Twin-tower separation and purification device for nitrogen-containing heterocyclic compounds

Abstract

The utility model relates to the technical field of purification processes, in particular to a double-tower type separation and purification device for nitrogen-containing heterocyclic compounds. The utility model provides a double-tower type separation and purification device for nitrogen-containing heterocyclic compounds. The double-tower type separation and purification device comprises a first tower type reactor, a second tower type reactor, a first pretreatment device, a second pretreatment device, an acid liquor dropwise adding tank, an alkali liquor dropwise adding tank, a stirring assembly, a transmission assembly, a material mixing assembly, a filtering assembly and a cleaning assembly, according to the separation and purification device, the double-tower type separation and purification structure is arranged, when the double-tower type separation and purification device is used, solvents and raw materials in the first tower type reactor and the second tower type reactor can be mixed and stirred through the two stirring structures respectively, the filtering structure can be cleaned through the cleaning structure, and in addition, the filtering structure can be cleaned through the cleaning structure. The device realizes the purpose of efficiently extracting and purifying the azacyclo-compounds from a mixed primary extracting solution through a double-tower structural design and in combination with a specific extraction strategy.

Description

Technical Field

[0001] The utility model relates to the technical field of purification processes, and particularly relates to a dual-tower separation and purification device for nitrogen-containing heterocyclic compounds. Background Art

[0002] Separation and purification devices are common equipment in the field of biological purification processes. Plants contain proteins, free amino acids, alkaloids (such as nicotine, nornicotine, anabasine, and anatabine, flavonoids, etc.). These compounds are of great significance in drug research and development and can be used as lead compounds or active pharmaceutical ingredients of drugs. However, in the actual use process, the introduction of ultrasonic-assisted technology can save extraction time, reduce solvent consumption and equipment costs, reduce energy input and improve extraction efficiency. However, it is difficult to scale up production and it is difficult to be put into industrial production, thus making it inconvenient to achieve the problem of efficiently extracting and purifying nitrogen heterocyclic compounds from the mixed primary extract. Content of the Utility Model

[0003] In order to overcome the problem that in the process of using the separation and purification device, the introduction of ultrasonic-assisted technology can save extraction time, reduce solvent consumption and equipment costs, reduce energy input and improve extraction efficiency, but it is difficult to scale up production and it is difficult to be put into industrial production, thus making it inconvenient to achieve the problem of efficiently extracting and purifying nitrogen heterocyclic compounds from the mixed primary extract.

[0004] The technical solution of the utility model is: a dual-tower separation and purification device for nitrogen-containing heterocyclic compounds, comprising a support frame, a first tower reactor, a second tower reactor, a first pretreatment device, a second pretreatment device, an upper end outlet, an alkali liquid dropping tank, an acid liquid dropping tank, a stirring component, a transmission component, a mixing component, a filtering component, and a cleaning component; a first tower reactor is arranged above the support frame, a first pretreatment device is arranged above the support frame, a second pretreatment device is arranged above the support frame, a second tower reactor is arranged above the support frame, an acid liquid dropping tank is arranged above the first pretreatment device, an alkali liquid dropping tank is arranged above the second pretreatment device, an upper end outlet is arranged above the first tower reactor, an upper end outlet is arranged above the second tower reactor, the tops of the two pretreatment devices are both connected to the acid dropping tank and the alkali dropping tank through valves, the bottom of the first tower reactor is connected to the bottom of the pretreatment device through a pipeline valve, and the bottom of the second tower reactor is connected to the bottom of the pretreatment device through a pipeline valve.

[0005] Preferably, when the double-tower separation and purification device is in use, first, the plant waste is pretreated, and the mixed primary extract is introduced into the first pretreatment device through a pipeline. Then, acid solution is introduced into the first pretreatment device to convert the fat-soluble mixed solution into a water-soluble sulfate solution. After the reaction in the first pretreatment device is sufficient, the pipeline valve is adjusted to continuously introduce the water-soluble sulfate solution from the lower end into the first tower reactor containing clean solvent and water. Under continuous stirring and the action of Pall rings, the solvents in the system are fully mixed, and the upper-layer fat-soluble impurities are discharged from the upper outlet. After 12 hours, the sulfate solution in the lower-layer aqueous phase is added to the second pretreatment device, and alkali solution is added to adjust the pH of the system to 11-13 to reduce it to a nitrogen-containing heterocyclic compound. After stirring and mixing evenly, the valve is adjusted again to directly transfer it into the second tower reactor. In the second tower separation device, clean solvent is introduced into the bottom and stirred continuously. After a period of time, after stirring and extraction in the second tower reactor, it is left to stand and layer. The pipeline valve is adjusted to transfer the oil-phase solution into the subsequent purification system, and nitrogen-containing heterocyclic compounds with different purity requirements can be obtained.

[0006] Preferably, the stirring assembly includes a stirring motor, a stirring shaft, and stirring rods; a stirring motor is arranged above the first tower reactor, a stirring shaft is arranged at the output end of the stirring motor, stirring rods are arranged on the side wall of the stirring shaft, multiple groups of stirring rods are provided, two groups of stirring assemblies are provided, and the other stirring assembly is arranged inside the second tower reactor; starting the stirring motor can drive the stirring shaft to rotate, and the stirring shaft can drive multiple groups of stirring rods to rotate. Through the multiple groups of stirring rods, the solvent and raw materials inside the first tower reactor can be mixed and stirred. At the same time, through the transmission assembly, the other stirring assembly can be driven to rotate, so that the solvent and raw materials inside the second tower reactor can be mixed and stirred.

[0007] Preferably, the transmission assembly includes a driving shaft, a driving wheel, and a transmission belt; one end of the stirring shaft is provided with a driving shaft, a driving wheel is arranged on the side wall of the driving shaft, a transmission belt is arranged outside the driving wheel, and the driving wheel is rotationally connected to the transmission belt; the stirring shaft can drive the driving shaft to rotate, and the driving shaft can drive the transmission belt to rotate through the driving wheel.

[0008] Preferably, the transmission assembly further includes a driven wheel and a driven shaft; one end of the other stirring assembly is provided with a driven shaft, a driven wheel is arranged on the side wall of the driven shaft, the driven wheel is arranged inside the transmission belt, and the driven wheel is rotationally connected to the transmission belt; the transmission belt can drive the driven wheel to rotate, and the driven wheel can drive the other stirring assembly to rotate through the driven shaft, so that the synchronous transmission and stirring effect of the two groups of stirring assemblies can be achieved.

[0009] Preferably, the mixing component includes Pall rings and mounting rings; mounting rings are provided on the inner wall of the first tower reactor, multiple groups of mounting rings are provided, Pall rings are arranged above the mounting rings, multiple groups of Pall rings are provided, two groups of mixing components are provided, and the other mixing component is arranged inside the second tower reactor; by adding a large number of Pall rings to the interiors of the first tower reactor and the second tower reactor, the solvent and the raw material can be promoted to fully contact, and the solvent leaching rate can be increased.

[0010] Preferably, the filtering component includes a filter screen and a liquid outlet; a liquid outlet is formed in the bottom wall of the first tower reactor, a filter screen is provided on the inner wall of the liquid outlet, two groups of filtering components are provided, and the other filtering component is arranged inside the second tower reactor; by designing a filter screen at the first liquid outlet, partial waste residues can be prevented from falling, and thus the situation of pipeline blockage can be avoided.

[0011] Preferably, the cleaning component includes a connecting rod and a cleaning brush plate; a connecting rod is provided on the bottom wall of the stirring rod, one end of the connecting rod is provided with a cleaning brush plate, and the cleaning brush plate is in contact connection with the filter screen; the stirring rod can drive the cleaning brush plate to rotate through the connecting rod, and the waste residues adhering to the upper part of the filter screen can be cleaned through the cleaning brush plate, and thus the situation of pipeline blockage can be avoided.

[0012] The beneficial effects of the present utility model are as follows:

[0013] 1. Compared with the traditional separation and purification device during use, the introduction of the ultrasonic-assisted technology can save extraction time, reduce solvent consumption and equipment costs, reduce energy input and improve extraction efficiency. However, it is difficult to scale up production and it is difficult to be put into industrial production, thus making it inconvenient to solve the problem of efficiently extracting and purifying nitrogen heterocyclic compounds from the mixed primary extract. By setting a double-tower separation and purification structure, when the double-tower separation and purification device is in use, the solvent and the raw material inside the first tower reactor and the second tower reactor can be respectively mixed and stirred through two groups of stirring structures. Moreover, the filtering structure can be cleaned through the cleaning structure. In addition, through the double-tower structure design and in combination with a specific extraction strategy, the purpose of efficiently extracting and purifying nitrogen heterocyclic compounds from the mixed primary extract is achieved.

[0014] 2. When the dual-tower separation and purification device is in use, first, the plant waste is pretreated, and the mixed primary extract is fed into the pretreatment device through a pipeline. Then, acid solution is introduced into the first pretreatment device to convert the fat-soluble mixed solution into a water-soluble sulfate solution. After the reaction in the first pretreatment device is sufficient, the pipeline valve is adjusted to continuously feed the water-soluble sulfate solution from the lower end into the first tower reactor containing clean solvent and water. Under continuous stirring and the action of Pall rings, the solvents in the system are fully mixed, and the upper-layer fat-soluble impurities are discharged from the upper outlet. After 12 hours, the sulfate solution in the lower water phase is added to the second pretreatment device, and alkali solution is added to adjust the pH of the system to 11 - 13 to reduce it to a nitrogen-containing heterocyclic compound. After stirring and mixing evenly, the valve is adjusted again to directly transfer it into the second tower reactor. In the second tower separation device, clean solvent is continuously fed into the bottom and stirred. After a period of time, after stirring and extraction in the second tower reactor, it is allowed to stand and layer. The pipeline valve is adjusted to transfer the oil-phase solution into the subsequent purification system, and nitrogen-containing heterocyclic compounds with different purity requirements can be obtained. Among them, starting the stirring motor can drive the stirring shaft to rotate, and the stirring shaft can drive multiple groups of stirring rods to rotate. Through the multiple groups of stirring rods, the solvents and raw materials inside the first tower reactor can be mixed and stirred. At the same time, through the transmission component, another stirring component can be driven to rotate, so as to mix and stir the solvents and raw materials inside the second tower reactor to achieve the purpose of energy saving.

[0015] 3. When it is necessary to clean the waste residue, the stirring rod can drive the cleaning brush plate to rotate through the connecting rod, and the cleaning brush plate can clean the waste residue adhering above the filter screen, thereby avoiding the occurrence of pipeline blockage. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 FIG. 9 shows a first three-dimensional structural schematic diagram of the dual-tower separation and purification device for nitrogen-containing heterocyclic compounds of the present invention;

[0017] Figure 2 FIG. 13 shows a first partial three-dimensional structural schematic diagram of the dual-tower separation and purification device for nitrogen-containing heterocyclic compounds of the present invention;

[0018] Figure 3 FIG. 17 shows a second partial three-dimensional structural schematic diagram of the dual-tower separation and purification device for nitrogen-containing heterocyclic compounds of the present invention;

[0019] Figure 4 FIG. 21 shows a third partial three-dimensional structural schematic diagram of the dual-tower separation and purification device for nitrogen-containing heterocyclic compounds of the present invention;

[0020] Description of the reference numerals: 1, stirring assembly; 2, transmission assembly; 3, mixing assembly; 4, filtering assembly; 5, cleaning assembly; 7, support frame; 8, first tower reactor; 9, second tower reactor; 10, first pretreatment device; 11, second pretreatment device; 12, upper outlet; 13, lye dropping tank; 14, acid dropping tank; 101, stirring motor; 102, stirring shaft; 103, stirring rod; 201, driving shaft; 202, driving wheel; 203, transmission belt; 204, driven wheel; 205, driven shaft; 301, Pall ring; 302, mounting ring; 401, filter screen; 402, liquid outlet; 501, connecting rod; 502, cleaning brush plate. Detailed implementation manners

[0021] The present utility model will be further described below in conjunction with the accompanying drawings and embodiments.

[0022] Please refer to Figure 1 , the present utility model provides an embodiment: a dual-tower separation and purification device for nitrogen-containing heterocyclic compounds, including a support frame 7, a first tower reactor 8, a second tower reactor 9, a first pretreatment device 10, a second pretreatment device 11, an upper outlet 12, an acid dropping tank 14, a lye dropping tank 13, a stirring assembly 1, a transmission assembly 2, a mixing assembly 3, a filtering assembly 4 and a cleaning assembly 5; above the support frame 7 is provided with a first tower reactor 8, above the support frame 7 is provided with a first pretreatment device 10, above the support frame 7 is provided with a second pretreatment device 11, above the support frame 7 is provided with a second tower reactor 9, above the first pretreatment device 10 is provided with an acid dropping tank 14, above the second pretreatment device 10 is provided with a lye dropping tank 13, above the first tower reactor 8 is provided with an upper outlet 12, above the second tower reactor 9 is provided with an upper outlet 12, the tops of the two pretreatment devices 10 are both connected to the acid dropping tank and the lye dropping tank through valves, the bottom of the first tower reactor 8 is connected to the bottom of the pretreatment device 10 through a pipeline valve, and the bottom of the second tower reactor 9 is connected to the bottom of the pretreatment device 10 through a pipeline valve.

[0023] Please refer to Figure 2, the stirring assembly 1 includes a stirring motor 101, a stirring shaft 102 and stirring rods 103; a stirring motor 101 is arranged above the first tower reactor 8, the output end of the stirring motor 101 is provided with a stirring shaft 102, and stirring rods 103 are arranged on the side wall of the stirring shaft 102. There are multiple groups of stirring rods 103, and two groups of stirring assemblies 1 are provided. Another stirring assembly 1 is arranged inside the second tower reactor 9; starting the stirring motor 101 can drive the stirring shaft 102 to rotate, and the stirring shaft 102 can drive multiple groups of stirring rods 103 to rotate. Through the multiple groups of stirring rods 103, the solvent and raw materials inside the first tower reactor 8 can be mixed and stirred. At the same time, through the transmission assembly 2, another stirring assembly 1 can be driven to rotate, so that the solvent and raw materials inside the second tower reactor 9 can be mixed and stirred; the transmission assembly 2 includes a driving shaft 201, a driving wheel 202 and a transmission belt 203; one end of the stirring shaft 102 is provided with a driving shaft 201, a driving wheel 202 is arranged on the side wall of the driving shaft 201, and a transmission belt 203 is arranged outside the driving wheel 202. The driving wheel 202 is rotatably connected to the transmission belt 203; the stirring shaft 102 can drive the driving shaft 201 to rotate, and the driving shaft 201 can drive the transmission belt 203 to rotate through the driving wheel 202; the transmission assembly 2 further includes a driven wheel 204 and a driven shaft 205; one end of another stirring assembly 1 is provided with a driven shaft 205, a driven wheel 204 is arranged on the side wall of the driven shaft 205, the driven wheel 204 is arranged inside the transmission belt 203, and the driven wheel 204 is rotatably connected to the transmission belt 203; the transmission belt 203 can drive the driven wheel 204 to rotate, and the driven wheel 204 can drive another stirring assembly 1 to rotate through the driven shaft 205, so as to drive the two stirring assemblies 1 to achieve the effect of synchronous transmission and stirring.

[0024] Please refer to Figures 3 - 4, in this embodiment, the mixing component 3 includes Pall rings 301 and mounting rings 302; mounting rings 302 are provided on the inner wall of the first tower reactor 8, and multiple groups of mounting rings 302 are provided. Above the mounting rings 302, multiple groups of Pall rings 301 are provided. Two groups of mixing components 3 are provided, and another mixing component 3 is arranged inside the second tower reactor 9; by adding a large number of Pall rings 301 to the interiors of the first tower reactor 8 and the second tower reactor 9, the solvent and the raw material can be promoted to fully contact, thereby improving the solvent leaching rate; the filtering component 4 includes a filter screen 401 and a liquid outlet 402; a liquid outlet 402 is opened on the bottom wall of the first tower reactor 8, and a filter screen 401 is provided on the inner wall of the liquid outlet 402. Two groups of filtering components 4 are provided, and another filtering component 4 is arranged inside the second tower reactor 9; by designing a filter screen 401 at the first liquid outlet 402, some waste residues can be prevented from falling, thereby avoiding the occurrence of pipeline blockage; the cleaning component 5 includes a connecting rod 501 and a cleaning brush plate 502; a connecting rod 501 is provided on the bottom wall of the stirring rod 103, and a cleaning brush plate 502 is provided at one end of the connecting rod 501. The cleaning brush plate 502 is in contact connection with the filter screen 401; the stirring rod 103 can drive the cleaning brush plate 502 to rotate through the connecting rod 501, and the waste residues adhering to the upper part of the filter screen 401 can be cleaned by the cleaning brush plate 502, thereby avoiding the occurrence of pipeline blockage;

[0025] When the dual-tower separation and purification device is in use, first, the plant waste is pretreated, and the mixed preliminary extraction liquid enters through a pipeline into;

[0026] Then, acid solution is added to the top of the first pretreatment device 10 to convert the fat-soluble mixed liquid into a water-soluble sulfate solution. Starting the stirring motor 101 can drive the stirring shaft 102 to rotate, and the stirring shaft 102 can drive multiple groups of stirring rods 103 to rotate. Through the multiple groups of stirring rods 103, the solvent and the raw material inside the first tower reactor 8 can be mixed and stirred;

[0027] Meanwhile, through the transmission component 2, another stirring component 1 can be driven to rotate, so that the solvent and the raw material inside the second tower reactor 9 can be mixed and stirred;

[0028] After the first pretreatment device reacts sufficiently, adjust the pipeline valve to continuously introduce the water-soluble sulfate solution into the first tower reactor containing clean solvent and water from the lower end. Under continuous stirring and the action of Pall rings, the solvents in the system are fully mixed, and the fat-soluble impurities in the upper layer are discharged from the upper outlet 12. After 12 hours, the sulfate solution in the lower aqueous phase is added to the second pretreatment device; in the second pretreatment device, add an alkali solution to adjust the pH of the system to 11-13 to reduce it to a nitrogen-containing heterocyclic compound; after stirring and mixing evenly, adjust the valve to directly transfer it to the second tower reactor; finally, in the second tower separation device, continuously introduce clean solvent into the bottom and stir. After a period of time, after stirring and extracting in the second tower reactor, let it stand and separate layers, adjust the pipeline valve to transfer the oil-phase solution to the subsequent purification system, and nitrogen-containing heterocyclic compounds with different purity requirements can be obtained.

[0029] Through the above steps, when the double-tower separation and purification device is in use, first, pretreat the plant waste, and introduce the mixed primary extract into the pretreatment device 10 through a pipeline. Then, add an acid solution to the pretreatment device 10 to convert the fat-soluble mixed solution into a water-soluble sulfate solution. After the first pretreatment device reacts sufficiently, adjust the pipeline valve to continuously introduce the water-soluble sulfate solution into the first tower reactor 8 containing clean solvent and water from the lower end. Under continuous stirring and the action of Pall rings, the solvents in the system are fully mixed, and the fat-soluble impurities in the upper layer are discharged from the upper outlet 12. After 12 hours, the sulfate solution in the lower aqueous phase is added to the second pretreatment device, and an alkali solution is added to adjust the pH of the system to 11-13 to reduce it to a nitrogen-containing heterocyclic compound. After stirring and mixing evenly, adjust the valve to directly transfer it to the second tower reactor 9. In the second tower separation device, continuously introduce clean solvent into the bottom and stir. After a period of time, after stirring and extracting in the second tower reactor, let it stand and separate layers, adjust the pipeline valve to transfer the oil-phase solution to the subsequent purification system, and nitrogen-containing heterocyclic compounds with different purity requirements can be obtained.

[0030] The above has described the embodiments of the present invention in detail with reference to the accompanying drawings. However, the present invention is not limited to the above embodiments. Within the scope of knowledge possessed by those skilled in the art, various changes can be made without departing from the gist of the present invention.

Claims

1. A dual-tower separation and purification device for nitrogen-containing heterocyclic compounds, comprising a support frame (7), characterized in that: It also includes a first tower reactor (8), a second tower reactor (9), a first pretreatment device (10), a second pretreatment device (11), an upper end outlet (12), an alkali liquid dropping tank (13), an acid liquid dropping tank (14), a stirring assembly (1), a transmission assembly (2), a mixing assembly (3), a filtering assembly (4) and a cleaning assembly (5); above the support frame (7), there is a first tower reactor (8), above the support frame (7), there is a first pretreatment device (10), above the support frame (7), there is a second pretreatment device (11), above the support frame (7), there is a second tower reactor (9), above the first pretreatment device (10), there is an acid liquid dropping tank (14), above the second pretreatment device (11), there is an alkali liquid dropping tank (13), above the first tower reactor (8), there is an upper end outlet (12), above the second tower reactor (9), there is an upper end outlet (12), the tops of the two pretreatment devices (10) are both connected to the acid dropping tank and the alkali dropping tank through valves, the bottom of the first tower reactor (8) is connected to the bottom of the pretreatment device (10) through a pipeline valve, and the bottom of the second tower reactor (9) is connected to the bottom of the pretreatment device (10) through a pipeline valve.

2. The dual-tower separation and purification device for nitrogen-containing heterocyclic compounds according to claim 1, wherein: The stirring assembly (1) includes a stirring motor (101), a stirring shaft (102) and stirring rods (103); above the first tower reactor (8), there is a stirring motor (101), the output end of the stirring motor (101) is provided with a stirring shaft (102), and stirring rods (103) are arranged on the side wall of the stirring shaft (102). There are multiple groups of stirring rods (103), and there are two groups of stirring assemblies (1). Another stirring assembly (1) is arranged inside the second tower reactor (9).

3. The dual-tower separation and purification device for nitrogen-containing heterocyclic compounds according to claim 2, wherein: The transmission assembly (2) includes a driving shaft (201), a driving wheel (202) and a transmission belt (203); one end of the stirring shaft (102) is provided with a driving shaft (201), a driving wheel (202) is arranged on the side wall of the driving shaft (201), and a transmission belt (203) is arranged outside the driving wheel (202). The driving wheel (202) is rotationally connected to the transmission belt (203).

4. The dual-tower separation and purification device for nitrogen-containing heterocyclic compounds according to claim 1, wherein: The transmission assembly (2) also includes a driven wheel (204) and a driven shaft (205); one end of another stirring assembly (1) is provided with a driven shaft (205), a driven wheel (204) is arranged on the side wall of the driven shaft (205), the driven wheel (204) is arranged inside the transmission belt (203), and the driven wheel (204) is rotationally connected to the transmission belt (203).

5. The dual-tower separation and purification device for nitrogen-containing heterocyclic compounds according to claim 1, characterized in that: The mixing assembly (3) includes Pall rings (301) and mounting rings (302); mounting rings (302) are arranged on the inner wall of the first tower reactor (8). There are multiple groups of mounting rings (302), and Pall rings (301) are arranged above the mounting rings (302). There are multiple groups of Pall rings (301), and there are two groups of mixing assemblies (3). Another mixing assembly (3) is arranged inside the second tower reactor (9).

6. The dual-tower separation and purification device for nitrogen-containing heterocyclic compounds according to claim 1, wherein: The filtering component (4) includes a filter screen (401) and a liquid outlet (402); a liquid outlet (402) is formed in the bottom wall of the first tower reactor (8), a filter screen (401) is arranged on the inner wall of the liquid outlet (402), two groups of filtering components (4) are provided, and another filtering component (4) is arranged inside the second tower reactor (9).

7. A dual-tower separation and purification device for nitrogen-containing heterocyclic compounds according to claim 2, characterized in that: The cleaning component (5) includes a connecting rod (501) and a cleaning brush plate (502); a connecting rod (501) is arranged on the bottom wall of the stirring rod (103), one end of the connecting rod (501) is provided with a cleaning brush plate (502), and the cleaning brush plate (502) is in contact connection with the filter screen (401).

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