Preparation device and method of perfluorotripropylamine

Abstract

The invention relates to the technical field of chemical preparation, and discloses a perfluorotripropylamine preparation device and a method thereof.The perfluorotripropylamine preparation device comprises a reaction kettle body and a kettle cover detachably connected to the top of the reaction kettle body; a stirring assembly extending to the inner cavity of the reaction kettle body is arranged in the inner cavity of the kettle cover; the stirring assembly comprises a stirring shaft rotationally connected to an inner cavity of the kettle cover, and materials can be pushed to form up-down circulating flow through guide vanes which are alternately and obliquely arranged; the gas-phase raw material can be fully dispersed to a liquid-phase main body by matching the shearing effect of the zigzag turbulent flow teeth at the edges of the blades on the gas-phase raw material, the intensifying effect of the turbulent flow protrusions on the surface on the material turbulent flow and the cross-flow guide of the middle flow guide holes on the upper-layer and lower-layer materials, and the wall-attached circular flow is broken by combining the turbulent flow beads on the inner wall of the kettle body, so that the gas-phase raw material can be fully dispersed to the liquid-phase main body. And finally, a dead-angle-free three-dimensional mixed flow field is constructed, so that the phenomena of gas-phase aggregation and liquid-phase retention caused by density difference are fundamentally improved, and the contact area and the reaction interface between raw materials are greatly increased.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical preparation, in particular to a preparation device and method of perfluorotripropylamine. BACKGROUND

[0002] Perfluorotripropylamine, as a kind of fluorine-containing fine chemical with excellent performance, has the characteristics of strong chemical stability, good insulation, high and low temperature resistance, etc., and is widely used in high-end fields such as electronic coolant, gas chromatography stationary liquid, fire extinguishing agent, etc. Its preparation process usually involves core steps such as fluorination reaction. The reaction is mostly based on fluorine gas and fluorine-containing intermediates as raw materials, or solid catalysts are added to form a gas-liquid or liquid-solid reaction system. The uniformity of the dispersion of the raw materials directly determines the reaction rate, product selectivity and raw material utilization rate. At present, the preparation of perfluorotripropylamine in industry mostly uses a single stirring type reaction kettle as the core reaction equipment, and the stirring assembly is generally a flat blade structure. The design of this traditional stirring structure is relatively simple, and the blades are arranged horizontally along the radial direction of the stirring shaft. When rotating, the material is mainly pushed in a circular direction by the flat blades, which lacks the shearing, guiding and dispersion strengthening mechanism for the material. For the typical gas-liquid or liquid-solid system in the preparation of perfluorotripropylamine, this structure has significant limitations: in the gas-liquid system, due to the large difference in density between fluorine gas and fluorine-containing intermediates, the flat blades are difficult to effectively shear the light gas phase raw material into small bubbles and disperse it into the liquid phase main body, which easily leads to the "stratified retention" phenomenon that the gas phase is gathered in the upper part of the kettle and the liquid phase is retained in the lower part. Stratified retention directly leads to limited contact area between raw materials and insufficient reaction interface, which in turn causes incomplete reaction, and the unreacted raw materials are discharged with the product, resulting in reduced raw material utilization rate. In view of this, the present application provides a preparation device and method of perfluorotripropylamine to solve the above technical problems. SUMMARY

[0003] In view of the deficiencies in the above background art, the present application provides a technical solution of a preparation device and method of perfluorotripropylamine. The alternating inclined guide vanes can push the material to form an up-down circulating flow. Combined with the shearing action of the serrated turbulence teeth on the edge of the blade, the intensification effect of the surface turbulence protrusions on the material turbulence, and the through-flow guidance of the middle guide holes to the upper and lower layers of material, the gas phase raw material can be fully dispersed into the liquid phase main body. In combination with the turbulence protrusions on the inner wall of the kettle, the dead angle of the three-dimensional mixing flow field is broken, which fundamentally improves the gas aggregation and liquid retention caused by density difference, and greatly improves the contact area between raw materials and the reaction interface.

[0004] The present application provides the following technical solution: a preparation device and method of perfluorotripropylamine, comprising a reaction kettle body and a kettle cover detachably connected to the top of the reaction kettle body. The inner cavity of the kettle cover is provided with a stirring assembly extending into the inner cavity of the reaction kettle body; The stirring assembly comprises a stirring shaft rotatably connected to the inner cavity of the kettle cover, the surface of the stirring shaft is embedded with a plurality of connecting seats, the surface of each connecting seat is connected with a group of guide vanes through an adjusting structure, the number of each group of guide vanes is four and they are uniformly distributed in the circumferential direction, and a plurality of groups of guide vanes are arranged in an up-down alternating inclined manner. The surface of each guide vane is provided with a sawtooth-shaped turbulence tooth, one end of each guide vane is fixedly connected with a plurality of turbulence protrusions, and a plurality of guide holes are formed in the middle of one end of each guide vane. The inside of the reaction kettle body is fixedly connected with a plurality of turbulence protrusions in an annular array.

[0005] As a preferred technical solution of the present application, the adjusting structure comprises a plurality of rotating discs rotatably connected to the inner cavity of the connecting seat, one end of each rotating disc is provided with two adjusting grooves, a bolt is arranged in the inner cavity of each adjusting groove, one end of the bolt is fixedly connected with the surface of the connecting seat, a fixed knob is threadedly connected with the surface of the bolt, and the surface of the guide vane is fixedly connected with one end of the rotating disc.

[0006] As a preferred technical solution of the present application, one end of the stirring shaft is connected with a driving member through a shaft coupling, the driving member is fixedly connected to the top of the kettle cover, and the driving member is a servo motor.

[0007] As a preferred technical solution of the present application, the top of the reaction kettle body is fixedly connected with a discharge pipe, and the top of the kettle cover is fixedly connected with a feeding pipe.

[0008] As a preferred technical solution of the present application, one end of the discharge pipe and the feeding pipe is fixedly connected with a connecting flange, and the inner cavity of the discharge pipe is provided with an electromagnetic valve.

[0009] As a preferred technical solution of the present application, the top of the reaction kettle body is provided with a positioning groove, one end of the kettle cover is fixedly connected with a positioning block matched with the positioning groove, and the mating surface of the positioning block and the positioning groove is provided with a sealing gasket.

[0010] As a preferred technical solution of the present application, the hole of the guide hole is provided with a rounded corner structure, and the cross section of the turbulence protrusion is trapezoidal.

[0011] As a preferred technical solution of the present application, S1, check the positioning block and the positioning groove of the reaction kettle body and the kettle cover, adjust the alternating inclination angle of a plurality of groups of guide vanes through the adjusting structure, and tighten the fixed knob to complete positioning.

[0012] S2. Gas-phase raw materials and liquid-phase raw materials are introduced into the reactor body through the feed pipe at the top of the reactor lid. The gas-phase raw material is fluorine gas, and the liquid-phase raw material is a fluorine-containing intermediate. The feed rate is controlled according to the reaction ratio. S3. Start the drive unit to drive the stirring shaft to rotate, so that the guide vanes stir the gas-liquid mixture system in the reactor body. The serrated turbulence teeth shear and disperse the bubbles, and the turbulence of the material is enhanced by the turbulence protrusions and guide holes. Together with the turbulence protrusions on the inner wall of the reactor, a three-dimensional mixing flow field is formed. S4. According to the reaction stage, manually fine-tune the angle of the guide vanes by adjusting the structure, and combine it with the speed control of the drive component to maintain the uniform mixing state of the reaction system until the reaction is completed. S5. After the reaction is complete, turn off the drive unit and open the solenoid valve of the discharge pipe to discharge the reaction product from the reactor body, thus completing the preparation of perfluorotripropylamine. S6. Introduce the cleaning medium through the feed pipe, start the stirring assembly for short-term stirring and cleaning, and discharge the waste liquid through the discharge pipe after cleaning.

[0013] Compared with the prior art, the present invention has the following beneficial effects: Compared to the limitations of existing technologies where straight blades can only create circumferential flow, this device uses alternately inclined guide blades to push materials into an up-and-down circulating flow. Combined with the shearing effect of the serrated turbulence teeth on the blade edges, the aggravating effect of the surface turbulence protrusions on the material turbulence, and the flow guidance of the middle guide holes for the material to pass through the upper and lower layers, the gaseous raw materials can be fully dispersed into the liquid phase. In addition, the turbulence protrusions on the inner wall of the vessel break the wall-attached circulation, ultimately constructing a three-dimensional mixing flow field without dead angles. This fundamentally improves the gas phase aggregation and liquid phase retention phenomena caused by density differences, and significantly increases the contact area between raw materials and the reaction interface.

[0014] The device is equipped with a blade angle adjustment structure, which can finely adjust the blade tilt angle according to the mixing requirements of different stages of the reaction. Combined with the control of the rotation speed by the drive component, it can maintain the optimal mixing state without relying on a single stirring mode. Compared with the fixed straight blade structure in the existing technology, it can better adapt to the reaction characteristics of different stages in the preparation of perfluorotripropylamine. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the structure of the present invention; Figure 2 This is an exploded view of the present invention; Figure 3 This is a schematic diagram of the adjustment structure of the present invention; Figure 4 This is a schematic diagram of the turbulence-causing protrusion structure of the present invention.

[0016] In the figure: 1, reaction kettle body; 101, kettle cover; 2, stirring shaft; 201, connecting seat; 202, guide vane; 203, serrated spoiler tooth; 204, spoiler protrusion; 205, guide hole; 206, spoiler convex rib; 3, rotating disc; 301, adjusting groove; 302, bolt; 303, fixed knob; 4, driving piece; 5, discharge pipe; 501, feed pipe; 6, connecting flange; 7, positioning groove. DETAILED DESCRIPTION

[0017] 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 those skilled in the art without creative labor fall within the scope of protection of the present application.

[0018] Please refer to Figures 1-4 As shown in the figure, a preparation device and method of perfluorotripropylamine, comprising a reaction kettle body 1 and a kettle cover 101 detachably connected to the top of the reaction kettle body 1; The inner cavity of the kettle cover 101 is provided with a stirring assembly extending into the inner cavity of the reaction kettle body 1; The stirring assembly comprises a stirring shaft 2 rotatably connected to the inner cavity of the kettle cover 101, and the surface of the stirring shaft 2 is embedded with a plurality of connecting seats 201. The surface of each connecting seat 201 is connected to a set of guide vanes 202 through adjusting structure. Each set of guide vanes 202 is four in number and is uniformly distributed in the circumferential direction, and the plurality of sets of guide vanes 202 are arranged alternately in an upward and downward inclined manner. The surface of each guide vane 202 is provided with a serrated spoiler tooth 203, one end of each guide vane 202 is fixedly connected with a plurality of spoiler protrusions 204, and a plurality of guide holes 205 are formed in the middle of one end of each guide vane 202. The inside of the reaction kettle body 1 is fixedly connected with a plurality of spoiler convex ribs 206 in an annular array.

[0019] The adjusting structure comprises a plurality of rotating discs 3 rotatably connected to the inner cavity of the connecting seat 201. One end of each rotating disc 3 is provided with two adjusting grooves 301, and a bolt 302 is arranged in the inner cavity of each adjusting groove 301. One end of the bolt 302 is fixedly connected to the surface of the connecting seat 201, and a fixed knob 303 is threadedly connected to the surface of the bolt 302. The surface of the guide vane 202 is fixedly connected to one end of the rotating disc 3.

[0020] One end of the stirring shaft 2 is connected with a driving piece 4 through a shaft coupling, and the driving piece 4 is fixedly connected to the top of the kettle cover 101. The driving piece 4 is a servo motor.

[0021] The top of the reaction kettle body 1 is fixedly connected with a discharge pipe 5, and the top of the kettle cover 101 is fixedly connected with a feeding pipe 501.

[0022] The one end of the discharge pipe 5 and the feeding pipe 501 is fixedly connected with a connecting flange 6, and the inner cavity of the discharge pipe 5 is provided with a solenoid valve.

[0023] The top of the reaction kettle body 1 is provided with a positioning groove 7, and one end of the kettle cover 101 is fixedly connected with a positioning block matched with the positioning groove 7.

[0024] The orifice of the flow guide hole 205 is provided with a rounded corner structure, and the cross section of the turbulence protruding rib 206 is trapezoidal.

[0025] S1, check the cooperation and sealing of the positioning block and the positioning groove 7 of the reaction kettle body 1 and the kettle cover 101, adjust the alternate inclination angles of the multiple groups of flow guide vanes 202 through the adjusting structure, and tighten the fixing knob 303 to complete the positioning.

[0026] S2, respectively pass the gas phase raw material and the liquid phase raw material into the reaction kettle body 1 through the feeding pipe 501 at the top of the kettle cover 101, wherein the gas phase raw material is fluorine gas, and the liquid phase raw material is a fluorine-containing intermediate, and the feeding rate is controlled according to the reaction ratio; S3, start the driving part 4 to drive the stirring shaft 2 to rotate, so that the flow guide vane 202 stirs the gas-liquid mixed system in the reaction kettle body 1, shears and disperses the bubbles through the serrated turbulence teeth 203, strengthens the material turbulence by using the turbulence protrusion 204 and the flow guide hole 205, and forms a three-dimensional mixed flow field in cooperation with the turbulence protruding rib 206 on the inner wall of the reaction kettle; S4, according to the reaction stage, manually fine-tune the angle of the flow guide vane 202 through the adjusting structure, and combine the speed control of the driving part 4 to maintain the uniform mixing state of the reaction system until the reaction is completed; S5, after the reaction is completed, the driving part 4 is closed, the solenoid valve of the discharge pipe 5 is opened, and the reaction product is discharged from the reaction kettle body 1, and the preparation of perfluorotripropylamine is completed; S6, pass the cleaning medium through the feeding pipe 501, start the stirring assembly for a short time to stir and clean, and then discharge the waste liquid through the discharge pipe 5 after cleaning.

[0027] When assembling, the positioning block of the kettle cover 101 is embedded into the positioning groove 7 of the reaction kettle body 1, the sealing gasket on the cooperation surface of the positioning block and the positioning groove 7 can enhance the sealing property of the connection between the two, and avoid leakage of corrosive raw materials or products during the reaction; at the same time, the inclination angle of the flow guide vane 202 is adjusted through the adjusting structure, the flow guide vane 202 reaches the preset angle by rotating the rotating disc 3, the angle is adapted by sliding the adjusting groove 301 along the bolt 302, the rotating disc 3 is fixed with the connecting seat 201 by tightening the fixing knob 303, and the parameter preset of the stirring assembly is completed. Liquid raw materials such as fluorine-containing intermediates and gaseous raw materials such as fluorine are introduced through the feed pipe 501 at the top of the reactor lid 101. The connecting flange 6 at the end of the feed pipe 501 facilitates connection with external conveying pipelines. At this time, the solenoid valve inside the discharge pipe 5 is in the closed state to ensure that a closed reaction space is formed inside the reactor body 1. The start-up drive unit 4 (servo motor) drives the stirring shaft 2 to rotate via a coupling. The connecting seat 201 on the surface of the stirring shaft 2 rotates synchronously with the shaft, thereby driving each set of guide vanes 202 to rotate. Because the multiple sets of guide vanes 202 are arranged with alternating vertical inclination and each set has four circumferentially evenly distributed, they can push the material to form an up-and-down circulating flow when rotating. The serrated turbulence teeth 203 on the edge of the guide vanes 202 can shear and disperse the gas phase raw material to form microbubbles. The turbulence protrusions 204 on the surface further intensify the material turbulence. The guide hole 205 in the middle promotes the flow exchange between the upper and lower layers of material. Together with the turbulence protrusions 206 (trapezoidal cross section) of the annular array on the inner wall of the reactor body 1, the wall-attached circulation is broken, and finally a three-dimensional mixing flow field without dead angles is formed, which improves the raw material contact efficiency. The rounded corner structure of the orifice of the guide hole 205 can reduce the material flow resistance and avoid raw material stagnation and blockage. During the reaction, stirring can be stopped according to the needs of the reaction stage. The angle of the guide vane 202 can be manually adjusted repeatedly, or the speed can be adjusted by the drive component 4 to maintain the optimal mixing state. After the reaction is completed, the drive component 4 is turned off and the solenoid valve of the discharge pipe 5 is opened. The product is discharged through the discharge pipe 5. The connecting flange 6 at the end of the discharge pipe 5 facilitates connection to subsequent separation equipment to complete the perfluorotripropylamine preparation process.

[0028] It should be noted that, in this document, relational terms such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Additionally, in the accompanying drawings of this invention, the fill patterns are merely for distinguishing layers and do not constitute any other limitation.

[0029] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. An apparatus for the preparation of perfluorotripropylamine comprising: The reaction kettle body (1) and the kettle cover (101) detachably connected to the top of the reaction kettle body (1); Characterized in that: the inner cavity of the kettle cover (101) is provided with a stirring assembly extending into the inner cavity of the reaction kettle body (1); The stirring assembly comprises a stirring shaft (2) rotatably connected to the inner cavity of the kettle cover (101), the surface of the stirring shaft (2) is embedded with a plurality of connecting seats (201), the surface of each connecting seat (201) is connected with a group of guide vanes (202) through adjusting structure, the number of each group of guide vanes (202) is four and is uniformly distributed in the circumferential direction, and a plurality of groups of guide vanes (202) are arranged alternately in an upward and downward inclined manner; The surface of each guide vane (202) is provided with a sawtooth turbulence tooth (203), one end of each guide vane (202) is fixedly connected with a plurality of turbulence protrusions (204), and a plurality of guide holes (205) are formed in the middle of one end of each guide vane (202). The inside of the reaction kettle body (1) is fixedly connected with a plurality of turbulence convex edges (206) in an annular array.

2. The apparatus for preparing perfluorotripropylamine according to claim 1, characterized by: The adjusting structure comprises a plurality of rotating discs (3) rotatably connected to the inner cavity of the connecting seat (201), one end of each rotating disc (3) is provided with two adjusting grooves (301), the inner cavity of each adjusting groove (301) is provided with a bolt (302), one end of the bolt (302) is fixedly connected with the surface of the connecting seat (201), the surface of the bolt (302) is threadedly connected with a fixed knob (303), and the surface of the guide vane (202) is fixedly connected with one end of the rotating disc (3).

3. The apparatus of claim 1, wherein: One end of the stirring shaft (2) is connected with a driving member (4) through a shaft coupling, the driving member (4) is fixedly connected to the top of the kettle cover (101), and the driving member (4) is a servo motor.

4. The apparatus of claim 1, wherein: The top of the reaction kettle body (1) is fixedly connected with a discharge pipe (5), and the top of the kettle cover (101) is fixedly connected with a feed pipe (501).

5. The apparatus of claim 4, wherein: One end of the discharge pipe (5) and the feed pipe (501) is fixedly connected with a connecting flange (6), and the inner cavity of the discharge pipe (5) is provided with an electromagnetic valve.

6. The apparatus of claim 1, wherein: The top of the reaction kettle body (1) is provided with a positioning groove (7), one end of the kettle cover (101) is fixedly connected with a positioning block matched with the positioning groove (7), and the matching surface of the positioning block and the positioning groove (7) is provided with a sealing gasket.

7. The apparatus of claim 1, wherein: The orifice of the guide hole (205) is provided with a fillet structure, and the cross section of the turbulence convex edge (206) is trapezoidal.

8. A device for preparing perfluorotripropylamine and a method thereof according to claim 1, wherein A kind of multi-kind chemotherapy drug injection control device according to any one of claims 1-7, specific method includes the following steps: S1, check the positioning block and the positioning groove (7) of the reaction kettle body (1) and the kettle cover (101) cooperation sealing, adjust the alternate inclination angle of a plurality of guide vanes (202) by adjusting structure, tighten the fixed knob (303) to complete positioning; S2, respectively into the reaction kettle body (1) through the feed pipe (501) on the top of the kettle cover (101) gas phase raw materials and liquid phase raw materials, wherein the gas phase raw material is fluorine gas, liquid phase raw material is fluorine containing intermediate, according to the reaction ratio control feed rate; S3, start driving element (4) drive stirring shaft (2) rotation, make guide vane (202) to the gas liquid mixing system in the reaction kettle body (1) is stirred, through the serrated spoiler (203) shear dispersion bubble, use spoiler convex (204) and guide hole (205) to strengthen material turbulence, cooperate with the reaction kettle inner wall spoiler convex (206) form three-dimensional mixed flow field; S4, according to the reaction stage by adjusting the structure manual fine tuning guide vane (202) angle, combined with the speed control of driving element (4), maintain the uniform mixing state of the reaction system, until the reaction is completed; S5, after the reaction is completed, close the driving element (4), open the electromagnetic valve of the discharge pipe (5), the reaction product is discharged from the reaction kettle body (1), complete the preparation of perfluorotripropylamine; S6, through the feed pipe (501) into the cleaning medium, start the stirring assembly for a short time to stir and clean, after cleaning through the discharge pipe (5) to discharge waste liquid.

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