Full-automatic three-liquid-phase extraction device

Abstract

The utility model relates to the field of extraction devices, in particular to a full-automatic three-liquid-phase extraction device. The device comprises an injection pump, a selector valve, a first phase container, a second phase container, a third phase container, a first collection container, a second collection container, a third collection container, a storage and detection assembly and a waste liquid container, the selector valve is provided with a common port and eight selection ports, and one of the common port is communicated with the selection ports; the first phase container, the second phase container and the third phase container are respectively communicated with three selection ports of the selection valve; the first collection container, the second collection container and the third collection container are respectively communicated with the other three selection ports of the selection valve; the storage and detection assembly comprises a sample tube, a base and a connecting tube which are sequentially communicated, and a conductivity detector and a capacitance detector which are arranged on the connecting tube. The device disclosed by the utility model can realize quantitative injection, automatic oscillation and mixing, automatic judgment of layering positions after standing and layering, and automatic receiving of three different-phase liquids obtained by extraction respectively.

Description

Technical Field

[0001] The utility model relates to the field of extraction devices, in particular to a full-automatic three-liquid phase extraction device. Background Art

[0002] The liquid-liquid-liquid three-phase extraction system refers to an extraction and separation system containing three liquid phases, which is an extension of the traditional two-phase liquid-liquid extraction method.

[0003] Due to the complex extraction conditions in three-phase extraction systems, optimization requires extensive experimental testing. Key tasks involve quantifying the phase volumes and separation conditions at varying volume ratios of the three phases, as well as the concentration of the target compound in each phase. Liquid metering and extraction processes are complex, and in some systems, the interfaces between the liquid phases are unclear, often leading to misjudgment of the phase interfaces during manual separation. Currently used liquid-liquid extraction instruments are essentially replicas of manual liquid-liquid extraction processes. This is achieved by using different types of pumps to pump the two liquids to be mixed and extracted into a separatory funnel. An online oscillator is used to mix the two phases and wait for the liquids to separate. The stopcock in the separatory funnel is then manually opened to collect the separated liquid. The device has a low level of automation and is unable to automatically determine the position of the liquid separation, preventing automatic collection. Designed solely for two-phase liquid-liquid extraction, these issues are particularly pronounced when performing three-phase extraction. For devices with similar functions, please refer to the fully automatic liquid-liquid extractor announced in Chinese Patent Publication No. CN212236075U and the new liquid-liquid extractor announced in Chinese Patent Publication No. CN214130389U.

[0004] The existing extraction device has a low degree of automation, does not support the quantitative automatic extraction process of three different solutions, cannot automatically determine the stratification position of the liquid, and has no automatic receiving port, so it cannot automatically receive. Utility Model Content

[0005] The purpose of the utility model is to solve the problems existing in the background technology and propose a fully automatic three-phase liquid extraction device, which can realize quantitative injection, automatic oscillation mixing, automatic judgment of the stratification position after static stratification, and automatically receive the three different phases of liquid obtained by extraction.

[0006] The technical solution of the utility model is a fully automatic three-phase extraction device, comprising an injection pump, a selection valve, a first phase container, a second phase container, a third phase container, a first collecting container, a second collecting container, a third collecting container, a storage and detection component and a waste liquid container; the selection valve has a common port and eight selection ports evenly distributed around the common port, and one of the common ports is selectively connected to the selection port; a buffer ring is connected between the injection pump and the common port of the selection valve; the first phase container, the second phase container and the third phase container are respectively connected to three of the selection ports of the selection valve; the first collection container, the second collection container and the third collection container are respectively connected to the other three selection ports of the selection valve; the storage and detection component comprises a sample tube, a base and a connecting tube that are connected in sequence, and a conductivity detector and a capacitance detector arranged on the connecting tube; the waste liquid container and the connecting tube are respectively connected to the remaining two selection ports of the selection valve.

[0007] Preferably, the volume of the buffer ring is consistent with the range specification of the injection pump.

[0008] Preferably, the selection valve includes a valve body, a stator arranged in the middle of the valve body and a rotor rotatably arranged on the stator. The common port and the selection port are both located on the valve body. The outer end of the rotor has a slot and the inside has a passage. When the slot faces any selection port, the port is connected to the common port.

[0009] Preferably, the top of the base has an opening for inserting the sample tube, a through hole is provided below the opening, and the connecting tube is connected to the through hole.

[0010] Preferably, a Luer connector is used to connect the base and the sample tube.

[0011] Preferably, a vibration motor is provided on the base.

[0012] Preferably, the conductivity detector is a flow-through detector, where the liquid is introduced into the conductivity detector inlet and taken out from the conductivity detector outlet; the capacitance detector is a clamp-tube detector, where the connecting tube is fixed between two measuring electrodes for measurement.

[0013] Preferably, the buffer ring is an inert pipeline, the selection valve material is stainless steel or polyetheretherketone, the base material is stainless steel, the sample tube material is polypropylene, and the connecting tube material is polytetrafluoroethylene.

[0014] Compared with the prior art, the present invention has the following beneficial technical effects:

[0015] The utility model can realize quantitative injection, automatic oscillation mixing, automatic determination of the stratification position after static stratification of the three-phase system for extraction, and automatic reception of the three different phases of liquid obtained by extraction, thereby facilitating a large number of condition experiments in liquid-liquid-liquid three-phase extraction research. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a structural schematic diagram of an embodiment of the present utility model.

[0017] Figure numerals: 1. Injection pump; 2. Buffer ring; 3. Selection valve; 41. First phase container; 42. Second phase container; 43. Third phase container; 51. First collecting container; 52. Second collecting container; 53. Third collecting container; 6. Waste liquid container; 7. Conductivity detector; 8. Capacitance detector; 9. Base; 10. Sample tube; 11. Vibration motor; 12. Data system. DETAILED DESCRIPTION

[0018] like Figure 1 As shown, a fully automatic three-phase liquid extraction device proposed in this embodiment includes a syringe pump 1, a selection valve 3, a first phase container 41, a second phase container 42, a third phase container 43, a first collection container 51, a second collection container 52, a third collection container 53, a storage and detection component and a waste liquid container 6, and an external data system 12 controls the entire extraction device.

[0019] The storage and detection component includes a sample tube 10, a base 9 and a connecting tube connected in sequence, and a conductivity detector 7 and a capacitance detector 8 arranged on the connecting tube. The top of the base 9 has an opening for plugging in the sample tube 10, and a through hole is provided below the opening, and the connecting tube is connected to the through hole. When injecting liquid into the sample tube 10, it is sucked or injected from the bottom end of the sample tube 10 through the corresponding port of the selection valve 3. The base 9 and the sample tube 10 are connected using a Luer connector. A vibration motor 11 is provided on the base 9. The sample tube 10 is used to hold the three phases of extraction and mix and oscillate them. The base 9 is made of stainless steel, the sample tube 10 is made of polypropylene, and the connecting tube is made of polytetrafluoroethylene, which is an insulating material and does not affect the detection of the conductivity detector 7 and the capacitance detector 8.

[0020] The conductivity detector 7 is a flow-through detector, where liquid is introduced into the inlet of the conductivity detector 7 and discharged from the outlet of the conductivity detector 7. The capacitance detector 8 is a clamp-tube detector, where a connecting tube is fixed between two measuring electrodes for measurement.

[0021] In liquid-liquid-liquid three-phase extraction, several different solvents may be used, including three of the four types: hydrophobic organic solvents (hexane, etc.), hydrophilic organic solvents (alcohols, etc.), polymer solutions (dextran, perfluoropolymers, etc.), and aqueous solutions of inorganic salts (magnesium sulfate, etc.). Therefore, the capacitance and conductivity properties of the phase separation solvents are significantly different, as shown in Table 1 below.

[0022] Table 1. Conductivity and dielectric constant of four solvents

[0023]

[0024] By measuring the conductivity and dielectric constant of the flowing liquid using the conductivity detector 7 and the capacitance detector 8 , the type of the flowing liquid can be determined.

[0025] Selector valve 3 has a common port and eight selector ports evenly distributed around the common port. The common port selectively connects to one of the selector ports. The eight selector ports are Port A, Port B, Port C, Port D, Port E, Port F, Port G, and Port H. Selector valve 3 is made of stainless steel or polyetheretherketone (PEEK), an inert material that does not react with the target substance being extracted or the reagents used. Selector valve 3 includes a valve body, a stator disposed in the middle of the valve body, and a rotor rotatably mounted on the stator. Both the common port and the selector ports are located on the valve body. The rotor has a slot at its outer end and a passageway within it. When the slot faces any selector port, that port connects to the common port.

[0026] A buffer ring 2 is connected between the common port of the syringe pump 1 and the selector valve 3. The buffer ring 2 is an inert pipeline. The volume of the buffer ring 2 is consistent with the range specification of the syringe pump 1. This ensures that when the syringe pump 1 draws a fixed amount of liquid, the drawn liquid only enters the buffer ring 2 and does not enter the syringe pump 1, preventing contamination of the syringe pump 1.

[0027] The first phase container 41, the second phase container 42 and the third phase container 43 are connected to the port A, port B and port C of the selection valve 3 respectively. The three containers generally store a sample to be extracted and two extraction solvents. The first collection container 51, the second collection container 52 and the third collection container 53 are connected to the port F, port G and port H of the selection valve 3 respectively. The three containers are used to collect the three extracted solutions. The waste liquid container 6 is connected to the port E of the selection valve 3. Specifically, the port E is connected to an open pipe, and the waste liquid container 6 is placed below. The outlet of the pipe is at the height of the bottle mouth and does not enter below the liquid level of the waste liquid. When inhaling, it can be used as an air inlet, and when pushing out, the waste liquid can be discharged to the waste liquid container 6 as a waste liquid outlet. The connecting pipe is connected to the port D of the selection valve 3.

[0028] This three-phase liquid extraction device can achieve the following three functions:

[0029] 1. Three-phase quantitative injection and capacitance and conductance measurement;

[0030] 2. Automatic oscillation extraction;

[0031] 3. Automatic layer judgment and three-phase automatic reception.

[0032] The implementation steps of the above three functions are carried out in sequence, among which, the implementation method of function one is as follows:

[0033] To draw a volume V of a phase from any of ports A, B, and C, push it into sample tube 10 for mixed extraction, and drain the line afterward, take the solution injected into port A as an example (the process for injecting solutions into ports B and C is the same, only the ports are different). The specific process is as follows: Steps A1-A7:

[0034] A1. Insert the empty sample tube 10 into the sample base 9. The volume of the sample tube 10 should be 2-3 times the total volume of the three extraction phases.

[0035] A2, selector valve 3 switches to port E, pushing out all the current remaining, and the piston in syringe pump 1 reaches the farthest end;

[0036] A3. Keep port E connected and use syringe pump 1 to draw 2 mL of air.

[0037] A4. Switch the selector valve 3 to the designated aspiration port A, and take out a liquid volume of V+δv mL. The extra aspirated δv volume is 0.2-0.5 mL, which is used to exchange the remaining volume in the pipeline.

[0038] A5, switch the selector valve 3 to the port D where output is required, push the piston of the syringe pump 1 out to a volume of V, and push the liquid with a volume of V sucked into the buffer ring from port A to port D;

[0039] A6. When the first phase in the first phase container 41 flows through the conductivity detector 7 and the capacitance detector 8, the two detectors measure the conductivity and capacitance of the first phase and send them to the data system 12 for recording;

[0040] A7. After the infusion is completed, select valve 3 to switch to port E to push out the remaining solvent and the previously inhaled air to achieve self-cleaning of the pipeline.

[0041] Function 2 is implemented as follows:

[0042] The sample extraction process is implemented in the sample tube 10 inserted into the sample base 9. According to the process in function one, the three phases in the first phase container 41, the second phase container 42 and the third phase container 43 are injected into the sample tube 10 according to the specified volume, and after measuring and recording the conductivity and capacitance values ​​of each phase, the oscillation extraction is implemented as follows: the vibration motor 11 is turned on to realize the oscillation function. Bubbling mixing can be added during the process. The implementation method is to switch the selection valve 3 to port E, inhale air to full scale, and then switch the selection valve 3 to the sample tube port D to be output, push the piston of the injection pump 1, and blow the absorbed air out from the lower end of the sample tube 10, so as to achieve the effect of bubbling assisted mixing during the oscillation extraction process.

[0043] Function three is implemented as follows:

[0044] When the oscillation mixing process is completed, the device will pause and wait for the three phases to separate, specifically the following steps B1-B5:

[0045] B1. After the solution in the sample tube 10 has been layered, the selection valve 3 is switched to port E to push out all the current residue, and the piston of the syringe pump 1 reaches the farthest end. Then, keep port E connected, and the syringe pump 1 draws 2mL of air. Thereafter, the selection valve 3 is switched to port D to connect to the common port, and the piston is withdrawn at a slow speed. At this time, the bottom layer of liquid will flow through the capacitance detector 8 and the conductivity detector 7. The two detectors measure the conductivity and capacitance values ​​of the inhaled bottom layer of liquid, and compare them with the corresponding values ​​of the three phases measured in the function one step. The conductivity and capacitance values ​​will be consistent with one of the phases. When the piston of the syringe pump 1 has drawn the bottom layer of liquid into the syringe pump 1, the two detectors will detect the changes in conductivity and capacitance. At this time, it means that the bottom layer of liquid has been completely drawn into the buffer ring 2. The syringe pump 1 stops withdrawing, and the selection valve 3 is switched to port F to connect to the common port, and the syringe pump 1 is completely pushed out. At this time, the bottom layer of liquid inhaled will be injected into the first collection container. The 2mL of air in the buffer ring 2 can discharge all the residues in the pipeline into the first collection container 51;

[0046] B2. Then the selection valve 3 is switched to port E to push out all the current remaining liquid, and the piston of the injection pump 1 reaches the farthest end. Then keep port E connected, and the injection pump 1 draws 2mL of air. The selection valve 3 is switched to port D to connect with the common port, and the piston of the injection pump 1 is withdrawn at a slow speed. At this time, the remaining liquid in the sample tube 10 will flow through the capacitance detector 8 and the conductivity detector 7. At this time, the injection pump 1 inhales the emulsion layer that may exist on the interface between the lower and middle liquid layers. The two detectors will measure the conductivity and capacitance values ​​of the inhaled emulsion layer liquid and compare them with the three phases measured in the function one step. When its capacitance and conductivity values ​​gradually change from the values ​​of the lower liquid to the values ​​of the middle liquid, it means that the emulsion layer liquid has been completely drawn into the buffer ring 2, and the injection pump 1 stops withdrawing, and the selection valve 3 is switched to port E to connect with the common port, and the injection pump 1 is completely pushed out. At this time, the inhaled emulsion layer liquid will be pushed out of the waste port. The 2mL of air in the buffer ring 2 can completely drain all the residues in the pipeline;

[0047] B3. Then, the selection valve 3 switches to port E, pushing out all the current remaining liquid, and the syringe pump 1 piston reaches the farthest end. Then, keep port E connected, and syringe pump 1 draws in 2mL of air. The selection valve 3 switches to port D to connect to the common port, and the syringe pump 1 piston draws out at a slow speed. At this time, the remaining liquid in the sample tube 10 (i.e., the extracted middle layer) will flow through the capacitance detector 8 and the conductivity detector 7. The two detectors will measure the conductivity and capacitance values ​​of the extracted middle layer liquid, and compare them with the three phases measured in the function step 1. The conductivity and capacitance values ​​will be consistent with one of the phases. When the syringe pump 1 piston draws all the extracted middle layer liquid into the syringe pump 1, the two detectors will detect the changes in conductivity and capacitance. At this point, it means that the extracted middle layer liquid has been completely drawn into the buffer ring 2. The syringe pump 1 stops drawing out, and the selection valve 3 switches to port G to connect to the common port, and the syringe pump 1 is completely pushed out. At this time, the extracted middle layer liquid drawn in will be injected into the second collection container 52. The 2mL of air in the buffer ring 2 can completely discharge all the residue in the pipeline into the second collection container 52;

[0048] B4. Then the selection valve 3 is switched to port E to push out all the current remaining liquid, and the piston of the injection pump 1 reaches the farthest end. Then keep port E connected, and the injection pump 1 draws in 2mL of air. The selection valve 3 is switched to port D to connect with the common port, and the piston of the injection pump 1 is withdrawn at a slow speed. At this time, the remaining liquid in the sample tube 10 will flow through the capacitance detector 8 and the conductivity detector 7. At this time, the injection pump 1 inhales the emulsion layer that may exist at the interface between the middle and upper liquid layers. The two detectors will measure the conductivity and capacitance values ​​of the inhaled emulsion layer liquid and compare them with the three phases measured in the function one step. When its capacitance and conductivity values ​​gradually change from the values ​​of the middle layer liquid to the values ​​of the upper layer liquid, it means that the emulsion layer liquid has been completely drawn into the buffer ring 2, and the injection pump 1 stops withdrawing, and the selection valve 3 is switched to port E to connect with the common port, and the injection pump 1 is completely pushed out. At this time, the inhaled emulsion layer liquid will be pushed out of the waste port. The 2mL of air in the buffer ring 2 can completely drain all the residues in the pipeline;

[0049] B5. Then the selection valve 3 is switched to port E to push out all the current residue, and the piston of the injection pump 1 reaches the farthest end. Then keep port E connected, and the injection pump 1 draws 2mL of air. The selection valve 3 is switched to port D to connect with the common port, and the piston of the injection pump 1 extracts the remaining liquid in the sample tube. The two detectors will measure the conductivity and capacitance values ​​of the inhaled extraction middle liquid. When the measured values ​​are equal to the conductivity and capacitance of the air, it means that the sample tube 10 has been completely evacuated, and the extracted upper liquid has all entered the buffer ring 2. The injection pump 1 stops extracting, and the selection valve 3 is switched to port H to connect with the common port, and the injection pump 1 is completely pushed out. At this time, the inhaled extraction upper liquid will be injected into the third collection container 53. The 2mL of air in the buffer ring 2 can discharge all the residues in the pipeline into the third collection container 53.

[0050] This embodiment can achieve quantitative injection, automatic oscillation mixing, and automatic determination of the stratification position after static stratification of the three-phase system to be extracted, and automatically receive the three different phases of liquid obtained by extraction. It has a high degree of automation and can conveniently optimize and automatically process the liquid-liquid-liquid three-phase extraction conditions, providing convenience for a large number of condition experiments in liquid-liquid-liquid three-phase extraction research.

[0051] Furthermore, this extraction device is also backward compatible, enabling a simpler two-phase liquid-liquid extraction process. The liquid-liquid extraction process is also fully automated, eliminating the need for manual liquid separation and interface determination. This is particularly advantageous for determining the location of delamination in extraction systems with unclear interfaces and emulsion interference.

[0052] The embodiments of the present invention are described in detail above with reference to the accompanying drawings, but the present invention is not limited thereto. Various changes can be made within the knowledge scope of those skilled in the art without departing from the purpose of the present invention.

Claims

1. A fully automatic three-phase liquid extraction device, characterized in that: include: A selection valve (3) having a common port and eight selection ports evenly distributed around the common port, wherein one of the common ports is selectively connected to the selection port; A buffer ring (2) is connected between the injection pump (1) and the common port of the selection valve (3); a first phase container (41), a second phase container (42) and a third phase container (43) respectively connected to three selection ports of the selection valve (3); a first collecting container (51), a second collecting container (52) and a third collecting container (53) respectively connected to the other three selection ports of the selection valve (3); A storage and detection assembly comprising a sample tube (10), a base (9) and a connecting tube connected in sequence, and a conductivity detector (7) and a capacitance detector (8) arranged on the connecting tube; The waste liquid container (6) and the connecting pipe are respectively connected to the remaining two selection ports of the selection valve (3).

2. A fully automatic three-liquid phase extraction device according to claim 1, characterized in that, The volume of the buffer ring (2) is consistent with the range specification of the injection pump (1).

3. A fully automatic three-liquid phase extraction device according to claim 1, characterized in that: The selection valve (3) comprises a valve body, a stator arranged in the middle of the valve body and a rotor rotatably arranged on the stator. The common port and the selection port are both located on the valve body. The outer end of the rotor has a slot and the interior has a passage. When the slot faces any selection port, the port is connected to the common port.

4. A fully automatic three-phase liquid extraction device according to claim 1, characterized in that: The top of the base (9) is provided with an opening for inserting the sample tube (10), a through hole is provided below the opening, and the connecting tube is communicated with the through hole.

5. A fully automatic three-liquid phase extraction device according to claim 4, characterized in that: The base (9) and the sample tube (10) are connected using a Luer connector.

6. A fully automatic three-phase liquid extraction device according to claim 1, characterized in that: A vibration motor (11) is provided on the base (9).

7. The fully automatic three-liquid phase extraction device according to claim 1, characterized in that: The conductivity detector (7) is a flow-through detector, wherein the liquid is introduced into the inlet of the conductivity detector (7) and taken out from the outlet of the conductivity detector (7); the capacitance detector (8) is a clamp-tube detector, wherein the connecting tube is fixed between two measuring electrodes for measurement.

8. The fully automatic three-liquid phase extraction device according to claim 1, characterized in that: The buffer ring (2) is an inert pipeline, the selection valve (3) is made of stainless steel or polyetheretherketone, the base (9) is made of stainless steel, the sample tube (10) is made of polypropylene, and the connecting tube is made of polytetrafluoroethylene.

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