Condensation kettle convenient to sample and used for flonicamid production
By using a hollow connecting column and peristaltic pump system in the condensation kettle for fluoridaimide production, the problem of real-time sampling in the fluoridaimide production process is solved, and stable sampling of reaction materials and continuous reactions are achieved.
Patent Information
- Application Number
- CN202422376724.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-29
- Publication Date
- 2025-07-18
- Estimated Expiration
- 2034-09-29
AI Technical Summary
In the production process of fluoridamid, it is difficult for the prior art to achieve real-time sampling without interfering with the reaction process in the reactor, and the sampling mechanism is prone to cause interactions between inside and outside the reactor.
A condensation kettle for the production of fluoridinamide that is convenient for sampling is designed. It adopts a hollow structure connecting column and sampling mechanism. By aspirating peristaltic pump and discharge peristaltic pump, the circulating sampling of reaction materials is realized, and the interaction between inside and outside the reactor is avoided.
Real-time sampling of reaction materials at different time periods is achieved, and the sampling process does not affect the normal reaction in the reaction kettle, ensuring the continuity and stability of the reaction.
Smart Images
Figure CN223113069U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the field of sampling of condensation reactors, and specifically relates to a condensation kettle for flonicamid production that is convenient for sampling. Background Art
[0002] When preparing flonicamid, 4-trifluoromethylnicotinic acid is used as the starting material, and the reaction of acyl chloride and amine is carried out directly. And 4-trifluoromethylnicotinic acid uses methyl 3-methoxyacrylate and 4-amino-1,1,1-trifluoro-3-buten-2-one as the starting materials, and under alkaline conditions, it undergoes condensation, cyclization, and hydrolysis reactions in sequence.
[0003] During the reaction process, real-time sampling is required. When performing real-time sampling, it is necessary to pay attention to avoiding interaction between the inside and outside of the reaction kettle, and during the process of the sampling mechanism, the normal reaction process inside the reaction kettle shall not be disturbed. Summary of the Utility Model
[0004] The purpose of the utility model is to provide a condensation kettle for flonicamid production that is convenient for sampling in order to solve the problems raised in the above background art.
[0005] To achieve the above purpose, the utility model provides the following technical solution: A condensation kettle for flonicamid production that is convenient for sampling, including a reaction kettle, a stirrer extending into the interior of the reaction kettle is installed at the top of the reaction kettle, a connecting column that penetrates to the outside of the reaction kettle is fixedly installed outside the stirrer inside the reaction kettle. The connecting column is of a hollow structure, and the bottom end of the connecting column is of an open structure, and the top end of the connecting column is of a closed structure. A sampling mechanism extending to the outside of the reaction kettle is installed inside the connecting column. The sampling mechanism includes a support plate fixedly connected to the outside of the reaction kettle through a bracket, a connecting head penetrating below the support plate is fixedly installed at the top end of the support plate, and a sampling bottle is threadedly connected to the outer wall of the connecting head below the support plate.
[0006] As a further solution of the utility model: The sampling mechanism further includes a connecting pipe and a circulation pipe. The output end of the connecting pipe penetrates the connecting head and extends into the inner cavity of the sampling bottle. The input end of the circulation pipe penetrates the connecting head and extends into the inner cavity of the sampling bottle. The height of the output end of the connecting pipe is located at the height of the input end of the circulation pipe.
[0007] As a further solution of the utility model: The sampling mechanism further includes a suction peristaltic pump connected to the input end of the connecting pipe and a discharge peristaltic pump connected to the output end of the circulation pipe. The input end of the suction peristaltic pump is connected to a sampling pipe, and the output end of the discharge peristaltic pump is connected to a reflux pipe. Valves are installed on both the sampling pipe and the reflux pipe.
[0008] As a further solution of the utility model: both the sample injection tube and the reflux tube penetrate through the top of the connecting column and extend into the inside of the connecting column, and sealing rings are arranged at the contact positions between the connecting column and the sample injection tube and the reflux tube.
[0009] As a further solution of the utility model: the end of the output end of the reflux tube is bent at a right angle, a round hole is formed in the side wall of the connecting column, and the end of the output end of the reflux tube is located in the round hole.
[0010] As a further solution of the utility model: the input end of the sample injection tube is flush with the bottom end of the connecting column.
[0011] Compared with the prior art, the beneficial effects of the utility model are:
[0012] 1. By setting the sampling mechanism, the reactants at different time periods can be sampled in real time, and there is no interaction between the inside and outside of the reaction kettle during the sampling process, and the normal progress of the reaction will not be affected. BRIEF DESCRIPTION OF THE DRAWINGS
[0013] Figure 1 is a structural schematic diagram of the utility model;
[0014] Figure 2 is a structural schematic diagram of the sampling mechanism of the utility model;
[0015] Figure 3 is a structural schematic diagram of the inside of the connecting column of the utility model.
[0016] In the figure: 1, reaction kettle; 2, stirrer; 3, connecting column; 4, round hole; 5, bracket; 6, support plate; 7, sample injection tube; 8, reflux tube; 9, discharge peristaltic pump; 10, suction peristaltic pump; 11, valve; 12, connecting pipe; 13, connector; 14, sampling bottle; 15, circulation pipe. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0017] Next, the technical solutions in the embodiments of the present utility model will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present utility model. Obviously, the described embodiments are only a part of the embodiments of the present utility model, rather than all the embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present utility model.
[0018] Please refer to Figures 1 to 3, in the embodiment of the present utility model, a condensation kettle for the production of flonicamid that is convenient for sampling includes a reaction kettle 1. A stirrer 2 extending into the interior of the reaction kettle 1 is installed at the top of the reaction kettle 1. Inside the reaction kettle 1, a connecting column 3 that penetrates to the outside of the reaction kettle 1 is fixedly installed on the outside of the stirrer 2. The connecting column 3 is of a hollow structure, and the bottom end of the connecting column 3 is of an open structure, while the top of the connecting column 3 is of a closed structure. A sampling mechanism extending to the outside of the reaction kettle 1 is installed inside the connecting column 3. The sampling mechanism includes a support plate 6 fixedly connected to the outside of the reaction kettle 1 through a bracket 5. At the top end of the support plate 6, a connecting head 13 penetrating below the support plate 6 is fixedly installed. A sampling bottle 14 is threadedly connected to the outer wall of the connecting head 13 below the support plate 6.
[0019] In this embodiment: When preparing flonicamid, 4-trifluoromethylnicotinic acid is used as the starting material, and it is prepared by the reaction of acyl chloride and amine. And 4-trifluoromethylnicotinic acid can use methyl 3-methoxyacrylate and 4-amino-1,1,1-trifluoro-3-buten-2-one as the starting materials. Under alkaline conditions, through condensation, cyclization, and hydrolysis reactions in sequence, 4-trifluoromethylnicotinic acid is prepared. During the condensation reaction process, the reaction is carried out in the reaction kettle. During the reaction process, by starting the sampling mechanism, the sampling mechanism sucks the materials in the reaction process into the sampling bottle 14 and then circulates back into the reaction kettle 1 through the sampling bottle 14 again. Therefore, when it is necessary to remove the sampling bottle 14 at the corresponding time period, by closing the two valves 11 and respectively closing the suction peristaltic pump 10 and the discharge peristaltic pump 9, at this time, the sampling bottle 14 can be rotated and unscrewed, and a new sampling bottle 14 can be threadedly connected to the connecting head 13, thus realizing the sampling of the reactants at different time periods.
[0020] Please refer specifically to Figure 1 、 Figure 2 and Figure 3 , the sampling mechanism further includes a connecting pipe 12 and a circulation pipe 15. The output end of the connecting pipe 12 penetrates the connecting head 13 and extends into the inner cavity of the sampling bottle 14. The input end of the circulation pipe 15 penetrates the connecting head 13 and extends into the inner cavity of the sampling bottle 14. The height of the output end of the connecting pipe 12 is located at the height of the input end of the circulation pipe 15. The sampling mechanism further includes a suction peristaltic pump 10 connected to the input end of the connecting pipe 12 and a discharge peristaltic pump 9 connected to the output end of the circulation pipe 15. The input end of the suction peristaltic pump 10 is connected to a sampling pipe 7, and the output end of the discharge peristaltic pump 9 is connected to a reflux pipe 8. Valves 11 are installed on both the sampling pipe 7 and the reflux pipe 8. The sampling pipe 7 and the reflux pipe 8 both penetrate to the top of the connecting column 3 and extend into the inside of the connecting column 3, and seals are provided at the contact positions between the connecting column 3 and the sampling pipe 7 and the reflux pipe 8.
[0021] In this embodiment: During the reaction process, by opening two valves 11, the suction peristaltic pump 10, and the discharge peristaltic pump 9, the started suction peristaltic pump 10 sucks the reaction material into the connecting pipe 12 through the sampling pipe 7. The reaction material enters the sampling bottle 14 through the connecting pipe 12. The reaction material that enters the sampling bottle 14 is sucked again by the operating discharge peristaltic pump 9 and returns to the reaction kettle 1 through the circulation pipe 15 and the reflux pipe 8. Therefore, reaction materials with different reaction times and degrees can enter the sampling bottle 14. When sampling, by closing the suction peristaltic pump 10, the discharge peristaltic pump 9, and the two valves 11, the sampling bottle 14 can be rotated and unscrewed, and a new sampling bottle 14 can be taken and threadedly connected to the connector 13. After connection, the two valves 11, the suction peristaltic pump 10, and the discharge peristaltic pump 9 can be opened, and the reaction material can continuously pass through the sampling bottle 14 again.
[0022] Please refer specifically to Figure 1 and Figure 3 , the end of the output end of the reflux pipe 8 is bent at a right angle. A round hole 4 is opened on the side wall of the connecting column 3. The end of the output end of the reflux pipe 8 is located in the round hole 4. The input end of the sampling pipe 7 is flush with the bottom end of the connecting column 3.
[0023] In this embodiment: Since the ports of the reflux pipe 8 and the sampling pipe 7 are in a vertically misaligned state, the reaction material that returns to the reaction kettle 1 through the reflux pipe 8 will not be sucked into the sampling pipe 7 again while being discharged.
[0024] The above is only the preferred specific implementation manner of the present utility model, but the protection scope of the present utility model is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present utility model, according to the technical solution of the present utility model and its inventive concept, makes equivalent substitutions or changes, and all should be covered within the protection scope of the present utility model.
Claims
1. A condensation kettle for the production of flonicamid that is convenient for sampling, comprising a reaction kettle (1), wherein a stirrer (2) extending into the interior of the reaction kettle (1) is installed at the top of the reaction kettle (1), and is characterized in that, A connecting column (3) which is fixedly installed outside the stirrer (2) inside the reactor (1) penetrates to the outside of the reactor (1). The connecting column (3) is of a hollow structure, and the bottom end of the connecting column (3) is of an open structure, and the top of the connecting column (3) is of a closed structure. A sampling mechanism extending to the outside of the reactor (1) is installed inside the connecting column (3). The sampling mechanism includes a support plate (6) fixedly connected to the outside of the reactor (1) through a bracket (5). The top end of the support plate (6) is fixedly installed with a connecting head (13) penetrating below the support plate (6). A sampling bottle (14) is threadedly connected to the outer wall of the connecting head (13) below the support plate (6).
2. The condensation kettle for flonicamid production that is convenient for sampling according to claim 1, wherein The sampling mechanism further includes a connecting pipe (12) and a circulating pipe (15). The output end of the connecting pipe (12) penetrates the connecting head (13) and extends into the inner cavity of the sampling bottle (14). The input end of the circulating pipe (15) penetrates the connecting head (13) and extends into the inner cavity of the sampling bottle (14). The height of the output end of the connecting pipe (12) is located at the height of the input end of the circulating pipe (15).
3. The condensation kettle for flonicamid production that is convenient for sampling according to claim 2, wherein, The sampling mechanism further includes a suction peristaltic pump (10) connected to the input end of the connecting pipe (12) and a discharge peristaltic pump (9) connected to the output end of the circulating pipe (15). The input end of the suction peristaltic pump (10) is connected with a sampling pipe (7). The output end of the discharge peristaltic pump (9) is connected with a reflux pipe (8). Valves (11) are installed on both the sampling pipe (7) and the reflux pipe (8).
4. A condensation kettle for flonicamid production that is convenient for sampling according to claim 3, characterized in that, Both the sampling pipe (7) and the reflux pipe (8) penetrate to the top of the connecting column (3) and extend into the inside of the connecting column (3). Sealing rings are arranged at the contact positions between the connecting column (3) and the sampling pipe (7) and the reflux pipe (8).
5. The condensation kettle for flonicamid production that is convenient for sampling according to claim 4, wherein, The output end of the reflux pipe (8) is bent at a right angle. A round hole (4) is formed in the side wall of the connecting column (3). The output end of the reflux pipe (8) is located in the round hole (4).
6. The condensation kettle for flonicamid production that is convenient for sampling according to claim 5, wherein, The input end of the sampling pipe (7) is flush with the bottom end of the connecting column (3).