schematic structural diagram of the U-shaped tubular extraction equipment provided in Embodiment 7 of the present invention.

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

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

[0101] Figure 12It is the aqueous phase holdup map obtained by performing CFD simulation on the extraction process provided in Application Example 1 of the present invention.

[0102] Figure 13 It is the aqueous phase holdup map obtained by performing CFD simulation on the extraction process provided in Application Example 5 of the present invention.

[0103] Figure 14 It is the map of Hf 4+ ion content in the aqueous phase obtained by performing CFD simulation on the extraction process provided in Application Example 4 of the present invention.

[0104] Figure 15 It is the map of Hf 4+ ion content in the organic phase obtained by performing CFD simulation on the extraction process provided in Application Example 4 of the present invention.

[0105] Figure 16 It is a schematic diagram showing the change of single-stage extraction efficiency of the present invention with the throughput of the extraction solvent / feed liquid.

[0106] Among them, 1-U-shaped pipe; 101-first vertical section; 102-horizontal 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-horizontal 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 sensor; 17-level sensor; 1701-first level sensor; 1702-second level sensor; 1703-third level sensor; 18-pressure sensor; 1801-first pressure sensor; 1802-second pressure sensor; 19-extraction feed inlet, 20-material outlet; 21-material inlet; 22-external pipe; 23-heat exchange sleeve; 24-vane; 25-impeller; 26-central shaft; 27-first pipe; 28-second pipe; 29-third pipe; 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 implementation mode

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

[0108] Example 1

[0109] This embodiment provides a U-tube extraction device, as Figure 1 shown. The U-tube extraction device includes a U-shaped pipe 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 40 mm, and the total length is 1200 mm, that is, the ratio of the length to the diameter of the U-shaped pipe 1 is 30:1. The U-shaped pipe 1 includes a first vertical section 101, a transverse section 102, and a second vertical section 103 connected in sequence. The first vertical section 101, the transverse section 102, and the second vertical section 103 are connected by an arc-shaped corner. An extraction raw material inlet 19 is provided on the first vertical section 101. 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. A heat exchange sleeve 23 is provided outside the U-shaped pipe 1.

[0111] The stirring device is an axial flow pump 2. The axial flow pump 2 is located in the transverse section 102 of the U-shaped pipe 1. The structural schematic diagram of the rotating part of the axial flow pump 2 is as Figure 4 shown. The axial flow pump 2 includes an impeller 25 and a central shaft 26 that overlap in the geometric center and are connected to each other. Four downward pressing blades 24 with a downward pressing angle of 50° are provided in the circumferential direction of the impeller. The structural schematic diagram of the blade 24 is as Figure 5 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. 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-tube extraction device is connected to the second vertical section 103 of the U-shaped pipe 1 through a flange with a static mixer 13 provided with a flow disturbing member inside. The specific structure of the static mixer 13 is as Figure 2 and Figure 3 shown. The static mixer includes a cylindrical pipe made of stainless steel and a flow disturbing member in the shape of a spiral fin.

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

[0114] The separation device 3 is an internal cavity container with a horizontal rectangular parallelepiped structure having a length, width, and height of 400 mm, 50 mm, and 400 mm respectively. Its internal cavity sequentially includes a clarification chamber 6 and a mixing chamber 7 from top to bottom. The two chambers are separated by a transverse baffle 12, such that the space volume ratio of the clarification chamber 6 to the mixing chamber 7 is 3:1. The material outlet 20 of the mixing chamber and the material inlet 21 of the clarification chamber are connected by an outer pipe 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 separation weir 9 close to the first vertical section 101 are arranged inside the clarification chamber 6; adjacent two of the vertical partitions 8 are staggeredly distributed; the clarification chamber includes a light phase discharge port 10 and a heavy phase discharge port 11. Among them, the light phase discharge port 10 and the heavy phase discharge port 11 are arranged on the side far from the material inlet 21 of the clarification chamber and close to the first vertical section 101, and the heavy phase discharge port 11 is arranged below the light phase discharge port 10.

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

[0117] The U-shaped tube extraction equipment further includes a flow sensor 14, a solenoid valve 15, a temperature sensor 16, a liquid level sensor 17, and a pressure sensor 18. Among them, 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 pipe, 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] Embodiment 2

[0119] This embodiment provides a U-shaped tube extraction equipment, 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 500 mm, and its total length is 5000 mm. That is, the ratio of the length to the diameter of the U-shaped pipe 1 is 10:1. The U-shaped pipe 1 includes a first vertical section 101, a transverse section 102, and a second vertical section 103 that are connected in sequence. The first vertical section 101, the transverse section 102, and the second vertical section 103 are connected by an arc-shaped corner. An extraction raw material inlet 19 is provided on the first vertical section 101. 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. A heat exchange sleeve 23 is provided outside the U-shaped pipe 1.

[0121] The stirring device is an axial flow pump 2. The axial flow pump 2 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 shaft 26 that overlap geometrically and are connected to each other. Four downward pressing blades 24 with a downward pressing angle of 15° are provided 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. 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 equipment is connected to the second vertical section 103 of the U-shaped pipe 1 through a flange with a static mixer 13 provided with a flow disturbing member inside.

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

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

[0125] Ten vertical partitions 8 and an overflow phase separation weir 9 close to the first vertical section are provided inside the clarification chamber 6. Two adjacent vertical partitions 8 are staggered; the clarification chamber includes a light phase discharge port 10 and a heavy phase discharge port 11. Among them, the light phase discharge port 10 and the heavy phase discharge port 11 are provided on the side away from the material inlet 21 of the clarification chamber and close to the first vertical section 101, and the heavy phase discharge port 11 is provided below the light phase discharge port 10.

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

[0127] The U-tube type extraction equipment further includes a flow sensor 14, a solenoid valve 15, a temperature sensor 16, a liquid level sensor 17 and a pressure sensor 18. Among them, 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-tube type extraction equipment, 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 pipeline 1 is polytetrafluoroethylene (PTFE-BP), its diameter is 30 mm, and the total length is 3000 mm, that is, the ratio of the length to the diameter of the U-shaped pipeline 1 is 100:1. The U-shaped pipeline 1 includes a first vertical section 101, a transverse section 102 and a second vertical section 103 connected in sequence. The first vertical section 101, the transverse section 102 and the second vertical section 103 are connected by an arc-shaped corner. 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 2 / 9:1. A heat exchange sleeve 23 is arranged outside the U-shaped pipeline 1.

[0131] The stirring device is an axial flow pump 2. The axial flow pump 2 is located in the transverse section 102 of the U-shaped pipeline 1. The axial flow pump 2 includes an impeller 25 and a central shaft 26 with overlapping geometric centers and connected to each other. Four downward pressing blades 24 with a downward pressing 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 pipeline 1 to the diameter of the U-shaped pipeline 1 is 2:1, and the ratio of the outermost dimension of the blade 24 to the diameter of the U-shaped pipeline 1 is 0.5:1.

[0132] The U-shaped tube extraction equipment connects a static mixer 13 with a turbulator 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 part of the separation device 3 is respectively communicated with the tops of the first vertical section 101 and the second vertical section 103.

[0134] The separation device 3 is an internal cavity container with a horizontal cylindrical structure with a diameter of 300 mm and a length of 1000 mm. Its internal cavity sequentially 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 volume ratio of the clarification chamber 6 to the mixing chamber 7 is 20:1. The material outlet 20 of the mixing chamber and the material inlet 21 of the clarification chamber are connected by an outer pipe 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] One vertical partition 8 and an overflow phase separation weir 9 close to the first vertical section are arranged inside the clarification chamber 6; adjacent two vertical partitions 8 are staggered; the clarification chamber includes a light phase discharge port 10 and a heavy phase discharge port 11. Among them, the light phase discharge port 10 and the heavy phase discharge port 11 are arranged on the side far from the material inlet 21 of the clarification chamber and close to the first vertical section 101, and the heavy phase discharge port 11 is arranged below the light phase discharge port 10.

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

[0137] The U-shaped tube extraction equipment further includes a flow sensor 14, a solenoid valve 15, a temperature sensor 16, a liquid level sensor 17 and a pressure sensor 18. Among them, 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 pipe, 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 example provides a U-tube extraction device. The difference from Example 1 is only that, except that no static mixer 13 is provided on the second vertical section 103, the rest are the same as in Example 1.

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

[0141] Example 5

[0142] This example provides a U-tube extraction device. The difference from Example 1 is only 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 port 10 and the heavy phase discharge port 11 are arranged on the side close to the second vertical section 103, and the material is kept flowing through the vertical partition 8 and the overflow phase separation weir 9 in sequence in the clarification chamber, and the third liquid level sensor 1703 is arranged between the vertical partition 8 and the overflow phase separation weir 9, the rest are the same as in Example 1.

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

[0144] Example 6

[0145] This example provides a U-tube extraction device. The difference from Example 1 is only that, except that connecting the material outlet 20 of the mixing chamber and the material inlet 21 of the clarification chamber through the outer tube 22 is replaced by opening a channel 30 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, the rest are the same as in Example 1.

[0146] This example cannot control the ratio of the mixed liquid entering the clarification chamber to the mixed liquid in the mixing chamber. The U-tube extraction device described in this example is as Figure 8 shown.

[0147] Example 7

[0148] This example provides a U-tube extraction device. The difference from Example 1 is only that, except that the mixing chamber 7 and the clarification chamber 6 of the separation device are adjusted from being arranged side by side up and down to being arranged side by side left and right, and the mixing chamber 7 and the clarification chamber 6 are arranged in sequence along the material flow direction, and accordingly the mixing chamber 7 and the clarification chamber 6 are separated by a vertical baffle 31, the rest are the same as in Example 1.

[0149] The U-tube extraction device described in this example is as Figure 9 shown.

[0150] Example 8

[0151] This embodiment provides a U-tube extraction device, which is different from that of Embodiment 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 are the same as those of Embodiment 1.

[0152] Example 9

[0153] This embodiment provides a U-tube extraction device, which is different from that of Embodiment 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 are the same as those of Embodiment 1.

[0154] Example 10

[0155] This embodiment provides a U-tube extraction device, which is different from that of Embodiment 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 are the same as those of Embodiment 1.

[0156] Example 11

[0157] This embodiment provides a U-tube extraction device, which is different from that of Embodiment 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 are the same as those of Embodiment 1.

[0158] Comparative Example 1

[0159] This comparative example provides a U-tube extraction device, which is different from that of Embodiment 1 only in that, 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 vertically placed, the rest are the same as those of Embodiment 1.

[0160] The U-tube extraction device described in this comparative example is as Figure 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 30 mm, and the effective height of the extraction section is 1500 mm, ensuring that the effective extraction volume is the same as that of the U-tube extraction device. The packing uses Raschig rings 36 with a diameter of 10 mm, a thickness of 2.5 mm, and a height of 2.5 mm. The light-phase liquid enters from the light-phase inlet 32 at the bottom of the extraction tower, and the heavy-phase liquid enters from the heavy-phase inlet 33 at the top of the extraction tower. The two-phase liquids flow countercurrently to complete the extraction process. After extraction, the light-phase liquid is discharged from the light-phase outlet 34, and the heavy-phase liquid after extraction is discharged from the heavy-phase outlet 35.

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

[0164] Application Example 1

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

[0166] (1) Pre-mix an extraction solvent with a flow rate of 0.22 m 3 / h and a raw material liquid with a flow rate of 0.22 m 3 / h, and then input them to the extraction raw material inlet on the U-shaped pipe;

[0167] (2) Start the axial flow pump so that the rotational 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 secondary mixing;

[0169] (4) After the secondary mixing by the static mixer, 30% of the materials in the U-shaped pipe enter the clarification chamber of the separation device for separation, and the light-phase liquid and the 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 materials continue to enter the U-shaped pipe through the mixing chamber of the separation device for circulating mixing.

[0170] Use the U-tube type extraction equipment described in Example 1 to perform CFD simulation on the extraction process of the Hf 4+ solution, and the water phase holdup diagram obtained is as Figure 12 shown. It can be seen from Figure 12 that when the water phase holdup is 100%, it is red, and when the organic phase holdup is 100%, it is blue. Figure 12 The color distribution in

[0171] is relatively uniform, indicating that the liquid-liquid two-phase contact is good during the extraction process.

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

[0173] (1) Pre-mix an extraction solvent with a flow rate of 10 m 3 / h and a raw material liquid with a flow rate of 10 m 3 / h, and then input them to the extraction raw material inlet on the U-shaped pipe;

[0174] (2) Start the axial flow pump so that the rotational 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 secondary mixing;

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

[0177] Application Example 3

[0178] This application example provides a usage method of the U-shaped tube extraction equipment described in Example 3. The usage method includes:

[0179] (1) Premix an extraction solvent with a flow rate of 0.1 m 3 / h and a raw material liquid with a flow rate of 0.1 m 3 / h, and then input it to the extraction raw material inlet on the U-shaped pipe;

[0180] (2) Start the axial flow pump so that the rotational 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 secondary mixing;

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

[0183] Application Example 4

[0184] This application example provides a usage method of the U-shaped tube extraction equipment described in Example 4. Except that the usage method is carried out using the U-shaped tube extraction equipment provided in Example 4 and no secondary mixing of the static mixer is performed after the axial flow pump mixes and transports, the rest is the same as that of Application Example 1.

[0185] Use the U-shaped tube extraction equipment described in Example 4 to perform CFD simulation on the extraction process of Hf 4+ solution. The obtained Hf 4+ ion content diagrams in the aqueous phase and the Hf 4+ ion content diagrams in the organic phase are respectively as shown in Figure 14 and Figure 15 shown. It can be seen from Figure 14 that Hf 4+When the ion content is 2.49 g / kg, it is red. As the Hf 4+ ion content decreases, the color gradually changes to blue. At the feed inlet, it is red, that is, the Hf 4+ ion content in the aqueous phase is the highest during feeding. Along the material flow direction, the blue color gradually deepens, that is, along the material flow rate, the extraction efficiency gradually increases. Similarly, from Figure 15 it can be seen that when the Hf 4+ ion content is 0 g / kg, it is blue. As the Hf 4+ ion content increases, the color gradually changes to yellow. At the feed inlet, it is blue, that is, the Hf 4+ ion content in the organic phase is 0 g / kg during feeding. Along the material flow direction, the yellow color gradually deepens, that is, along the material flow rate, the extraction efficiency gradually increases.

[0186] Meanwhile, in order to better verify the influence of the throughput on the extraction effect, on the basis of Application Example 4, the throughput is adjusted to 0.0022 m 3 / h, 0.022 m 3 / h, 0.11 m 3 / h and 0.44 m 3 / h respectively, and the single-stage extraction efficiency is tested. The results are as Figure 16 shown. From Figure 16 it can be seen that as the throughput increases, the single-stage extraction efficiency gradually decreases.

[0187] Application Example 5

[0188] This application example provides a method for using the U-tube type extraction equipment described in Example 5. The method is carried out using the U-tube type extraction equipment provided in Example 5, and step (4) is adjusted as follows: After the second mixing by the static mixer, when 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. The light-phase liquid and the 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 and mixing. The rest is the same as in Application Example 1.

[0189] Perform CFD simulation on the extraction process of the Hf 4+ solution using the U-tube type extraction equipment described in Example 5. The obtained aqueous-phase holdup diagram is as Figure 13 shown. From Figure 13 it can be seen that when the aqueous-phase holdup is 100%, it is red, and when the organic-phase holdup is 100%, it is blue. Figure 13 The blue distribution within the dashed box is relatively concentrated, indicating that the organic phase aggregates there and the liquid-liquid two-phase contact is poor, which will ultimately lead to a decrease in the extraction efficiency.

[0190] Application Example 6

[0191] This application example provides a method for using the U-tube type extraction equipment described in Example 6. The method is carried out using the U-tube type extraction equipment provided in Example 6, and step (4) is adjusted as follows: After the second mixing in the static mixer, part of the materials in the U-shaped pipe enter the clarification chamber of the separation device for separation. The light-phase liquid and the 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 materials continue to enter the U-shaped pipe through the mixing chamber of the separation device for circulating mixing. The rest is the same as that in Application Example 1.

[0192] Application Example 7

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

[0194] Application Example 8

[0195] This application example provides a method for using the U-tube type extraction equipment described in Example 8. The method is the same as that in Application Example 1.

[0196] Application Example 9

[0197] This application example provides a method for using the U-tube type extraction equipment described in Example 9. The method is the same as that in Application Example 1.

[0198] Application Example 10

[0199] This application example provides a method for using the U-tube type extraction equipment described in Example 10. The method is the same as that in Application Example 1.

[0200] Application Example 11

[0201] This application example provides a method for using the U-tube type extraction equipment described in Example 11. The method 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-tube type extraction equipment described in Comparative Example 1. The method 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 type extraction equipment described in Comparative Example 2. The method includes:

[0206] (1) Feed 0.0022 m 3 / h of the extraction solvent and 0.0022 m 3 / h of the feed liquid are respectively added into the packed tower extraction equipment from the light-phase inlet and the heavy-phase inlet;

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

[0208] (3) After the extraction is completed, the light-phase liquid is stratified above the packed tower extraction equipment and discharged from the light-phase outlet; the heavy-phase liquid is stratified below the packed tower extraction equipment and discharged from the heavy-phase outlet.

[0209] Using the usage methods described in the above Application Examples 1-11 and Comparative Application Examples 1-2, the extraction processes of Hf 4+ solutions in the corresponding extraction equipment are respectively subjected to CFD simulations. Among them, the extraction system is the MIBK-HSCN system, and the Hf 4+ ion concentration in the feed liquid is 2.49 g / kg. During the simulation process, the ion concentrations in the heavy-phase liquid and the light-phase liquid at the outlet are detected. After the ion concentrations are stable, the extraction efficiency is calculated according to the formula where C 萃原水相 is the concentration of hafnium in the feed liquid before extraction, with the unit of g / kg, and C 萃余水相 is the concentration of hafnium in the liquid discharged from the heavy-phase outlet after extraction, with the unit of g / kg. The detection results are shown in Table 1.

[0210] Table 1

[0211]

[0212] It can be seen from the test results that:

[0213] (1) It can be seen from Application Examples 1 to 3 that by combining the U-shaped pipe and the separation device in the present invention, the whole equipment forms a circulating tubular structure, and by controlling the inlet and outlet flows of the mixed liquid, the residence time of the mixed liquid is controlled, the single-stage extraction efficiency and the throughput are improved, 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, greatly reducing the floor area of the equipment, being easy to scale up industrially, and being applicable to the industrial extraction process of large-flow and 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 equipment 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 equipment 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, preventing liquid stratification and improving the extraction efficiency.

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

[0216] (4) It can be seen from Application Example 1 and Application Example 6 that in the U-shaped tube extraction equipment used in Application Example 1, 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 its single-stage extraction efficiency is 60.5%; while in the U-shaped tube extraction equipment used in Application Example 6, a hole 30 is opened on the transverse baffle between the mixing chamber 7 and the clarification chamber 6 of the separation device, and the hole is close to the second vertical section 103, so that the mixed liquid enters the clarification chamber 6 through the hole 30, and its single-stage extraction efficiency is 46.0%. This shows that by connecting the mixing chamber and the clarification chamber with an outer tube, the present invention 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) From Application Example 1 and Comparative Application Example 1, it can be seen that by arranging the axial flow pump below the horizontal section of the U-shaped pipe, the present invention can shear the mixed material to promote the breakup of droplets, reduce the droplet size, increase the contact area between the liquid-liquid two phases, and thus improve the extraction efficiency.

[0221] (9) From Application Example 1 and Comparative Application Example 2, it can be seen that by combining the U-shaped pipe and the separation device, the present invention makes the whole device form a circulating tubular structure, which can improve the single-stage extraction efficiency and throughput. Under the condition of the same extraction volume of the device, the U-shaped tubular extraction device of the present invention has higher extraction efficiency. At the same time, since the flow of the liquid-liquid two phases in the packed tower extraction device is only driven by the density difference, its throughput is low, while the throughput of the U-shaped tubular extraction device of the present invention can reach about 100 times that of the packed tower extraction device.

[0222] In summary, by combining the U-shaped pipe and the separation device, the present invention makes the whole device form a circulating tubular structure, and by controlling the inlet and outlet flow rates of the mixed liquid and the residence time of the mixed liquid, the single-stage extraction efficiency and throughput are improved. At the same time, by arranging the separation device above the U-shaped pipe, the floor area of the device is greatly reduced, which is easy to scale up industrially and is applicable to the industrial extraction process of liquid-liquid two-phase systems with large flow rates and high solid content rates.

[0223] The applicant declares that the above description is only the specific implementation manner 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 fall within the protection scope and the disclosure scope of the present invention.

Claims

1. A U-tube extraction device, characterized in that, The U-shaped tube extraction equipment includes a U-shaped pipe, a stirring device and a separation device; The U-shaped pipe includes a first vertical section, a horizontal section and a second vertical section connected in sequence; the U-shaped pipe further includes an extraction raw material inlet provided on the first vertical section; The stirring device is located in the horizontal 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 respectively communicated with the tops of the first vertical section and the second vertical section; The separation device includes a light phase discharge port and a heavy phase discharge port, wherein the light phase discharge port and the heavy phase discharge port are provided on the side of the separation device; The internal cavity of the separation device sequentially includes a clarification chamber and a mixing chamber from top to bottom; And a horizontal baffle is provided between the mixing chamber and the clarification chamber, and the horizontal baffle isolates the clarification chamber and the mixing chamber into two independent spaces; The mixing chamber and the clarification chamber are connected by an outer pipe, and the outer pipe is connected to a material outlet provided on the mixing chamber and a material inlet provided on the clarification chamber; the material inlet and the material outlet are respectively provided on the side of the clarification chamber and the mixing chamber; The material outlet is provided on the side of the mixing chamber close to the second vertical section.

2. The U-tube extraction device according to claim 1, wherein A mixer is further included inside the U-shaped pipe; wherein, the stirring device and the mixer are sequentially arranged along the material flow direction; The mixer is arranged in the second vertical section; The mixer includes a static mixer.

3. The U-tube type extraction device 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-tube type extraction device according to claim 1, 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; two adjacent vertical partitions are distributed in a staggered manner.

5. The U-tube extraction device according to claim 1, characterized in that, The heavy phase discharge port and the light phase discharge port are provided 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 provided on the side of the clarification chamber far from the material inlet.

6. A method for using the U-tube type extraction device according to any one of claims 1 to 5, characterized in that, The usage method includes: feeding a heavy phase raw material liquid and a light phase extraction solvent into the extraction raw material inlet of the U-shaped pipe, and starting the stirring device to enable the material to flow through the stirring device and the separation device in sequence for liquid-liquid extraction and separation.

7. The usage method according to claim 6, characterized in that, The usage method further includes: using a mixer to perform secondary mixing on the heavy phase raw material liquid and the light phase extraction solvent between the stirring device and the separation device.

8. The usage method according to claim 6 or 7, characterized in that, When the material flows through the separation device, wherein, a first part of the material enters the clarification chamber of the separation device for separation, and a second part of the material continues to enter the U-shaped pipe through the mixing chamber of the separation device for cyclic mixing.

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