Extraction unit for extraction column, combined extraction column and extraction method

Abstract

The present invention discloses an extraction unit, a combined extraction column and an extraction method for an extraction column, and belongs to the field of extraction technology. The combined extraction column of the present invention is composed of a plurality of extraction units connected in series. The extraction unit includes a shell, a filtering mechanism, a solid adsorbent, a stirring mechanism, etc.; the shell includes an intra-tube channel, a liquid inlet and a liquid outlet; the solid adsorbent is arranged in the shell, and the solid adsorbent occupies 1-95% of the volume of the shell; the filtering mechanism blocks the solid adsorbent so that the solid adsorbent is retained in the shell; the stirring mechanism is arranged in the shell for stirring the solid adsorbent. The present invention achieves the function of stirring and extracting in the extraction column by splitting the extraction column into a plurality of extraction units, and then leaving a movable space for the solid adsorbent in each extraction unit and adding a stirring mechanism. In the actual extraction process, the adsorbent and the extracted liquid form an extraction system of a suspension, thereby achieving the effect of rapid extraction.

Description

Technical Field

[0001] The invention belongs to the field of extraction technology or synthetic ester purification, and particularly relates to an extraction unit for an extraction column, a combined extraction column and an extraction method. Background Art

[0002] In the production of synthetic esters, such as ININ (isononyl isononanoate), water washing or alkali washing is usually used to remove the impurity acid (formic acid, acetic acid and other organic acids) or salts in the product. The alkali washing or water washing process will waste a lot of water resources and a lot of time waiting for the emulsion layer to break.

[0003] Solid adsorbents can save water resources, but they are not suitable for industrial adsorption and acid removal production. Currently, one way to use solid adsorbents for extraction is chromatography columns, which are formed by filling solid adsorbents to form chromatography columns for extraction. The solid adsorbent is in a compacted state. Especially when the viscosity of the organic product is high, the flow rate of the mobile phase in the chromatography column will be low, the efficiency is slow, and it is not easy to replace the solid adsorbent, making the extraction column unsuitable for industrial production. Another way to use solid adsorbents for extraction is to directly mix the solid adsorbent with the extract, stir it for adsorption, and then filter and separate it; when ordinary solid adsorbents are mixed and stirred with the extract for extraction, they do not have the plate effect of the chromatography column, resulting in a low adsorption efficiency.

[0004] On the other hand, the current single-tube chromatography columns are only suitable for using a single type of adsorbent filler. When multiple adsorbents are used to form multi-layer chromatography, the solid adsorbents in each layer are in direct contact, which is not conducive to the recovery of the solid adsorbent.

[0005] Therefore, it is particularly important to provide an extraction column that can achieve continuous extraction and can save solvent, improve extraction production efficiency, and facilitate replacement and recovery of solid adsorbents. Summary of the invention

[0006] The present invention aims to solve the technical problems existing in the prior art. To this end, the present invention proposes an extraction unit for an extraction column, wherein a plurality of extraction units can be sequentially connected in series to form an integral combined extraction column, the extraction column can save solvent, improve extraction production efficiency, facilitate replacement and recovery of solid adsorbents, and can be used for industrial extraction production.

[0007] The inventive concept of the present invention is as follows: by splitting the extraction column into multiple extraction units, the length of the extraction column, the types of solid adsorbents, and the number of adsorbents in each extraction unit can be flexibly combined according to actual production needs; at the same time, the connection between the various extraction units can simulate the plate effect of the chromatography column to ensure the extraction and adsorption efficiency; leaving room for movement for the solid adsorbent in each extraction unit and adding a stirring mechanism, so that during extraction, the solid adsorbent and the extracted liquid are mixed to form a suspension system, and the suspension extraction and adsorption system is conducive to the flow of the extracted liquid, thereby achieving a rapid extraction effect.

[0008] The plate effect mentioned in the present invention can be understood as follows: one extraction unit is equivalent to one theoretical plate in a chromatography column, and adsorption-desorption rapidly reaches equilibrium in each theoretical plate.

[0009] The main purpose of the present invention is to provide an extraction unit for an extraction column. The extraction unit comprises a housing, a filtering mechanism, a solid adsorbent and a connecting mechanism; wherein:

[0010] The shell comprises an inner tube channel, and a liquid inlet and a liquid outlet respectively located at two ends of the inner tube channel;

[0011] The filtering mechanism is arranged in the inner tube channel of the shell, and the filtering mechanism is close to the liquid outlet end, and the filtering mechanism is used to filter the extracted liquid and block the solid adsorbent so that the solid adsorbent is retained in the inner tube channel of the shell;

[0012] The solid adsorbent is arranged in the tube channel of the shell and laid on the filtering mechanism, and the volume occupied by the solid adsorbent is smaller than the volume of the tube channel of the shell; the solid adsorbent is used to adsorb impurities in the extracted liquid; preferably, the solid adsorbent is at least one of an inorganic solid adsorbent or an organic solid adsorbent; the inorganic solid adsorbent includes at least one of activated carbon, kaolin, alumina, zeolite, and silica gel, and the organic solid adsorbent includes at least one of adsorption resin, protein, polysaccharide, chitin, glucose, and animal and plant fiber.

[0013] The connecting mechanism is used to connect the two extraction units into a whole;

[0014] In addition, a stirring mechanism is provided in the inner channel of the shell, and the stirring mechanism is used to stir the solid adsorbent. Stirring the solid adsorbent can mix the solid adsorbent with the extracted liquid to form a suspension. The extraction adsorption system of the suspension is conducive to the flow of the extracted liquid, thereby achieving a rapid extraction effect.

[0015] Furthermore, the present invention also includes a receiving plate, which is arranged below the filtering mechanism, and is fixedly connected to the shell for supporting the filtering mechanism; the receiving plate is provided with a through hole for the extracted liquid to flow through.

[0016] Compared with the prior art, the present invention can flexibly combine the length of the extraction column, the type of solid adsorbent, and the number of solid adsorbents in each extraction unit according to actual production needs by splitting the extraction column into multiple extraction units; at the same time, each extraction unit is independent of each other, so it can simulate the plate effect of the chromatography column to ensure the extraction and adsorption efficiency; leave room for the solid adsorbent in each extraction unit to move, and cooperate with the stirring mechanism to form a suspension system during extraction. The suspension extraction and adsorption system is conducive to the flow of the extracted liquid, achieving the effect of rapid extraction. The solid adsorbents between the extraction units are separated by a filtering mechanism, which facilitates the replacement and recovery of the solid adsorbents.

[0017] Further, the connecting mechanism includes a first connecting mechanism and / or a second connecting mechanism, the first connecting mechanism is at least one of a threaded structure, a nested structure, and a slot structure arranged on the shell wall of the liquid inlet and the liquid outlet of the shell, and the first connecting mechanism realizes the docking of two adjacent extraction units; the second connecting mechanism is a connecting shaft that passes through the filtering mechanism and is stably mounted on the central axis position of the shell, the connecting shaft is a hollow tube or a solid rod, and the upper and lower ends of the connecting shaft have matching connecting parts, and the upper and lower extraction units are connected to each other as a whole through the connecting parts of their respective connecting shafts; preferably, the connecting parts are adapter nuts and adapter threads respectively located at both ends of the connecting shaft. In a preferred embodiment, the connecting shaft is fixedly arranged on the receiving plate or the filtering mechanism, and in another preferred embodiment, the connecting shaft is relatively rotatably connected to the receiving plate or the filtering mechanism through a bearing or a bushing.

[0018] The number of extraction units in a complete extraction column determines the length of the extraction column, and the solid adsorbent in different extraction units can be freely selected according to the purpose of extraction. The extraction units are connected in an end-to-end arrangement. The end-to-end connection can be understood as that the liquid outlet of the extraction unit at the upper position and the liquid inlet at the lower position are butt-sealed, and the connection between the upper and lower butt-jointed extraction units is achieved through a connecting mechanism. As mentioned above, the connecting mechanism can be a threaded structure, a nested structure, a slot structure separately arranged on the liquid outlet or the liquid inlet, or it can be achieved through a connecting shaft. For greater stability, the extraction unit can have both connecting mechanisms.

[0019] Preferably, the extraction unit further comprises a pressurizing mechanism, which is used to inflate the space between the liquid inlet and the filtering mechanism during the extraction process so that the space forms a high-pressure environment. The pressurizing mechanism is arranged on the liquid inlet and / or the shell; further preferably, the pressurizing mechanism comprises at least one of a pressurizing air valve and a pressurizing pump. Preferably, in a stirring scheme using a mechanical stirring structure, in order to reduce the driving load of the driving mechanism, the air outlet of the pressurizing air valve or the pressurizing pump is aligned with the stirring blade, so that the gas ejected from the pressurizing air valve or the pressurizing pump drives the stirring blade to rotate. Correspondingly, in order to prevent the pressurizing mechanism from continuously ejecting air so that the air pressure in the shell is too high, a pressure relief valve can also be arranged on the shell.

[0020] Preferably, the stirring mechanism is a gas stirring structure or a magnetic stirrer; in this case, the selection of the connection mechanism in the extraction unit can be arbitrary, and it is only necessary to ensure that the shells of the upper and lower connected extraction units are docked and sealed. Preferably, the gas stirring mechanism includes an air pump and an air outlet pipe connected to the air outlet of the air pump, and the air outlet end of the air outlet pipe is buried in the solid adsorbent, and the solid adsorbent is stirred by blowing.

[0021] Furthermore, the stirring mechanism is preferably a mechanical stirring structure; a preferred solution may be that the mechanical stirring structure includes stirring blades. In this case, the connection structure of the present invention may preferably be in the form of a connecting shaft, so that the stirring blades may be fixedly mounted on the connecting shaft, or may be rotatably mounted on the connecting shaft. The movement of the stirring blades may be driven in different ways for different connection methods. If the stirring blades are connected to the connecting shaft by rotatable mounting, the stirring blades may be rotated by blowing air or by direct driving of an additional driving mechanism; if the stirring blades are fixedly connected to the connecting shaft, they may be driven by adding a driving motor, and the driving shaft of the driving motor drives the movement of the connecting shaft and then drives the movement of the stirring blades. At this time, the connection between the connecting shaft and the receiving plate may be connected by a bearing or a sleeve to achieve the connection stability between the connecting shaft and the receiving plate. The advantage of using a motor drive shaft to drive the connecting shaft and then drive the stirring blades to move is that, because each extraction unit is provided with a connecting shaft, and when multiple extraction units are combined into an extraction column, the connecting shafts of all extraction units are connected end to end, so the additional driving mechanism drives the connecting shaft of the extraction unit at the top to move, which can drive the connecting shafts of all extraction units to move, thereby driving the stirring blades in all extraction units to move. The driving mechanism is a rotating motor or a telescopic motor, and the driving shaft of the driving mechanism is connected to the connecting part of the connecting shaft of the extraction unit at the top, so that the driving shaft drives the stirring blades to move, and the movement is rotation or up and down reciprocating motion, which can realize the stirring function. Among them, the rotating motor drives the rotation of the connecting shaft and then drives the stirring blades to rotate to stir the solid adsorbent, and at this time, the connection between the connecting shaft and the carrier plate can be a bearing connection; and the driving shaft of the telescopic motor can also drive the connecting shaft to reciprocate up and down and then drive the stirring blades to move up and down to stir the solid adsorbent, and at this time, the connection between the connecting shaft and the carrier plate can be a sleeve connection. In the present invention, the stirring blades can be in various shapes, such as common blade type, rod type, two-blade paddle type, three-blade paddle type, spiral type, frame type, turbine type, etc. In addition to the additional drive mechanism driving the rotating blades, it has been mentioned above that the rotation of the rotating blades can be driven by the airflow blown by the pressurizing mechanism. Therefore, the rotation of the rotating blades can also be achieved by the airflow of the pressurizing mechanism alone. At this time, the pressurizing mechanism provides a high-pressure environment in the shell and drives the rotating blades at the same time, killing two birds with one stone.

[0022] In the present invention, the number of extraction units in an extraction column can be selected according to specific production needs. When facing organic products with more impurities, more extraction units can be connected in series to improve the extraction and adsorption effect. When facing organic products with fewer impurities, fewer extraction units can be connected in series to reduce the consumption of solid adsorbents and improve the corresponding extraction efficiency.

[0023] For example, for the extraction of organic products with more impurities, the number of extraction units of an extraction column can reach 20 to 50 or more, or even more than 100; and for the extraction of organic products with fewer impurities, the number of extraction units of an extraction column can be 10 to 20 or less, or even less than 3.

[0024] Preferably, the shell of the extraction unit is in the shape of a cylindrical tube, and the top and bottom surfaces of the cylindrical tube are the liquid inlet and liquid outlet, respectively. Further preferably, the cylindrical tube is a cylindrical tube, and more preferably, the diameters of any cross sections of the cylindrical tube are equal.

[0025] Preferably, the cylindrical tube of the shell of the extraction unit is composed of two semi-cylindrical pieces, and the joint of the two semi-cylindrical pieces has corresponding hinge structures and / or snap structures to lock the two semi-cylindrical pieces. In addition, preferably, a sealing gasket is provided at the joint of the two semi-cylindrical pieces to achieve sealing.

[0026] The bearing plate is an annular baffle plate provided at the end near the liquid outlet in the inner tube channel of the shell or on the liquid outlet of the shell. Correspondingly, the outer edge of the annular baffle plate is fixedly connected to the inner wall of the inner tube channel of the shell or the outer edge of the annular baffle plate is fixedly connected to the peripheral edge of the liquid outlet of the shell. Generally speaking, the annular baffle plate is a circular ring baffle plate. Preferably, the bearing plate is perpendicular to the central axis of the shell.

[0027] Preferably, the filter mechanism is arranged at the end of the tube channel of the shell near the liquid outlet. Specifically, the outer edge of the filter mechanism is in contact with or connected to the inner wall of the tube channel of the shell, or the outer edge of the filter mechanism is in contact with or connected to the peripheral edge of the liquid outlet.

[0028] Preferably, the pore size of the filtering mechanism in the present invention is smaller than the particle size of the solid adsorbent.

[0029] Preferably, the filtering mechanism includes at least one of a sand core filter plate, a sieve plate, a filter paper, a filter screen, a ceramic filter plate, and a cotton filter plate.

[0030] In the present invention, the types of solid adsorbents include at least one of inorganic solid adsorbents and organic solid adsorbents; wherein, the inorganic solid adsorbents include at least one of activated carbon, kaolin, alumina, zeolite, and silica gel, and the organic solid adsorbents include at least one of adsorption resins, proteins, polysaccharides, chitin, glucose, and animal and plant fibers. Technicians can select the type of solid adsorbent in each extraction unit according to specific production needs to achieve the purpose of adsorbing different impurities, such as adding an extraction unit with activated carbon to achieve the purpose of adsorbing impurities such as pigments and heavy metals. At the same time, different types of solid adsorbents and different amounts of solid adsorbents added can be selected in different extraction units in an extraction column to meet actual production needs.

[0031] In the present invention, technicians can select the mesh size of each solid adsorbent in different extraction units according to specific production needs. Preferably, the mesh size of the solid adsorbent is 10-5000 mesh; more preferably, the mesh size of the solid adsorbent is 30-500 mesh. The selection of the mesh size depends not only on the adsorption effect, but also on the stirring difficulty of the stirring mechanism. The larger the mesh size, the greater the stirring difficulty.

[0032] The volume occupied by the solid adsorbent should be smaller than the volume of the space formed by the shell and the filter mechanism. The amount of solid adsorbent added should not only take into account the adsorption effect, but also the difficulty of stirring by the stirring mechanism. Preferably, the volume occupied by the solid adsorbent is 1-95% of the volume of the space formed by the shell and the filter mechanism.

[0033] Preferably, in the present invention, the extraction column composed of a plurality of extraction units further includes a liquid collecting funnel, which is located on the liquid outlet of the shell of the lowest extraction unit and is used to collect the extracted liquid. Furthermore, the upper end of the liquid collecting funnel is connected to the liquid outlet of the shell of the lowest extraction unit to form a seal. At this time, the liquid collecting funnel is also connected to a decompression mechanism, which is used to evacuate the liquid collecting funnel to form a low-pressure environment in the liquid collecting funnel. Specifically, the decompression mechanism can be arranged at least at one place on the liquid outlet or the wall of the liquid collecting funnel. The decompression mechanism includes at least one of a decompression valve and a vacuum pump.

[0034] The method for extracting using the combined extraction column of the present invention comprises the following steps:

[0035] The same or different solid adsorbents are added to different extraction units respectively, and multiple extraction units are connected in series to form an extraction column, and a liquid collecting funnel is connected to the bottom of the extraction column;

[0036] The extracted liquid is added from the liquid inlet of the uppermost extraction unit, and the sealing cover of the first extraction unit is closed;

[0037] Turn on the stirring mechanism, the pressurizing mechanism and the decompressing mechanism;

[0038] The extracted liquid flows out from the liquid collecting funnel after multi-stage extraction and is recovered.

[0039] Preferably, the mass ratio of the total amount of the solid adsorbent to the extracted liquid is (0.1-1000):100, more preferably (1-100):100; further preferably (1-50):100, and further preferably (1-20):100.

[0040] Preferably, the number of extraction units in a combined extraction column is greater than 2, and the mass of the solid adsorbent in one extraction unit is 0.1%-80% of the total mass of the solid adsorbent; more preferably 1%-50%; and even more preferably 5%-50%.

[0041] Preferably, the mass of the solid adsorbent used in the extraction unit is greater than the mass of the solid adsorbent used in the next extraction unit.

[0042] Preferably, before the extraction of the extracted liquid begins, the pressurizing mechanism and / or the decompressing mechanism are started to set the air pressure of each extraction unit and the air pressure at the liquid collecting funnel from top to bottom, and the air pressure in all extraction units is greater than the air pressure in the liquid collecting funnel, and the air pressure in the previous extraction unit is greater than the air pressure in the next extraction unit. For example, in an extraction column composed of 5 extraction units, the air pressures in the 5 extraction units and the liquid collecting funnel are P1, P2, P3, P4, P5, and P6, respectively, and the air pressure relationship is: P1>P2>P3>P4>P5>P6.

[0043] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0044] (1) The connection of each extraction unit can simulate the plate effect of the chromatography column to ensure the extraction and adsorption efficiency;

[0045] (2) The length of the extraction column, the type and mesh size of the solid adsorbent, and the number of solid adsorbents in each extraction unit can be flexibly combined according to actual production needs;

[0046] (3) A space for movement is left for the solid adsorbent in each extraction unit and a stirring mechanism is added, so that the solid adsorbent forms a suspension system during extraction. The suspension extraction adsorption system is conducive to the flow of the extracted liquid, thereby achieving a rapid extraction effect.

[0047] Under the condition of the same ratio of solid adsorbent to extracted liquid, using the combined extraction column of the present invention, it only takes 25 minutes to reduce the acid value of 100g of ININ (isononyl isononanoate) organic product from 0.4087mgKOH / g to 0.0198mgKOH / g; and after the solid adsorbent and the extracted liquid were mixed and stirred for 150 minutes, the acid value of the ININ organic product only decreased from 0.4025mgKOH / g to 0.02971mgKOH / g. BRIEF DESCRIPTION OF THE DRAWINGS

[0048] Figure 1 Schematic diagram of the extraction column of Example 1;

[0049] Figure 2 This is a schematic cross-sectional view of the extraction column at the pressurized gas valve of Example 1;

[0050] Reference numerals:

[0051] Shell 100 , annular partition plate 110 , sand core filter plate 200 , alumina powder 300 , rotating stirring blade 400 , round rod 510 , adapter nut 520 , pressurizing air valve 601 , decompressing air valve 602 , and liquid collecting funnel 700 . DETAILED DESCRIPTION

[0052] In order to make the technical scheme of the present invention more clearly understood by those skilled in the art, the following embodiments are listed for illustration. It should be pointed out that the following embodiments do not limit the protection scope of the present invention.

[0053] Unless otherwise specified, the raw materials, reagents or devices used in the following examples can be obtained from conventional commercial sources or by existing known methods.

[0054] In the present invention, the extracted liquid used is: isononanoic acid and isononanol are reacted at a molar ratio of 1:1, and the catalyst is sodium bisulfate and activated carbon. The acid value of the organic product ININ (isononyl isononanoate) is between 0.429-0.3904 mgKOH / g after 12 hours of reaction. The solid adsorbent is alumina powder (Al2O3) (100-200 mesh), and the qualified index of extraction is that the acid value of the ININ organic product is less than 0.03 mgKOH / g.

[0055] Example 1

[0056] like Figure 1 A combined extraction column is shown, and the extraction column includes the following structure:

[0057] 5 extraction units and a liquid collecting funnel 700, in which a pressure reducing air valve 602 is installed, each extraction unit comprises: a cylindrical shell 100 (tube diameter 8cm), a sand core filter plate 200 (filtering mechanism), alumina powder 300 (solid adsorbent), a rotating stirring blade 400 (stirring mechanism), a connecting mechanism composed of a round rod 510 (connecting shaft) and a transfer nut 520, and a pressurizing air valve 601. A circular partition 110 is fixedly provided inside the inner channel of the cylindrical shell 100 near the liquid outlet; Figure 2 The cross-sectional view of the extraction column of Example 1 at the pressurized air valve 601 is shown. The pressurized air valve 601 is disposed on the cylindrical housing 100. The air outlet of the pressurized air valve 601 faces the upper half of the rotating stirring blade 400. The rotating stirring blade 400 can rotate around the round rod 510. The cylindrical housing 100 is a cylindrical glass tube. The cylindrical housing 100 has an inner tube channel, a liquid inlet and a liquid outlet. The housing 100 at the liquid inlet and the liquid outlet has mutually docking grooves to ensure docking of the upper and lower extraction units. An annular partition 110 is connected to the inner bottom surface of the cylindrical shell 100 around the liquid outlet, and the annular partition 110 is used to support the sand core filter plate 200 to prevent the sand core filter plate 200 from falling; the sand core filter plate 200 is circular and is placed on the annular partition 110. The diameter of the sand core filter plate 200 is larger than the inner ring diameter of the annular partition 110. The sand core filter plate 200 blocks the alumina powder 300, so that the alumina powder 300 is retained in the shell 100; the round rod 510 vertically passes through the center of the sand core filter plate 200 and is connected to the sand core filter plate 200. There are adapter threads at both ends of the round rod 510, which can be connected to the round rod 510 of the next extraction unit through the adapter nut 520; the rotating stirring blade 400 is set on the round rod 510, which is used to stir the alumina powder 300;

[0058] The pressurizing air valve 601 is arranged on the shell 100, and the gas outlet of the pressurizing air valve 601 is aligned with the blades of the upper half of the rotating stirring blade 400, and is connected to the pressurizing air pump, so that the shell can be pressurized, and the gas ejected from the pressurizing air valve 601 can drive the rotating stirring blade 400 to rotate around the round rod 510 (in order to control the air pressure in the shell 100 in this scheme, a pressure gauge and a pressure relief valve are synchronously equipped, which are not shown in the figure); the decompression air valve 602 is arranged on the liquid collecting funnel 700, and is used to decompress the liquid collecting funnel 700; the five extraction units are connected by a card slot The aluminum oxide powder 300 is arranged and connected from top to bottom; the aluminum oxide powder 300 is arranged in the shell 100, and from top to bottom, the mass ratios of the aluminum oxide powder 300 to the extracted liquid in each extraction unit are 0.6:100, 0.5:100, 0.4:100, 0.3:100, and 0.2:100, respectively, and the particle size (100-200 mesh) is smaller than the pore size (20-30μm) of the sand core filter plate 200. From top to bottom, the extraction units are named the first extraction unit, the second extraction unit, the third extraction unit, the fourth extraction unit, and the fifth extraction unit, respectively.

[0059] In addition to the extraction column, it is also equipped with: a sealing cover for sealing the liquid inlet of the shell 100 of the extraction unit at the uppermost end of the extraction column, a pressurizing air pump connected to the pressurizing air valve 601, a decompression air pump connected to the decompression air valve 602, and a liquid collecting bottle connected to the liquid collecting funnel 700. The combination of the liquid collecting bottle, the liquid collecting funnel 700, the decompression air valve 602 and the decompression air pump can form a decompression filtration operation with the extraction unit connected to the liquid collecting funnel 700.

[0060] The extraction method comprises the following steps:

[0061] (1) Add 100 g of the extracted liquid ININ from the liquid inlet and cover with a sealing cap;

[0062] (2) Start the pressurizing air valve and the decompressing air pump, and set the air pressure of each extraction unit and the air pressure at the liquid collecting funnel to P1, P2, P3, P4, P5, and P6 from top to bottom, respectively, so that P1>P2>P3>P4>P5>P6; at the same time, the gas ejected from the pressurizing air valve drives the rotating stirring blade to rotate, stirring so that the alumina powder and the extracted liquid form a suspension system; the air pressure data in each extraction unit can be controlled in real time by the matching pressure gauge and pressure relief valve. For example, in an actual production batch, P1 can be controlled at about 1.45MPa, P2 at about 1.4MPa, P3 at about 1.35MPa, P4=about 1.3MPa, P5 at about 1.2MPa, and P6 at about 0.6MPa.

[0063] (3) Recover the extracted liquid from the collecting funnel.

[0064] It took 25 minutes from starting the air pump to completing the extraction.

[0065] The acid values ​​of the extracted liquid before and after extraction in each extraction unit were measured and recorded in Table 1 from top to bottom. The extraction units from top to bottom were named the first extraction unit, the second extraction unit, the third extraction unit, the fourth extraction unit, and the fifth extraction unit.

[0066] This embodiment shows an example of using less solid adsorbent. Those skilled in the art can add or further reduce the amount of adsorbent according to actual production needs. According to common sense, the larger the ratio of adsorbent to extracted liquid, the better the adsorption effect, the better the extraction effect, and the corresponding extraction time will be slightly longer.

[0067] In a normal chromatography column, the adsorbent filler is in a compacted state. Especially when the viscosity of the organic product is high, the flow rate of the mobile phase in the chromatography column will be low. During ordinary mixed stirring extraction, the pedal effect of the chromatography column will be destroyed, resulting in a small adsorption effect. Therefore, the present invention simulates the plate effect of the chromatography column by arranging multiple extraction units in the extraction column, and at the same time forms a suspension extraction system in each extraction unit to achieve a rapid extraction effect.

[0068] Another advantage of the present invention is that the number of extraction units, the number and type of adsorbents in each extraction unit can be flexibly combined to suit actual industrial production; for example, if a batch of ININ organic products produced has a low acid value, such as 0.164 mgKOH / g, then those skilled in the art can directly disassemble the first extraction unit and the second extraction unit to save the use of adsorbents; for example, an extraction unit with an activated carbon adsorbent can be added to the extraction column in Example 1 to achieve the purpose of adsorbing other impurities such as pigments.

[0069] It should be noted that, for the case where the diameter of the extraction column is less than 10 cm, the stirring method of Example 1 can be used, that is, the stirring blades can be rotated by blowing air through the pressure mechanism. However, if the diameter of the extraction column is larger, such as reaching 15-20 cm, the airflow of the pressure mechanism will be difficult to push the stirring blades. At this time, the stirring blades need to be equipped with an additional motor to drive the stirring blades to move and achieve the stirring of the solid adsorbent. The motor-driven method also has great advantages. For example, since the connecting shafts of the extraction units are interconnected, and the connecting shafts are connected to the receiving plate through bearings or sleeves, the mobility of the connecting shafts is ensured. The driving shaft of the motor can drive the top connecting shaft to move. Therefore, one motor can easily complete the control of the stirring blades of all extraction units.

[0070] Comparative Example 1

[0071] The difference between this comparative example 1 and the embodiment 1 is that each extraction unit of the extraction column of the comparative example 1 does not have a rotating stirring blade, and the rest of the structure is the same as the extraction method. (No stirring)

[0072] It took 25 minutes from starting the air pump to completing the extraction.

[0073] The acid values ​​of the extracted liquid before and after extraction in each extraction unit were measured from top to bottom and recorded in Table 1.

[0074] Comparative Example 2

[0075] The difference between Comparative Example 2 and Example 1 is that the extraction column of Comparative Example 2 has only three extraction units, and from top to bottom, the mass ratio of alumina powder to the extracted liquid in each extraction unit is 1:100, 0.7:100, and 0.3:100, respectively. (less grading)

[0076] It took 15 minutes from starting the air pump to completing the extraction.

[0077] From top to bottom, the extraction units are named the first extraction unit, the second extraction unit, and the third extraction unit, respectively. The acid values ​​of the extracted liquid before and after extraction in each extraction unit are measured and recorded in Table 1.

[0078] From the results of Comparative Example 2, it can be seen that although three extraction units are set in the extraction column, the extracted liquid obtained by extraction with the same mass (2g) of alumina powder still does not meet the passing index, and the plate effect of the chromatography column is not obvious enough.

[0079] Comparative Example 3

[0080] The difference between this comparative example 3 and comparative example 2 is that each extraction unit of the extraction column of comparative example 2 does not have a rotating stirring plate, and the remaining extraction devices and extraction methods are the same. (No stirring)

[0081] It took 15 minutes from starting the air pump to completing the extraction.

[0082] From top to bottom, the extraction units are named the first extraction unit, the second extraction unit, and the third extraction unit, respectively. The acid values ​​of the extracted liquid before and after extraction in each extraction unit are measured and recorded in Table 1.

[0083] Comparative Example 4

[0084] The difference between Comparative Example 4 and Example 1 is that the extraction column of Comparative Example 4 has only one extraction unit, and the mass ratio of alumina powder to the extracted liquid is 2:100. (Ungraded)

[0085] It took 5 minutes from starting the air pump to completing the extraction.

[0086] The acid value of the extracted solution before and after extraction was measured and recorded in Table 1.

[0087] Comparative Example 5

[0088] In this comparative example 5, 2 g of the same (100-200 mesh) alumina powder as in Example 1 was spread evenly in a sand core funnel with a pore size of 20-30 μm, and 100 g of the extracted liquid was filtered under reduced pressure without stirring. The reduced pressure pump was the same as in Example 1.

[0089] It took 5 minutes from starting the air pump to completing the extraction.

[0090] The acid value of the extracted solution before and after extraction was measured and recorded in Table 1.

[0091] Comparative Example 6

[0092] The difference between Comparative Example 6 and Example 1 is that the extraction column of Comparative Example 6 has only 4 extraction units and each extraction unit has no rotating stirring blades. From top to bottom, the mass ratio of alumina powder to the extracted liquid in each extraction unit is 0.5:100, 0.5:100, 0.5:100, and 0.5:100, respectively. (less grading and no stirring)

[0093] It took 20 minutes from starting the air pump to completing the extraction.

[0094] The extraction units from top to bottom are named the first extraction unit, the second extraction unit, the third extraction unit, and the fourth extraction unit, respectively. The acid values ​​of the extracted liquid before and after extraction in each extraction unit are measured and recorded in Table 1.

[0095] Table 1 Acid value of the extracted liquid before and after extraction in each extraction unit

[0096]

[0097] Comparative Example 7

[0098] In this comparative example 7, 2 g (100-200 mesh) of alumina powder was mixed with 100 g of the extracted liquid, first stirred at room temperature for 150 min, then heated and stirred at 80°C for 60 min, and the acid value of the extracted liquid was measured at 30 min, 60 min, 90 min, 120 min, 150 min of stirring at room temperature and 60 min of heating and stirring, and recorded in Table 2.

[0099] Table 2 Changes in acid value after mixing alumina powder and extract

[0100] Acid value / (mgKOH / g) Acid value / (mgKOH / g) Initial acid value 0.4025 Stir at room temperature for 120 minutes 0.0303 Stir at room temperature for 30 minutes 0.0971 Stir at room temperature for 150 minutes 0.02971 Stir at room temperature for 60 minutes 0.03945 Heating and stirring for 60 minutes 0.0271 Stir at room temperature for 90 minutes 0.0353

[0101] Under the condition of the same ratio of adsorbent to extracted liquid, the extraction column of the present invention only needs 25 minutes to reduce the acid value of 100g of ININ organic product from 0.4087mgKOH / g to 0.0198mgKOH / g; and after the adsorbent and the extracted liquid were mixed and stirred for 150 minutes, the acid value of the ININ organic product only decreased from 0.4025mgKOH / g to 0.02971mgKOH / g, just reaching the passing level of the ININ organic product acid value of less than 0.03mgKOH / g.

[0102] The above description of the embodiments is to facilitate the understanding and application of the present invention by those skilled in the art. It is obvious that those skilled in the art can easily make various modifications to these embodiments and apply the general principles described herein to other embodiments without creative work. Therefore, the present invention is not limited to the embodiments herein, and improvements and modifications made to the present invention by those skilled in the art based on the disclosure of the present invention should be within the scope of protection of the present invention.

Claims

1. A combined extraction column, characterized in that: It comprises a plurality of extraction units, which are connected in series into a columnar structure through a connecting mechanism, and a liquid collecting funnel is provided on the liquid outlet of the shell of the extraction unit at the lowest end for collecting the extracted liquid; The extraction unit comprises a housing, a filtering mechanism, a solid adsorbent, and a connecting mechanism; wherein: The shell comprises an inner tube channel, and a liquid inlet and a liquid outlet respectively located at two ends of the inner tube channel; The filtering mechanism is arranged in the inner channel of the shell, and is used to filter the extracted liquid; The solid adsorbent is arranged in the inner channel of the shell and laid on the filtering mechanism; the solid adsorbent is used to adsorb impurities in the extracted liquid; the mesh number of the solid adsorbent is 30-500 mesh; The solid adsorbent is at least one of an inorganic solid adsorbent or an organic solid adsorbent; the inorganic solid adsorbent includes at least one of activated carbon, kaolin, alumina, zeolite, and silica gel; the organic solid adsorbent includes at least one of adsorption resin, protein, polysaccharide, chitin, glucose, and animal and plant fiber; The connecting mechanism is used to connect the two extraction units into a whole; A stirring mechanism is also provided in the inner tube channel of the shell, and the stirring mechanism is used to stir the solid adsorbent after the extract is added; The connecting mechanism includes a first connecting mechanism and / or a second connecting mechanism, wherein the first connecting mechanism is at least one of a threaded structure, a nested structure, and a slot structure provided on the shell wall of the liquid inlet and the liquid outlet of the shell, and the first connecting mechanism realizes the docking of two adjacent extraction units; the second connecting mechanism is a connecting shaft that passes through the filtering mechanism and is stably mounted at the central axis position of the shell, the connecting shaft is a hollow tube or a solid rod, and the upper end and the lower end of the connecting shaft have an adaptive connecting portion, and the two extraction units are connected to each other as a whole through the connecting portions of their respective connecting shafts; The extraction unit further comprises a pressurizing mechanism, and the pressurizing structure is used to inflate the space between the liquid inlet and the filtering mechanism during the extraction process so that the space forms a high-pressure environment.

2. A combined extraction column as claimed in claim 1, characterized in that: It also includes a receiving plate, which is arranged below the filter mechanism and fixedly connected to the shell for supporting the filter mechanism; the receiving plate is provided with a through hole for the extracted liquid to flow through.

3. A combined extraction column as claimed in claim 2, characterized in that: The receiving plate is an annular partition plate arranged at the end near the liquid outlet in the tube channel of the shell or on the liquid outlet of the shell. Correspondingly, the outer edge of the annular partition plate is fixedly connected to the inner wall of the tube channel of the shell or the outer edge of the annular partition plate is fixedly connected to the peripheral edge of the liquid outlet of the shell.

4. A combined extraction column as claimed in claim 1, characterized in that: The connecting part is a transfer nut and a transfer thread respectively located at two ends of the connecting shaft. The connecting shaft is fixed on the receiving plate or the filter mechanism or is relatively rotatably connected to the receiving plate or the filter mechanism through a bearing or a sleeve.

5. A combined extraction column as claimed in claim 1, characterized in that: The stirring mechanism is a gas stirring mechanism or a magnetic stirrer; wherein, the gas stirring mechanism comprises an air pump and an air outlet pipe connected to the air outlet of the air pump, the air outlet end of the air outlet pipe is buried in the solid adsorbent, and stirring of the solid adsorbent is achieved by blowing and bubbling.

6. A combined extraction column as claimed in claim 1, characterized in that: The stirring mechanism is a mechanical stirring structure, which includes stirring blades. The stirring blades are fixedly or movably mounted on the connecting shaft. The stirring blades are blown by a pressurizing mechanism or directly driven by an additional driving mechanism alone or by an additional driving mechanism to drive the connecting shaft, thereby driving the stirring blades to move with the connecting shaft.

7. A combined extraction column as claimed in claim 6, characterized in that: The stirring blade is rotated by the airflow from the blowing port of the pressurizing mechanism; or the stirring blade is driven to move by an additional driving mechanism to drive the connecting shaft, and the driving mechanism is a rotating motor or a telescopic motor, and the driving shaft of the rotating motor or the telescopic motor is connected to the connecting part of the connecting shaft of the uppermost extraction unit, and the driving shaft drives the stirring blade to move, and the movement is rotation or up and down reciprocating motion.

8. A combined extraction column as claimed in claim 1, characterized in that: The upper end of the liquid collecting funnel is sealed with the liquid outlet of the shell of the lowest extraction unit. The liquid collecting funnel is also connected to a decompression mechanism, which includes at least one of a decompression valve and a vacuum pump for vacuuming or exhausting the liquid collecting funnel.

9. A combined extraction column as claimed in claim 8, characterized in that: The upper end of the liquid collecting funnel is sealed with the liquid outlet of the shell of the lowest extraction unit. The liquid collecting funnel is also connected to a decompression mechanism, which includes at least one of a decompression valve and a vacuum pump for vacuuming or exhausting the liquid collecting funnel.

10. An extraction method, characterized in that: The combined extraction column according to any one of claims 1 to 9 is used to extract the extracted liquid.

Images