Production equipment of aziridine cross-linking agent

Abstract

The utility model belongs to the technical field of cross-linking agent production, and particularly relates to aziridine cross-linking agent production equipment which comprises esterification equipment, cyclization equipment, addition equipment and storage equipment which are sequentially connected through pipelines. The esterification equipment is used for esterification reaction of isopropanolamine and concentrated sulfuric acid, and comprises mixing equipment, a preheating kettle I and a reaction kettle I which are sequentially connected through pipelines; the cyclization equipment is used for cyclization reaction of ammonium sulfate and alkali, and comprises a reaction kettle II and a dehydration device which are sequentially connected through a pipeline; the addition equipment is used for a Michael addition reaction of aziridine and alkali, and comprises a reaction kettle III, a standing device and a separation device which are sequentially connected through a pipeline; the number of the standing devices is at least two, and the standing devices are arranged in parallel. Esterification equipment, cyclization equipment, addition equipment and storage equipment which are sequentially connected through pipelines are arranged, so that the production of the aziridine cross-linking agent is continuous.

Description

Technical Field

[0001] The present application belongs to the technical field of cross-linking agent production, and specifically relates to a production device for an aziridine cross-linking agent. Background Art

[0002] Trimethylolpropane tris[3-(2-methylaziridinyl)propionate], also known as an aziridine crosslinker, is a chemical intermediate with a wide range of applications: improving the water, wash, chemical, and high-temperature resistance of leather coatings; improving the water, alcohol, wash, chemical, and abrasion resistance of water-based parquet varnishes, water-based plastic paints, and water-based metal paints; and improving the water and wash resistance of water-based printing inks. The preparation of aziridine crosslinkers involves three steps: the first step is the esterification reaction of isopropanolamine with concentrated sulfuric acid; the second step is the cyclization reaction of the ammonium sulfate salt with a base; and the third step is the addition reaction of aziridine. However, existing aziridine crosslinker production equipment performs all three steps in a single reactor, making it unsuitable for continuous production.

[0003] For example, "CN201921113529.9 A 2-Methylaziridine Cross-linking Agent Production Reactor" and "202321309872.7 A Synthesis Reactor for Intermediates for the Production of Aziridine Cross-linking Agents" both disclose production equipment for aziridine cross-linking agents. However, since the reaction of aziridine consists of three steps, the reaction conditions for each step are different. The first step is at 4-6°C, the second step is at 190-210°C, and the third step is at 4-6°C. If only one reactor is used in the production process, the temperature needs to be lowered to the reaction conditions in the first step, the temperature needs to be raised to the reaction conditions in the second step, and the temperature needs to be lowered to the reaction conditions in the third step. Cooling down, heating up, and cooling down again take time, which affects the progress of industrial production and consumes too much energy. Summary of the Invention

[0004] In order to solve the problems of the prior art, the present application provides a production device for an aziridine crosslinker, which is achieved through the following scheme:

[0005] A production device for an aziridine cross-linking agent, comprising an esterification device, a cyclization device, an addition device, and a storage device connected in sequence through pipelines;

[0006] The esterification equipment is used for the esterification reaction of isopropanolamine and concentrated sulfuric acid, and includes a mixing device, a preheating kettle, and a reaction kettle connected in sequence through pipelines;

[0007] The cyclization equipment is used for the cyclization reaction of ammonium sulfate with a base, and comprises a second reactor and a dehydration device connected in sequence through pipelines;

[0008] The addition equipment is used for the Michael addition reaction of aziridine and base, and includes a reactor 3, a static device, and a separation device connected in sequence through pipelines; the number of the static devices is at least 2 and they are arranged in parallel.

[0009] The storage device is used to store the aziridine cross-linking agent, and includes a pre-storage device and a packaging device. The number of the pre-storage devices is at least 2 and they are arranged in parallel.

[0010] Furthermore, the esterification equipment also includes a receiver and a pressure reducing device. The reactor 1 is connected to the receiver through a pipeline, and the receiver is connected to the pressure reducing device through a pipeline.

[0011] Furthermore, the cyclization equipment also includes an alkali tank, which is connected to the reactor 2 through a pipeline 1, and a flow valve 1 is provided on the pipeline 1.

[0012] Furthermore, the alkali tank is connected to the reactor phase 3 through pipeline 2, and a flow valve 2 is provided on the pipeline 2.

[0013] Furthermore, the pre-storage device is connected to the separation device through a reflux pipe.

[0014] Furthermore, a stirring rod is provided in the reactor three, a frame-shaped stirring rack is provided on the stirring rod, and a brush is provided on the outer wall of the frame-shaped stirring rack.

[0015] Furthermore, two connecting rods are provided on the upper inner wall of the frame-shaped stirring rack, namely a left connecting rod and a right connecting rod. The left connecting rod is provided with a sub-frame-shaped stirring rack, and the right connecting rod is provided with a stirring blade.

[0016] Furthermore, the connecting rod is rotatable.

[0017] Furthermore, the production equipment of the aziridine cross-linking agent also includes a water bath heating tank, and the mixing device and the reactor three are arranged in the same water bath heating tank.

[0018] Beneficial effects: an esterification device, a cyclization device, an addition device and a storage device connected in sequence through pipelines are provided, so that the production of the aziridine cross-linking agent is continuous; by providing a receiver and a pressure reducing device, the water generated by the esterification reaction is removed by pressure reduction during the esterification reaction, which helps the reaction to proceed in the positive direction, and the water generated by the reaction is removed in time to reduce the dilution of concentrated sulfuric acid, which helps the reaction to proceed in the positive direction; the cross-linking agent in the pre-storage device is tested to see if it is qualified, and if it is qualified, it is packaged; if it is unqualified, it is sent to the separation device through a reflux pipe for further purification until it is qualified; due to the high viscosity of the aziridine cross-linking agent, a brush is provided on the outer wall of the stirring rod to prevent the cross-linking agent from adhering to the inner wall of the reactor for a long time and causing solidification; by providing two connecting rods, and providing sub-frame-shaped stirring racks or stirring blades on the two connecting rods, the stirring force is increased; the two connecting rods are rotatable, and the connecting rods rotate with the stirring rods. The movement of the reaction liquid in the reactor can drive the rotation of the connecting rods themselves, further increasing the stirring force. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] To more clearly illustrate the technical solutions in the embodiments of this application, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some preferred embodiments of this application, not all embodiments. Regarding the preferred embodiments of this application, it is clear that those skilled in the art can derive other embodiments and drawings based on these embodiments and drawings without inventive effort, and all of them fall within the scope of protection of this application.

[0020] Figure 1 This is a schematic diagram of the structure of an embodiment of the present application;

[0021] Figure 2 This is a schematic diagram of the internal stirring structure of the reactor 3 in the embodiment of the present application;

[0022] In the figure, 1. mixing equipment, 2. preheating kettle 1, 3. reactor 1, 4. reactor 2, 5. dehydration device, 6. reactor 3, 7. standing device, 8. separation device, 9. pre-storage device, 10. packaging device, 11. receiver, 12. pressure reducing device, 13. alkali tank, 14. pipeline 1, 15. flow valve 1, 16. pipeline 2, 17. flow valve 2, 18. stirring rod, 19. frame-shaped stirring rack, 20. left connecting rod, 21. right connecting rod, 22. sub-frame-shaped stirring rack, 23. stirring plate, 24. stirring blade, 25. motor. DETAILED DESCRIPTION

[0023] To make the objectives, technical solutions, and advantages of this application more clear, the embodiments of this application will be described in further detail below. It should be understood that the terms "upper," "lower," "top," "bottom," "inner," "outer," and the like indicate positions or location relationships based on the positions or location relationships shown in the accompanying drawings. The foregoing definitions are merely for the purpose of describing this application and simplifying the description, and do not indicate or imply that the structures referred to must have a specific orientation, be constructed, or operate in a specific orientation. Therefore, they should not be construed as limitations on this application.

[0024] Example 1

[0025] A production equipment for an aziridine cross-linking agent, such as Figure 1 The process shown includes an esterification device, a cyclization device, an addition device and a storage device connected in sequence through pipelines;

[0026] The esterification equipment is used for the esterification reaction of isopropanolamine and concentrated sulfuric acid, and includes a mixing device 1, a preheating kettle 2, and a reaction kettle 3 connected in sequence through pipelines;

[0027] The cyclization equipment is used for the cyclization reaction of ammonium sulfate and base, including a reactor 2 4 and a dehydration device 5 connected in sequence through pipelines;

[0028] The addition device is used for the Michael addition reaction of aziridine and base, comprising a reactor 6, a stationary device 7, and a separation device 8 connected in sequence by pipelines; the number of the stationary devices 7 is at least two and they are arranged in parallel;

[0029] The storage device is used to store the aziridine cross-linking agent, including a pre-storage device 9 and a packaging device 10, and the number of the pre-storage devices 9 is at least 2 and arranged in parallel;

[0030] An esterification device, a cyclization device, an addition device, and a storage device connected in sequence by pipelines are provided to continuously produce an aziridine crosslinker; specifically, isopropanolamine is first added to a mixing device, concentrated sulfuric acid is added to the mixing device at a low temperature and under stirring, and the mixture is continuously stirred and mixed evenly, the mixed material is transported to a preheating kettle 1, heated to a reaction temperature, and then transported to a reactor 1, an esterification reaction occurs in the reactor 1 to generate ammonium sulfate salt, the ammonium sulfate salt undergoes a cyclization reaction under alkaline conditions in the reactor 2 to generate aziridine, most of the water generated by the reaction is removed by a dehydration device, an addition reaction occurs in the reactor 3 to obtain an aziridine crosslinker, and finally the target product aziridine crosslinker is obtained by static separation and impurity removal, and the target product aziridine crosslinker is stored in a pre-storage device, and packaged after passing the test;

[0031] Since the static time is too long, at least one static device should be set up for replacement to ensure uninterrupted production line;

[0032] By setting at least 2 pre-stored devices, they can be used interchangeably;

[0033] Furthermore, the esterification equipment further includes a receiver 11 and a pressure reducing device 12, the reactor 11 is connected to the receiver via a pipeline, and the receiver is connected to the pressure reducing device via a pipeline;

[0034] By setting up a receiver and a pressure reducing device, the water generated by the esterification reaction is removed by reducing pressure during the esterification reaction, which helps the reaction proceed in the positive direction. In addition, the water generated by the reaction is removed in time, which reduces the dilution of concentrated sulfuric acid and helps the reaction proceed in the positive direction.

[0035] Furthermore, the cyclization equipment further includes an alkali tank 13, which is connected to the reactor 2 4 via a pipeline 14, and a flow valve 15 is provided on the pipeline 14; by providing the alkali tank, alkali solution is introduced into the reactor 3 and the reactor 2;

[0036] Furthermore, the alkali tank 13 is connected to the reactor 3 6 via a second pipeline 16 , and a second flow valve 17 is provided on the second pipeline 16 ;

[0037] Furthermore, the pre-storage device 9 is connected to the separation device 8 via a reflux pipe;

[0038] The cross-linking agent in the pre-storage device is tested to see if it is qualified. If it is qualified, it is packaged. If it is unqualified, it is sent to the separation device through the reflux pipe for further purification until it is qualified.

[0039] Example 2

[0040] On the basis of Example 1, Figure 2 In at least one embodiment, a stirring rod 18 is provided in the reactor 3, a frame-shaped stirring frame 19 is provided on the stirring rod 18, and a brush is provided on the outer wall of the frame-shaped stirring frame 19;

[0041] Furthermore, two connecting rods are provided on the upper inner wall of the frame-shaped stirring frame 19, namely a left connecting rod 20 and a right connecting rod 21. The left connecting rod 20 is provided with a sub-frame-shaped stirring frame 22, and the sub-frame-shaped stirring frame is provided with a stirring disk 23. The right connecting rod 21 is provided with a stirring blade 24.

[0042] Furthermore, in one embodiment, the left connecting rod 20 and the right connecting rod 21 are fixedly arranged on the upper inner wall of the frame-shaped stirring frame 19; in another embodiment, the left connecting rod 20 and the right connecting rod 21 are rotatably connected to the upper inner wall of the frame-shaped stirring frame 19.

[0043] Reactor 3 is provided with a motor 25 matched with the stirring shaft.

[0044] Due to the high viscosity of the aziridine cross-linking agent, a brush is provided on the outer wall of the stirring rod to prevent the cross-linking agent from adhering to the inner wall of the reactor for a long time and causing solidification. The stirring force is increased by providing two connecting rods, each of which is provided with a sub-frame-shaped stirring rack or stirring blade. The two connecting rods are rotatable, and the connecting rods rotate with the stirring rods. The movement of the reaction liquid in the reactor can drive the rotation of the connecting rods themselves, further increasing the stirring force.

[0045] Furthermore, in at least one embodiment, the production equipment of the aziridine cross-linking agent also includes a water bath heating tank, and the mixing device and the reactor three are arranged in the same water bath heating tank.

[0046] The mixing and addition reaction of concentrated sulfuric acid and isopropanolamine are both at about 5°C. The mixing equipment and reactor 3 are set in a water bath heating tank to make rational use of resources.

[0047] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application and are not limiting. Although the present application has been described in detail with reference to the preferred embodiments, ordinary technicians in this field should understand that the technical solutions of the present application can be modified or replaced by equivalents without departing from the purpose and scope of the technical solutions of the present application, which should be included in the scope of the claims of the present application.

Claims

1. A production equipment for an aziridine crosslinking agent, characterized in that, It includes esterification equipment, cyclization equipment, addition equipment and storage equipment connected in sequence through pipelines; The esterification equipment is used for the esterification reaction of isopropanolamine and concentrated sulfuric acid, and includes a mixing device, a preheating kettle, and a reaction kettle connected in sequence through pipelines; The cyclization equipment is used for the cyclization reaction of ammonium sulfate with a base, and comprises a second reactor and a dehydration device connected in sequence through pipelines; The addition device is used for the Michael addition reaction of aziridine and base, and includes a reactor 3, a static device, and a separation device connected in sequence by pipelines; the number of the static devices is at least 2 and they are arranged in parallel; The storage device is used for storing the aziridine cross-linking agent and includes a pre-storage device and a packaging device. The number of the pre-storage devices is at least 2 and they are arranged in parallel.

2. The production equipment of an aziridine crosslinking agent according to claim 1, characterized in that: The esterification equipment further includes a receiver and a pressure reducing device. The reactor 1 is connected to the receiver through a pipeline, and the receiver is connected to the pressure reducing device through a pipeline.

3. The production equipment of an aziridine crosslinking agent according to claim 1, characterized in that, The cyclization equipment further comprises an alkali tank, which is connected to the reactor 2 via a first pipeline, and a flow valve 1 is provided on the first pipeline.

4. The production equipment of an aziridine crosslinking agent according to claim 3, characterized in that, The alkali tank is connected to the reactor through a second pipeline, and a second flow valve is provided on the second pipeline.

5. The production equipment of an aziridine crosslinking agent according to claim 1, characterized in that, The pre-storage device is connected to the separation device through a reflux pipe.

6. The production equipment of an aziridine crosslinking agent according to claim 1, characterized in that: A stirring rod is provided in the reactor three, a frame-shaped stirring rack is provided on the stirring rod, and a brush is provided on the outer wall of the frame-shaped stirring rack.

7. The production equipment of an aziridine cross-linking agent according to claim 6, characterized in that: Two connecting rods are provided on the upper inner wall of the frame-shaped stirring frame, namely a left connecting rod and a right connecting rod. The left connecting rod is provided with a sub-frame-shaped stirring frame, and the right connecting rod is provided with a stirring blade.

8. The production equipment of an aziridine cross-linking agent according to claim 7, characterized in that: The connecting rod is rotatable.

9. The production equipment of an aziridine cross-linking agent according to claim 1, characterized in that: The production equipment of the aziridine cross-linking agent also includes a water bath heating tank, and the mixing device and the reactor three are arranged in the same water bath heating tank.

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