Liquid-phase amination reaction synthesis system

Abstract

The utility model belongs to a liquid-phase amination reaction synthesis system. Comprising a first liquid phase feeding pipeline and a second liquid phase feeding pipeline, the first liquid phase feeding pipeline is connected with an inlet in the middle of the reactor, a circulating material outlet in the bottom of the reactor and the second liquid phase feeding pipeline are connected with a circulating material inlet of the reactor through a reaction liquid cooler, and a material outlet is formed in the upper middle portion of the reactor; through the reaction of the two liquid-phase raw materials, the reaction efficiency is improved, the reaction heat is quickly removed, and the influence on the reaction process is avoided.

Description

Technical Field

[0001] The utility model belongs to the technical field of amination reaction, and particularly relates to a liquid-phase amination reaction synthesis system. Background Art

[0002] In the amination reaction, the reaction is mainly a heterogeneous reaction with gas and liquid phases. To ensure sufficient reaction, it is necessary to ensure the full mixing of raw materials in two different phases. To achieve the above purpose, the liquid-phase raw material is usually converted into gas phase, so that the two gas phases react with each other to meet the reaction requirements. The following defects exist in the above reaction process: 1. The mixing speed between the two gas phases is slow, resulting in a slow reaction speed; 2. The amination reaction is an exothermic reaction, and the traditional reactor is externally provided with a heat exchange jacket for timely removing the reaction heat; due to the gas-gas reaction inside the reactor, there are defects of slow reaction rate and unsatisfactory heat exchange effect; thus affecting the normal progress of the synthesis reaction. Summary of the Utility Model

[0003] The utility model provides a liquid-phase amination reaction synthesis system for solving the technical problems put forward in the above background art.

[0004] The technical solution of the utility model is as follows:

[0005] A liquid-phase amination reaction synthesis system includes a first liquid-phase feed pipeline and a second liquid-phase feed pipeline. The first liquid-phase feed pipeline is connected to the middle inlet of the reactor. The circulating material outlet at the bottom of the reactor and the second liquid-phase feed pipeline are connected to the circulating material inlet of the reactor through a reaction liquid cooler. A material outlet is provided in the upper middle part of the reactor.

[0006] The beneficial effect of the utility model is that the utility model abandons the form of the amination reaction with two gas-phase raw materials in the traditional technical solution, and improves the reaction efficiency through the reaction of two liquid-phase raw materials, and quickly removes the reaction heat to avoid affecting the reaction process. Specifically, the first liquid phase in the first liquid-phase feed pipeline of the utility model enters the reactor and reacts with the second liquid phase from the circulating material inlet. At the same time, it is cooled in the reaction liquid cooler during the circulation process to achieve the characteristics of full mixing between the two materials and timely removal of the reaction heat.

[0007] Preferably, the first liquid-phase feed pipeline is connected to a distributor inside the reactor.

[0008] Preferably, the second liquid-phase feed pipeline is connected to the first inlet of a mixer. The circulating material outlet at the bottom of the reactor is connected to the second inlet of the mixer through a circulating pump. The outlet of the mixer is connected to the tube-side inlet of the reaction liquid cooler. The tube-side outlet of the reaction liquid cooler is connected to the circulating material inlet of the reactor.

[0009] Preferably, a baffle is provided at the upper part of the tube side of the reaction liquid cooler. One side of the baffle is connected to the outlet of the mixer, and the other side of the baffle is connected to the recycled material outlet of the reactor. The inlet of the shell side of the reaction liquid cooler is connected to the cooling water supply pipeline, and the outlet of the shell side of the reaction liquid cooler is connected to the cooling water return pipeline.

[0010] Preferably, the first liquid phase feed pipeline is connected to the inlet of the distributor through a pressure sensor, a first flowmeter, and a first regulating valve.

[0011] Preferably, a second flowmeter and a second regulating valve are provided on the second liquid phase feed pipeline. The material outlet is connected to the subsequent process through a pipeline with an overflow valve.

[0012] Preferably, the recycled material inlet of the reactor is connected to the liquid phase inlet of an ejector provided at the top of the reactor. The air inlet of the ejector is connected to the gas phase outlet at the top of the reactor, and the outlet of the ejector is arranged inside the reactor.

[0013] Preferably, a main vent pipeline with a vent regulating valve is provided at the top gas phase safety outlet of the reactor. A tee is provided between the gas phase safety outlet and the vent regulating valve, and the third end of the tee is connected to a safety pipeline with a pressure safety valve.

[0014] Preferably, the spray head of the distributor is arranged at the top of the distributor.

[0015] A liquid phase amination reaction synthesis system made according to the above solution can change the heat exchange form of the original gas-gas reaction in the reactor to the reaction liquid in the reaction liquid cooler outside the reactor circulating and cooling, so as to achieve the characteristic of timely removing the reaction heat. In addition, the present invention adopts the method that the first liquid phase in the first liquid phase feed pipeline enters the reactor, and the second liquid phase in the second liquid phase feed pipeline enters through the recycled material inlet, so as to realize the full mixing of the two liquid phases. Further, the second liquid phase in the second liquid phase feed pipeline and the material in the reactor can be initially mixed in the mixer, then mixed again in the ejector, and finally enter the reactor for three times of mixing, so as to realize the full mixing between the two materials, so as to realize the characteristic of improving the amination reaction rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 is a schematic structural diagram of the present invention.

[0017] Reference numerals in the figure: 1. First liquid-phase feed pipeline; 2. Second liquid-phase feed pipeline; 3. Reactor; 4. Reaction liquid cooler; 5. Material outlet; 6. Distributor; 7. Mixer; 8. Circulation pump; 9. Baffle; 10. Cooling water supply pipeline; 11. Cooling water return pipeline; 12. First flowmeter; 13. Pressure sensor; 14. First regulating valve; 15. Second flowmeter; 16. Second regulating valve; 17. Injector; 18. Vent regulating valve; 19. Pressure safety valve; 20. Safety pipeline; 21. Overflow valve; 22. Sprinkler head. Detailed implementation mode

[0018] In order to enable those skilled in the art to better understand the technical solution of the present utility model, the present utility model will be described in detail below with reference to the accompanying drawings. The description of this part is only exemplary and explanatory, and should not have any restrictive effect on the protection scope of the present utility model.

[0019] It should be noted that similar reference numerals and letters represent similar items in the following drawings. Therefore, once an item is defined in one drawing, it does not need to be further defined and explained in subsequent drawings.

[0020] It should be noted that the orientation or positional relationship indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. is based on the orientation or positional relationship shown in the drawings, or the orientation or positional relationship in which the product of this utility model is usually placed during use. It is only for the convenience of describing the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation to the present utility model. In addition, the terms "first", "second", "third", etc. are only used for distinguishing descriptions and cannot be understood as indicating or implying relative importance.

[0021] In addition, terms such as "horizontal", "vertical", "overhanging", etc. do not mean that the components are required to be absolutely horizontal or overhanging, but can be slightly inclined. For example, "horizontal" only means that its direction is more horizontal relative to "vertical", and does not mean that the structure must be completely horizontal, but can be slightly inclined.

[0022] In the description of the present utility model, it should also be noted that unless otherwise clearly specified and defined, the terms "set", "installed", "connected", "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, and can be the communication inside two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present utility model can be understood according to specific situations.

[0023] As Figure 1 shown, the utility model is a liquid-phase amination reaction synthesis system, including a first liquid-phase feed pipeline 1 and a second liquid-phase feed pipeline 2. The first liquid-phase feed pipeline 1 is connected to the middle inlet of a reactor 3. The recycle material outlet at the bottom of the reactor 3 and the second liquid-phase feed pipeline 2 are connected to the recycle material inlet of the reactor 3 through a reaction liquid cooler 4. A material outlet 5 is provided in the upper-middle part of the reactor 3. Compared with the traditional amination reaction, the utility model adopts a reaction mode of liquid-phase mixing, and adopts a form that one liquid-phase directly enters the reactor 3, and the other liquid-phase is mixed and cooled externally with the liquid-phase in the reactor 3 and then enters the reactor 3 for reaction, so as to improve the mixing efficiency and quickly remove the reaction heat, so as to realize the rapid progress of the amination reaction; compared with the other two liquid-phase material mixing reactions, the utility model can realize the two-time mixing of the materials, so as to achieve the characteristic of improving the mixing efficiency.

[0024] Furthermore, the first liquid-phase feed pipeline 1 is connected to a distributor 6 inside the reactor 3. In the utility model, the first liquid-phase in the first liquid-phase feed pipeline 1 enters the reactor 3 through the distributor 6, so as to realize the uniform distribution of the first liquid-phase, thus achieving the characteristics of improving the mixing efficiency and accelerating the reaction process.

[0025] Furthermore, the second liquid-phase feed pipeline 2 is connected to the first inlet of a mixer 7. The recycle material outlet at the bottom of the reactor 3 is connected to the second inlet of the mixer 7 through a recycle pump 8. The outlet of the mixer 7 is connected to the tube-side inlet of the reaction liquid cooler 4. The tube-side outlet of the reaction liquid cooler 4 is connected to the recycle material inlet of the reactor 3. By arranging the mixer 7 in front of the mixer 7, the utility model enables the second liquid-phase to be fully mixed with the liquid-phase material from the reactor 3, so as to achieve the characteristics of improving the mixing efficiency and initially cooling the liquid-phase material in the reactor 3, laying a foundation for further cooling in the reaction liquid cooler 4 subsequently.

[0026] Furthermore, a baffle 9 is provided in the upper part of the tube side of the reaction liquid cooler 4. One side of the baffle 9 is connected to the outlet of the mixer 7, and the other side of the baffle 9 is connected to the recycle material outlet of the reactor 3. The shell-side inlet of the reaction liquid cooler 4 is connected to a cooling water supply pipeline 10, and the shell-side outlet of the reaction liquid cooler 4 is connected to a cooling water return pipeline 11. By providing the baffle 9 in the upper part of the tube side of the reaction liquid cooler 4, the utility model can make one side of the upper part of the tube side of the reaction liquid cooler 4 be the recycle material inlet and the other side be the recycle material outlet, so as to extend the heat exchange path of the recycle material, so as to achieve the characteristic of fully heat-exchanging the recycle material.

[0027] Further, the first liquid-phase feed pipe 1 is connected to the inlet of the distributor 6 through a pressure sensor 13, a first flowmeter 12, and a first regulating valve 14. Through the above settings, it is possible to monitor the pressure and flow rate of the first liquid phase to meet the requirements of subsequent reactions.

[0028] Further, a second flowmeter 15 and a second regulating valve 16 are provided on the second liquid-phase feed pipe 2; the material outlet 5 is connected to the subsequent process through a pipe with an overflow valve 21. Through the foregoing settings, it is possible to monitor the flow rate of the second liquid phase to meet the requirements of subsequent reactions.

[0029] Further, the recycle material inlet of the reactor 3 is connected to the liquid-phase inlet of an ejector 17 provided at the top of the reactor 3; the air inlet of the ejector 17 is connected to the gas-phase outlet at the top of the reactor 3, and the outlet of the ejector 17 is arranged inside the reactor 3. Through the above settings, it is possible to achieve full mixing and uniform distribution of the materials, so as to facilitate uniform mixing with the first liquid phase uniformly distributed in the reactor 3 during the subsequent process, thereby achieving the characteristic of improving the reaction efficiency.

[0030] Further, a main vent pipe with a vent regulating valve 18 is provided on the gas-phase safety outlet at the top of the reactor 3, a tee is provided between the gas-phase safety outlet and the vent regulating valve 18, and the third end of the tee is connected to a safety pipe 20 with a pressure safety valve 19. Through the above settings, it is possible to ensure the long-term safe and stable operation of the reactor 3; the non-condensable gas accumulated in the reactor 3 after long-term reaction is processed through the main vent pipe with a vent regulating valve 18; when the internal pressure of the reactor 3 rises, it can be discharged through the safety pipe 20 with a pressure safety valve 19.

[0031] Further, the material outlet 5 is connected to the subsequent process through a pipe with an overflow valve 21.

[0032] Further, the nozzle 22 of the distributor 6 is arranged at the top of the distributor 6.

[0033] The working principle of the present utility model is as follows: A method for synthesizing liquid-phase amination reaction, the method comprising the following steps: Step 1: The first liquid phase in the first liquid-phase feed pipe 1 enters the distributor 6 inside the reactor 3 through the first flowmeter 12 and the pressure sensor 13 and is distributed into a fine material flow from bottom to top, and finally enters the lower part of the distributor 6 by gravity; Step 2: The second liquid phase in the second liquid-phase feed pipe 2 enters the first inlet of the mixer 7 through the second flowmeter 15 and the second regulating valve 16; Step 3: The liquid phase in the reactor 3 enters the second inlet of the mixer 7 through the circulating material outlet at the bottom of the reactor 3 and the circulating pump 8; Step 4: The second liquid phase entering the mixer 7 in Step 2 and the liquid phase in the reactor entering the mixer 7 in Step 3 are mixed to form a mixed liquid, and the mixed liquid enters the tube side of the reaction liquid cooler 4 to exchange heat with the cooling water in the shell side of the reaction liquid cooler 4, and can timely remove the reaction heat in the reactor 3; Step 5: The mixed liquid after heat exchange and cooling enters the liquid-phase inlet of the ejector 17, and the gas phase in the reactor 3 enters the air inlet of the ejector 17. After the two are further mixed, they move downward from the upper part of the reactor 3 in a dispersed state through the outlet of the ejector 17; The material in the ejector 17 moves from top to bottom and makes full contact and mixing with the first liquid phase distributed into a fine material flow from bottom to top in Step 1; The above materials are fully contacted and mixed and undergo an amination reaction at the temperature and pressure in the reactor 3; The temperature in the reactor 3 is 40 to 50 °C, and the pressure is 0.01 to 0.05 Mpa; Step 6: The materials that have undergone the amination reaction and the materials that have not undergone the amination reaction are at the inner bottom of the reactor 3. Repeating the aforementioned Steps 2 to 5 can achieve full mixing between the materials and remove the reaction heat; Step 7: Through the continuous reaction of the foregoing process, the liquid level rises step by step, and the reaction liquid is sent to the subsequent section through the pipeline with the overflow valve 21. It has the characteristics of reasonable process design, can achieve full mixing between liquid-phase materials and timely remove the reaction heat to improve the efficiency of the amination reaction; Using the traditional method, the reaction time is 6 hours. Through the above process of the present utility model, the whole reaction time is 4 to 4.5 hours, and the reaction heat can be timely removed to avoid the problem that the high temperature and high pressure in the reactor 3 during the reaction affect the reaction process; The process of removing the reaction heat in the present utility model includes the temperature reduction of the kettle liquid in the reactor 3 and the second liquid phase mixing in the mixer 7, and the second temperature reduction of heat exchange and cooling in the reaction liquid cooler 4; The mixing in the present utility model includes the mixing in the mixer 7, the mixing during the heat exchange process in the reaction liquid cooler 4, the mixing in the ejector 17, and the mixing in the reactor 3. Through the above mixing, full mixing between the materials can be achieved to improve the reaction rate.

[0034] The standard parts used in this application document can all be purchased from the market, and can also be customized according to the descriptions in the specification and the drawings. The specific connection methods of each part all adopt conventional means such as bolts, rivets, and welding that are mature in the prior art. The machines, parts, and equipment all adopt conventional models in the prior art. The control method is to automatically control through a controller. The control circuit of the controller can be realized by simple programming by those skilled in the art, which belongs to the common general knowledge in this field. And this utility model is mainly used to protect mechanical devices, so the control method and circuit connection of this utility model will not be explained in detail. Moreover, the peripheral controller mentioned in the specification can play a control role for the electrical components mentioned in this article, and this peripheral controller is a conventional known device.

[0035] It should be noted that in this article, the term "including", "comprising" or any other variant thereof is intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements not only includes those elements, but also includes other elements not expressly listed, or further includes elements inherent to such process, method, article or device.

[0036] Specific examples are used in this article to elaborate on the principle and implementation manner of this utility model. The description of the above examples is only used to help understand the method and its core idea of this utility model. The above are only the preferred implementation manners of this utility model. It should be pointed out that due to the limited nature of written expression and the objectively infinite specific structures, for those of ordinary skill in the art in this technical field, without departing from the principle of this utility model, several improvements, refinements or changes can also be made, or the above technical features can be combined in an appropriate manner; these improvements, changes or combinations, or directly applying the concept and technical solution of the utility model to other occasions without improvement, should all be regarded as the protection scope of this utility model.

Claims

1. A liquid-phase amination reaction synthesis system, comprising a first liquid-phase feed pipeline (1) and a second liquid-phase feed pipeline (2), characterized in that: The first liquid-phase feed pipe (1) is connected to the middle inlet of the reactor (3). The recycle material outlet at the bottom of the reactor (3) and the second liquid-phase feed pipe (2) are connected to the recycle material inlet of the reactor (3) through the reaction liquid cooler (4). A material outlet (5) is provided in the upper middle part of the reactor (3).

2. The liquid-phase amination reaction synthesis system according to claim 1, wherein: The first liquid-phase feed pipe (1) is connected to the distributor (6) inside the reactor (3).

3. The liquid-phase amination reaction synthesis system according to claim 1, wherein: The second liquid-phase feed pipe (2) is connected to the first inlet of the mixer (7). The recycle material outlet at the bottom of the reactor (3) is connected to the second inlet of the mixer (7) through the recycle pump (8). The outlet of the mixer (7) is connected to the tube-side inlet of the reaction liquid cooler (4). The tube-side outlet of the reaction liquid cooler (4) is connected to the recycle material inlet of the reactor (3).

4. The liquid-phase amination reaction synthesis system according to claim 3, wherein: A baffle (9) is provided in the upper part of the tube side of the reaction liquid cooler (4). One side of the baffle (9) is connected to the outlet of the mixer (7), and the other side of the baffle (9) is connected to the recycle material outlet of the reactor (3). The shell-side inlet of the reaction liquid cooler (4) is connected to the cooling water supply pipe (10), and the shell-side outlet of the reaction liquid cooler (4) is connected to the cooling water return pipe (11).

5. The liquid-phase amination reaction synthesis system according to claim 2, characterized in that: The first liquid-phase feed pipe (1) is connected to the inlet of the distributor (6) through the pressure sensor (13), the first flowmeter (12), and the first regulating valve (14).

6. The liquid-phase amination reaction synthesis system according to claim 1, characterized in that: A second flowmeter (15) and a second regulating valve (16) are provided on the second liquid-phase feed pipe (2). The material outlet (5) is connected to the subsequent process section through a pipe with an overflow valve (21).

7. A liquid-phase amination reaction synthesis system according to claim 1 or 3 or 4, characterized in that: The recycle material inlet of the reactor (3) is connected to the liquid-phase inlet of the ejector (17) provided at the top of the reactor (3). The air inlet of the ejector (17) is connected to the gas-phase outlet at the top of the reactor (3), and the outlet of the ejector (17) is arranged inside the reactor (3).

8. The liquid-phase amination reaction synthesis system according to claim 7, wherein: A main vent pipe with a vent regulating valve (18) is provided on the top gas-phase safety outlet of the reactor (3). A tee is provided between the gas-phase safety outlet and the vent regulating valve (18), and the third end of the tee is connected to a safety pipe (20) with a pressure safety valve (19).

9. The liquid-phase amination reaction synthesis system according to claim 2, wherein: The nozzle (22) of the distributor (6) is arranged at the top of the distributor (6).

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