Monomethyl cyclopentadiene dropwise adding type cyclic sodium reaction device

Abstract

The utility model belongs to the technical field of organic synthesis equipment, and particularly relates to a monomethyl cyclopentadiene dripping type cyclic sodium reaction device which comprises a support frame, a cyclic sodium reaction kettle, two liquid storage tanks, a mounting frame, a driving component, a hollow shaft, a stirring component, two dripping feeding components and a reaction endpoint judging component, the cyclic sodium reaction kettle and the two liquid storage tanks are fixedly installed on the supporting frame, the two liquid storage tanks are located on the two sides of the cyclic sodium reaction kettle respectively, the two dropwise adding and feeding assemblies are arranged on the cyclic sodium reaction kettle and connected with the corresponding liquid storage tanks respectively, and the installation frame is fixedly installed at the top of the cyclic sodium reaction kettle. The hollow shaft is rotatably mounted on the sodium annulus reaction kettle, and the driving assembly is arranged on the mounting frame and is connected with the hollow shaft. The reaction kettle is reasonable in design, has the advantages of compact structure, good stirring effect, accurate dropwise adding, accurate reaction endpoint judgment, convenience in operation and the like, and has higher practical value and application prospect.

Description

Technical Field

[0001] This utility model relates to the field of organic synthesis equipment technology, and in particular to a monomethylcyclopentadiene dropwise sodium cyclosynthetic reaction apparatus. Background Technology

[0002] In the field of organic synthesis, the reaction of monomethylcyclopentadiene with sodium cyclopentadiene is a key step in the preparation of certain important organic compounds. However, traditional monomethylcyclopentadiene dropwise sodium cyclopentadiene reaction apparatus has many drawbacks.

[0003] From the perspective of device structure, the early reaction devices had unstable connections between various components, which were prone to loosening and displacement during long-term use. This not only affected the stability of the device but also may lead to safety issues such as leakage during the reaction process, seriously reducing the durability and service life of the device.

[0004] In the material mixing stage, previous equipment lacked effective stirring components, resulting in uneven mixing of materials in the reactor, leading to low reaction efficiency and inconsistent product quality. This not only increased production costs but also made it difficult to meet the requirements of industrial production for product quality stability.

[0005] In terms of material drop addition, conventional drop addition methods are difficult to control precisely, cannot guarantee that the material is added at the predetermined rate and amount, and lack reasonable dispersion design, so that the material cannot be quickly and evenly dispersed after entering the reactor, which further affects the mixing rate and reaction effect.

[0006] Traditional methods for determining the reaction endpoint rely primarily on observing single bubbles, which is highly susceptible to human error and lacks accuracy and reliability. This can lead to over- or under-reaction, affecting product yield and quality.

[0007] In summary, existing monomethylcyclopentadiene dropwise sodium cyclocarbon reaction apparatuses have significant shortcomings in terms of structural stability, stirring effect, dropwise accuracy, and reaction endpoint determination. There is an urgent need for a more rationally designed and superior reaction apparatus to improve reaction efficiency and product quality. Based on this, this utility model provides a novel monomethylcyclopentadiene dropwise sodium cyclocarbon reaction apparatus.

[0008] The information disclosed in this background section is intended only to enhance the understanding of the overall background of this utility model and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Utility Model Content

[0009] The purpose of this invention is to address the shortcomings mentioned in the background section by providing a monomethylcyclopentadiene dropwise sodium cycloaddition reaction apparatus.

[0010] The above-mentioned technical objective of this utility model is achieved through the following technical solution: a monomethylcyclopentadiene drop-type sodium cyclocarbon reaction device, comprising a support frame, a sodium cyclocarbon reaction vessel, two storage tanks, a mounting frame, a drive assembly, a hollow shaft, a stirring assembly, two drop-feeding assemblies, and a reaction endpoint determination assembly;

[0011] The sodium cyclic reactor and two storage tanks are fixedly mounted on the support frame, and the two storage tanks are located on both sides of the sodium cyclic reactor. Two drip feeding components are set on the sodium cyclic reactor and connected to the corresponding storage tanks. The mounting frame is fixedly mounted on the top of the sodium cyclic reactor. The hollow shaft is rotatably mounted on the sodium cyclic reactor. The drive component is set on the mounting frame and connected to the hollow shaft. The stirring component is set on the hollow shaft. The reaction endpoint determination component is set on the support frame and connected to the hollow shaft. Multiple air inlets are opened at the upper middle position of the hollow shaft.

[0012] The bottom of the sodium cyclic reactor is fixedly equipped with a discharge pipe, and a discharge control valve is fixedly installed on the discharge pipe.

[0013] Preferably, the stirring assembly includes multiple stirring rods and multiple stirring paddles. Multiple stirring rods and multiple stirring paddles are radially fixedly mounted on a hollow shaft. The multiple stirring rods are all located above the multiple stirring paddles, and the contour of the stirring paddles on the side away from the hollow shaft is adapted to the inner wall of the sodium ring reactor.

[0014] Preferably, the drive assembly includes a motor, a drive gear, and a driven gear. The motor is fixedly mounted on the mounting bracket, the drive gear is fixedly sleeved on the output shaft of the motor, and the driven gear is fixedly sleeved on the hollow shaft. The drive gear and the driven gear mesh with each other.

[0015] Preferably, the drip feeding assembly includes a delivery pipe, a metering pump, and a dispersing pipe. Two delivery pipes are symmetrically fixedly installed on the sodium cyclohexane reactor based on the mounting frame. The ends of the two delivery pipes away from the sodium cyclohexane reactor extend into the corresponding storage tanks. A metering pump is installed on the delivery pipe. One end of the delivery pipe extends into the sodium cyclohexane reactor and is fixedly installed with an arc-shaped dispersing pipe. The dispersing pipe has multiple downward-facing through holes.

[0016] Preferably, the reaction endpoint determination component includes a bubble observer, an air inlet pipe, an exhaust pipe, and an observation mirror. The bubble observer is fixedly installed on the support frame, and the observation mirror is fixedly installed at the center of the top of the bubble observer. The exhaust pipe and the air inlet pipe are fixedly installed on the bubble observer, and the air inlet pipe is rotatably and sealed to the top of the hollow shaft.

[0017] Preferably, the reaction endpoint determination component further includes a potential measuring instrument and three electrodes. The potential measuring instrument is fixedly installed on the front side of the bubble observer, and three electrodes extending into the bubble observer are connected to the potential measuring instrument.

[0018] Preferably, the three electrodes are a reference electrode, a working electrode, and a counter electrode.

[0019] Preferably, an inlet pipe is fixedly installed on the liquid storage tank, and the inlet of the inlet pipe is set downward.

[0020] The beneficial effects of this utility model are:

[0021] 1. The structure is compact and the design is reasonable. The connection between the components is stable and reliable, which improves the overall stability and durability of the reaction device.

[0022] 2. The stirring components ensure that the materials are fully stirred and mixed in the sodium ring reactor, thereby improving reaction efficiency and product quality.

[0023] 3. The design of the drip feeding component, through the combined use of a metering pump and a dispersion tube, enables precise dripping and initial dispersion of materials, further improving the mixing rate and reaction effect.

[0024] 4. The introduction of the reaction endpoint determination component not only allows for the determination of the reaction endpoint by observing bubbles, but also by monitoring the potential changes in the reaction system, thereby improving the accuracy and reliability of the reaction endpoint determination.

[0025] In summary, this monomethylcyclopentadiene dropwise sodium cycloaddition reaction apparatus has advantages such as compact structure, reasonable design, good stirring effect, precise dropwise addition, accurate determination of reaction endpoint, and convenient operation. It is suitable for the reaction process of monomethylcyclopentadiene and sodium cycloaddition and has high practical value and application prospects. Attached Figure Description

[0026] To more clearly illustrate the technical solutions in the embodiments of this utility model, the drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0027] Figure 1 This is a three-dimensional structural schematic diagram of a monomethylcyclopentadiene dropwise sodium cyclorea reaction apparatus proposed in this utility model;

[0028] Figure 2 for Figure 1 A schematic diagram of the cross-sectional structure;

[0029] Figure 3 This is a schematic diagram of the drive assembly, hollow shaft, stirring assembly, and air inlet portion proposed in this utility model.

[0030] Figure 4 This is a schematic diagram of the structure of the drip feeding component proposed in this utility model;

[0031] Figure 5 This is a schematic diagram of the reaction endpoint determination component proposed in this utility model;

[0032] Figure 6 This is a schematic diagram of the electrode and potential measuring instrument components proposed in this utility model.

[0033] In the diagram: 1. Support frame; 2. Sodium cyclic reactor; 201. Discharge pipe; 202. Mounting frame; 21. Hollow shaft; 211. Stirring rod; 212. Stirring paddle; 22. Motor; 221. Drive gear; 222. Driven gear; 3. Storage tank; 31. Delivery pipe; 32. Metering pump; 33. Dispersion pipe; 4. Bubble observer; 401. Air inlet pipe; 402. Exhaust pipe; 41. Sight glass; 42. Potentiometer; 421. Electrode. Detailed Implementation

[0034] The technical solution of this utility model will now be clearly and completely described with reference to specific embodiments. Obviously, the described embodiments are only a part of the embodiments of this utility model, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this utility model without creative effort are within the scope of protection of this utility model.

[0035] Reference Figure 1-6A monomethylcyclopentadiene drop-type sodium cyclocarbonate reaction device includes a support frame 1, a sodium cyclocarbonate reaction vessel 2, two storage tanks 3, a mounting frame 202, a drive assembly, and a hollow shaft 21. The sodium cyclocarbonate reaction vessel 2 and the two storage tanks 3 are fixedly mounted on the support frame 1, with the two storage tanks 3 located on opposite sides of the sodium cyclocarbonate reaction vessel 2. Two delivery pipes 31 are symmetrically fixedly mounted on the sodium cyclocarbonate reaction vessel 2, centered on the mounting frame 202. The ends of the two delivery pipes 31 away from the sodium cyclocarbonate reaction vessel 2 extend into their respective storage tanks 3. A metering pump 32 is installed on each delivery pipe 31. One end of each delivery pipe 31 extends into the sodium cyclocarbonate reaction vessel 2 and is fixedly mounted with an arc-shaped dispersion pipe 33. The dispersion pipe 33 has multiple downward-facing through holes, allowing material to be added to the sodium cyclocarbonate reaction vessel 2 via drop-feeding. Simultaneously, during the drop-feeding operation... The initial dispersion is achieved, thereby increasing the mixing rate. The mounting bracket 202 is fixedly installed on the top of the sodium cyclic reactor 2. The hollow shaft 21 is rotatably installed on the sodium cyclic reactor 2, and multiple air inlets are opened in the upper middle part of the hollow shaft 21. The mounting bracket 202 is fixedly installed with a motor 22. The output shaft of the motor 22 is fixedly fitted with a drive gear 221, and the hollow shaft 21 is fixedly fitted with a driven gear 222. The drive gear 221 and the driven gear 222 mesh with each other and can provide driving force for the hollow shaft 21. Multiple stirring rods 211 and multiple stirring paddles 212 are radially fixedly installed on the hollow shaft 21. The multiple stirring rods 211 are all located above the multiple stirring paddles 212, and the contour of the side of the stirring paddle 212 away from the hollow shaft 21 is adapted to the inner side wall of the sodium cyclic reactor 2, so that the material can be stirred when the hollow shaft 21 rotates.

[0036] A bubble observer 4 is fixedly installed on the support frame 1. An observation mirror 41 is fixedly installed at the center of the top of the bubble observer 4. An exhaust pipe 402 and an air inlet pipe 401 are fixedly installed on the bubble observer 4. The air inlet pipe 401 is sealed and rotatably connected to the top of the hollow shaft 21. The reaction endpoint can be determined by manually observing the bubbles. A potential measuring instrument 42 is fixedly installed on the front side of the bubble observer 4. Three electrodes 421 extending into the bubble observer 4 are connected to the potential measuring instrument 42. The reaction endpoint can be determined by monitoring the potential change of the reaction system, so as to more accurately determine the reaction endpoint. The three electrodes 421 are the reference electrode 421, the working electrode 421, and the counter electrode 421, respectively.

[0037] A discharge pipe 201 is fixedly installed at the bottom of the sodium cyclic reactor 2, and a discharge control valve is fixedly installed on the discharge pipe 201.

[0038] In this embodiment, in order to ensure the air pressure balance in the storage tank 3 when the metering pump 32 extracts materials through the delivery pipe 31, and to facilitate the addition of materials to the storage tank 3, an inlet pipe is fixedly installed on the storage tank 3, and the inlet of the inlet pipe is set downward.

[0039] The circuits, electronic components, and module mechanisms involved all employ existing technologies, which can be fully implemented by those skilled in the art, and need no further explanation. The content protected by this application does not involve any improvement to the software, circuits, or methods.

[0040] Working principle: In operation, first connect the power supply, add the monomethylcyclopentadiene and sodium cyclopentadiene to be reacted into the two storage tanks 3 respectively, and then control the dripping rate of the materials through the metering pump 32. The materials enter the dispersion tube 33 through the conveying pipe 31, and then enter the sodium cyclopentadiene reaction vessel 2 by dripping through the through hole on the dispersion tube 33. During the dripping process, preliminary dispersion is carried out, thereby improving the mixing rate. At the same time, the motor 22 is started. The output shaft of the motor 22 drives the drive gear 221 to rotate, the drive gear 221 drives the driven gear 222 to rotate, and the driven gear 222 drives the hollow shaft 21. The hollow shaft 21 rotates, driving the stirring rod 211 and the stirring paddle 212 to rotate, stirring the materials in the sodium cyclic reactor 2, so that the materials can be fully mixed and the reaction efficiency can be improved. During the reaction, the bubble situation in the bubble observer 4 can be observed through the sight glass 41 to determine the reaction endpoint. At the same time, the potential measuring instrument 42 monitors the potential change of the reaction system in real time. When the potential reaches the preset value, the reaction endpoint can also be determined, thereby improving the accuracy and reliability of the reaction endpoint determination. After the reaction is completed, the discharge control valve is opened to discharge the reaction products from the discharge pipe 201.

[0041] The above provides a detailed description of the monomethylcyclopentadiene dropwise sodium cyclocarbon reaction apparatus provided by this utility model. Specific embodiments have been used to illustrate the principle and implementation of this utility model. The descriptions of the embodiments above are only for the purpose of helping to understand the method and core idea of ​​this utility model. It should be noted that those skilled in the art can make several improvements and modifications to this utility model without departing from the principle of this utility model, and these improvements and modifications also fall within the protection scope of the claims of this utility model.

Claims

1. A single methyl cyclopentadiene dropwise ring sodium reaction apparatus, characterized by, The device comprises a support frame (1), a ring sodium reaction kettle (2), two liquid storage tanks (3), a mounting frame (202), a driving assembly, a hollow shaft (21), a stirring assembly, two drop feeding assemblies and a reaction endpoint judgment assembly. The ring sodium reaction kettle (2) and the two liquid storage tanks (3) are fixedly installed on the support frame (1), and the two liquid storage tanks (3) are respectively located on the two sides of the ring sodium reaction kettle (2). The two drop feeding assemblies are arranged on the ring sodium reaction kettle (2) and are respectively connected with the corresponding liquid storage tanks (3). The mounting frame (202) is fixedly installed on the top of the ring sodium reaction kettle (2). The hollow shaft (21) is rotatably installed on the ring sodium reaction kettle (2). The driving assembly is arranged on the mounting frame (202) and is connected with the hollow shaft (21). The stirring assembly is arranged on the hollow shaft (21). The reaction endpoint judgment assembly is arranged on the support frame (1) and is connected with the hollow shaft (21). A plurality of air inlet holes are formed in the upper middle part of the hollow shaft (21). The bottom of the ring sodium reaction kettle (2) is fixedly installed with a discharge pipe (201), and the discharge pipe (201) is fixedly installed with a discharge control valve.

2. The single methyl cyclopentadiene dropwise ring sodium reaction device according to claim 1, characterized in that: The stirring assembly comprises a plurality of stirring rods (211) and a plurality of stirring paddles (212). The hollow shaft (21) is fixedly installed with the plurality of stirring rods (211) and the plurality of stirring paddles (212) in a radial direction. The plurality of stirring rods (211) are located above the plurality of stirring paddles (212), and the profile of the stirring paddles (212) away from the hollow shaft (21) is matched with the inner side wall of the ring sodium reaction kettle (2).

3. The single methyl cyclopentadiene dropwise ring sodium reaction device according to claim 1, characterized in that: The driving assembly comprises a motor (22), a driving gear (221) and a driven gear (222). The motor (22) is fixedly installed on the mounting frame (202). The output shaft of the motor (22) is fixedly sleeved with the driving gear (221). The hollow shaft (21) is fixedly sleeved with the driven gear (222). The driving gear (221) and the driven gear (222) are engaged.

4. The single methyl cyclopentadiene drop feed cyclo sodium reaction device according to claim 1, characterized in that: The drop feeding assembly comprises a conveying pipe (31), a quantitative pump (32) and a dispersing pipe (33). The ring sodium reaction kettle (2) is fixedly installed with two conveying pipes (31) in a symmetrical manner based on the mounting frame (202) as the center. The ends of the two conveying pipes (31) away from the ring sodium reaction kettle (2) respectively extend into the corresponding liquid storage tanks (3). The conveying pipe (31) is provided with the quantitative pump (32). The conveying pipe (31) is fixedly installed with the arc-shaped dispersing pipe (33) extending into the ring sodium reaction kettle (2). A plurality of downwardly arranged through holes are formed in the dispersing pipe (33).

5. The single methyl cyclopentadiene drop feed cyclo sodium reaction apparatus according to claim 1, characterized in that: The reaction endpoint judgment assembly comprises a bubble observer (4), an air inlet pipe (401), an air outlet pipe (402) and an observation mirror (41). The bubble observer (4) is fixedly installed on the support frame (1). The observation mirror (41) is fixedly installed on the top of the bubble observer (4) in a central position. The bubble observer (4) is fixedly installed with the air outlet pipe (402) and the air inlet pipe (401). The air inlet pipe (401) is sealingly and rotatably connected with the top end of the hollow shaft (21).

6. The single methyl cyclopentadiene drop feed cyclo sodium reaction apparatus according to claim 5, characterized in that: The reaction end point judging assembly further comprises a potential measuring instrument (42) and three electrodes (421), the front side of the bubble observer (4) is fixedly provided with the potential measuring instrument (42), and the potential measuring instrument (42) is connected with the three electrodes (421) extending into the bubble observer (4).

7. The single methyl cyclopentadiene drop feed cyclo sodium reaction apparatus according to claim 6, characterized in that: The three electrodes (421) are respectively a reference electrode (421), a working electrode (421) and a counter electrode (421).

8. The single methyl cyclopentadiene drop feed cyclo sodium reaction apparatus of claim 1, wherein: The liquid inlet pipe is fixedly installed on the liquid storage tank (3), and the inlet of the liquid inlet pipe is downwardly arranged.

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