An adsorption extraction tower

Abstract

The utility model relates to the technical field of extraction towers, and proposes an adsorption extraction tower, including a tower body, wherein the top of the tower body has a light phase outlet and a heavy phase inlet, and the bottom of the tower body has a light phase inlet and a heavy phase outlet; a discharge bin, wherein the discharge bin is arranged at the bottom of the tower body, and the bottom of the discharge bin has a slag discharge port, and the cross-sectional area of ​​the discharge bin gradually decreases from close to far from the tower body, and an extraction chamber is formed between the tower body and the discharge bin; a rotating shaft, wherein the rotating shaft is rotatably arranged on the tower body and is located in the extraction chamber, and the light phase outlet, the heavy phase inlet, the light phase inlet, the heavy phase outlet and the slag discharge port are all connected to the extraction chamber; and a spiral scraper, wherein the spiral scraper is arranged on the rotating shaft and is located above the slag discharge port. Through the above technical scheme, the problem that the heavy phase liquid outlet of the adsorption extraction tower in the prior art may be blocked by settled solids is solved.

Description

Technical Field

[0001] The utility model relates to the technical field of extraction towers, and specifically relates to an adsorption-type extraction tower. Background Art

[0002] 2-chloro-5-chloromethylpyridine (CCMP) is a key intermediate of the new and highly effective pesticides imidacloprid and acetamiprid, and is also the most insecticidal part of this type of pesticide molecule. Currently, 2-chloro-2-chloromethyl-4-cyanobutyraldehyde and phosphorus oxychloride are used to produce dichloropentachloromethylpyridine by cyclization, and then hydrolyzed. The oil phase after hydrolysis is combined with toluene extracted from the hydrolyzed acid water, and dichloropentachloromethylpyridine is obtained by desolventization and distillation. During the process of toluene extraction and hydrolysis of acid water, the oil phase contains slag, and the residual dichloropentachloromethylpyridine in the acid water is high, and the yield is low. Therefore, an extraction tower is used to replace the traditional kettle reactor for water washing to improve efficiency and yield.

[0003] There are many types of extraction towers, among which the structure of the adsorption extraction tower is different from other traditional extraction towers. Traditional packed extraction towers or turntable extraction towers mainly rely on packing and turntables for liquid-liquid separation. In contrast, the adsorption extraction tower has extraction tower plates distributed inside. The extraction tower plates have the characteristics of optimizing the dispersion effect and improving the mass transfer process. At the same time, they can reduce the back-mixing rate in the extraction process and there is no need to increase the proportion of extraction solvent.

[0004] However, directly applying the adsorption extraction tower to the acid-water extraction step will have the following problems: the heavy phase outlet of the extraction tower may be blocked by settled solids, and the internal mixing effect of the adsorption extraction tower still needs to be improved. Utility Model Content

[0005] The utility model provides an adsorption type extraction tower, which solves the problem in the related art that the heavy phase liquid outlet of the adsorption type extraction tower may be blocked by settled solids.

[0006] The technical solution of the utility model is as follows:

[0007] An adsorption extraction tower, comprising:

[0008] A tower body, wherein the top of the tower body has a light phase outlet and a heavy phase inlet, and the bottom of the tower body has a light phase inlet and a heavy phase outlet;

[0009] A discharge bin, which is arranged at the bottom of the tower body, has a slag discharge port at the bottom of the discharge bin, and the cross-sectional area of ​​the discharge bin gradually decreases from close to the tower body to far away from the tower body, and an extraction chamber is formed between the tower body and the discharge bin;

[0010] A rotating shaft, the rotating shaft is rotatably arranged on the tower body and is located in the extraction chamber, the light phase outlet, the heavy phase inlet, the light phase inlet, the heavy phase outlet and the slag discharge port are all connected to the extraction chamber;

[0011] A spiral scraper is arranged on the rotating shaft and is located above the slag discharge port.

[0012] As a further technical solution, the discharge bin is V-shaped, the spiral scraper is located directly above the slag discharge port, and the spiral scraper abuts against the inner wall of the discharge bin.

[0013] As a further technical solution, the light phase outlet, the heavy phase inlet, the light phase inlet, the heavy phase outlet and the slag discharge port are arranged in sequence from the top to the bottom of the tower body.

[0014] As a further technical solution, it also includes a plurality of stirring units, wherein the plurality of stirring units are arranged on the rotating shaft, and the plurality of stirring units are arranged at intervals along the length direction of the rotating shaft, and the stirring units include:

[0015] A stirring horizontal plate and a stirring vertical plate, wherein the stirring horizontal plate and the stirring vertical plate are both arranged on the rotating shaft, and the stirring vertical plate is located directly above the stirring horizontal plate.

[0016] As a further technical solution, it also includes:

[0017] A vertical baffle and two transverse baffles, wherein the vertical baffle and the transverse baffle are both arranged on the inner wall of the tower body, the vertical baffles are arranged along the circumference of the vertical stirring plate, and the transverse stirring plate is located between the two transverse baffles.

[0018] As a further technical solution, it also includes:

[0019] Two fixed annular plates, both of which are arranged on the inner wall of the tower body, the fixed annular plates are located between the two transverse baffles, and the stirring transverse plate is located between the two fixed annular plates, and the minimum cross-sectional area of ​​the fixed annular plates is larger than the cross-sectional area of ​​the stirring transverse plate.

[0020] As a further technical solution, an adsorption device is also included, and the adsorption device is arranged on the inner wall of the tower body and located between two adjacent stirring units. The adsorption device includes:

[0021] A plurality of upward members and a plurality of downward members, wherein the upward members and the downward members are both arranged vertically;

[0022] A light phase adsorption layer, wherein the light phase adsorption layer is arranged on the top of the upward member;

[0023] A heavy phase adsorption layer is arranged at the bottom of the descending member.

[0024] As a further technical solution, there is a gap between the upper member and the lower member, and further comprising:

[0025] A sealing member is disposed in the gap.

[0026] The working principle and beneficial effects of the utility model are:

[0027] The utility model discloses a post-hydrolysis extraction process of dichloropentachloromethylpyridine, which comprises: extracting dichloropentachloromethylpyridine in hydrolysis acid water with toluene through a reaction kettle, and then removing solvent and distilling to obtain dichloropentachloromethylpyridine. However, the efficiency of using the reaction kettle still needs to be improved, so an extraction tower with a body reaction kettle is used, which greatly improves the water washing efficiency, can realize continuous operation, reduce labor and energy consumption, and can also reduce the slag in the oil phase and improve the yield. However, when a traditional extraction tower is used in the acid water extraction step, the heavy phase liquid outlet may be blocked by the settled solid, and the internal mixing effect of the adsorption extraction tower still needs to be improved. In order to solve the above problems, an adsorption extraction tower is provided.

[0028] During use, a normal tower body needs to have a light phase outlet, a heavy phase inlet, a light phase inlet and a heavy phase outlet. The four are arranged in sequence from the top to the bottom of the tower body. Working process: Before water washing, you need to prepare the materials, which are the acid water after hydrolysis and the toluene extracted from the desolvation. Turn on the light phase tank feed pump switch, and pump toluene to the light phase inlet of the extraction tower until the liquid level reaches the upper clarification section and submerges the heavy phase inlet. Stop pumping toluene, then start the extraction tower stirring, and turn on the heavy phase tank feed pump switch. Set the feed speed, start feeding from the heavy phase inlet, and start extraction in the effective section. When the acid water phase reaches the lower clarification section and there is an obvious interface, turn on the light phase tank feed pump to continuously pump toluene into the extraction chamber, set the feed speed, and start continuous extraction. When the system runs stably, take samples from the light phase outlet and the heavy phase outlet to detect the content of each component.

[0029] In order to deal with the solid slag produced during the extraction process, a discharge bin with a gradually decreasing cross-sectional area is installed at the bottom of the tower body. Unlike the traditional cylindrical discharge bin, it can better gather the solid slag, facilitate centralized treatment, and discharge it from the discharge port. At the same time, the power of the rotating shaft is used to drive the spiral scraper in the discharge bin to rotate, and the solid slag attached to the inner wall of the discharge bin is scraped off. The design of the spiral scraper, on the one hand, better fits the discharge bin with a changing cross-sectional area, and on the other hand, the continuous spiral form can ensure that the rotating shaft rotates one circle, so as to more comprehensively remove the solid slag on the inner wall of the discharge bin. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] The preferred implementation modes will be described below in a clear and understandable manner with reference to the accompanying drawings to further illustrate the above-mentioned characteristics, technical features, advantages and implementation methods of the present utility model.

[0031] Figure 1 This is a schematic diagram of the structure of an adsorption extraction tower in the utility model;

[0032] Figure 2 For this utility model Figure 1 Enlarged view of part A in the middle;

[0033] Figure 3 This is a schematic diagram of the structure of the stirring unit in the utility model;

[0034] Figure 4 This is a schematic diagram of the structure of the adsorption device in the utility model;

[0035] In the figure: 1. tower body, 101. light phase outlet, 102. heavy phase inlet, 103. light phase inlet, 104. heavy phase outlet, 105. extraction chamber, 2. discharge bin, 201. slag discharge port, 3. rotating shaft, 4. spiral scraper, 5. stirring unit, 501. stirring horizontal plate, 502. stirring vertical plate, 6. vertical baffle, 7. horizontal baffle, 8. fixed annular plate, 9. adsorption device, 901. upward member, 902. downward member, 903. light phase adsorption layer, 904. heavy phase adsorption layer, 10. sealing member. DETAILED DESCRIPTION

[0036] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the specific implementation methods of the utility model will be described below with reference to the accompanying drawings. Obviously, the accompanying drawings described below are only some embodiments of the utility model. For ordinary technicians in this field, other drawings and other implementation methods can be obtained based on these drawings without creative work.

[0037] In order to simplify the drawings, only the parts related to the utility model are schematically shown in each figure, and they do not represent the actual structure of the product. In addition, in order to simplify the drawings and facilitate understanding, in some figures, only one of the parts with the same structure or function is schematically shown, or only one of them is marked. In this article, "one" not only means "only one", but also means "more than one", and "several" includes "two" and "more than two".

[0038] In this article, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in this utility model can be understood according to specific circumstances.

[0039] In addition, in the description of the present application, the terms "first", "second", etc. are only used to distinguish the description and cannot be understood as indicating or implying relative importance.

[0040] Reference Figure 1~Figure 4 , which is the first embodiment of the utility model, proposes an adsorption extraction tower, comprising:

[0041] A tower body 1, wherein the top of the tower body 1 has a light phase outlet 101 and a heavy phase inlet 102, and the bottom of the tower body 1 has a light phase inlet 103 and a heavy phase outlet 104;

[0042] A discharge bin 2, the discharge bin 2 is arranged at the bottom of the tower body 1, the bottom of the discharge bin 2 has a slag discharge port 201, and the cross-sectional area of ​​the discharge bin 2 gradually decreases from close to the tower body 1 to far away from the tower body 1, and an extraction chamber 105 is formed between the tower body 1 and the discharge bin 2;

[0043] A rotating shaft 3, the rotating shaft 3 is rotatably disposed on the tower body 1 and is located in the extraction chamber 105, and the light phase outlet 101, the heavy phase inlet 102, the light phase inlet 103, the heavy phase outlet 104 and the slag discharge port 201 are all connected to the extraction chamber 105;

[0044] The spiral scraper 4 is arranged on the rotating shaft 3 and is located above the slag discharge port 201 .

[0045] In this embodiment, the extraction process after hydrolysis of dichloropentachloromethylpyridine is: through a reactor, dichloropentachloromethylpyridine in the hydrolysis acid water is extracted with toluene, and then desolventized and distilled to obtain dichloropentachloromethylpyridine, but the efficiency of using the reactor still needs to be improved, so the extraction tower with a reactor is used, which greatly improves the water washing efficiency, can realize continuous operation, reduce labor and reduce energy consumption, and at the same time, can also reduce the residue in the oil phase and improve the yield. However, the application of traditional extraction towers in the acid water extraction step may cause the heavy phase outlet to be blocked by the settled solids, and the internal mixing effect of the adsorption extraction tower still needs to be improved. In order to solve the above problems, an adsorption extraction tower is set.

[0046] During use, the normal tower body 1 needs to have a light phase outlet 101, a heavy phase inlet 102, a light phase inlet 103 and a heavy phase outlet 104, and the four are arranged in sequence from the top to the bottom of the tower body 1. Working process: before water washing, materials need to be prepared first, namely the acid water after hydrolysis and the toluene extracted from the desolvation, turn on the light phase tank feed pump switch, and pump toluene into the light phase inlet 103 of the extraction tower until the liquid level reaches the upper clarification section and submerges the heavy phase inlet 102, stop pumping toluene, then start the extraction tower stirring, and turn on the heavy phase tank feed pump switch, set the feed speed, start feeding from the heavy phase inlet 102, and start extraction in the effective section during this period. When the acid water phase reaches the lower clarification section and there is an obvious interface, turn on the light phase tank feed pump to continuously pump toluene into the extraction chamber 105, set the feed speed, and start continuous extraction. When the system runs stably, samples are taken from the light phase outlet 101 and the heavy phase outlet 104 to detect the content of each component.

[0047] In order to process the solid-phase slag produced during the extraction process, a discharge bin 2 with a gradually decreasing cross-sectional area is installed at the bottom of the tower body 1. Unlike the traditional cylindrical discharge bin 2, it can better gather the solid-phase slag, which is convenient for centralized treatment and discharged from the slag discharge port 201. At the same time, the power of the rotating shaft 3 is used to drive the spiral scraper 4 in the discharge bin 2 to rotate, and the solid-phase slag attached to the inner wall of the discharge bin 2 is scraped off. The design of the spiral scraper 4, on the one hand, better fits the discharge bin 2 with a changing cross-sectional area, and on the other hand, the continuous spiral form can ensure that the rotating shaft 3 rotates one circle, so that the solid-phase slag on the inner wall of the discharge bin 2 can be more comprehensively discharged.

[0048] Furthermore, the discharge bin 2 is V-shaped, the spiral scraper 4 is located directly above the slag discharge port 201 , and the spiral scraper 4 abuts against the inner wall of the discharge bin 2 .

[0049] Furthermore, the light phase outlet 101 , the heavy phase inlet 102 , the light phase inlet 103 , the heavy phase outlet 104 and the slag discharge port 201 are arranged in sequence from the top to the bottom of the tower body 1 .

[0050] In this embodiment, the cross-section of the discharge bin 2 is limited to a V-shape, which is convenient for early production and processing and ensures that the discharge bin 2 functions normally. The spiral scraper 4 abuts against the inner wall of the discharge bin 2 and smoothly scrapes off the residual solid slag on the inner wall after rotation. The slag discharge port 201 at the bottom directly discharges the solid slag.

[0051] Furthermore, it also includes a plurality of stirring units 5, which are all arranged on the rotating shaft 3, and are arranged at intervals along the length direction of the rotating shaft 3. The stirring units 5 include:

[0052] The stirring horizontal plate 501 and the stirring vertical plate 502 are both arranged on the rotating shaft 3 , and the stirring vertical plate 502 is located directly above the stirring horizontal plate 501 .

[0053] Furthermore, it also includes:

[0054] A vertical baffle 6 and two transverse baffles 7 , wherein the vertical baffle 6 and the transverse baffle 7 are both arranged on the inner wall of the tower body 1 , the vertical baffle 6 is arranged along the circumference of the stirring vertical plate 502 , and the stirring transverse plate 501 is located between the two transverse baffles 7 .

[0055] Furthermore, it also includes:

[0056] Two fixed annular plates 8, both of which are arranged on the inner wall of the tower body 1, the fixed annular plates 8 are located between the two transverse baffles 7, and the stirring transverse plate 501 is located between the two fixed annular plates 8, and the minimum cross-sectional area of ​​the fixed annular plates 8 is larger than the cross-sectional area of ​​the stirring transverse plate 501.

[0057] In this embodiment, the rotating shaft 3 drives several stirring units 5 to rotate in the extraction chamber 105 to improve the mass transfer effect and the extraction efficiency. The stirring units 5 are arranged at equal intervals along the length direction of the rotating shaft 3 to achieve comprehensive stirring of each area in the extraction chamber 105. At the same time, the stirring unit 5 is provided with two groups of stirring plates, namely, a stirring horizontal plate 501 and a stirring vertical plate 502, that is, axial flow stirring and paddle stirring are used in combination, and the two are alternated in sequence to improve the mixing effect.

[0058] Further, a plurality of groups of limit plates consisting of a vertical plate and two horizontal baffles 7 are fixedly installed on the inner wall of the tower body 1. One stirring unit 5 is equipped with a group of limit plates, wherein the vertical baffles 6 are arranged along the circumference of the stirring vertical plate 502, the stirring horizontal plate 501 is located between the two horizontal baffles 7, and two additional fixed annular plates 8 are fixedly installed between the two horizontal baffles 7, which are respectively located on both sides of the stirring horizontal plate 501. The combination of the horizontal and vertical baffles 6 and the fixed annular plates 8 restricts the stirring unit 5 to a certain area, fully stirs the materials in the limited area, and improves the mixing efficiency. At the same time, in order to ensure the smooth transfer of materials in the extraction tower and prevent them from being blocked by the fixed annular plates 8, the minimum cross-sectional area of ​​the fixed annular plates 8 is set to be larger than the cross-sectional area of ​​the stirring horizontal plate 501.

[0059] Furthermore, it also includes an adsorption device 9, which is arranged on the inner wall of the tower body 1 and located between two adjacent stirring units 5. The adsorption device 9 includes:

[0060] A plurality of upward members 901 and a plurality of downward members 902, wherein the upward members 901 and the downward members 902 are both arranged vertically;

[0061] A light phase adsorption layer 903, wherein the light phase adsorption layer 903 is arranged on the top of the upward member 901;

[0062] The heavy phase adsorption layer 904 is arranged at the bottom of the descending member 902 .

[0063] Further, there is a gap between the upper member 901 and the lower member 902, and further comprising:

[0064] A sealing member 10 is arranged in the gap.

[0065] In this embodiment, the adsorption device 9 includes a plurality of vertically arranged upward parts 901 and downward parts 902, and is respectively provided with a light phase adsorption layer 903 and a heavy phase adsorption layer 904. The light phase adsorption layer 903 allows the light phase in the liquid to flow upward and blocks the heavy phase in the liquid from flowing. The heavy phase adsorption layer 904 allows the heavy phase in the liquid to flow downward and blocks the light phase in the liquid from flowing. It is located between two adjacent stirring units 5. Since the heavy phase and the light phase are immiscible and repel each other, the heavy phase formed after stratification in the upward part 901 cannot pass through the area where the light phase is located, and a barrier type layer that gathers the light phase is formed on the top of the upward part 901. In the area, a small amount of extracted light phase formed after stratification in the upward component 901 will be adsorbed near the barrier area. As more and more extracted light phases gather at the bottom of the barrier area, the buoyancy of the extracted light phase becomes larger and larger, and the extracted light phase can pass upward from the barrier area where the extracted light phase is gathered relatively smoothly. The extracted light phase formed after stratification in the downward component 902 cannot pass through the area where the extracted heavy phase is located. The barrier area where the extracted heavy phase is gathered is formed in the adsorption material box area at the bottom of the downward component 902. The extracted light phase repels the barrier area where the extracted heavy phase is gathered formed in the adsorption material box area. Therefore, the extracted light phase cannot flow from the downward component 902 from top to bottom. In addition, because a barrier area where the heavy phase of extraction is gathered is formed at the bottom of the descending member 902, a small amount of heavy phase of extraction formed after stratification in the descending member 902 will be adsorbed near the barrier area. As more and more heavy phase of extraction gathers on the top of the barrier area, the gravity formed by the heavy phase of extraction becomes greater and greater. The heavy phase of extraction can pass downward from the barrier area where the heavy phase of extraction is gathered relatively smoothly, ensuring that the descending member 902 only passes through the heavy phase of extraction while blocking the passage of the light phase of extraction, and a sealing member 10 is installed in the gap between the two to ensure the extraction quality of the extraction tower and to fully play the role of the stirring unit 5 in the adjacent extraction area.

[0066] It should be noted that the above embodiments are only used to illustrate the technical solution of the utility model rather than to limit it. Although the utility model has been described in detail with reference to the preferred embodiments, ordinary technicians in the field should understand that the technical solution of the utility model can be modified or replaced by equivalents without departing from the spirit and scope of the technical solution of the utility model, which should be included in the scope of the claims of the utility model.

Claims

1. An adsorption extraction tower, characterized in that: include: A tower body (1), wherein the top of the tower body (1) is provided with a light phase outlet (101) and a heavy phase inlet (102), and the bottom of the tower body (1) is provided with a light phase inlet (103) and a heavy phase outlet (104); A discharge bin (2), the discharge bin (2) being arranged at the bottom of the tower body (1), the discharge bin (2) having a slag discharge port (201) at the bottom, and the cross-sectional area of ​​the discharge bin (2) gradually decreasing from close to the tower body (1) to far away from the tower body (1), and an extraction chamber (105) being formed between the tower body (1) and the discharge bin (2); a rotating shaft (3), the rotating shaft (3) being rotatably disposed on the tower body (1) and being located in the extraction chamber (105); the light phase outlet (101), the heavy phase inlet (102), the light phase inlet (103), the heavy phase outlet (104) and the slag discharge port (201) are all connected to the extraction chamber (105); A spiral scraper (4), wherein the spiral scraper (4) is arranged on the rotating shaft (3) and is located above the slag discharge port (201).

2. An adsorption extraction tower according to claim 1, characterized in that: The discharge bin (2) is V-shaped, the spiral scraper (4) is located directly above the slag discharge port (201), and the spiral scraper (4) abuts against the inner wall of the discharge bin (2).

3. The adsorption extraction tower according to claim 1, characterized in that: The light phase outlet (101), the heavy phase inlet (102), the light phase inlet (103), the heavy phase outlet (104) and the slag discharge port (201) are arranged in sequence from the top to the bottom of the tower body (1).

4. The adsorption extraction tower according to claim 1, characterized in that: It also comprises a plurality of stirring units (5), wherein the plurality of stirring units (5) are arranged on the rotating shaft (3), and the plurality of stirring units (5) are arranged at intervals along the length direction of the rotating shaft (3), and the stirring units (5) comprise: A stirring horizontal plate (501) and a stirring vertical plate (502), wherein the stirring horizontal plate (501) and the stirring vertical plate (502) are both arranged on the rotating shaft (3), and the stirring vertical plate (502) is located directly above the stirring horizontal plate (501).

5. An adsorption extraction tower according to claim 4, characterized in that: Also includes: A vertical baffle (6) and two transverse baffles (7), wherein the vertical baffle (6) and the transverse baffle (7) are both arranged on the inner wall of the tower body (1), the vertical baffle (6) is arranged along the circumference of the stirring vertical plate (502), and the stirring transverse plate (501) is located between the two transverse baffles (7).

6. The adsorption extraction tower according to claim 5, characterized in that: Also includes: Two fixed annular plates (8), both of which are arranged on the inner wall of the tower body (1), the fixed annular plates (8) are located between the two transverse baffles (7), and the stirring transverse plate (501) is located between the two fixed annular plates (8), and the minimum cross-sectional area of ​​the fixed annular plates (8) is greater than the cross-sectional area of ​​the stirring transverse plate (501).

7. The adsorption extraction tower according to claim 4, characterized in that: It also includes an adsorption device (9), which is arranged on the inner wall of the tower body (1) and located between two adjacent stirring units (5), and the adsorption device (9) includes: A plurality of upward members (901) and a plurality of downward members (902), wherein the upward members (901) and the downward members (902) are both arranged vertically; A light phase adsorption layer (903), wherein the light phase adsorption layer (903) is arranged on the top of the upward member (901); A heavy phase adsorption layer (904), wherein the heavy phase adsorption layer (904) is arranged at the bottom of the descending member (902).

8. An adsorption extraction tower according to claim 7, characterized in that: There is a gap between the upper member (901) and the lower member (902), and further comprises: A sealing member (10) is arranged in the gap.

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