CN113082767A - Device and method for micro-fine extraction - Google Patents
Device and method for micro-fine extraction Download PDFInfo
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- CN113082767A CN113082767A CN202110321274.0A CN202110321274A CN113082767A CN 113082767 A CN113082767 A CN 113082767A CN 202110321274 A CN202110321274 A CN 202110321274A CN 113082767 A CN113082767 A CN 113082767A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0484—Controlling means
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Abstract
The invention relates to a device and a method for micro-fine extraction, the device comprising: an extraction pipe with an upper opening; manifold located at the side of and in communication with the extraction tubes: the end part of the manifold is also provided with micropores; a stirring component which can extend into the extraction tube; and the air pressure adjusting component can be arranged at the opening of the extraction pipe and used for adjusting the pressure condition in the extraction pipe. Compared with the prior art, the invention can realize micro fine liquid-liquid extraction, and has the advantages of simple operation, short separation time, high extraction efficiency, good use safety and the like.
Description
Technical Field
The invention belongs to the technical field of fine extraction, and relates to a device and a method for micro fine extraction.
Background
Extraction refers to the separation and purification of a substance by transferring the substance from one solvent to another solvent by utilizing the difference of solubility or partition coefficient of the substance in two solvents which are not soluble (or slightly soluble) or reactive with each other. The extracted substances enter the extractant through an interphase interface until the distribution of the components between the two phases is substantially balanced, and then the extracted substances are settled by standing and separated into two layers of liquid, namely an extraction liquid converted from the extractant and a raffinate liquid converted from the feed liquid. At present, most extraction devices are long in separation time and complicated in operation steps, and need more manual intervention, and if a separating funnel is used as the extraction separation device, raffinate often enters the extraction liquid carelessly, so that the whole extraction test is influenced. The tower-type extraction separation device has the advantages of complex structure, higher cost, higher energy consumption, lower efficiency and certain potential safety hazard.
Therefore, in order to solve the above-mentioned disadvantages of the prior art, it is necessary to design a micro fine extraction device with high safety, simplicity and high efficiency to meet the needs of different industries in production process.
Disclosure of Invention
The invention aims to provide a device and a method for micro-fine extraction, so as to realize micro-fine liquid-liquid extraction.
The purpose of the invention can be realized by the following technical scheme:
one of the technical schemes of the invention provides a device for micro-fine extraction, which comprises:
an extraction pipe with an upper opening;
manifold located at the side of and in communication with the extraction tubes: the end part of the manifold is also provided with micropores;
a stirring component which can extend into the extraction tube;
and the air pressure adjusting component can be arranged at the opening of the extraction pipe and used for adjusting the pressure condition in the extraction pipe.
Furthermore, the device also comprises a base and a clamping fixture which is arranged on the base and can rotate in a vertical plane, and the extraction tube is fixed on the clamping fixture and is driven by the clamping fixture to rotate.
Furthermore, the clamping fixture is rotatably connected with the base through a horizontal pin shaft, and a pitching adjusting knob which enables the clamping fixture to be locked with the base is further arranged on the horizontal pin shaft.
Furthermore, the air pressure adjusting assembly comprises an adjustable rubber air bag and a connecting pipe which is arranged on the rubber air bag and can be connected with the opening of the extraction pipe.
Furthermore, the air pressure adjusting assembly further comprises an adjusting frame with an inner cavity, the rubber air bag is arranged in the adjusting frame, the connecting pipe on the rubber air bag extends out of the adjusting frame, and an adjusting rod used for extruding the rubber air bag is further arranged on the adjusting frame.
More preferably, the adjusting rod is arranged on the adjusting frame in a threaded manner, one end of the adjusting rod extends into the adjusting frame and abuts against the rubber air bag, and the other end of the adjusting rod extends out of the adjusting frame and is provided with an adjusting button.
Further, the stirring subassembly include be connected and can stretch into with outside agitator the interior stirring rod of extraction tube still installs on the stirring rod and is used for sealing extraction tube upper portion open-ended rubber buffer.
Furthermore, the stirrer is an electric stirrer.
Furthermore, the length of the stirring rod extending into the extraction tube satisfies the following conditions: the stirring blade installed on the stirring rod is completely immersed in the mixed liquid in the extraction tube.
The second technical scheme of the invention provides a method for micro-fine extraction, which is implemented by adopting the device, and the method comprises the following steps:
(1) introducing a solution to be separated and an extracting agent into a vertically placed extraction pipe, and installing a stirring assembly to mix and stir uniformly;
(2) when the solution to be separated is fully mixed with the extracting agent, the stirring component is detached, and the air pressure adjusting component is installed;
(3) the air pressure in the extraction pipe is adjusted to be negative pressure through the air pressure adjusting assembly, and the angle of the extraction pipe is adjusted at the same time, so that the mixed solution in the extraction pipe flows into the manifold until the manifold is in a vertical state;
(4) after the mixed solution in the manifold is stood for settling and separated into two layers of liquid, the air pressure adjusting assembly is adjusted to change negative pressure into positive pressure in the extraction pipe, so that the layered liquid is pressed out of the manifold from the micropores, and micro-fine extraction is realized.
Compared with the prior art, the invention has the following advantages:
1) the disassembly and assembly are rapid, the operation is convenient, and the safety is good;
2) the pressure in the extraction pipe can be adjusted through the adjusting button, the speed is controlled, and the raffinate is prevented from entering the extraction liquid during liquid separation;
3) the extraction device has wide application range, can adjust the solvent, the pressure and the extraction time, can perform micro-continuous extraction, and obviously improves the extraction efficiency.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic representation of an extraction process;
the notation in the figure is:
1-manifold, 2-micropore, 3-stirring rod, 4-electric stirrer, 5-clamping fixture, 6-pitching adjusting knob, 7-base, 8-adjusting knob, 9-adjusting rod, 10-rubber air bag, 11-connecting pipe, 12-adjusting frame and 13-extracting pipe.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following embodiments or examples, functional components or structures that are not specifically described are all conventional components or structures that are adopted in the art to achieve the corresponding functions.
The apparatus for the fine micro-extraction will be described first.
In order to realize micro fine liquid-liquid extraction, the invention provides a device for micro fine extraction, the structure of which is shown in figure 1, and the device comprises:
an extraction pipe with an upper opening;
manifold 1 located at the side of and communicating with the extraction tubes: the end part of the manifold 1 is also provided with micropores 2;
a stirring component which can extend into the extraction tube;
and the air pressure adjusting component can be arranged at the opening of the extraction pipe and used for adjusting the pressure condition in the extraction pipe.
In some embodiments, referring to fig. 1 again, the apparatus further includes a base 7, and a holding fixture 5 disposed on the base 7 and capable of rotating in a vertical plane, wherein the extraction tube is fixed on the holding fixture 5 and is driven by the holding fixture 5 to rotate.
In a more specific embodiment, the clamping fixture 5 and the base 7 are rotatably connected through a horizontal pin, and a pitch adjusting knob 6 for locking the clamping fixture 5 and the base 7 is further arranged on the horizontal pin. Every single move adjust knob 6 here can adopt the screw form cover to establish on horizontal pin axle, when every single move adjust knob 6 was screwed up, namely made between centre gripping anchor clamps 5 and the base 7 relatively fixed, when every single move adjust knob 6 was unscrewed, the free rotation state that resumes promptly between centre gripping anchor clamps 5 and the base 7, at this moment, can be through making centre gripping anchor clamps 5 rotate around horizontal pin axle promptly to adjust the angle of placing of its fixed extraction tube of centre gripping.
In some embodiments, referring to fig. 1 again, the air pressure adjusting assembly includes an adjustable rubber air bag 10 and a connecting pipe 11 disposed on the rubber air bag 10 and capable of connecting with the opening of the extraction pipe, so that the air pressure in the extraction pipe can be adjusted by adjusting the degree of squeezing the rubber air bag 10, and the air pressure in the extraction pipe can complete the conversion process of positive pressure-negative pressure-positive pressure, thereby achieving micro fine liquid-liquid extraction.
In a more specific embodiment, the air pressure adjusting assembly further comprises an adjusting frame 12 having an inner cavity, the rubber air bag 10 is disposed in the adjusting frame 12, the connecting pipe 11 of the rubber air bag 10 extends out of the adjusting frame 12, and an adjusting rod 9 for pressing the rubber air bag 10 is further disposed on the adjusting frame 12. More preferably, the adjusting rod 9 is arranged on the adjusting frame 12 in a threaded manner, one end of the adjusting rod extends into the adjusting frame 12 and abuts against the rubber air bag 10, the other end of the adjusting rod extends out of the adjusting frame 12 and is provided with an adjusting button 8, and the adjusting button 8 can be arranged to conveniently adjust the length of the adjusting rod 9 screwed into the adjusting frame 12, so that the extrusion degree of the rubber air bag 10 can be adjusted.
In some embodiments, referring to fig. 1 again, the stirring assembly includes a stirring rod 3 connected to an external stirrer and extending into the extraction tube, and a rubber stopper is mounted on the stirring rod 3 for sealing the upper opening of the extraction tube.
In a more specific embodiment, the agitator is an electric agitator 4.
In a more specific embodiment, the length of the stirring rod 3 extending into the extraction tube is as follows: the stirring blade installed on the stirring rod 3 is completely immersed in the mixed liquid in the extraction tube.
Next, the method of the fine micro-extraction will be described.
In order to overcome the defects of the conventional extraction device, the invention provides the device and simultaneously discloses an operation method thereof to realize micro-fine extraction, and please refer to fig. 1 and 2, wherein the method comprises the following steps:
(1) introducing a solution to be separated and an extracting agent into a vertically placed extraction pipe, and installing a stirring assembly to mix and stir uniformly;
(2) when the solution to be separated is fully mixed with the extracting agent, the stirring component is detached, and the air pressure adjusting component is installed;
(3) the air pressure in the extraction pipe is adjusted to be negative pressure through the air pressure adjusting assembly, and the angle of the extraction pipe is adjusted at the same time, so that the mixed solution in the extraction pipe flows into the manifold 1 until the manifold 1 is in a vertical state, and at the moment, the mixed solution cannot flow out of the micropores 2 because the air pipe is in negative pressure;
(4) after the mixed solution in the manifold 1 is stood for settling and separated into two layers of liquid, the air pressure adjusting assembly is adjusted, so that negative pressure in the extraction pipe is changed into positive pressure, layered liquid is pressed out of the manifold 1 from the micropores 2, and micro fine extraction is realized.
The above embodiments will be described in detail with reference to specific examples.
Example 1:
in order to realize the micro fine liquid-liquid extraction, the present embodiment provides an apparatus for micro fine extraction, the structure of which is shown in fig. 1, and the apparatus comprises:
an extraction pipe with an upper opening;
manifold 1 located at the side of and communicating with the extraction tubes: the end part of the manifold 1 is also provided with micropores 2;
a stirring component which can extend into the extraction tube;
and the air pressure adjusting component can be arranged at the opening of the extraction pipe and used for adjusting the pressure condition in the extraction pipe.
Referring to fig. 1 again, the apparatus further includes a base 7, and a clamping fixture 5 disposed on the base 7 and capable of rotating in a vertical plane, wherein the extraction tube is fixed on the clamping fixture 5 and is driven by the clamping fixture 5 to rotate. The clamping fixture 5 is rotatably connected with the base 7 through a horizontal pin shaft, and a pitching adjusting knob 6 for locking the clamping fixture 5 and the base 7 is further arranged on the horizontal pin shaft. Every single move adjust knob 6 here can adopt the screw form cover to establish on horizontal pin axle, when every single move adjust knob 6 was screwed up, namely made between centre gripping anchor clamps 5 and the base 7 relatively fixed, when every single move adjust knob 6 was unscrewed, the free rotation state that resumes promptly between centre gripping anchor clamps 5 and the base 7, at this moment, can be through making centre gripping anchor clamps 5 rotate around horizontal pin axle promptly to adjust the angle of placing of its fixed extraction tube of centre gripping.
Referring to fig. 1 again, the air pressure adjusting assembly includes an adjustable rubber air bag 10 and a connecting pipe 11 disposed on the rubber air bag 10 and capable of connecting with the opening of the extraction tube, so that the air pressure in the extraction tube can be adjusted by adjusting the extrusion degree of the rubber air bag 10 and the volume of the rubber air bag 10, and the air pressure in the extraction tube can complete the conversion process of positive pressure-negative pressure-positive pressure, thereby realizing micro fine liquid-liquid extraction. The air pressure adjusting assembly further comprises an adjusting frame 12 with an inner cavity, the rubber air bag 10 is arranged in the adjusting frame 12, the connecting pipe 11 on the rubber air bag 10 extends out of the adjusting frame 12, and an adjusting rod 9 used for extruding the rubber air bag 10 is further arranged on the adjusting frame 12. More preferably, the adjusting rod 9 is arranged on the adjusting frame 12 in a threaded manner, one end of the adjusting rod extends into the adjusting frame 12 and abuts against the rubber air bag 10, the other end of the adjusting rod extends out of the adjusting frame 12 and is provided with an adjusting button 8, and the adjusting button 8 can be arranged to conveniently adjust the length of the adjusting rod 9 screwed into the adjusting frame 12, so that the extrusion degree of the rubber air bag 10 can be adjusted.
Referring to fig. 1 again, the stirring assembly includes a stirring rod 3 connected to an external electric stirrer 4 and extending into the extraction tube, a rubber stopper is further mounted on the stirring rod 3 for sealing the opening at the upper portion of the extraction tube, the rubber stopper is configured to ensure the stability of the stirring rod 3 during rotation, and the solution to be separated and the extractant in the extraction tube are fully mixed and intimately contacted under strong shearing force. After the material to be extracted reaches equilibrium distribution between the two phases, the stirring rod 3 is removed. The length of the stirring rod 3 extending into the extraction tube satisfies the following conditions: the stirring blade installed on the stirring rod 3 is completely immersed in the mixed liquid in the extraction tube.
Referring to fig. 1 and fig. 2 again, the method for realizing micro-scale and fine extraction by using the above device comprises the following steps:
(1) introducing a solution to be separated and an extracting agent into a vertically placed extraction pipe, and installing a stirring assembly to mix and stir uniformly;
(2) when the solution to be separated is fully mixed with the extracting agent, the stirring component is detached, and the air pressure adjusting component is installed;
(3) the air pressure in the extraction pipe is adjusted to be negative pressure through the air pressure adjusting assembly, and the angle of the extraction pipe is adjusted at the same time, so that the mixed solution in the extraction pipe flows into the manifold 1 until the manifold 1 is in a vertical state, and at the moment, the mixed solution cannot flow out of the micropores 2 because the air pipe is in negative pressure;
(4) after the mixed solution in the manifold 1 is stood for settling and separated into two layers of liquid, the air pressure adjusting assembly is adjusted, so that negative pressure in the extraction pipe is changed into positive pressure, layered liquid is extruded out of the manifold 1 from the micropores 2, trace fine extraction is realized, and at the moment, the speed of extruding layered liquid can be adjusted by adjusting the size of the positive pressure in the extraction pipe.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. An apparatus for micro-fine extraction, comprising:
an extraction pipe with an upper opening;
manifold located at the side of and in communication with the extraction tubes: the end part of the manifold is also provided with micropores;
a stirring component which can extend into the extraction tube;
and the air pressure adjusting component can be arranged at the opening of the extraction pipe and used for adjusting the pressure condition in the extraction pipe.
2. The apparatus of claim 1, further comprising a base, and a holding fixture disposed on the base and capable of rotating in a vertical plane, wherein the extraction tube is fixed on the holding fixture and driven by the holding fixture to rotate.
3. The apparatus of claim 2, wherein the holding fixture is rotatably connected to the base by a horizontal pin, and a pitch adjusting knob is further provided on the horizontal pin to lock the holding fixture to the base.
4. The apparatus of claim 1, wherein the air pressure adjusting assembly comprises an adjustable rubber bladder and a connecting tube disposed on the rubber bladder and connected to the opening of the extraction tube.
5. The apparatus of claim 4, wherein the air pressure adjusting assembly further comprises an adjusting frame having an inner cavity, the rubber bladder is disposed in the adjusting frame, the connecting tube of the rubber bladder extends out of the adjusting frame, and an adjusting rod for pressing the rubber bladder is disposed on the adjusting frame.
6. The apparatus as claimed in claim 5, wherein the adjusting rod is threaded on the adjusting frame, one end of the adjusting rod extends into the adjusting frame and abuts against the rubber air bag, and the other end of the adjusting rod extends out of the adjusting frame and is provided with an adjusting knob.
7. The apparatus as claimed in claim 1, wherein the stirring assembly comprises a stirring rod connected to an external stirrer and extending into the extraction tube, and a rubber stopper mounted on the stirring rod for sealing the upper opening of the extraction tube.
8. An apparatus for micro fine extraction as claimed in claim 7, wherein the agitator is an electric agitator.
9. An apparatus as claimed in claim 7, wherein the stirring rod extends into the extraction tube for a length of: the stirring blade installed on the stirring rod is completely immersed in the mixed liquid in the extraction tube.
10. A method for micro-fine extraction, carried out with a device according to any one of claims 1 to 9, characterized in that it comprises the following steps:
(1) introducing a solution to be separated and an extracting agent into a vertically placed extraction pipe, and installing a stirring assembly to mix and stir uniformly;
(2) when the solution to be separated is fully mixed with the extracting agent, the stirring component is detached, and the air pressure adjusting component is installed;
(3) the air pressure in the extraction pipe is adjusted to be negative pressure through the air pressure adjusting assembly, and the angle of the extraction pipe is adjusted at the same time, so that the mixed solution in the extraction pipe flows into the manifold until the manifold is in a vertical state;
(4) after the mixed solution in the manifold is stood for settling and separated into two layers of liquid, the air pressure adjusting assembly is adjusted to change negative pressure into positive pressure in the extraction pipe, so that the layered liquid is pressed out of the manifold from the micropores, and micro-fine extraction is realized.
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| CN202110321274.0A CN113082767B (en) | 2021-03-25 | 2021-03-25 | Device and method for micro-fine extraction |
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| CN202110321274.0A CN113082767B (en) | 2021-03-25 | 2021-03-25 | Device and method for micro-fine extraction |
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| CN113082767B CN113082767B (en) | 2022-11-25 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113499606A (en) * | 2021-07-23 | 2021-10-15 | 上海化工研究院有限公司 | Multi-connected reciprocating extrusion-discharge type micro-extraction-separation integrated device and use method thereof |
| CN113552279A (en) * | 2021-07-21 | 2021-10-26 | 常州民生环境检测有限公司 | Quick sample preparation equipment for ion chromatographic analysis test |
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| CN212262452U (en) * | 2020-05-29 | 2021-01-01 | 内蒙古伊利实业集团股份有限公司 | Saponification extraction container |
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2021
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2926557A1 (en) * | 1979-06-30 | 1981-01-22 | Heinz Ludwig | Laboratory extraction and separation flask - being flat bottomed conical flask with side branch for venting and with run=off cock attached on the top |
| JPH03148500A (en) * | 1989-07-21 | 1991-06-25 | Helena Lab Corp | Discharging device of contents from sealed vessel |
| CN2785678Y (en) * | 2005-02-03 | 2006-06-07 | 中国科学院新疆理化技术研究所 | Extraction and detachment device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113552279A (en) * | 2021-07-21 | 2021-10-26 | 常州民生环境检测有限公司 | Quick sample preparation equipment for ion chromatographic analysis test |
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| CN113082767B (en) | 2022-11-25 |
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