Preparation device

Abstract

The utility model discloses a preparation device which is characterized in that the output end of a solvent mixing kettle is connected with a solvent dripping kettle, and the output end of the solvent dripping kettle is connected with a preparation tower; a first feeding device is connected above the preparation tower, and the output end of the preparation tower is connected with the addition tower; the addition tower is connected with a second feeding device, and the output end of the addition tower is connected with a continuous phase splitting device; the output end of the continuous phase splitting device is connected with a rectifying tower, the top of the rectifying tower is connected with a first condenser, the output end of the first condenser is connected with a first storage tank, the bottom of the rectifying tower is connected with a second condenser, and the output end of the second condenser is connected with a second storage tank; quantitative continuous adding is achieved in the solvent mixing kettle for adding raw materials, the solvent dropwise adding kettle and the first feeding device, the speed of the reaction process is controlled, cooling control is further conducted through the rectifying tower and the condenser after a cooling layer is designed on the preparation tower and passes through the continuous phase splitting device, safety is higher, and continuous production of the prothioconazole intermediate is achieved.

Description

Technical Field

[0001] This utility model relates to the field of chemical synthesis, and in particular to a preparation apparatus. Background Technology

[0002] Prothioconazole is a novel broad-spectrum triazole thione fungicide developed by Bayer AG. It is primarily used to control numerous diseases in cereal, wheat, and legume crops. Prothioconazole has low toxicity, no teratogenic or mutagenic effects, is non-embryonic, and safe for humans and the environment. Its mechanism of action involves inhibiting the demethylation at the 14-position of lanosterol or 24-methylenedihydroguanidine, precursors of sterols in fungi.

[0003] In existing technologies, the synthetic route of prothioconazole mostly uses o-chlorobenzyl chloride as a raw material, and proceeds through the preparation of Grignard reagents, Grignard addition reactions, epoxidation reactions, substitution reactions, ring-closing reactions, and oxidation reactions to synthesize the final product. Among these steps, the preparation of Grignard reagents and the Grignard addition reactions are highly exothermic, therefore the production of prothioconazole is mostly carried out in a batch operation mode, which is labor-intensive and has low production efficiency. Furthermore, the low heat exchange efficiency of the batch production process makes temperature control difficult; inaccurate temperature control can easily lead to the generation of large amounts of coupling impurities, or even serious accidents such as overheating and material spraying. Utility Model Content

[0004] The purpose of this invention is to address the shortcomings of existing technologies by proposing a preparation device.

[0005] To achieve the above objectives, the present invention adopts the following technical solution: a preparation apparatus, comprising:

[0006] Solvent mixing vessel;

[0007] The output end of the solvent mixing vessel is connected to the solvent dropping vessel, and the output end of the solvent dropping vessel is connected to the preparation tower;

[0008] The preparation tower is connected to a first feeding device at the top, and the output end of the preparation tower is connected to an addition tower;

[0009] The addition tower is connected to a second feeding device, and the output end of the addition tower is connected to a continuous phase separation device;

[0010] The output end of the continuous phase separation device is connected to a distillation column, the top of the distillation column is connected to a first condenser, the output end of the first condenser is connected to a first storage tank, the bottom of the distillation column is connected to a second condenser, and the output end of the second condenser is connected to a second storage tank. The second storage tank is used to store the prepared prothioconazole intermediate.

[0011] As a further description of the above technical solution: a first stirring rod is provided on the solvent mixing vessel;

[0012] The solvent dropper is equipped with a solvent feed pump at its output end, which is connected to the bottom of the preparation tower.

[0013] As a further description of the above technical solution: the inner side of the preparation tower is divided into several interconnected cavities by a perforated sieve plate, the inner side of the cavities is filled with packing material, and the inner and outer sides of the preparation tower are provided with cooling layers.

[0014] As a further description of the above technical solution: the preparation tower is provided with a solvent inlet, a first material inlet, a first top outlet and a first bottom outlet, and the bottom of the preparation tower is also provided with a first waste discharge outlet. The first top outlet and the first bottom outlet are connected to the addition tower through a first transfer pump.

[0015] As a further description of the above technical solution: the first feeding device includes a storage bin, a first motor and a first rotary rod are provided on the storage bin, a conveying pipe is provided at the outlet below the storage bin, a second motor and a second rotary rod are provided on the conveying pipe, and the output end of the conveying pipe is connected to the first material inlet at the top of the preparation tower.

[0016] As a further description of the above technical solution: the inner side of the addition tower is provided with a diversion tower plate, and the upper and lower sides of the diversion tower plate are provided with a number of protrusions, and adjacent diversion tower plates are staggered through the protrusions.

[0017] As a further description of the above technical solution: the addition tower is provided with a reagent inlet, a second material inlet, a second top outlet and a second bottom outlet, and the bottom of the addition tower is also provided with a second waste outlet. The second top outlet and the second bottom outlet are connected to the continuous phase separation device through a second transfer pump.

[0018] As a further description of the above technical solution: the continuous phase separation device is provided with a crude product inlet, a water inlet, a water outlet, and a crude product outlet;

[0019] The inner side of the continuous phase separation device is provided with a second stirring rod and a phase separation plate.

[0020] As a further description of the above technical solution: the crude product outlet of the continuous phase separation device is connected to the distillation column via a feed pump, and a third condenser is provided inside the distillation column.

[0021] As a further description of the above technical solution: the distillation column is provided with a third top outlet and a third bottom outlet.

[0022] The above technical solution has the following advantages or beneficial effects:

[0023] The preparation apparatus designed in this application enables quantitative and continuous addition of raw materials in the solvent mixing vessel, solvent dropping vessel, and first feeding device, controlling the reaction rate. Furthermore, by designing a cooling layer in the preparation tower and further controlling the temperature through a distillation tower and condenser after a continuous phase separation device, the safety is enhanced, achieving continuous production of prothioconazole intermediates. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the preparation device proposed in this utility model.

[0025] Figure 2 This is a schematic diagram of the structural principle of the preparation tower in this utility model;

[0026] Figure 3 This is a schematic diagram of the addition tower in this utility model.

[0027] Legend:

[0028] 1. Solvent mixing vessel; 101. First stirring rod; 2. Solvent dropping vessel; 201. Solvent feed pump; 3. Preparation tower; 301. Sieve tray; 302. Packing; 303. Cooling layer; 304. Solvent inlet; 305. First material inlet; 306. First top outlet; 307. First bottom outlet; 308. First waste outlet; 309. First transfer pump; 4. First feeding device; 401. Storage bin; 402. First motor; 403. First rotary shaft; 404. Conveying pipe; 405. Second motor; 406. Second rotary shaft; 5. Addition tower; 501. Diverting tray; 502. Test 503. Second material inlet; 504. Second top outlet; 505. Second bottom outlet; 506. Second waste outlet; 507. Second transfer pump; 6. Second feeding device; 7. Continuous phase separation device; 701. Crude product inlet; 702. Water inlet; 703. Water outlet; 704. Crude product outlet; 705. Second stirring rod; 706. Phase separation plate; 707. Feed pump; 8. Distillation column; 801. Third condenser; 802. Third top outlet; 803. Third bottom outlet; 9. First condenser; 10. First storage tank; 11. Second condenser; 12. Second storage tank. Detailed Implementation

[0029] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0030] Reference Figures 1-3 An embodiment of this utility model provides a preparation apparatus, comprising: a solvent mixing vessel 1; the output end of the solvent mixing vessel 1 is connected to a solvent dropping vessel 2, and the output end of the solvent dropping vessel 2 is connected to a preparation tower 3; a first feeding device 4 is connected above the preparation tower 3, and the output end of the preparation tower 3 is connected to an addition tower 5; the addition tower 5 is connected to a second feeding device 6, and the output end of the addition tower 5 is connected to a continuous phase separation device 7; the output end of the continuous phase separation device 7 is connected to a distillation tower 8, the top of the distillation tower 8 is connected to a first condenser 9, the output end of the first condenser 9 is connected to a first storage tank 10, the bottom of the distillation tower 8 is connected to a second condenser 11, and the output end of the second condenser 11 is connected to a second storage tank 12, the second storage tank 12 being used to store the prepared prothioconazole intermediate.

[0031] In this embodiment, o-chlorobenzyl chloride solvent is placed in solvent mixing vessel 1, and the output end of solvent mixing vessel 1 is connected to solvent dropping vessel 2. ， The output end of the solvent dropping vessel 2 is connected to the preparation tower 3 to achieve quantitative and continuous addition and control the reaction process speed. Magnesium shavings are placed inside the first feeding device 4 and added from above the preparation tower 3 to prepare Grignard reagent. The Grignard reaction is carried out through the addition tower 5 to generate crude product. The aqueous phase and organic phase are then mixed and separated by the continuous phase separation device 7 to separate the solvent and prothioconazole intermediate. The intermediate is then condensed by the first condenser 9 and the second condenser 11 and transported to the first storage tank 10 and the second storage tank 12 for storage, realizing the continuous production of prothioconazole intermediate.

[0032] Specifically, a first stirring rod 101 is provided on the solvent mixing vessel 1; a solvent feed pump 201 is provided at the output end of the solvent dropping vessel 2, and the solvent feed pump 201 is connected to the bottom of the preparation tower 3.

[0033] In this embodiment, the solvent mixing vessel 1 stirs the o-chlorobenzyl chloride solvent with the first stirring rod 101 to ensure that the solvent is uniformly delivered to the solvent dropping vessel 2. The output end of the solvent mixing vessel 1 is interlocked with the solvent dropping vessel 2 by a level gauge. When the liquid level in the solvent dropping vessel 2 reaches the low value, the valve at the output end of the solvent mixing vessel 1 is opened to feed the solvent dropping vessel 2. When the liquid level in the solvent dropping vessel 2 reaches the high value, the valve at the output end of the solvent mixing vessel 1 is closed to stop feeding.

[0034] The inner side of the preparation tower 3 is divided into several interconnected cavities by a sieve plate 301. The inner side of the cavities is filled with packing 302. Cooling layers 303 are provided on the inner and outer sides of the preparation tower 3. The preparation tower 3 is provided with a solvent inlet 304, a first material inlet 305, a first top outlet 306 and a first bottom outlet 307. The bottom of the preparation tower 3 is also provided with a first waste outlet 308. The first top outlet 306 and the first bottom outlet 307 are connected to the addition tower 5 through a first transfer pump 309.

[0035] In this embodiment, filters are provided at the first top outlet 306 and the first bottom outlet 307 to prevent the added magnesium shavings from leaking out. A check valve and a switching valve are provided between the bottom solvent inlet 304 and the solvent feed pump 201. The flow rate of the solvent feed pump 201 is controlled by the control system of the preparation tower 3, and the feed rate of o-chlorobenzyl chloride solvent can be controlled by adjusting the flow rate.

[0036] The sieve holes of the perforated tray 301 are smaller than the diameter of the upper packing 302 and the number of holes is greater than the number of packings in contact with the perforated tray 301. The diameter of the upper packing 302 is greater than the diameter of the lower packing 302. The depth of the upper packing 302 is greater than the depth of the lower packing 302. The number of packing layers and the number of perforated trays are five or more. The packing 302 is made of materials such as metal, ceramic, and plastic.

[0037] The cooling layer 303 of the preparation tower 3 includes an external shell cooling and an internal coil cooling. The external shell cooling is normally open, and the internal coil cooling switch valve is interlocked with the temperature of the preparation tower 3. When the temperature of the preparation tower 3 is at a high value, the internal coil cooling switch valve is opened, and when the temperature drops to a low value, the internal coil cooling switch valve is closed.

[0038] The first bottom outlet 307 is connected to the first top outlet 306, and then to the inlet valve of the first transfer pump 309. At the same time, the first top outlet 306 is also connected to the outlet valve of the first transfer pump 309. Valves are provided at each connection point. The first bottom outlet 307 and the first transfer pump 309 are normally closed, and the first top outlet 306 is normally open. When production stops, the first top outlet 306 is closed, and the first bottom outlet 307 and the first transfer pump 309 are opened to transfer the material in the preparation tower 3 to the next process to continue the reaction.

[0039] The first feeding device 4 includes a storage bin 401, a first motor 402 and a first rotary rod 403 installed on the storage bin 401, a conveying pipe 404 installed at the outlet below the storage bin 401, a second motor 405 and a second rotary rod 406 installed on the conveying pipe 404, and the output end of the conveying pipe 404 is connected to the first material inlet 305 at the top of the preparation tower 3.

[0040] In this embodiment, the outlet of the storage bin 401 is connected to the inlet of the conveying pipe 404, and the outlet of the conveying pipe 404 is connected to the preparation tower 3. The first swivel 403 is vertically installed in the storage bin 401 and is driven to rotate by the first motor 402 to convey magnesium shavings to the conveying pipe 404 below. The length of the second swivel 406 is the length from the inlet of the conveying pipe 404 to the outlet of the magnesium shavings conveying pipe, which is less than the overall length of the conveying pipe 404. A mechanical seal is used between the second swivel 406 and the conveying pipe 404. The second swivel 406 is controlled by the second motor 405, which is responsible for conveying magnesium shavings from the inlet to the outlet of the conveying pipe 404. The second motor 405 is controlled by the magnesium shavings feeding control system.

[0041] The inner side of the addition tower 5 is provided with a diversion tower plate 501. Several protrusions are provided on the upper and lower sides of the diversion tower plate 501, and adjacent diversion tower plates 501 are arranged in an alternating manner through the protrusions.

[0042] In this embodiment, the diversion tray 501 is provided with protrusions so that the upper and lower adjacent diversion trays 501 are staggered, forming a Y-shaped cavity between the diversion trays, which plays a diversion role for the reactants in each cavity, increases the contact area of ​​the reactants and reduces the amount of reactants per unit volume.

[0043] The addition tower 5 is provided with a reagent inlet 502, a second material inlet 503, a second top outlet 504 and a second bottom outlet 505. The bottom of the addition tower 5 is also provided with a second waste outlet 506. The second top outlet 504 and the second bottom outlet 505 are connected to the continuous phase separation device 7 through a second transfer pump 507.

[0044] In this embodiment, the reagent inlet 502 is connected to the first transfer pump 309, the second bottom outlet 505 is connected to the second top outlet 504 and then to the inlet valve of the second transfer pump 507, and the second top outlet 504 is also connected to the outlet valve of the second transfer pump 507. Valves are provided at all the connections. The second bottom outlet 505 and the second transfer pump 507 are normally closed, and the second top outlet 504 is normally open. When production stops, the second top outlet 504 is closed, and the second bottom outlet 505 and the second transfer pump 507 are opened to transfer the material in the addition tower 5 to the next process to continue the reaction.

[0045] Furthermore, the second feeding device 6 is equipped with 2-chloro-1-(1-chlorocyclopropyl)ethyl ketone, which is connected to the second material inlet 503 and conveyed to the bottom of the addition tower 5. The second material inlet 503 is equipped with a check valve and a switching valve. The switching valve is controlled by the control system of the addition tower 5. The position of the second top outlet 504 is lower than the position of the first top outlet 306 of the preparation tower 3.

[0046] Furthermore, the addition tower 5 is also equipped with a cooling layer 303, which includes an external shell cooling and an internal coil cooling. The external shell cooling of the tower body is in a normally open state, and the internal coil cooling switch valve is interlocked with the temperature of the addition tower 5. When the tower body temperature is at a high value, the internal coil cooling switch valve is opened, and when the temperature drops to a low value, the internal coil cooling switch valve is closed.

[0047] The continuous phase separation device 7 is provided with a crude product inlet 701, a water inlet 702, a water outlet 703 and a crude product outlet 704; a second stirring rod 705 and a phase separation plate 706 are provided on the inner side of the continuous phase separation device 7.

[0048] In this embodiment, the water inlet 702 and the crude product inlet 701 are located at the top and are both equipped with check valves and on / off valves. The top water inlet 702 is in a normally open state with a fixed opening degree to ensure that the water level in the continuous phase separation device 7 remains stable. The water outlet 703 is located at the bottom and the crude product outlet 704 is located in the middle. Both the water outlet 703 and the crude product outlet 704 are equipped with density sensors to monitor the status of the outlet material.

[0049] The crude product outlet 704 of the continuous phase separation device 7 is connected to the distillation column 8 via the feed pump 707. The distillation column 8 is equipped with a third condenser 801. The distillation column 8 is equipped with a third top outlet 802 and a third bottom outlet 803.

[0050] In this embodiment, the third top outlet 802 is connected to the first condenser 9. After cooling, the product is transferred to the first storage tank 10 to recover the solvent, which can be used in the Grignard reaction. The third bottom outlet 803 is connected to the second condenser 11. After being cooled by the condenser, the product is transported to the second storage tank 12 for storing the prothioconazole intermediate. The distillation column 8 can be any type of plate column, packed column, membrane column, etc.

[0051] Finally, it should be noted that the above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Although the present utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. A preparation apparatus, characterized in that, include: Solvent mixing vessel (1); The output end of the solvent mixing vessel (1) is connected to the solvent dropping vessel (2), and the output end of the solvent dropping vessel (2) is connected to the preparation tower (3); The preparation tower (3) is connected to a first feeding device (4) above it, and the output end of the preparation tower (3) is connected to an addition tower (5); The addition tower (5) is connected to a second feeding device (6), and the output end of the addition tower (5) is connected to a continuous phase separation device (7); The output end of the continuous phase separation device (7) is connected to the distillation column (8). The top of the distillation column (8) is connected to the first condenser (9). The output end of the first condenser (9) is connected to the first storage tank (10). The bottom of the distillation column (8) is connected to the second condenser (11). The output end of the second condenser (11) is connected to the second storage tank (12). The second storage tank (12) is used to store the prepared prothioconazole intermediate.

2. The preparation apparatus according to claim 1, characterized in that: The solvent mixing vessel (1) is equipped with a first stirring rod (101); The output end of the solvent dropping vessel (2) is equipped with a solvent feed pump (201), which is connected to the bottom of the preparation tower (3).

3. The preparation apparatus according to claim 1, characterized in that: The inner side of the preparation tower (3) is divided into several interconnected cavities by a perforated tower plate (301). The inner side of the cavities is filled with packing material (302), and the inner and outer sides of the preparation tower (3) are provided with cooling layers (303).

4. The preparation apparatus according to claim 1, characterized in that: The preparation tower (3) is provided with a solvent inlet (304), a first material inlet (305), a first top outlet (306) and a first bottom outlet (307). The bottom of the preparation tower (3) is also provided with a first waste outlet (308). The first top outlet (306) and the first bottom outlet (307) are connected to the addition tower (5) through a first transfer pump (309).

5. The preparation apparatus according to claim 4, characterized in that: The first feeding device (4) includes a storage bin (401), on which a first motor (402) and a first rotary rod (403) are provided. A conveying pipe (404) is provided at the outlet below the storage bin (401). A second motor (405) and a second rotary rod (406) are provided on the conveying pipe (404). The output end of the conveying pipe (404) is connected to the first material inlet (305) at the top of the preparation tower (3).

6. The preparation apparatus according to claim 1, characterized in that: The inner side of the addition tower (5) is provided with a diversion tower plate (501), and the upper and lower sides of the diversion tower plate (501) are provided with a number of protrusions, and the adjacent diversion tower plates (501) are staggered through the protrusions.

7. The preparation apparatus according to claim 1, characterized in that: The addition tower (5) is provided with a reagent inlet (502), a second material inlet (503), a second top outlet (504) and a second bottom outlet (505). The bottom of the addition tower (5) is also provided with a second waste outlet (506). The second top outlet (504) and the second bottom outlet (505) are connected to the continuous phase separation device (7) through a second transfer pump (507).

8. The preparation apparatus according to claim 1, characterized in that: The continuous phase separation device (7) is provided with a crude product inlet (701), a water inlet (702), a water outlet (703) and a crude product outlet (704); The inner side of the continuous phase separation device (7) is provided with a second stirring rod (705) and a phase separation plate (706).

9. The preparation apparatus according to claim 8, characterized in that: The crude product outlet (704) of the continuous phase separation device (7) is connected to the distillation column (8) via a feed pump (707), and the distillation column (8) is equipped with a third condenser (801).

10. The preparation apparatus according to claim 1, characterized in that: The distillation column (8) is provided with a third top outlet (802) and a third bottom outlet (803).

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