2-amino-4-trifluoromethyl-pyridine synthesis device and method

Abstract

The invention relates to the technical field of chemical synthesis, in particular to a 2-amino-4-trifluoromethyl-pyridine synthesis device and method.The 2-amino-4-trifluoromethyl-pyridine synthesis device comprises a reaction kettle and a stirring shaft, a plurality of first stirring blades are arranged on the stirring shaft in the circumferential direction, and a plurality of second stirring blades are movably installed on the first stirring blades; a plurality of sliding rods are arranged on the first stirring blade and the second stirring blade in a sliding mode, turbulent flow blades are rotationally arranged on the sliding rods, and mixing strengthening units connected with the turbulent flow blades are arranged on the first stirring blade and the second stirring blade and used for pushing out the turbulent flow blades in the initial stage of reactant mixing. When the 2-amino-4-trifluoromethyl-pyridine synthesis device and method are used, the efficiency and safety of a synthesis process are remarkably improved through cooperation of a dynamic turbulent flow structure and a boundary layer control structure, in the initial stage of reactant mixing, the small turbulent flow blades contained in the stirring blades are accurately pushed out, the turbulence degree of fluid is enhanced, and the efficiency of the synthesis process is improved. And rapid dispersion of a reactant solution is realized.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of chemical synthesis, in particular to a 2-amino-4-trifluoromethyl-pyridine synthesis device and method. BACKGROUND

[0002] 2-amino-4-trifluoromethylpyridine is a pyridine ring derivative with specific substituents, and the amino group at the 2nd position and the trifluoromethyl group at the 4th position in the molecular structure jointly determine its unique chemical properties and functional characteristics. The compound has important application value in the fields of medicinal chemistry, pesticide synthesis and material science, and is often used as a key intermediate to participate in the construction of complex molecules with biological activity. Its synthesis process usually involves multiple organic reactions, including but not limited to nucleophilic substitution, cyclization and amination steps. In the reaction system, the full contact of reactants and the optimization of mass transfer efficiency need to be realized through mixing and stirring operations. At the same time, the reaction conditions need to be accurately controlled to avoid the generation of by-products. In the preparation process, the homogenization degree of mixing and stirring directly affects the reaction rate, product purity and final yield.

[0003] In the mixing reaction process of vinyl ether and trifluoroacetic anhydride in a traditional kettle reactor, due to the limited mass transfer efficiency of mechanical stirring, the reactants need to undergo a long diffusion process to realize molecular-level contact, which leads to uneven distribution of reactant concentration in the local reaction area. This non-uniform mixing state easily causes local enrichment of trifluoroacetic anhydride, which in turn induces its hydrolysis or self-condensation and other side reactions, generating by-products such as trifluoroacetic acid, resulting in a decrease in the chemical purity and yield of the target product 2-amino-4-trifluoromethylpyridine. To solve this problem, the existing technology enhances the mixing efficiency by increasing the shear force and turbulence of high-speed turbine stirrers. However, under high-speed conditions, high-speed shearing of the blade easily causes solid particles to migrate and deposit towards the kettle wall, forming dead zones and reducing reaction efficiency. Moreover, the heat transfer between the local turbulent zone and the dead zone is uneven, leading to large temperature fluctuations in the reaction system and increasing the risk of side reactions. At the same time, maintaining high speed requires a significant increase in motor power, resulting in low energy efficiency. Therefore, we propose a 2-amino-4-trifluoromethyl-pyridine synthesis device and method. SUMMARY

[0004] One technical problem to be solved by the present application is that high-speed shearing of the blade easily causes solid particles to migrate and deposit towards the kettle wall, forming dead zones and reducing reaction efficiency. Moreover, the heat transfer between the local turbulent zone and the dead zone is uneven, leading to large temperature fluctuations in the reaction system and increasing the risk of side reactions. At the same time, maintaining high speed requires a significant increase in motor power, resulting in low energy efficiency.

[0005] To solve the above technical problems, the embodiment of the present application provides a 2-amino-4-trifluoromethyl-pyridine synthesis device and method, which comprises a reaction kettle and a stirring shaft, a plurality of stirring blades one are arranged on the stirring shaft in a circumferential direction, a plurality of stirring blades two are movably arranged on the stirring blades one, a plurality of sliding rods are slidably arranged on the stirring blades one and the stirring blades two, turbulence blades are rotatably arranged on the sliding rods, mixing enhancement units connected with the turbulence blades are arranged on the stirring blades one and the stirring blades two, so as to push out the turbulence blades at the initial stage of mixing of the reactants, and the turbulence mixing of the reactants is carried out, and a heat dissipation unit is arranged in the reaction kettle, so as to dissipate the heat accumulation points generated at the initial stage of mixing due to uneven mixing.

[0006] In some embodiments, the mixing enhancement unit comprises unfolding members arranged on the stirring blades one and the stirring blades two, the turbulence blades are pushed out through the unfolding members, and boundary turbulence members are arranged on the stirring blades two, so as to destroy the boundary laminar flow state of the reaction kettle wall during mixing.

[0007] In some embodiments, the unfolding members comprise receiving bins opened on opposite sides of the stirring blades one and the stirring blades two, the receiving bins on the stirring blades one are communicated with an external gas source through a pipeline, moving grooves are opened on the stirring blades one and the stirring blades two, both ends of the sliding rods extend into the moving grooves, both ends of the sliding rods located in the moving grooves are provided with limiting plates one which are slidably connected with the moving grooves, sliding grooves are opened on the stirring blades one and the stirring blades two, stretch rods are slidably arranged in the sliding grooves, both ends of the stretch rods located in the sliding grooves are provided with limiting plates two, the stretch rods located in the sliding grooves are sleeved with return springs, a fixed plate is arranged on the stirring blades two, an inclined groove is opened in the fixed plate, an inertia ball is movably arranged in the inclined groove, and a one-way valve is arranged on the receiving bin.

[0008] In some embodiments, the boundary turbulence members comprise mounting bins arranged on the stirring blades two, lifting plates are slidably arranged in the mounting bins, a plurality of turbulence rods are arranged on the lifting plates, one end of the turbulence rods penetrates through the mounting bins and is slidably connected with the mounting bins, telescopic rods are arranged in the mounting bins, one end of the telescopic rods is connected with the lifting plates, telescopic springs are sleeved on the telescopic rods, a triangular plate is arranged on the side of the lifting plate away from the turbulence rods, a pushing block is slidably arranged in the mounting bin, the pushing block is in contact with the triangular plate, a positioning plate is arranged in the mounting bin, extrusion springs are arranged on the positioning plate, one end of the extrusion springs is connected with the pushing block, a traction rope is arranged on the pushing block, the traction rope passes through holes in the mounting bin and the moving groove in sequence and is connected with the limiting plate one.

[0009] In some embodiments, the heat dissipation unit comprises a heat conducting member arranged in the reaction kettle, and the heat conducting member is used to dissipate heat from the heat accumulation point in the reactant; a rotating member is arranged on the heat conducting member, and the rotating member is used to drive the heat conducting member to rotate; and an oscillating member is arranged on the heat conducting member, and the oscillating member is used to change the motion state of the heat conducting member after the reactant is mixed.

[0010] In some embodiments, the heat conducting member comprises a mounting plate arranged to rotate in the reaction kettle, a plurality of mounting tubes are arranged to rotate on the mounting plate, one end of the mounting tube penetrates the mounting plate, a plurality of rotating shafts are arranged on the mounting tube, a plurality of hollow heat dissipation blades are arranged on the rotating shaft, and the heat dissipation blades are in communication with the external refrigerant through the pipeline.

[0011] In some embodiments, the rotating member comprises a rotating gear arranged on the mounting tube, and the rotating gear is located at the end of the mounting tube away from the stirring blade; a rotating gear ring is arranged to rotate on the mounting plate, a clamping cavity is arranged on the rotating gear ring, a clamping block is arranged to slide on the stirring shaft, a pressing plate connected with the clamping block is arranged to slide on the stirring shaft, a plurality of connecting rods I are arranged to rotate on the stirring shaft, an oscillating ball is arranged at the end of the connecting rod I, a connecting rod II is arranged to rotate on the connecting rod I, and the connecting rod II is connected with the pressing plate in rotation; a limiting plate III is arranged on the stirring shaft, and a pushing spring is arranged on the stirring shaft between the limiting plate III and the pressing plate.

[0012] In some embodiments, the oscillating member comprises an oscillating gear arranged on the rotating shaft, a connecting rod is arranged to slide in the mounting tube, an oscillating rack engaged with the oscillating gear is arranged on the connecting rod, a pressing spring is arranged at the bottom of the mounting tube, one end of the pressing spring is connected with the connecting rod, a pressing rod is arranged on the connecting rod, one end of the pressing rod penetrates the mounting plate, a pressing block matched with the pressing rod is arranged on the pressing plate, and the pressing block is an arc-shaped block.

[0013] In some embodiments, the adjacent sides of the stirring blade I and the stirring blade II are provided with sawtooth plates.

[0014] In some embodiments, the synthesis method is as follows:

[0015] S1, install the reaction kettle, the stirring shaft and the auxiliary components in place; add trifluoroacetic anhydride, pyridine derivatives and other raw materials into the reaction kettle in proportion;

[0016] S2, the stirring shaft works to drive stirring blade one and stirring blade two to rotate, and the inertial ball slides along the chute under centrifugal force when the stirring shaft rotates, so that stirring blade two is moved under the action of centrifugal force to overcome the elastic force of the return spring, and the sliding rod is moved synchronously, the spoiler blade is pushed out of the storage bin and exposed in the reactant, and at this time the spoiler blade rotates under the push of the reactant to mix the solution in the reactant;

[0017] S3, when stirring blade two is pushed to be close to the side wall of the reaction kettle under centrifugal force, the boundary spoiler works synchronously to push the spoiler rod on the lifting plate out, the spoiler rod is stretched out to be close to the inner wall of the reaction kettle, the boundary layer flow state is destroyed, and the mixing dead angle is eliminated;

[0018] S4, the heat dissipation unit is started, the external refrigerant is input into the hollow heat dissipation blade through the pipeline; the rotating shaft drives the heat dissipation blade to rotate, and accelerates the heat exchange between the refrigerant and the reactant;

[0019] S5, in the initial stage of mixing, the stirring shaft drives the clamping block and the clamping bin to drive the rotating gear ring and the rotating gear to rotate, drives the heat dissipation blade to rotate at high speed, and quickly absorbs the heat of local heat accumulation points;

[0020] S6, in the later stage of reaction, the stirring shaft speed is reduced, so that the pressing plate is lowered, at this time the pressing rod is cyclically extruded by the pressing plate, drives the oscillating gear to reciprocate, switches the heat dissipation blade to oscillation mode, uniformly dissipates heat, and avoids damaging the product crystal.

[0021] The present application has at least the following beneficial effects:

[0022] 1, through the cooperation of the dynamic spoiler structure and the boundary layer control structure, the efficiency and safety of the synthesis process are significantly improved, in the initial stage of reactant mixing, the small spoiler blade stored in the stirring blade is accurately pushed out, the fluid turbulence degree is strengthened, the reactant solution is quickly dispersed, and the side reaction caused by local heat release is effectively reduced; after mixing, the spoiler blade is automatically retracted into the storage bin, inert gas is injected to completely purge the residual reactant, material corrosion caused by the retention of corrosive media such as trifluoroacetic anhydride is avoided, and the synchronous starting of the boundary layer optimization structure can drive the spoiler rod to extend radially, so that it operates with a small gap from the inner wall of the reaction kettle, directly destroys the boundary layer stagnation area, eliminates the traditional stirring dead angle, and ensures the uniformity of mass transfer in the whole reaction system. The design guarantees the mixing efficiency, realizes the double optimization of long-term operation and maintenance of the equipment and reaction selectivity through the dynamic adaptation of the telescopic mechanism;

[0023] 2. The reaction system achieves full-cycle heat dissipation optimization through a dynamic switching mode that adapts to the rotation speed. In the initial stage of mixing, the stirring shaft drives the locking block and locking chamber to mesh, triggering the linkage effect between the rotating gear ring and the rotating gear, driving the heat dissipation blades into a high-speed rotation state, and specifically enhancing the forced convection heat dissipation in the local heat accumulation area. In the later stage of the reaction, as the stirring shaft speed decreases, the pressure plate descends under the action of gravity and periodically squeezes the pressing rod. The linkage oscillating gear drives the heat dissipation blades to switch to a reciprocating oscillation mode. While maintaining the temperature balance across the entire range, the risk of damage to the product lattice structure by high-speed rotation is avoided by reducing the mechanical shear strength. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the overall structure of the present invention;

[0025] Figure 2 This is a schematic diagram of the cross-sectional structure of the reaction vessel of the present invention;

[0026] Figure 3 This is a schematic diagram of the hybrid reinforcement unit structure of the present invention;

[0027] Figure 4 This is a schematic cross-sectional view of stirring blade one and stirring blade two of the present invention;

[0028] Figure 5 For the present invention Figure 4 Enlarged structural diagram of area A in the middle;

[0029] Figure 6 This is a schematic diagram of the exploded structure of stirring blade one and stirring blade two of the present invention;

[0030] Figure 7 This is a schematic diagram of the heat dissipation unit structure of the present invention;

[0031] Figure 8 This is a schematic diagram of the rotating component structure of the present invention;

[0032] Figure 9 This is a schematic diagram of the swing component structure of the present invention;

[0033] Figure 10 For the present invention Figure 9 Enlarged structural diagram of area B in the middle;

[0034] Figure 11 This is a schematic diagram of the structure of Embodiment 2 of the present invention.

[0035] In the figure: 1, reaction kettle; 2, stirring shaft; 3, stirring blade one; 31, stirring blade two; 4, sliding rod; 5, spoiler blade; 6, mixing enhancement unit; 7, unfolding piece; 71, storage bin; 72, moving groove; 73, limit plate one; 74, sliding groove; 75, extension rod; 76, limit plate two; 77, return spring; 78, fixed plate; 79, chute; 710, inertia ball; 711, one-way valve; 8, boundary spoiler; 81, mounting bin; 82, lifting plate; 83, spoiler rod; 84, telescopic rod; 85, telescopic spring; 86, triangular plate; 87, pushing block; 88, positioning plate; 89, extrusion spring; 810, traction rope; 9, heat dissipation unit; 10, heat conduction piece; 101, mounting plate; 102, mounting pipe; 103, rotating shaft; 104, heat dissipation blade; 11, rotating piece; 111, rotating gear; 112, rotating gear ring; 113, clamping bin; 114, clamping block; 115, pressing plate; 116, connecting rod one; 117, swing ball; 118, connecting rod two; 119, limit plate three; 1110, pushing spring; 12, swinging piece; 121, swinging gear; 122, connecting rod; 123, swinging rack; 124, pressing spring; 125, pressing rod; 126, pressing block; 13, sawtooth plate. DETAILED DESCRIPTION

[0036] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative work fall within the scope of protection of the present application.

[0037] Embodiment 1: Please refer to Figures 1-10 The present application provides a technical solution: a 2-amino-4-trifluoromethyl-pyridine synthesis device and method, comprising a reaction kettle 1 and a stirring shaft 2, a plurality of stirring blades one 3 are arranged circumferentially on the stirring shaft 2, a plurality of stirring blades two 31 are movably installed on the stirring blades one 3, a plurality of sliding rods 4 are slidably arranged on the stirring blades one 3 and the stirring blades two 31, spoiler blades 5 are rotatably arranged on the sliding rods 4, mixing enhancement units 6 connected with the spoiler blades 5 are arranged on the stirring blades one 3 and the stirring blades two 31, so as to push out the spoiler blades 5 at the initial stage of mixing of the reactants, and the spoiler blades 5 are used for spoiler mixing of the reactants, a heat dissipation unit 9 is arranged in the reaction kettle 1, so as to dissipate heat accumulation points generated at the initial stage of mixing due to uneven mixing.

[0038] The mixing reinforcing unit 6 comprises unfolding members 7 arranged on the stirring blade one 3 and the stirring blade two 31, and the disturbing blades 5 are pushed out through the unfolding members 7, and the stirring blade two 31 is provided with boundary disturbing members 8 for destroying the boundary layer flow state of the reactor 1 wall during the mixing process.

[0039] The unfolding members 7 comprise receiving bins 71 arranged on opposite sides of the stirring blade one 3 and the stirring blade two 31, and the receiving bin 71 on the stirring blade one 3 is communicated with an external gas source through a pipeline, and the stirring blade one 3 and the stirring blade two 31 are both provided with moving grooves 72, both ends of the sliding rod 4 extend into the moving grooves 72, both ends of the sliding rod 4 located in the moving grooves 72 are both provided with limiting plates one 73 in sliding connection with the moving grooves 72, the stirring blade one 3 and the stirring blade two 31 are both provided with sliding grooves 74, the sliding grooves 74 are both provided with extension rods 75 in sliding connection, both ends of the extension rod 75 located in the sliding grooves 74 are both provided with limiting plates two 76, both ends of the extension rod 75 located in the sliding grooves 74 are both provided with return springs 77, the stirring blade two 31 is provided with a fixed plate 78, the fixed plate 78 is provided with an inclined groove 79, the inclined groove 79 is movably provided with an inert ball 710, and the receiving bin 71 is provided with a one-way valve 711.

[0040] When the reactants are injected into the reactor 1 for synthesis, the stirring shaft 2 starts to work and rotates, and the stirring shaft 2 drives the stirring blade one 3 and the stirring blade two 31 mounted on the stirring shaft 2 to rotate synchronously, at this time, under the action of centrifugal force, the stirring blade two 31 moves away from the stirring blade one 3 by overcoming the elastic force of the return spring 77, at this time, the sliding rod 4 and the disturbing blade 5 located in the stirring blade one 3 are exposed to the reactant solution, and the disturbing blade 5 is rotated by the liquid during rotation, so as to strengthen the degree of fluid turbulence, realize the rapid dispersion of the reactant solution, and effectively reduce the side reaction caused by local heat release, and when the mixing is completed, the stirring blade two 31 is recombined with the stirring blade one 3 by the pushing of the return spring 77, the disturbing blade 5 is retracted into the receiving bin 71, and at the same time, the inert gas is injected into the receiving bin 71 through the external gas tank to discharge the reactants from the one-way valve 711, so as to avoid the material corrosion caused by the stagnation of corrosive media such as trifluoroacetic anhydride.

[0041] The spacing between the stirring blade two 31 and the stirring blade one 3 is dynamically adjusted by the centrifugal force to expose the sliding rod 4 and the spoiler blade 5 to the reaction system during the stirring process. The spoiler blade 5 is passively rotated to generate multidirectional turbulence by using the principle of fluid mechanics, which significantly improves the uniformity of the reactant dispersion, effectively eliminates the local concentration gradient and temperature accumulation, and thus reduces the occurrence of side reactions. After the mixing is completed, the reset spring 77 is used to reset and store the spoiler assembly. Combined with the inert gas purging system and the one-way valve 711 discharge design, it not only prevents the corrosion of high corrosive medium residues on the key components of the equipment, but also ensures the effective isolation of the reaction system and the external environment. The overall structure improves the mixing efficiency while optimizing the durability of the equipment.

[0042] The boundary spoiler 8 comprises a mounting bin 81 arranged on the stirring blade two 31, a lifting plate 82 slidably arranged in the mounting bin 81, a plurality of spoiler rods 83 arranged on the lifting plate 82, one end of the spoiler rod 83 penetrating through the mounting bin 81 and being in sliding connection with the mounting bin 81, a telescopic rod 84 arranged in the mounting bin 81 and one end of the telescopic rod 84 being connected with the lifting plate 82, a telescopic spring 85 sleeved on the telescopic rod 84, a triangular plate 86 arranged on the side of the lifting plate 82 away from the spoiler rod 83, a pushing block 87 slidably arranged in the mounting bin 81, the pushing block 87 being in contact with the triangular plate 86, a positioning plate 88 arranged in the mounting bin 81, an extrusion spring 89 arranged on the positioning plate 88, one end of the extrusion spring 89 being connected with the pushing block 87, and a traction rope 810 arranged on the pushing block 87 and sequentially penetrating through the mounting bin 81 and the through hole of the moving groove 72 and being connected with the limiting plate one 73.

[0043] While the stirring blade two 31 moves, the limiting plate one 73 on the sliding rod 4 generates relative displacement, thereby pulling the traction rope 810. The traction rope 810 is pulled to drive the pushing block 87 to move against the elastic force of the spring, thereby pushing the triangular plate 86. The triangular plate 86 pushes the lifting plate 82 and the spoiler rod 83 fixed on the lifting plate 82 to extend out of the mounting bin 81 during the pushing process, so that they operate with a micro-gap distance from the inner wall of the reaction kettle 1, directly destroy the boundary layer stagnation zone, eliminate the traditional stirring dead angle, and ensure the uniformity of mass transfer in the whole reaction system. When the stirring blade two 31 is reset after the mixing is completed, the spoiler rod 83 is pushed back into the mounting bin 81 by the telescopic spring 85, thereby reducing the corrosion of the reactant to the spoiler rod 83.

[0044] The linkage mechanism of the traction rope 810 is triggered by the stirring blade two 31 displacement, and the synchronous extension and contraction movement of the spoiler rod 83 is accurately controlled: during the stirring process, the limiting plate one 73 traction rope 810 drives the push block 87 to push the triangular plate 86, so that the lifting plate 82 carries the spoiler rod 83 to run along the inner wall of the reaction kettle 1 with a micro interval, directly destroys the fluid boundary layer and eliminates the stirring dead angle; after the mixing is completed, the linkage mechanism is reset in reverse, and the spoiler rod 83 is retracted into the installation bin 81 to avoid the corrosive medium. This design realizes the intelligent switching of dynamic spoiler and static protection through pure mechanical structure, enhances the uniformity of global mass transfer, and significantly improves the durability and system reliability of key components in strong corrosion environment.

[0045] The heat dissipation unit 9 comprises a heat conduction piece 10 arranged in the reaction kettle 1, which is used for dissipating heat of heat accumulation points in the reactants, the heat conduction piece 10 is provided with a rotating piece 11, which is used for driving the heat conduction piece 10 to rotate, and the heat conduction piece 10 is provided with an oscillating piece 12, which is used for changing the movement state of the heat conduction piece 10 after the reactants are mixed.

[0046] The heat conduction piece 10 comprises a mounting plate 101 rotatably arranged in the reaction kettle 1, a plurality of mounting pipes 102 are rotatably arranged on the mounting plate 101, one end of the mounting pipe 102 penetrates the mounting plate 101, a plurality of rotating shafts 103 are arranged on the mounting pipe 102, a plurality of hollow heat dissipation blades 104 are arranged on the rotating shaft 103, and the heat dissipation blades 104 are communicated with the external refrigerant through the pipeline.

[0047] The rotating piece 11 comprises a rotating gear 111 arranged on the mounting pipe 102, and the rotating gear 111 is located at the end of the mounting pipe 102 away from the stirring blade one 3, a rotating gear ring 112 is rotatably arranged on the mounting plate 101, a clamping bin 113 is arranged on the rotating gear ring 112, a clamping block 114 is slidably arranged on the stirring shaft 2, a pressing plate 115 connected with the clamping block 114 is slidably arranged on the stirring shaft 2, a plurality of connecting rods one 116 are rotatably arranged on the stirring shaft 2, an oscillating ball 117 is arranged at the end of the connecting rod one 116, a connecting rod two 118 is rotatably arranged on the connecting rod one 116, and the connecting rod two 118 is rotatably connected with the pressing plate 115, a limiting plate three 119 is arranged on the stirring shaft 2, and a pushing spring 1110 is sleeved between the limiting plate three 119 and the pressing plate 115 on the stirring shaft 2.

[0048] When the stirring shaft 2 rotates, the circular mounting plate 101 connected with the stirring shaft 2 rotates synchronously, the mounting pipe 102 and the heat dissipation blades 104 rotatingly arranged on the mounting pipe 102 rotate synchronously around the stirring shaft 2, when the stirring shaft 2 rotates, the swing ball 117 arranged on the connecting rod one 116 drives the connecting rod one 116 to deflect under the action of centrifugal force, thereby driving the connecting rod two 118 rotatingly connected with the connecting rod one 116 to lift, further driving the pressing plate 115 and the clamping block 114 connected with the pressing plate 115 to rise, the clamping block 114 rises and is clamped with the clamping cavity 113 on the rotating gear ring 112, thereby driving the clamping cavity 113 to rotate synchronously, the clamping cavity 113 rotates and drives the rotating gear ring 112 to rotate, synchronously driving the rotating gear 111 meshing with the rotating gear ring 112 to rotate, the rotating gear 111 rotates and drives the mounting pipe 102 to rotate, and further drives the mounting pipe 102 to rotate, when the mounting pipe 102 rotates, the heat dissipation blades 104 arranged on the mounting pipe 102 rotate, and the heat dissipation blades 104 are designed to be at an angle with the horizontal plane, which can further improve the turbulence effect on the reactants.

[0049] The design realizes the multi-dimensional compound motion of the heat dissipation blades 104 through linkage, significantly improves the heat dissipation efficiency and uniformity of the reaction system, and the core advantage lies in that the centrifugal force generated by the rotation of the stirring shaft 2 is used as a power source to drive the connecting rod mechanism to automatically trigger the clamping device, so that the heat dissipation blades 104 generate rotational motion while revolving around the stirring shaft 2, the superposition effect of revolution and rotation greatly enhances the turbulence intensity of the heat dissipation blades 104 on the reactants, forms multidirectional turbulent flow, effectively breaks the temperature boundary layer, and accelerates heat diffusion, the inclination design of the heat dissipation blades 104 and the horizontal plane further optimizes the fluid dynamics performance, realizes larger heat exchange area and more efficient forced convection under low energy consumption conditions, and the whole transmission process is automatically completed depending on the mechanical structure, without additional power input, which not only ensures the reliability and stability of the system operation, but also realizes intelligent conversion of the motion form through a pure mechanical mode.

[0050] The swing member 12 comprises a swing gear 121 arranged on the rotating shaft 103, a connecting rod 122 is slidingly arranged in the mounting pipe 102, the connecting rod 122 is provided with a swing rack 123 meshing with the swing gear 121, a pressing spring 124 is arranged at the bottom of the mounting pipe 102, one end of the pressing spring 124 is connected with the connecting rod 122, a pressing rod 125 is arranged on the connecting rod 122, one end of the pressing rod 125 penetrates through the mounting plate 101, a pressing block 126 cooperating with the pressing rod 125 is arranged on the pressing plate 115, and the pressing block 126 is an arc-shaped block.

[0051] When the mixing is completed and the reaction stage is entered, the stirring shaft 2 is reduced in speed, at which time the pressing plate 115 is reduced under the action of the pressing spring 124 due to the weakening of the centrifugal force, and the pressing block 126 provided thereon is synchronously lowered, after the pressing block 126 is lowered, it is in contact with the pressing rod 125, and the pressing rod 125 and the connecting rod 122 connected with the pressing rod 125 are extruded, after the pressing block 126 rotates with the stirring shaft 2, the pressing rod 125 is separated, and the connecting rod 122 and the pressing rod 125 are pushed up again by the pressing spring 124, and because the pressing block 126 is provided with multiple, the multiple pressing blocks 126 are in a wave shape, so that the pressing rod 125 is continuously extruded in the process of contact with the pressing rod 125, so that the connecting rod 122 moves up and down in a cycle, the connecting rod 122 moves up and down to drive the oscillating rack 123 provided thereon to move, thereby driving the oscillating gear 121 meshing with the oscillating rack 123 to reciprocating rotate, the oscillating gear 121 rotates to drive the rotating shaft 103 to rotate, and finally drives the heat dissipation blade 104 to reciprocating swing, while maintaining the global temperature balance, the risk of destroying the product crystal lattice structure by reducing the mechanical shear strength is avoided.

[0052] The mechanical transmission design realizes the adaptation of the heat dissipation mode to the reaction process, ensures the uniformity of the temperature field while considering the integrity of the product structure, utilizes the spring reset mechanism triggered by the stirring shaft 2 speed reduction to convert the rotary motion into the periodic up-down displacement of the pressing rod 125, utilizes the continuous action of the wave-shaped multiple pressing blocks 126 to form regular pulsation, drives the oscillating rack 123-gear mechanism to complete the controllable reciprocating swing of the heat dissipation blade 104, this swing heat dissipation mode not only maintains the dynamic thermal balance of the reaction system, but also effectively weakens the fluid shear stress by reducing the blade movement amplitude and frequency, especially suitable for synthesis reactions sensitive to crystal morphology or molecular structure, the mechanical structure realizes the negative correlation of the heat dissipation strength and the stirring speed, avoids the risk of local overheating, and reduces the influence on the synthesis product.

[0053] The synthesis method is as follows:

[0054] S1, install the reaction kettle 1, the stirring shaft 2 and the auxiliary components in place; add trifluoroacetic anhydride, pyridine derivatives and other raw materials into the reaction kettle 1 in proportion;

[0055] S2, the stirring shaft 2 drives the stirring blade one 3 and the stirring blade two 31 to rotate, at the same time, the inertial ball 710 slides along the chute 79 under the centrifugal force when the stirring shaft 2 rotates, so that the stirring blade two 31 moves under the action of the centrifugal force to overcome the elastic force of the return spring 77, and synchronously moves the sliding rod 4, pushes the spoiler blade 5 out of the storage bin 71 and exposes it in the reaction material, at this time the spoiler blade 5 rotates under the push of the reaction material, and mixes the solution in the reaction material;

[0056] S3, when the stirring blade two 31 is pushed by the centrifugal force to be close to the side wall of the reaction kettle 1, the boundary spoiler 8 works synchronously to push the spoiler rod 83 on the lifting plate 82 out, the spoiler rod 83 is close to the inner wall of the reaction kettle 1 after being stretched out, the boundary layer flow state is destroyed, and the mixing dead angle is eliminated;

[0057] S4, the heat dissipation unit 9 starts to work, the external refrigerant is input into the hollow heat dissipation blade 104 through the pipeline; the rotating shaft 103 drives the heat dissipation blade 104 to rotate, and the heat exchange between the refrigerant and the reactant is accelerated;

[0058] S5, in the initial stage of mixing, the stirring shaft 2 drives the clamping block 114 and the clamping bin 113 to drive the rotating gear ring 112 and the rotating gear 111 to rotate, and drives the heat dissipation blade 104 to rotate at high speed, so as to quickly absorb the heat of the local heat accumulation point;

[0059] S6, in the later stage of the reaction, the stirring shaft 2 reduces the rotating speed, so that the pressing plate 115 descends, at this time, the pressing rod 125 is cyclically pressed by the pressing plate 115, drives the oscillating gear 121 to reciprocate, switches the heat dissipation blade 104 to the oscillation mode, uniformly dissipates heat, and avoids damaging the product crystal.

[0060] Embodiment 2: please refer to Figure 11 The present application provides a technical solution: the sawtooth plate 13 is arranged on the adjacent side of the stirring blade one 3 and the stirring blade two 31, the non-continuous geometric characteristics of the sawtooth break the laminar boundary layer, induce controllable turbulent vortex, greatly enhance the radial and axial mass transfer rate between the reaction medium, and the staggered layout forms a dynamic cutting network, a multi-scale shear field is established in the rotating process, so that the mixing consistency of the reactants and the energy consumption optimization in the mixing process are realized.

[0061] It should be noted that, in this document, the relationship terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between the entities or operations. Moreover, the terms "include", "contain" or any other variants thereof are intended to cover non-exclusive inclusion, so that the process, method, article or equipment including a series of elements not only includes those elements, but also includes other elements not explicitly listed or inherent to such process, method, article or equipment.

[0062] Although the embodiments of the present application have been shown and described, it can be understood by those skilled in the art that various changes, modifications, replacements and variations can be made to the embodiments without departing from the principles and spirits of the present application.

Claims

1. A 2-amino-4-trifluoromethyl-pyridine synthesis apparatus, comprising a reaction vessel (1) and a stirring shaft (2), characterized in that: The stirring shaft (2) is circumferentially provided with multiple stirring blades (3), and multiple stirring blades (31) are movably installed on the stirring blades (3). Multiple sliding rods (4) are slidably provided on the stirring blades (3) and the stirring blades (31). Turbulence blades (5) are rotatably provided on the sliding rods (4). Mixing enhancement units (6) connected to the turbulence blades (5) are provided on the stirring blades (3) and the stirring blades (31) to push out the turbulence blades (5) in the initial stage of reactant mixing and to turbulently mix the reactants. A heat dissipation unit (9) is provided in the reactor (1) to dissipate heat from the heat accumulation points caused by uneven mixing in the initial stage of mixing.

2. The 2-amino-4-trifluoromethyl-pyridine synthesis apparatus according to claim 1, characterized in that: The mixing enhancement unit (6) includes a deployer (7) provided on the first stirring blade (3) and the second stirring blade (31). The turbulence blade (5) is pushed out by the deployer (7). The second stirring blade (31) is provided with a boundary turbulence member (8) to disrupt the flow state of the boundary layer of the reactor (1) wall during the mixing process.

3. The 2-amino-4-trifluoromethyl-pyridine synthesis apparatus according to claim 2, characterized in that: The unfolding component (7) includes a storage compartment (71) on one side of the stirring blade (3) and the stirring blade (31), and the storage compartment (71) on the stirring blade (3) is connected to an external air source through a pipe. Both the stirring blade (3) and the stirring blade (31) are provided with a moving groove (72). Both ends of the sliding rod (4) extend into the moving groove (72). Both ends of the sliding rod (4) located within the moving groove (72) are provided with a limiting plate (73) that is slidably connected to the moving groove (72). The stirring blade (3) and the stirring blade (31)... 31) Each of the blades is provided with a sliding groove (74), and an extension rod (75) is slidably arranged in the sliding groove (74). Limiting plates (76) are provided at both ends of the extension rod (75) located in the sliding groove (74). Reset springs (77) are sleeved at both ends of the extension rod (75) located in the sliding groove (74). A fixing plate (78) is provided on the stirring blade (2) (31). An inclined groove (79) is provided in the fixing plate (78). An inertial ball (710) is movably arranged in the inclined groove (79). A one-way valve (711) is provided on the storage bin (71).

4. The 2-amino-4-trifluoromethyl-pyridine synthesis apparatus according to claim 3, characterized in that: The boundary turbulence-disrupting component (8) includes an installation chamber (81) disposed on the stirring blade (31). A lifting plate (82) is slidably disposed inside the installation chamber (81). Multiple turbulence-disrupting rods (83) are disposed on the lifting plate (82). One end of each turbulence-disrupting rod (83) passes through the installation chamber (81) and is slidably connected to the installation chamber (81). A telescopic rod (84) is disposed inside the installation chamber (81), and one end of the telescopic rod (84) is connected to the lifting plate (82). A telescopic spring (85) is sleeved on the telescopic rod (84). The lifting plate (82) is located away from the turbulence-disrupting rods. 83) A triangular plate (86) is provided on one side. A push block (87) is slidably provided in the installation chamber (81). The push block (87) is in contact with the triangular plate (86). A positioning plate (88) is provided in the installation chamber (81). A compression spring (89) is provided on the positioning plate (88). One end of the compression spring (89) is connected to the push block (87). A traction rope (810) is provided on the push block (87). The traction rope (810) passes through the through holes on the installation chamber (81) and the moving groove (72) in sequence and is connected to the limiting plate (73).

5. The 2-amino-4-trifluoromethyl-pyridine synthesis apparatus according to claim 4, characterized in that: The heat dissipation unit (9) includes a heat-conducting component (10) disposed in the reaction vessel (1). The heat-conducting component (10) is used to dissipate heat from the heat accumulation points in the reactants. A rotating component (11) is disposed on the heat-conducting component (10). The rotating component (11) is used to drive the heat-conducting component (10) to rotate. A swinging component (12) is disposed on the heat-conducting component (10). The swinging component (12) is used to change the motion state of the heat-conducting component (10) after the reactants are mixed.

6. The 2-amino-4-trifluoromethyl-pyridine synthesis apparatus according to claim 5, characterized in that: The heat-conducting component (10) includes a mounting plate (101) rotatably disposed inside the reactor (1). Multiple mounting tubes (102) are rotatably disposed on the mounting plate (101), and one end of the mounting tube (102) penetrates through the mounting plate (101). Multiple rotating shafts (103) are disposed on the mounting tubes (102), and multiple hollow heat dissipation blades (104) are disposed on the rotating shafts (103). The heat dissipation blades (104) are connected to the external refrigerant through pipes.

7. The 2-amino-4-trifluoromethyl-pyridine synthesis apparatus according to claim 6, characterized in that: The rotating component (11) includes a rotating gear (111) mounted on the mounting tube (102), and the rotating gear (111) is located at the end of the mounting tube (102) away from the stirring blade (3). A rotating gear ring (112) is rotatably mounted on the mounting plate (101), and a snap-fit ​​chamber (113) is provided on the rotating gear ring (112). A snap-fit ​​block (114) is slidably mounted on the stirring shaft (2), and a pressure plate connected to the snap-fit ​​block (114) is slidably mounted on the stirring shaft (2). (115) A plurality of connecting rods (116) are rotatably arranged on the stirring shaft (2). A swing ball (117) is provided at the end of the connecting rod (116). A connecting rod (118) is rotatably arranged on the connecting rod (116), and the connecting rod (118) is rotatably connected to the pressure plate (115). A limiting plate (119) is provided on the stirring shaft (2). A push spring (1110) is sleeved on the stirring shaft (2) between the limiting plate (119) and the pressure plate (115).

8. The apparatus for synthesizing 2-amino-4-trifluoromethyl-pyridine according to claim 7, characterized in that: The swing component (12) includes a swing gear (121) mounted on a rotating shaft (103), a connecting rod (122) slidably mounted inside the mounting tube (102), a swing rack (123) meshing with the swing gear (121) mounted on the connecting rod (122), a pressing spring (124) at the bottom of the mounting tube (102), one end of the pressing spring (124) being connected to the connecting rod (122), a pressing rod (125) mounted on the connecting rod (122), one end of the pressing rod (125) penetrating through the mounting plate (101), and a pressing block (126) cooperating with the pressing rod (125) mounted on the pressure plate (115), the pressing block (126) being an arc-shaped block.

9. The apparatus for synthesizing 2-amino-4-trifluoromethyl-pyridine according to claim 8, characterized in that: Serrated plates (13) are provided on the adjacent sides of the first stirring blade (3) and the second stirring blade (31).

10. A method for synthesizing 2-amino-4-trifluoromethyl-pyridine using the apparatus described in any one of claims 1 to 9, characterized in that: The synthesis method is as follows: S1. Install the reactor (1), stirring shaft (2) and auxiliary parts into place; add trifluoroacetic anhydride, pyridine derivative and other raw materials into the reactor (1) in proportion; S2. The working of the stirring shaft (2) drives the stirring blade one (3) and stirring blade two (31) to rotate. At the same time, the inertial ball (710) slides along the inclined groove (79) due to centrifugal force when the stirring shaft (2) rotates, so that stirring blade two (31) moves under the action of centrifugal force, overcoming the elastic force of the return spring (77), and simultaneously moves the sliding rod (4), pushing the turbulence blade (5) out of the storage chamber (71) and exposing it to the reactants. At this time, the turbulence blade (5) rotates under the push of the reactants, mixing the solution in the reactants. S3. When the stirring blade (31) is pushed close to the side wall of the reactor (1) by centrifugal force, the boundary turbulence element (8) works synchronously to push out the turbulence rod (83) on the lifting plate (82). After the turbulence rod (83) extends out, it is close to the inner wall of the reactor (1), which disrupts the boundary layer flow state and eliminates the mixing dead angle. S4. The heat dissipation unit (9) is started, and the external refrigerant is introduced into the hollow heat dissipation blades (104) through the pipe; the rotating shaft (103) drives the heat dissipation blades (104) to rotate, accelerating the heat exchange between the refrigerant and the reactants; S5. In the initial stage of mixing, the stirring shaft (2) drives the snap block (114) and snap chamber (113) to drive the rotating gear ring (112) and rotating gear (111) to rotate, driving the heat dissipation blades (104) to rotate at high speed and quickly absorb the heat from the local heat accumulation point. S6. In the later stage of the reaction, the speed of the stirring shaft (2) decreases, causing the pressure plate (115) to drop. At this time, the pressing rod (125) is squeezed by the pressure plate (115) in a cycle, which drives the swing gear (121) to rotate back and forth, switching the heat dissipation blade (104) to the swing mode, dissipating heat evenly, and avoiding damage to the crystallization of the product.

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