Continuous flow reaction device for amination synthesis of N-butyl pyrrolidone

Abstract

The invention discloses a continuous flow reaction device for amination synthesis of N-butyl pyrrolidone, the continuous flow reaction device comprises a reaction device and a base mounted at the bottom, the reaction device is composed of three-level structures, namely a physical mixing structure, a reaction mixing structure and a continuous reaction structure, the physical mixing structure is composed of a mixing thin tube, and the mixing thin tube is connected with the base. The reaction mixing structure is composed of a mixing and stirring reaction device, the continuous reaction structure is composed of a discharge pipe, and a mixing thin pipe capable of mixing input solutions is assembled at the head of the reaction device. The continuous flow reaction device for amination synthesis of N-butyl pyrrolidone has efficient mixing and reaction: by arranging a mixing and stirring reaction device in a reaction mixing structure and designing a plurality of layers of stirring rods and blocking plates, not only is a solution further mixed, but also the solution is divided into a plurality of chambers through partition plates; the cavities are communicated through the holes, so that sufficient reaction time and mixing opportunity are provided while the flow velocity of the solution is ensured, and the proportioned solution can react more completely and sufficiently.

Description

Technical Field

[0001] The invention relates to the technical field of chemical equipment, in particular to a continuous flow reaction device for synthesizing N-butylpyrrolidone by amination. Background Art

[0002] In the field of chemical synthesis, N-butylpyrrolidone, as an important organic solvent and chemical raw material, is widely used in coatings, inks, resins, dyes, pesticides, pharmaceuticals and other industries. There are various methods for its synthesis, among which the amination synthesis method has attracted much attention due to its easy availability of raw materials, mild reaction conditions and high yield. However, the traditional continuous flow reaction device for the synthesis of N-butylpyrrolidone by amination still faces many challenges in practical applications.

[0003] First, the mixing efficiency of the reaction solution is one of the key factors affecting the synthesis efficiency and product quality. Traditional mixing methods often rely on simple stirring or oscillation, which has a poor mixing effect and easily leads to uneven reaction, thus affecting the purity and yield of the product. Therefore, it is particularly important to develop a continuous flow reaction device that can efficiently mix the reaction solution.

[0004] Secondly, the control and operation of the reaction process are also important factors affecting the synthesis effect. Traditional reaction devices are often not flexible enough in controlling the discharge of the reaction solution, and it is difficult to achieve precise flow control and time control, which affects the subsequent processing and product quality. In addition, changes in pressure during the reaction process may also affect the reaction rate and yield, so a reaction device that can adjust the pressure of the input solution is needed.

[0005] Furthermore, the optimization of the heating system is also crucial to improving reaction efficiency and product quality. Traditional heating methods often have problems such as uneven heating, high energy consumption, and inaccurate temperature control, all of which may affect the reaction rate and product selectivity. Therefore, the development of a reaction device that can evenly heat the inside of the reaction device, with low energy consumption and precise temperature control has become a hot topic in the industry.

[0006] Finally, the compactness and practicality of the device are also important indicators for evaluating its performance. Traditional reaction devices are often large and complex in structure, which not only takes up a lot of space, but also increases production costs and maintenance difficulties. Therefore, it is of great significance to develop a reaction device with a compact structure, reasonable design, full use of space and easy maintenance.

[0007] In summary, in view of the problems of low mixing efficiency, inflexible control and operation, imperfect heating system and incompact structure in the traditional continuous flow reaction device for amination synthesis of N-butyl pyrrolidone, the present invention proposes a novel continuous flow reaction device for amination synthesis of N-butyl pyrrolidone. The device realizes efficient mixing of the reaction solution by setting up a physical mixing structure and a reaction mixing structure; flexible control and operation are realized by setting up valve groups such as solenoid valves and discharge pipes; the heating system is optimized by adopting a hot oil circulation heating method and an oil guide cavity opened in the partition; at the same time, the overall design of the device is compact and practical, which can make full use of space and improve production efficiency. These innovative designs effectively solve the problems existing in traditional reaction devices and provide a more efficient, flexible, energy-saving and easy-to-maintain reaction device for amination synthesis of N-butyl pyrrolidone. Summary of the invention

[0008] The object of the present invention is to provide a continuous flow reaction device for synthesizing N-butylpyrrolidone by amination, so as to solve the problem that the traditional mixing method mentioned in the above background technology often relies on simple stirring or oscillation, which has a poor mixing effect and easily leads to uneven reaction, thereby affecting the purity and yield of the product.

[0009] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: a continuous flow reaction device for synthesizing N-butylpyrrolidone by amination, comprising: a reaction device and a base installed at the bottom, and the reaction device is composed of three-level structures, namely a physical mixing structure, a reaction mixing structure and a continuous reaction structure, the physical mixing structure is composed of a mixing capillary, the reaction mixing structure is composed of a mixing stirring reaction device and the continuous reaction structure is composed of a discharge pipe, the head of the reaction device is equipped with a mixing capillary for mixing the input solution, the bottom discharge of the mixing capillary is provided with a mixing stirring reaction device, the bottom discharge port of the mixing stirring reaction device is provided with a reaction tube, the bottom of the reaction tube is connected with a discharge pipe, and a valve group such as a solenoid valve is installed at the connection between the reaction tube and the discharge pipe, the mixing capillary, the mixing stirring reaction device and the reaction tube are placed inside a heating device and provide a heating environment with a capping structure at both ends of the reaction device.

[0010] Preferably, the mixing tube includes at least two feed pipes, a pressure pump, and a discharge pipe. The feed pipe extends into the outside of the reaction device and is equipped with a pressure pump. The tail end of the feed pipe is connected to the discharge pipe, so that the solution input into the reaction device can be further physically mixed.

[0011] Preferably, the mixing and stirring reaction device includes a support frame, a motor, a rotating shaft, a stirring rod, and a blocking plate. Support frames fixed on a base are arranged on both sides of the reaction device, and a motor is installed on the outer side of the support frame. The rotating shaft on the motor passes through the reaction wall of the reaction device and extends to the interior. A stirring rod is located inside the reaction device and installed on the rotating shaft. The mixing and stirring reaction device can achieve mixing of the reaction solution, and a blocking plate is arranged while stirring and mixing to ensure a sufficient retention time of the solution and avoid rapid outflow of the reaction solution.

[0012] Preferably, the mixing and stirring reaction device is divided into multiple stages in series, and two adjacent stages are separated by a partition, and the two adjacent layers are connected end to end, so that the tail end of the solution of one layer flows out and flows into the head of the solution of another layer, thereby realizing the zigzag flow of the reaction solution.

[0013] Preferably, a blocking plate is provided between two adjacent stirring rods, and each level of the mixing and stirring reaction device can be separated into different chambers by the blocking plate.

[0014] Preferably, the blocking plate further comprises holes inside, and the holes are provided so that the reaction solution can flow into the next cavity through the holes, thereby achieving the purpose of preventing the solution from flowing quickly, so that the solution has a sufficient reaction time in the reaction device.

[0015] Preferably, the reaction tube is a stainless steel straw and is arranged in a spiral structure at the bottom layer of the reaction device. By arranging a longer reaction tube at the tail end, the reaction solution can maintain the reaction conditions for a period of time before being discharged, further avoiding the problem of insufficient reaction of the reaction solution.

[0016] Preferably, the heating device comprises an oil inlet pipe, an oil outlet pipe, and an oil storage chamber, and the two sides of the oil storage chamber are connected with the oil inlet pipe and the oil outlet pipe.

[0017] Preferably, the oil inlet pipe and the oil outlet pipe are respectively located at the lower end and the upper end of the reaction device, so that the poured hot oil can fully flow through the oil storage chamber inside the reaction device and then flow out from the oil outlet pipe, ensuring that the reaction temperature in the reaction device remains consistent.

[0018] Preferably, the mixing structure unit, the mixing reaction unit, and the coil reaction unit are all immersed in the heat transfer oil chamber, and the oil transfer chamber is connected to the oil storage chamber. Based on this structure, it can be ensured that the reaction solutions of the above two units can also ensure a sufficient reaction temperature, so that the reaction solution can maintain a uniform reaction temperature at any position.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] The continuous flow reaction device for synthesizing N-butylpyrrolidone by amination has efficient mixing and reaction: by setting up a physical mixing structure and a reaction mixing structure, the device can achieve efficient mixing of the reaction solution. The physical mixing structure utilizes the mutual impact of solutions input from different feed pipes to enhance the mixing effect of the solution. The mixing and stirring reaction device in the reaction mixing structure not only further mixes the solution through the design of multi-layer stirring rods and blocking plates, but also divides the solution into multiple chambers through partitions, and each chamber is connected through holes, thereby ensuring the flow rate of the solution while providing sufficient reaction time and mixing opportunities, so that the proportioned solution reacts more completely and fully.

[0021] The continuous flow reaction device for synthesizing N-butylpyrrolidone by amination has flexible control and operation. The valve group and discharge pipe such as the solenoid valve provided in the device can conveniently control the discharge of the reaction solution, which is convenient for subsequent treatment. At the same time, the application of the pressure pump can increase the pressure of the input solution, which is conducive to the mixing and reaction of the solution.

[0022] The continuous flow reaction device for synthesizing N-butylpyrrolidone by amination has an optimized heating system. The heating device adopts a hot oil circulation heating method. The oil inlet and outlet pipes are set to ensure that the hot oil can fully flow through the oil storage cavity, thereby forming a uniform heating environment inside the reaction device. The oil guide cavity opened in the partition further ensures that each level of the mixing and stirring reaction device can be fully heated, ensuring that the reaction temperature of the solution reaches the optimal state, and improving the reaction efficiency and product quality.

[0023] The continuous flow reaction device for synthesizing N-butylpyrrolidone by amination has a compact and practical structure. The overall design of the device is compact and the structure is reasonable, and the space can be fully utilized to improve production efficiency. At the same time, the reaction tube adopts a stainless steel straw and is arranged at the bottom of the reaction device in a spiral structure, which not only ensures sufficient reaction time of the reaction solution, but also enables the device to place a longer reaction tube in a limited space, thereby improving the reaction efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a schematic diagram of the main structure of the present invention;

[0025] Figure 2 It is a simplified structural schematic diagram of the reaction mixing structure of the present invention;

[0026] Figure 3 Schematic diagram of the blocking plate structure of the present invention

[0027] Figure 4 It is a schematic diagram of the structure of the solution of the present invention in a zigzag flow.

[0028] In the figure: 1. reaction device; 2. base; 3. mixing capillary; 31. feed pipe; 32. pressure pump; 33. discharge pipe; 4. support frame; 41. motor; 441. hole; 42. rotating shaft; 43. stirring rod; 44. blocking plate; 441. hole; 45. partition; 5. reaction tube; 6. solenoid valve and other valve groups; 7. discharge pipe; 8. heating device; 81. oil inlet pipe; 82. oil outlet pipe; 83. oil storage chamber. DETAILED DESCRIPTION

[0029] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] Example 1: Please refer to Figure 1 The present invention provides a technical solution: a continuous flow reaction device for synthesizing N-butylpyrrolidone by amination, comprising: a reaction device 1 and a base 2 installed at the bottom, and the reaction device 1 is composed of a three-level structure, namely a physical mixing structure, a reaction mixing structure and a continuous reaction structure, the physical mixing structure is composed of a mixing capillary 3, the head of the reaction device 1 is equipped with a mixing capillary 3 for mixing the input solution, the mixing capillary 3 includes at least two feed pipes 31, a pressure pump 32, and a discharge pipe 33, the feed pipe 31 extends into the outside of the reaction device 1, and the feed pipe 31 is installed with a pressure pump 32, and the tail end of the feed pipe 31 is connected to the discharge pipe 33.

[0031] The method of this embodiment is: the reaction solutions required for the synthesis of N-butylpyrrolidone by amination are mixed again and then respectively input into the reaction device 1 through different feed pipes 31. At this time, the pressure pump 32 can increase the pressure of the input solution. At the same time, the solutions input through different feed pipes 31 impact each other and flow in, thereby realizing a physical mixing process of the incoming solutions. This process can further mix the input mixed solution, thereby ensuring sufficient mixing of the solution.

[0032] Example 1: Please refer to Figure 1 , 23. The reaction mixing structure is composed of a mixing and stirring reaction device. The mixing and stirring reaction device is arranged at the bottom discharge of the mixing capillary 3. The bottom discharge port of the mixing and stirring reaction device is arranged with a reaction tube 5. The mixing and stirring reaction device comprises a support frame 4, a motor 41, a rotating shaft 42, a stirring rod 43, and a blocking plate 44. Support frames 4 fixed to the base 2 are arranged on both sides of the reaction device 1. The motor 41 is installed on the outer side of the support frame 4. The rotating shaft 42 on the motor 41 passes through the reaction wall of the reaction device 1 and extends to the inside. A stirring rod 43 is arranged inside the reaction device 1 and installed on the rotating shaft 42. The mixing and stirring reaction device is divided into at least two levels, and adjacent two levels are separated by a partition 45, and the two adjacent levels are connected end to end. A blocking plate 44 is arranged between two adjacent stirring rods 43, and the blocking plate 44 also includes a hole 441;

[0033] This embodiment starts the motor 41, which drives the rotating shaft 42 to rotate, so that the stirring rod 43 mixes the internal solution, so that the solution can be mixed again while ensuring a sufficient mixing reaction of the solution. The partition 45 can divide the mixing and stirring reaction device of each level into multiple chambers. The solution can be transported to the next chamber through the hole 441 between each chamber, so as to ensure a flow rate of the solution, provide a sufficient reaction time for the reaction solution, and ensure that the solution is fully mixed again, so that the proportioned solution reacts more completely and more fully.

[0034] Example 1: Please refer to Figure 1 , 3 The bottom of the reaction tube 5 is connected to a discharge pipe 7, and a valve group 6 such as a solenoid valve is installed at the connection between the reaction tube 5 and the discharge pipe 7. The reaction tube 5 is a stainless steel straw and is arranged in a spiral structure at the bottom layer of the reaction device 1.

[0035] The reaction tube 5 located in the last layer can fully guarantee the reaction time of the reaction solution. The spiral structure can be placed in the reaction device 1 for a longer length, thereby ensuring that the reaction solution has enough reaction time, and the reaction solution is discharged through the solenoid valve group 6 and the discharge pipe 7.

[0036] See also Figure 3 The mixing capillary 3, the mixing and stirring reaction device and the reaction tube 5 are placed inside the heating device 8 and form a heating environment inside the reaction device 1. The heating device 8 includes an oil inlet pipe 81, an oil outlet pipe 82, and an oil storage chamber 83. The two sides of the oil storage chamber 83 are connected with the oil inlet pipe 81 and the oil outlet pipe 82. The oil inlet pipe 81 and the oil outlet pipe 82 are respectively located at the lower end and the upper end of the reaction device 1. An oil guide chamber is opened in the partition 45, and the oil guide chamber is connected to the oil storage chamber 83.

[0037] The hot oil is transported to the interior of the oil storage chamber 83 through the oil inlet pipe 81 and discharged through the oil outlet pipe 82. By arranging the oil inlet pipe 81 at the bottom of the reaction device 1 and the oil outlet pipe 82 at the top of the reaction device 1, it can be ensured that the hot oil can fully pass through the oil storage chamber 83 before being discharged, thereby ensuring that the heat transfer oil can fully heat the interior of the reaction device 1. The oil transfer chamber is opened in the partition 45 to ensure that each level of the mixing and stirring reaction device is fully heated, thereby ensuring that the reaction temperature of the solution reaches a suitable reaction temperature.

[0038] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A continuous flow reaction device for synthesizing N-butylpyrrolidone by amination, characterized in that: include: A reaction device (1) and a base (2) installed at the bottom, and the reaction device (1) is composed of three-level structures, namely a physical mixing structure, a reaction mixing structure and a continuous reaction structure. The physical mixing structure is composed of a mixing capillary (3), the reaction mixing structure is composed of a mixing and stirring reaction device, and the continuous reaction structure is composed of a discharge pipe (7). The head of the reaction device (1) is equipped with a mixing capillary (3) capable of mixing an input solution, a mixing and stirring reaction device is arranged at the bottom discharge of the mixing capillary (3), a reaction tube (5) is arranged at the bottom discharge port of the mixing and stirring reaction device, the bottom of the reaction tube (5) is connected to a discharge pipe (7), and a valve group (6) such as a solenoid valve is installed at the connection between the reaction tube (5) and the discharge pipe (7), the mixing capillary (3), the mixing and stirring reaction device and the reaction tube (5) are placed inside a heating device (8) and provide a heating environment with a head structure at both ends of the reaction device (1).

2. A continuous flow reaction device for synthesizing N-butylpyrrolidone by amination according to claim 1, characterized in that: The mixing capillary (3) comprises at least two feed pipes (31), a pressure pump (32), and a discharge pipe (33); the feed pipe (31) extends into the outside of the reaction device (1), and a pressure pump (32) is installed on the feed pipe (31); the tail end of the feed pipe (31) is connected to the discharge pipe (33).

3. A continuous flow reaction device for synthesizing N-butylpyrrolidone by amination according to claim 1, characterized in that: The mixing and stirring reaction device comprises a support frame (4), a motor (41), a rotating shaft (42), a stirring rod (43), and a blocking plate (44); support frames (4) fixed to a base (2) are arranged on both sides of the reaction device (1); a motor (41) is installed on the outer side of the support frame (4); a rotating shaft (42) on the motor (41) passes through a reaction wall of the reaction device (1) and extends to the inside; a stirring rod (43) is located inside the reaction device (1) and is installed on the rotating shaft (42).

4. A continuous flow reaction device for synthesizing N-butylpyrrolidone by amination according to claim 3, characterized in that: The mixing and stirring reaction device is divided into at least two levels, and two adjacent levels are separated by a partition (45), and the two adjacent levels are connected end to end.

5. A continuous flow reaction device for synthesizing N-butylpyrrolidone by amination according to claim 3, characterized in that: A blocking plate (44) is arranged between two adjacent stirring rods (43).

6. A continuous flow reaction device for synthesizing N-butylpyrrolidone by amination according to claim 5, characterized in that: The blocking plate (44) further comprises a hole (441) therein.

7. The continuous flow reaction device for synthesizing N-butylpyrrolidone by amination according to claim 1, characterized in that: The reaction tube (5) is a stainless steel straw and is arranged in a spiral structure at the bottom layer of the reaction device (1).

8. The continuous flow reaction device for synthesizing N-butylpyrrolidone by amination according to claim 1, characterized in that: The heating device (8) comprises an oil inlet pipe (81), an oil outlet pipe (82), and an oil storage chamber (83); the two sides of the oil storage chamber (83) are connected to the oil inlet pipe (81) and the oil outlet pipe (82).

9. A continuous flow reaction device for synthesizing N-butylpyrrolidone by amination according to claim 8, characterized in that: The oil inlet pipe (81) and the oil outlet pipe (82) are respectively located at the lower end and the upper end of the reaction device (1).

10. A continuous flow reaction device for synthesizing N-butylpyrrolidone by amination according to claims 4 and 8, characterized in that: The mixing structure unit, the mixing reaction unit and the coil reaction unit are all immersed in the heat transfer oil cavity, and the oil transfer cavity is connected to the oil storage cavity (83).

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