Liquid-liquid extraction-nitrogen blowing integrated extraction and purification device

Abstract

The utility model relates to the technical field of chemical experiment equipment, and discloses a liquid-liquid extraction-nitrogen blowing integrated extraction and purification device, which comprises a first separating funnel, a second separating funnel and two nitrogen blowing shunting devices, the first separating funnel and the second separating funnel are connected in series, and are respectively connected with a nitrogen blowing shunting device. According to the device, layered liquid is separated by adopting the serially connected separating funnel group, so that upper and lower layers of extraction liquid are conveniently collected, the leakage phenomenon of the extraction liquid is avoided, the repeated extraction operation is more convenient, meanwhile, the extraction liquid can be added while nitrogen blowing is carried out, the device is more convenient and quicker, repeated liquid adding is not needed, and the continuous experiment operation is facilitated.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical experimental equipment, and particularly relates to a liquid-liquid extraction-nitrogen blowing integrated extraction and purification device. Background Technique

[0002] Liquid-liquid extraction technology utilizes the principle of similar solubility to extract target molecules into a solvent, thereby separating the target substance from impurities. Commonly used solvents mainly include organic solvents such as methanol, acetonitrile, toluene, dichloromethane, chloroform, n-hexane, etc. or composite solvents composed of several solvents. Among them, liquid-liquid extraction (LLE) is the most commonly used traditional liquid-liquid extraction method. By utilizing the difference in the distribution coefficient of the analyte between two immiscible liquids or phases, the purpose of separation and enrichment is achieved. It has the advantages of simple operation, simple equipment, good broad-spectrum property, low price, etc., and has been applied earlier and the technology is relatively mature in the pretreatment of food detection. In general laboratory tests, a single separatory funnel is commonly used to perform liquid-liquid separation and extraction on the components of the sample. The sample extraction solution A is placed in the separatory funnel, and another immiscible solution B is added. After manual shaking for a period of time, the target compound is transferred to solution B, thereby achieving the purification purpose. For the purified extraction solution, concentration is required. More and more standards adopt the nitrogen blowing concentration method, that is, nitrogen is blown onto the surface of the heated sample solution, and the sample is concentrated after the solvent is vaporized. It has the advantages of time-saving, convenient operation, easy control, etc. At the same time, the environment given by nitrogen blowing concentration to the sample is an inert environment, which protects the stability of the target compound in the sample solution. For example, the "Nitrogen Blowing Concentration Device for Analyzing Tobacco-Specific Nitrosamines in Cigarette Smoke" with the invention number CN201320164922.7 includes a nitrogen blowing instrument provided with a concentrated sampling tube, an exhaust pipe connected to the nitrogen blowing instrument, a nitrogen gas system connected to the nitrogen blowing instrument through a nitrogen gas pipe, and a sample bottle connected to the nitrogen blowing instrument through a concentrated liquid outlet pipe.

[0003] Although many standards and methods use separatory funnels for liquid-liquid extraction and purification of target compounds and nitrogen blowing for solvent concentration, there are the following defects: When using a single separatory funnel for liquid-liquid extraction, it is usually shaken by hand. Due to individual differences in shaking frequency and time, the extraction efficiency between samples will vary, resulting in large errors in detection results. When using a single separatory funnel for liquid-liquid extraction, after extraction and layering, generally, the upper or lower layer solution is taken according to needs for subsequent experiments, and the extraction is repeated 2-3 times. During the collection process of the extraction solution, leakage and other problems are likely to occur, resulting in sample loss. In order to completely extract the target compound from the sample solution, the extraction solution after liquid-liquid extraction is relatively large, generally about 20-50 mL. The specification of the nitrogen blowing concentration tube on the nitrogen blowing instrument is generally 10 mL, and the recommended sample loading amount is within 5 mL. Therefore, when concentrating the extraction solution after liquid-liquid extraction by nitrogen blowing, multiple samplings are required, which is troublesome, prone to intermediate losses, and when there are multiple samples, it is easy to add the samples to the wrong positions.

[0004] Therefore, it is necessary to improve the existing technology. Utility Model Content

[0005] The technical problem to be solved by the present utility model is to provide a liquid-liquid extraction-nitrogen blowing integrated extraction and purification device that is convenient to use and has a simple structure.

[0006] To solve the above technical problems, the present utility model provides a liquid-liquid extraction-nitrogen blowing integrated extraction and purification device, which includes a first separatory funnel and a second separatory funnel, and each of the first separatory funnel and the second separatory funnel is connected to a nitrogen blowing shunt device;

[0007] The nitrogen blowing shunt device includes a fourth polytetrafluoroethylene tube, a flow rate controller, a fifth polytetrafluoroethylene tube, and a nitrogen blowing tube inlet needle connected in sequence. The lower part of the nitrogen blowing tube inlet needle is located inside the nitrogen blowing concentration tube;

[0008] The lower parts of the first separatory funnel and the second separatory funnel are each provided with a liquid outlet. After the liquid outlet of the first separatory funnel passes through a first three-way control valve, one path is connected to the fourth polytetrafluoroethylene tube of a nitrogen blowing shunt device. After the liquid outlet of the second separatory funnel passes through a second three-way control valve, one path is connected to the fourth polytetrafluoroethylene tube of another nitrogen blowing shunt device. The remaining other path outlet of the second three-way control valve is connected to the other path outlet of the first three-way control valve through a second polytetrafluoroethylene tube.

[0009] As an improvement to the liquid-liquid extraction-nitrogen blowing integrated extraction and purification device of the present utility model:

[0010] The first and second separating funnels are each provided with a liquid adding port on their upper parts, an adjustable speed motor is installed on the liquid adding port of the first separating funnel, the adjustable speed motor housing is detachably connected to the liquid adding port of the first separating funnel, a stirring paddle is provided in the first separating funnel, and the stirring paddle is transmission-connected to the motor shaft of the adjustable speed motor via an adjustable stirring rod;

[0011] The second separating funnel liquid adding port is provided with a rotatable cover, and the rotatable cover is detachably connected to the second separating funnel liquid adding port.

[0012] As a further improvement of the liquid-liquid extraction-nitrogen blowing integrated extraction and purification device of the utility model:

[0013] A first switch valve is provided on the liquid outlet of the first separating funnel, and the first three-way control valve is connected to the first switch valve via a first polytetrafluoroethylene tube;

[0014] A second switch valve is provided on the liquid outlet of the second separating funnel, and the second three-way control valve is connected to the second switch valve via a third polytetrafluoroethylene tube.

[0015] As a further improvement of the liquid-liquid extraction-nitrogen blowing integrated extraction and purification device of the utility model:

[0016] The first separatory funnel is fixedly connected to the first fixing frame via a first adjustable fixing clamp to adjust the height of the first separatory funnel, and the second separatory funnel is fixedly connected to the second fixing frame via a second adjustable fixing clamp to adjust the height of the second separatory funnel.

[0017] As a further improvement of the liquid-liquid extraction-nitrogen blowing integrated extraction and purification device of the utility model:

[0018] The nitrogen blowpipe inflow needle is provided with a nitrogen blowpipe fixing buckle for fixing the nitrogen blowpipe inflow needle to the tube wall of the nitrogen blow concentration tube.

[0019] As a further improvement of the liquid-liquid extraction-nitrogen blowing integrated extraction and purification device of the utility model:

[0020] A nitrogen blowing needle is provided in the nitrogen blowing concentrator to blow nitrogen into the nitrogen blowing concentrator.

[0021] The beneficial effects of the present invention are mainly reflected in:

[0022] 1. The utility model uses a motor to shake and stir the liquid, and no other external force is required to mix and extract the liquid. The operation is simple and the target compound can be fully extracted.

[0023] 2. The utility model adopts a series of separating funnels to separately separate the layered liquids, which is more convenient for collecting the upper and lower layer extraction liquids. Through the adjustment of the height difference between the series of separating funnels, it is convenient to distribute the layered extraction liquids between the two, without causing liquid leakage of the extraction liquid, and is more convenient for repeated extraction operations.

[0024] 3. The utility model adopts a three-way valve to connect the liquid-liquid extraction device with the nitrogen blowing device, adding extraction liquid while nitrogen blowing, which is more convenient and fast, without the need for multiple liquid additions, and is convenient for continuous experimental operations. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] The following further elaborates on the specific implementation manners of the utility model in conjunction with the drawings.

[0026] Figure 1 It is a structural schematic diagram of the liquid-liquid extraction-nitrogen blowing integrated extraction and purification device of the utility model. SPECIFIC IMPLEMENTATION MANNERS

[0027] The following further describes the utility model in conjunction with specific embodiments, but the protection scope of the utility model is not limited thereto:

[0028] Example 1. The liquid-liquid extraction-nitrogen blowing integrated extraction and purification device, as Figure 1 shown, includes a first separating funnel 11 and a second separating funnel 31. Both the first separating funnel 11 and the second separating funnel 31 are made of polytetrafluoroethylene material, and have the same shape for convenient mutual replacement. The first separating funnel 11 and the second separating funnel 31 are connected in series. Among them, the first separating funnel 11 is the main separating funnel, whose function is to mix and extract the liquid, and the second separating funnel 31 is the auxiliary separating funnel, whose function is to distribute and isolate the lower layer liquid stratified in the first separating funnel 11. Through two series-connected separating funnels, the upper and lower layered liquids after extraction are distributed and stored in the two separating funnels, facilitating subsequent further extraction and nitrogen blowing operations.

[0029] The first separating funnel 11 is fixedly connected through a first adjustable fixing clip 7 and a first fixing bracket 8, and the second separating funnel 31 is fixedly connected through a second adjustable fixing clip 10 and a second fixing bracket 9. Among them, the first adjustable fixing clip 7 can move up and down along the first fixing bracket 8 to adjust the height and lock, and the second adjustable fixing clip 10 can move up and down along the second fixing bracket 9 and lock.

[0030] The first separating funnel 11 and the second separating funnel 31 are all opened up and down, and the top is a liquid adding port, and the bottom is a liquid outlet. An adjustable speed motor 21 is installed on the liquid adding port of the first separating funnel 11, and the adjustable speed motor 21 shell is connected with the first separating funnel 11 liquid adding ports by a thread, so that the bottom of the adjustable speed motor 21 can be screwed into the liquid adding port of the first separating funnel 11, and the effect of sealing the liquid adding port is played when fixing the adjustable speed motor 21. A stirring paddle 23 is provided in the first separating funnel 11, and the stirring paddle 23 is connected with the motor shaft of the adjustable speed motor 21 by an adjustable stirring rod 22, so that the liquid in the first separating funnel 11 can be rotated and stirred under the drive of the adjustable speed motor 21. The adjustable stirring rod 22 adopts a telescopic rod structure and can adjust the upper and lower positions of the stirring paddle 23 according to the liquid height. The adjustable stirring rod 22 and the stirring paddle 23 material are all stainless steel. By means of the adjustable speed motor 21 , the adjustable stirring rod 22 and the stirring paddle 23 , a controllable extraction operation can be performed in the first separating funnel 11 , thereby avoiding the inhomogeneity of the extraction rate between samples.

[0031] A rotatable lid 32 is provided on the liquid adding port of the second separating funnel 31. The rotatable lid 32 is made of polytetrafluoroethylene and is threadedly connected to the liquid adding port of the second separating funnel 31 to seal and prevent dust. When liquid needs to be distributed, the rotatable lid 32 can be unscrewed.

[0032] A first switch valve 13 is provided at the liquid outlet of the first separating funnel 11. The first switch valve 13 is connected to the inlet end of the first three-way control valve 41 through a first polytetrafluoroethylene tube 12. One outlet end of the first three-way control valve 41 is connected to one end of the second polytetrafluoroethylene tube 42, and the other outlet end is connected to the nitrogen blow diversion device.

[0033] A second switch valve 33 is provided at the liquid outlet of the second separating funnel 31. The second switch valve 33 is connected to the inlet end of the second three-way control valve 43 through a third polytetrafluoroethylene tube 34. One outlet end of the second three-way control valve 43 is connected to the other end of the second polytetrafluoroethylene tube 42, and the other outlet end of the second three-way control valve 43 is connected to another nitrogen blowing shunt device. The first three-way control valve 41 and the second three-way control valve 43 are used to control the flow direction of the liquid in the first separating funnel 11 and the second separating funnel 31 respectively. When the liquid extraction in the first separating funnel 11 is completed, rotate the first three-way control valve 41 to connect the first polytetrafluoroethylene tube 12 with the second polytetrafluoroethylene tube 42, and rotate the second three-way control valve 43 to connect the third polytetrafluoroethylene tube 34 with the second polytetrafluoroethylene tube 42, so that the first separating funnel 11 and the second separating funnel 31 are connected. Then, adjust the height of the first separating funnel 11 by the first adjustable fixing clip 7, or adjust the height of the second separating funnel 31 by the second adjustable fixing clip 10, and use the height difference to transfer and adjust the volume of the upper and lower layer liquids in the first separating funnel 11 and the second separating funnel 31. Through the height difference, the distribution of the stratified liquid can be adjusted at any time, and it flows in and out through a closed-loop system to prevent liquid loss.

[0034] The nitrogen blowing shunt device includes a fourth polytetrafluoroethylene tube 131, a flow rate controller 132, a fifth polytetrafluoroethylene tube 133, a nitrogen blowing tube inlet needle 135 and a nitrogen blowing concentration tube 17 connected in sequence. The fourth polytetrafluoroethylene tube 131 is used to connect the nitrogen blowing shunt device with the first three-way control valve 41, or to connect another set of nitrogen blowing shunt devices with the second three-way control valve 43. The flow rate controller 132 can adopt, for example, a hose flow rate regulator including a Robert clip and a damper, which is used to control the flow rate of the extraction solution flowing into the nitrogen blowing concentration tube 17 to prevent the inflow rate of the extraction solution from being greater than the drying rate of the extraction solution. A nitrogen blowing tube fixing buckle 134 is provided on the nitrogen blowing tube inlet needle 135, which is used to fix the nitrogen blowing tube inlet needle 135 on the wall of the nitrogen blowing concentration tube 17, and the nitrogen blowing tube inlet needle 135 is located inside the nitrogen blowing concentration tube 17, so that the liquid slowly flows into the nitrogen blowing concentration tube 17 along the wall through the nitrogen blowing tube inlet needle 135. Through the integrated design of the extraction system of the two separating funnels and the nitrogen blowing of the nitrogen blowing shunt device, the whole extraction and concentration process is carried out in a closed loop, reducing the loss in the experimental process and improving the experimental efficiency. A nitrogen blowing needle 19 is provided in the nitrogen blowing concentration tube 17, and the nitrogen blowing needle 19 is connected to an external nitrogen generating device, which is used to blow nitrogen into the nitrogen blowing concentration tube 17.

[0035] The specific usage method of the present utility model is as follows:

[0036] 1. Place the liquid-liquid extraction-nitrogen blowing integrated extraction and purification device of the present utility model in the fume hood in the analytical laboratory, and configure a nitrogen generating device and a constant temperature water bath device;

[0037] 2. Place the nitrogen-blowing concentration tubes 17 of the two nitrogen-blowing and shunting devices in a water bath constant temperature device; then connect the two nitrogen-blowing needles 19 to a nitrogen generation device respectively and place them in the two nitrogen-blowing concentration tubes 17 respectively.

[0038] 3. Close the first switching valve 13 and the second switching valve 33, unscrew the adjustable-speed motor 21 at the top of the first separating funnel 11, add the sample solution to be extracted and the extraction liquid from the liquid adding port of the first separating funnel 11, adjust the height of the stirring paddle 23 according to the liquid level height, and then screw in the adjustable-speed motor 21 and tighten it to fix it on the liquid adding port of the separating funnel 11.

[0039] Turn on the adjustable-speed motor 21 to stir the liquid in the first separating funnel 11 for a preset duration.

[0040] 4. After waiting for the liquid in the first separating funnel 11 to stand and separate into layers, loosen the adjustable-speed motor 21 and the rotatable lid 32, rotate the first three-way control valve 41 to connect the first polytetrafluoroethylene tube 12 with the second polytetrafluoroethylene tube 42, rotate the second three-way control valve 43 to connect the third polytetrafluoroethylene tube 34 with the second polytetrafluoroethylene tube 42, and then open the first switching valve 13 and the second switching valve 33 to connect the first separating funnel 11 and the second separating funnel 31, and transfer the lower layer liquid of the first separating funnel 11 to the second separating funnel 31; during the liquid transfer process, by adjusting the height of the first separating funnel 11 or the second separating funnel 31, make the upper and lower layer liquids completely separated into the two separating funnels.

[0041] If it is necessary to re-extract once, repeat the above steps 3 and 4.

[0042] Then close the first switching valve 13 and the second switching valve 33.

[0043] 5. Then select the solution to be extracted as needed, specifically:

[0044] (1) If the solution to be extracted is in the first separating funnel 11, then rotate the first three-way control valve 41 to connect the nitrogen-blowing and shunting device connected to the first three-way control valve 41 with the first polytetrafluoroethylene tube 12, and open the first switching valve 13 to make the liquid in the first separating funnel 11 flow into the nitrogen-blowing concentration tube 17 through the nitrogen-blowing and shunting device.

[0045] (2) If the solution to be extracted is in the second separating funnel 31, then rotate the second three-way control valve 43 to connect the nitrogen-blowing and shunting device connected to the second three-way control valve 43 with the third polytetrafluoroethylene tube 34, and open the second switching valve 33 to make the liquid in the second separating funnel 31 flow into the nitrogen-blowing concentration tube 17 through another nitrogen-blowing and shunting device.

[0046] (3) Turn on the nitrogen generator and the constant temperature water bath, perform nitrogen blowing and concentration through the nitrogen blow needle 19, and adjust the opening size of the flow rate controller 132 to select an appropriate liquid inflow rate to ensure a balance between the liquid drying rate and the liquid inflow rate. For example, if the extract is a n-hexane solution and the volume of the extract is 20 mL, about 5 mL of the extract is preliminarily flowed into the nitrogen blowing and concentration tube, and nitrogen blowing and concentration are performed through the nitrogen blow needle 19 at a drying rate of about 1 mL / min. At the same time, the flow rate controller 132 is controlled and adjusted so that the flow rate of the extract into the nitrogen blowing and concentration tube 17 is about 1 mL / min, which can ensure a balance between the extract concentration rate and the extract inflow rate.

[0047] Finally, it should be noted that the above examples are merely specific embodiments of the present invention. Obviously, the present invention is not limited to the above examples and is subject to numerous variations. All variations that can be directly derived or conceived by a person skilled in the art from the disclosure of the present invention should be considered within the scope of protection of the present invention.

Claims

1. Liquid-liquid extraction-nitrogen blowing integrated extraction and purification device, characterized in that: It includes a first separating funnel (11) and a second separating funnel (31), and each of the first separating funnel (11) and the second separating funnel (31) is connected to a nitrogen blowing shunt device; The nitrogen blowing shunt device includes a fourth polytetrafluoroethylene tube (131), a flow rate controller (132), a fifth polytetrafluoroethylene tube (133) and a nitrogen blowing tube inlet needle (135) connected in sequence. The lower part of the nitrogen blowing tube inlet needle (135) is located inside the nitrogen blowing concentration tube (17); The lower parts of the first separating funnel (11) and the second separating funnel (31) are both provided with liquid outlets. After the liquid outlet of the first separating funnel (11) passes through the first three-way control valve (41), one path is connected to the fourth polytetrafluoroethylene tube (131) of a nitrogen blowing shunt device. After the liquid outlet of the second separating funnel (31) passes through the second three-way control valve (43), one path is connected to the fourth polytetrafluoroethylene tube (131) of another nitrogen blowing shunt device. The remaining other path outlet of the second three-way control valve (43) is connected to the other path outlet of the first three-way control valve (41) through a second polytetrafluoroethylene tube (42).

2. The liquid-liquid extraction-nitrogen blowing integrated extraction and purification device according to claim 1, characterized in that: The upper parts of the first separating funnel (11) and the second separating funnel (31) are both provided with liquid adding ports. An adjustable speed motor (21) is installed on the liquid adding port of the first separating funnel (11). The outer shell of the adjustable speed motor (21) is detachably connected to the liquid adding port of the first separating funnel (11). A stirring paddle (23) is arranged inside the first separating funnel (11). The stirring paddle (23) is in transmission connection with the motor shaft of the adjustable speed motor (21) through an adjustable stirring rod (22); A rotatable lid (32) is provided on the liquid adding port of the second separating funnel (31). The rotatable lid (32) is detachably connected to the liquid adding port of the second separating funnel (31).

3. The liquid-liquid extraction-nitrogen blowing integrated extraction and purification device according to claim 2, characterized in that: A first switching valve (13) is provided at the liquid outlet of the first separating funnel (11). The first three-way control valve (41) and the first switching valve (13) are connected through a first polytetrafluoroethylene tube (12); A second switching valve (33) is provided at the liquid outlet of the second separating funnel (31). The second three-way control valve (43) and the second switching valve (33) are connected through a third polytetrafluoroethylene tube (34).

4. The liquid-liquid extraction-nitrogen blowing integrated extraction and purification device according to claim 3, characterized in that: The first separating funnel (11) is fixedly connected through a first adjustable fixing clip (7) and a first fixing frame (8) to adjust the height of the first separating funnel (11). The second separating funnel (31) is fixedly connected through a second adjustable fixing clip (10) and a second fixing frame (9) to adjust the height of the second separating funnel (31).

5. The liquid-liquid extraction-nitrogen blowing integrated extraction and purification device according to claim 4, characterized in that: A nitrogen blowing tube inlet needle (135) is provided with a nitrogen blowing tube fixing buckle (134) for fixing and clamping the nitrogen blowing tube inlet needle (135) on the tube wall of a nitrogen blowing concentration tube (17).

6. The liquid-liquid extraction-nitrogen blowing integrated extraction and purification device according to claim 5, characterized in that: A nitrogen blowing needle (19) is arranged in the nitrogen blowing concentration tube (17) for blowing nitrogen into the nitrogen blowing concentration tube (17).

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