Liquid-phase amination reaction synthesis system and synthesis method

Abstract

The invention belongs to a liquid-phase amination reaction synthesis system and a synthesis method. 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 invention belongs to the technical field of amination reaction, and in particular relates to a liquid phase amination reaction synthesis system and a synthesis method. Background Art

[0002] In the amination reaction, the reaction is mainly a heterogeneous reaction with gas and liquid as the main phases. In order to ensure sufficient reaction, it is necessary to ensure that the two raw materials in different phases are fully mixed. In order to achieve the above purpose, the liquid raw material is usually converted into a gas phase, so that the two gas phases react with each other to meet the reaction requirements; the above reaction process has the following defects: 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 a heat exchange jacket is provided on the outside of the traditional reactor to remove the reaction heat in time; since the reactor is a gas-gas reaction, it has the defects of slow reaction rate and unsatisfactory heat exchange effect; thus affecting the normal progress of the synthesis reaction. Summary of the invention

[0003] The present invention provides a liquid phase amination reaction synthesis system and a synthesis method, which are used to solve the technical problems raised in the above background technology.

[0004] The technical solution of the present invention is:

[0005] A liquid phase amination reaction synthesis system comprises a first liquid phase feed pipeline and a second liquid phase feed pipeline, wherein the first liquid phase feed pipeline is connected to the middle inlet of a reactor, a 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, and a material outlet is arranged at the middle and upper part of the reactor.

[0006] The beneficial effects of the present invention are as follows: the present invention abandons the traditional technical solution in which the amination reaction is in the form of reaction of two gaseous raw materials, and achieves the characteristics of improving the reaction efficiency and quickly removing the reaction heat to avoid affecting the reaction process through the reaction of two liquid raw materials; specifically, the first liquid phase in the first liquid phase feed pipeline of the present invention enters the reactor, reacts with the second liquid phase from the circulating material inlet, and is cooled in the reaction liquid cooler during the circulation process to achieve the characteristics of sufficient 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 the 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, and 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 on 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 circulating material outlet of the reactor; the shell side inlet of the reaction liquid cooler is connected to the cooling water supply pipeline, and the shell side outlet of the reaction liquid cooler is connected to the cooling water reflux pipeline.

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

[0011] Preferably, the second liquid phase feed pipeline is provided with a second flow meter and a second regulating valve; the material outlet is connected to the subsequent process section via a pipeline with an overflow valve.

[0012] Preferably, the circulating material inlet of the reactor is connected to the liquid phase inlet of the ejector arranged 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 vent main pipeline with a vent regulating valve is provided on 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 nozzle of the distributor is arranged on the top of the distributor.

[0015] The present invention also provides a liquid phase amination reaction synthesis method, which comprises the following steps:

[0016] Step 1: The first liquid phase in the first liquid phase feed pipeline enters the distributor inside the reactor through the first flow meter and the pressure sensor and is distributed into a fine material flow from bottom to top, and finally enters the lower part of the distributor by gravity;

[0017] Step 2: The second liquid phase in the second liquid phase feed pipeline passes through the second flow meter and the second regulating valve and enters the first inlet of the mixer;

[0018] Step 3: The liquid phase in the reactor enters the second inlet of the mixer through the circulating material outlet at the bottom of the reactor and the circulating pump;

[0019] Step 4: The second liquid phase entering the mixer in step 2 and the liquid phase in the reactor entering the mixer in step 4 are mixed to form a mixed liquid, and the mixed liquid enters the tube side of the reaction liquid cooler to exchange heat with the cooling water from the shell side of the reaction liquid cooler, so as to remove the reaction heat in the reactor in time;

[0020] Step 5: The mixed liquid after heat exchange and cooling enters the liquid phase inlet of the ejector, and the gas phase in the reactor enters the air inlet of the ejector. After further mixing, the two pass through the ejector outlet in a dispersed state and move downward from the upper part of the reactor;

[0021] The material in the ejector moves from top to bottom and is fully contacted and mixed with the first liquid phase distributed from bottom to top in step 1 into a fine material flow; the above materials are fully contacted and mixed, and an amination reaction is carried out at the temperature and pressure in the reactor; the temperature in the reactor is 40-50° C. and the pressure is 0.01-0.05 MPa;

[0022] Step 6: The materials that have undergone amination reaction and the materials that have not undergone amination reaction are at the bottom of the reactor. Repeating the above steps 2-5 can achieve sufficient mixing between the materials and remove the reaction heat;

[0023] Step 7: Through the continuous reaction of the above process, the liquid level is gradually increased, and the reaction liquid is sent to the subsequent section through a pipeline with an overflow valve.

[0024] A liquid-phase amination reaction synthesis system and a synthesis method prepared according to the above scheme can change the original gas-gas reaction heat exchange form in the reactor to liquid phase circulation cooling in the reaction liquid cooler outside the reactor by setting a reaction liquid cooler, so as to achieve the characteristic of timely removal of reaction heat; in addition, the present invention adopts a method in which 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 circulating material inlet, so as to achieve 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 mixed for the first time in the mixer, and then for the second time in the ejector, and finally enter the reactor for the third mixing, so as to achieve full mixing between the two materials, so as to achieve the characteristic of improving the amination reaction rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a structural schematic diagram of the present invention.

[0026] Numbers 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 flow meter; 13. pressure sensor; 14. first regulating valve; 15. second flow meter; 16. second regulating valve; 17. ejector; 18. vent regulating valve; 19. pressure safety valve; 20. safety pipeline; 21. overflow valve; 22. nozzle. DETAILED DESCRIPTION

[0027] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention is described in detail below in conjunction with the accompanying drawings. The description in this part is only exemplary and explanatory and should not have any limiting effect on the protection scope of the present invention.

[0028] It should be noted that similar reference numerals and letters denote similar items in the following drawings, and therefore, once an item is defined in one drawing, further definition and explanation thereof is not required in subsequent drawings.

[0029] It should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inside", "outside", etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the drawings, or are the orientation or positional relationship in which the invented product is usually placed when in use. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", "third", etc. are only used to distinguish the description, and cannot be understood as indicating or implying relative importance.

[0030] In addition, the terms "horizontal", "vertical", "overhanging" and the like do not mean that the components are required to be absolutely horizontal or overhanging, but can be slightly tilted. For example, "horizontal" only means that its direction is more horizontal than "vertical", and does not mean that the structure must be completely horizontal, but can be slightly tilted.

[0031] In the description of the present invention, it is also necessary to explain that, unless otherwise clearly specified and limited, the terms "set", "install", "connect", and "connect" 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 a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0032] like Figure 1As shown, the present invention is a liquid phase amination reaction synthesis system and synthesis method, and the synthesis system includes a first liquid phase feed pipeline 1 and a second liquid phase feed pipeline 2, wherein the first liquid phase feed pipeline 1 is connected to the middle inlet of the reactor 3, the circulating material outlet at the bottom of the reactor 3 and the second liquid phase feed pipeline 2 are connected to the circulating material inlet of the reactor 3 through a reaction liquid cooler 4, and a material outlet 5 is provided at the middle and upper part of the reactor 3. Compared with the traditional amination reaction, the present invention adopts a liquid phase mixing reaction mode, and adopts a form in which one liquid phase directly enters the reactor 3, and the other liquid phase is mixed and cooled with the liquid phase in the reactor 3 outside before entering the reactor 3 for reaction, so as to improve the mixing efficiency and quickly remove the reaction heat, so as to realize the characteristics of rapid amination reaction; compared with other two liquid phase material mixing reactions, the present invention can realize the double mixing of materials, thereby achieving the characteristics of improving the mixing efficiency.

[0033] Furthermore, the first liquid phase feed pipeline 1 is connected to the distributor 6 inside the reactor 3. In the present invention, the first liquid phase of the first liquid phase feed pipeline 1 enters the reactor 3 through the distributor 6 to achieve uniform distribution of the first liquid phase, thereby achieving the characteristics of improving mixing efficiency and accelerating the reaction process.

[0034] Furthermore, the second liquid phase feed pipeline 2 is connected to the first inlet of the mixer 7, the circulating material outlet at the bottom of the reactor 3 is connected to the second inlet of the mixer 7 through the circulating pump 8, the outlet of the mixer 7 is connected to the tube side inlet of the reaction liquid cooler 4, and the tube side outlet of the reaction liquid cooler 4 is connected to the circulating material inlet of the reactor 3. The present invention arranges the mixer 7 at the front of the mixer 7 to fully mix the second liquid phase with the liquid phase material from the reactor 3, so as to improve the mixing efficiency and realize the initial cooling of the liquid phase material in the reactor 3, which lays a foundation for further cooling in the reaction liquid cooler 4 later.

[0035] Furthermore, a baffle 9 is provided on 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 circulating material outlet of the reactor 3; the shell side inlet of the reaction liquid cooler 4 is connected to the cooling water supply pipeline 10, and the shell side outlet of the reaction liquid cooler 4 is connected to the cooling water reflux pipeline 11. The present invention provides a baffle 9 on the upper part of the tube side of the reaction liquid cooler 4, so that one side of the upper part of the tube side of the reaction liquid cooler 4 is the circulating material inlet, and the other side is the circulating material outlet, thereby extending the heat exchange path of the circulating material to achieve the characteristic of fully exchanging the circulating material.

[0036] Furthermore, the first liquid phase feed pipeline 1 is connected to the inlet of the distributor 6 via a pressure sensor 13, a first flowmeter 12 and a first regulating valve 14. The above arrangement enables monitoring of the pressure and flow of the first liquid phase to meet the requirements of subsequent reactions.

[0037] Furthermore, the second liquid phase feed pipeline 2 is provided with a second flow meter 15 and a second regulating valve 16; the material outlet 5 is connected to the subsequent process section via a pipeline with an overflow valve 21. The above arrangement enables monitoring of the flow of the second liquid phase to meet the needs of subsequent reactions.

[0038] Furthermore, the circulating material inlet of the reactor 3 is connected to the liquid phase inlet of the ejector 17 disposed 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 disposed inside the reactor 3. The above arrangement enables full mixing and uniform distribution of the materials, so that the materials can be uniformly mixed with the first liquid phase uniformly distributed in the reactor 3 in the subsequent process, thereby achieving the characteristic of improving the reaction efficiency.

[0039] Furthermore, a venting main pipeline with a venting 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 venting regulating valve 18, and the third end of the tee is connected to a safety pipeline 20 with a pressure safety valve 19. The above arrangement can 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 venting main pipeline with the venting regulating valve 18; when the internal pressure of the reactor 3 increases, it can be discharged through the safety pipeline 20 with the pressure safety valve 19.

[0040] Furthermore, the nozzle 22 of the distributor 6 is arranged on the top of the distributor 6 .

[0041] The present invention also provides a liquid phase amination reaction synthesis method, which comprises the following steps:

[0042] Step 1: The first liquid phase in the first liquid phase feed pipeline 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;

[0043] Step 2: The second liquid phase in the second liquid phase feeding pipeline 2 passes through the second flow meter 15 and the second regulating valve 16 and enters the first inlet of the mixer 7;

[0044] 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;

[0045] 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 from the shell side of the reaction liquid cooler 4, so that the reaction heat in the reactor 3 can be removed in time;

[0046] 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 further mixing, the mixed liquid passes through the outlet of the ejector 17 in a dispersed state and moves downward from the upper part of the reactor 3;

[0047] The material in the ejector 17 moves downward from top to bottom and is fully contacted and mixed with the first liquid phase distributed from bottom to top in step 1 into a fine material flow; the above materials are fully contacted and mixed, and amination reaction is carried out at the temperature and pressure in the reactor 3; the temperature in the reactor 3 is 40-50° C., and the pressure is 0.01-0.05 MPa;

[0048] Step 6: The materials that have undergone amination reaction and the materials that have not undergone amination reaction are at the inner bottom of the reactor 3. Repeating the above steps 2-5 can achieve sufficient mixing between the materials and remove the reaction heat;

[0049] Step 7: Through the continuous reaction of the above process, the liquid level is gradually increased, and the reaction liquid is sent to the subsequent section through a pipeline with an overflow valve 21.

[0050] The present invention has the characteristics of reasonable process design, capable of achieving full mixing between liquid phase materials and timely removing reaction heat to improve the efficiency of amination reaction; the reaction time is 6 hours in a traditional way, while the entire reaction time is 4 to 4.5 hours through the above process of the present invention, and the reaction heat can be removed in time to avoid the problem of high temperature and high pressure in the reactor 3 affecting the reaction process during the reaction; the process of removing the reaction heat in the present invention includes the cooling of the kettle liquid in the reactor 3 and the second liquid phase in the mixer 7, and the second cooling of the heat exchange cooling in the reaction liquid cooler 4; the mixing described in the present invention includes the mixing in the mixer 7, the mixing in the heat exchange process in the reaction liquid cooler 4, the mixing in the ejector 17, and the mixing in the reactor 3, and the above mixing can achieve full mixing between the materials to achieve the characteristic of improving the reaction rate.

[0051] Example 1

[0052] A liquid-phase amination reaction synthesis system comprises a first liquid-phase feed pipeline 1 and a second liquid-phase feed pipeline 2, wherein the first liquid-phase feed pipeline 1 is connected to the middle inlet of a reactor 3, the circulating material outlet at the bottom of the reactor 3 and the second liquid-phase feed pipeline 2 are connected to the circulating material inlet of the reactor 3 through a reaction liquid cooler 4, and a material outlet 5 is provided in the middle and upper part of the reactor 3. The first liquid-phase feed pipeline 1 is connected to a distributor 6 inside the reactor 3. The second liquid-phase feed pipeline 2 is connected to the first inlet of a mixer 7, the circulating material outlet at the bottom of the reactor 3 is connected to the second inlet of the mixer 7 through a circulation pump 8, the outlet of the mixer 7 is connected to the tube-side inlet of the reaction liquid cooler 4, and the tube-side outlet of the reaction liquid cooler 4 is connected to the circulating material inlet of the reactor 3. The reaction liquid cooler 4 is provided with a baffle 9 on the upper part of the tube side, 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 circulating material outlet of the reactor 3; the shell side inlet of the reaction liquid cooler 4 is connected to the cooling water supply pipeline 10, and the shell side outlet of the reaction liquid cooler 4 is connected to the cooling water reflux pipeline 11. The first liquid phase feed pipeline 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. The second liquid phase feed pipeline 2 is provided with a second flowmeter 15 and a second regulating valve 16; the material outlet 5 is connected to the back section through a pipeline with an overflow valve 21. The circulating material inlet of the reactor 3 is connected to the liquid phase inlet of the ejector 17 arranged 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. A venting main pipeline with a venting 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 venting regulating valve 18, and the third end of the tee is connected to a safety pipeline 20 with a pressure safety valve 19. The nozzle 22 of the distributor 6 is arranged on the top of the distributor 6.

[0053] The present invention also provides a liquid phase amination reaction synthesis method, which comprises the following steps:

[0054] Step 1: The first liquid phase in the first liquid phase feed pipeline 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;

[0055] Step 2: The second liquid phase in the second liquid phase feeding pipeline 2 passes through the second flow meter 15 and the second regulating valve 16 and enters the first inlet of the mixer 7;

[0056] 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;

[0057] 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 from the shell side of the reaction liquid cooler 4, so that the reaction heat in the reactor 3 can be removed in time;

[0058] 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 further mixing, the mixed liquid passes through the outlet of the ejector 17 in a dispersed state and moves downward from the upper part of the reactor 3;

[0059] The material in the ejector 17 moves downward from top to bottom and is fully contacted and mixed with the first liquid phase distributed from bottom to top in step 1 into a fine material flow; the above materials are fully contacted and mixed, and amination reaction is carried out at the temperature and pressure in the reactor 3; the temperature in the reactor 3 is 45° C. and the pressure is 0.03 MPa;

[0060] Step 6: The materials that have undergone amination reaction and the materials that have not undergone amination reaction are at the inner bottom of the reactor 3. Repeating the above steps 2-5 can achieve sufficient mixing between the materials and remove the reaction heat;

[0061] Step 7: Through the continuous reaction of the above process, the liquid level is gradually increased, and the reaction liquid is sent to the subsequent section through a pipeline with an overflow valve 21.

[0062] Example 2

[0063] A liquid-phase amination reaction synthesis system comprises a first liquid-phase feed pipeline 1 and a second liquid-phase feed pipeline 2, wherein the first liquid-phase feed pipeline 1 is connected to the middle inlet of a reactor 3, the circulating material outlet at the bottom of the reactor 3 and the second liquid-phase feed pipeline 2 are connected to the circulating material inlet of the reactor 3 through a reaction liquid cooler 4, and a material outlet 5 is provided in the middle and upper part of the reactor 3. The first liquid-phase feed pipeline 1 is connected to a distributor 6 inside the reactor 3. The second liquid-phase feed pipeline 2 is connected to the first inlet of a mixer 7, the circulating material outlet at the bottom of the reactor 3 is connected to the second inlet of the mixer 7 through a circulation pump 8, the outlet of the mixer 7 is connected to the tube-side inlet of the reaction liquid cooler 4, and the tube-side outlet of the reaction liquid cooler 4 is connected to the circulating material inlet of the reactor 3. The reaction liquid cooler 4 is provided with a baffle 9 on the upper part of the tube side, 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 circulating material outlet of the reactor 3; the shell side inlet of the reaction liquid cooler 4 is connected to the cooling water supply pipeline 10, and the shell side outlet of the reaction liquid cooler 4 is connected to the cooling water reflux pipeline 11. The first liquid phase feed pipeline 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. The second liquid phase feed pipeline 2 is provided with a second flowmeter 15 and a second regulating valve 16; the material outlet 5 is connected to the back section through a pipeline with an overflow valve 21. The circulating material inlet of the reactor 3 is connected to the liquid phase inlet of the ejector 17 arranged 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. A venting main pipeline with a venting 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 venting regulating valve 18, and the third end of the tee is connected to a safety pipeline 20 with a pressure safety valve 19. The nozzle 22 of the distributor 6 is arranged on the top of the distributor 6.

[0064] The present invention also provides a liquid phase amination reaction synthesis method, which comprises the following steps:

[0065] Step 1: The first liquid phase in the first liquid phase feed pipeline 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;

[0066] Step 2: The second liquid phase in the second liquid phase feeding pipeline 2 passes through the second flow meter 15 and the second regulating valve 16 and enters the first inlet of the mixer 7;

[0067] 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;

[0068] 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 from the shell side of the reaction liquid cooler 4, so that the reaction heat in the reactor 3 can be removed in time;

[0069] 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 further mixing, the mixed liquid passes through the outlet of the ejector 17 in a dispersed state and moves downward from the upper part of the reactor 3;

[0070] The material in the ejector 17 moves downward from top to bottom and is fully contacted and mixed with the first liquid phase distributed from bottom to top in step 1 into a fine material flow; the above materials are fully contacted and mixed, and amination reaction is carried out at the temperature and pressure in the reactor 3; the temperature in the reactor 3 is 50° C. and the pressure is 0.05 MPa;

[0071] Step 6: The materials that have undergone amination reaction and the materials that have not undergone amination reaction are at the inner bottom of the reactor 3. Repeating the above steps 2-5 can achieve sufficient mixing between the materials and remove the reaction heat;

[0072] Step 7: Through the continuous reaction of the above process, the liquid level is gradually increased, and the reaction liquid is sent to the subsequent section through a pipeline with an overflow valve 21.

[0073] Example 3

[0074] A liquid-phase amination reaction synthesis system comprises a first liquid-phase feed pipeline 1 and a second liquid-phase feed pipeline 2, wherein the first liquid-phase feed pipeline 1 is connected to the middle inlet of a reactor 3, the circulating material outlet at the bottom of the reactor 3 and the second liquid-phase feed pipeline 2 are connected to the circulating material inlet of the reactor 3 through a reaction liquid cooler 4, and a material outlet 5 is provided in the middle and upper part of the reactor 3. The first liquid-phase feed pipeline 1 is connected to a distributor 6 inside the reactor 3. The second liquid-phase feed pipeline 2 is connected to the first inlet of a mixer 7, the circulating material outlet at the bottom of the reactor 3 is connected to the second inlet of the mixer 7 through a circulation pump 8, the outlet of the mixer 7 is connected to the tube-side inlet of the reaction liquid cooler 4, and the tube-side outlet of the reaction liquid cooler 4 is connected to the circulating material inlet of the reactor 3. The reaction liquid cooler 4 is provided with a baffle 9 on the upper part of the tube side, 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 circulating material outlet of the reactor 3; the shell side inlet of the reaction liquid cooler 4 is connected to the cooling water supply pipeline 10, and the shell side outlet of the reaction liquid cooler 4 is connected to the cooling water reflux pipeline 11. The first liquid phase feed pipeline 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. The second liquid phase feed pipeline 2 is provided with a second flowmeter 15 and a second regulating valve 16; the material outlet 5 is connected to the back section through a pipeline with an overflow valve 21. The circulating material inlet of the reactor 3 is connected to the liquid phase inlet of the ejector 17 arranged 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. A venting main pipeline with a venting 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 venting regulating valve 18, and the third end of the tee is connected to a safety pipeline 20 with a pressure safety valve 19. The nozzle 22 of the distributor 6 is arranged on the top of the distributor 6.

[0075] The present invention also provides a liquid phase amination reaction synthesis method, which comprises the following steps:

[0076] Step 1: The first liquid phase in the first liquid phase feed pipeline 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;

[0077] Step 2: The second liquid phase in the second liquid phase feeding pipeline 2 passes through the second flow meter 15 and the second regulating valve 16 and enters the first inlet of the mixer 7;

[0078] 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;

[0079] 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 from the shell side of the reaction liquid cooler 4, so that the reaction heat in the reactor 3 can be removed in time;

[0080] 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 further mixing, the mixed liquid passes through the outlet of the ejector 17 in a dispersed state and moves downward from the upper part of the reactor 3;

[0081] The material in the ejector 17 moves downward from top to bottom and is fully contacted and mixed with the first liquid phase distributed from bottom to top in step 1 into a fine material flow; the above materials are fully contacted and mixed, and an amination reaction is carried out at the temperature and pressure in the reactor 3; the temperature in the reactor 3 is 40° C. and the pressure is 0.01 MPa;

[0082] Step 6: The materials that have undergone amination reaction and the materials that have not undergone amination reaction are at the inner bottom of the reactor 3. Repeating the above steps 2-5 can achieve sufficient mixing between the materials and remove the reaction heat;

[0083] Step 7: Through the continuous reaction of the above process, the liquid level is gradually increased, and the reaction liquid is sent to the subsequent section through a pipeline with an overflow valve 21.

[0084] It should be noted that, in this article, the terms "comprises", "includes" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article or apparatus that includes a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or apparatus.

[0085] This article uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. The above are only preferred implementation methods of the present invention. It should be pointed out that due to the limitations of textual expression, there are objectively infinite specific structures. For ordinary technicians in this technical field, without departing from the principles of the present invention, several improvements, modifications or changes can be made, and the above technical features can be combined in an appropriate manner; these improvements, changes or combinations, or the direct application of the inventive concept and technical solution to other occasions without improvement, should be regarded as the protection scope of the present invention.

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 pipeline (1) is connected to the middle inlet of the reactor (3), the circulating material outlet at the bottom of the reactor (3) and the second liquid-phase feed pipeline (2) are connected to the circulating material inlet of the reactor (3) through a reaction liquid cooler (4), and a material outlet (5) is provided in the middle and upper part of the reactor (3).

2. A liquid phase amination reaction synthesis system according to claim 1, characterized in that: The first liquid phase feed pipeline (1) is connected to a distributor (6) inside the reactor (3).

3. A liquid phase amination reaction synthesis system according to claim 1, characterized in that: The second liquid phase feed pipeline (2) is connected to the first inlet of the mixer (7), the circulating material outlet at the bottom of the reactor (3) is connected to the second inlet of the mixer (7) through a circulating pump (8), the outlet of the mixer (7) is connected to the tube side inlet of the reaction liquid cooler (4), and the tube side outlet of the reaction liquid cooler (4) is connected to the circulating material inlet of the reactor (3).

4. A liquid phase amination reaction synthesis system according to claim 3, characterized in that: A baffle (9) is provided on 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 circulating 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 reflux pipeline (11).

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

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

7. A liquid phase amination reaction synthesis system according to claim 1, 3 or 4, characterized in that: The circulating material inlet of the reactor (3) is connected to the liquid phase inlet of the ejector (17) arranged 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. A liquid phase amination reaction synthesis system according to claim 7, characterized in that: A venting main pipeline with a venting 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 venting regulating valve (18), and the third end of the tee is connected to a safety pipeline (20) with a pressure safety valve (19).

9. A liquid phase amination reaction synthesis system according to claim 2, characterized in that: The nozzle (22) of the distributor (6) is arranged on the top of the distributor (6).

10. A liquid phase amination reaction synthesis method according to any one of claims 1 to 9, characterized in that: The method comprises the following steps: Step 1: The first liquid phase in the first liquid phase feed pipeline (1) enters the distributor (6) inside the reactor (3) through the first flow meter (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 pipeline (2) passes through the second flow meter (15) and the second regulating valve (16) and then enters the first inlet of the mixer (7); 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 from the shell side of the reaction liquid cooler (4), so that the reaction heat in the reactor (3) can be removed in time; 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 further mixing, the mixed liquid passes through the outlet of the ejector (17) in a dispersed state and moves downward from the upper part of the reactor (3); The material in the ejector (17) moves downward from top to bottom and is fully contacted and mixed 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 an amination reaction is carried out at the temperature and pressure in the reactor (3); the temperature in the reactor (3) is 40-50°C, and the pressure is 0.01-0.05Mpa; Step 6: The materials that have undergone amination reaction and the materials that have not undergone amination reaction are at the bottom of the reactor (3). Repeating the above steps 2-5 can achieve sufficient mixing between the materials and remove the reaction heat; Step 7: Through the continuous reaction of the above process, the liquid level is gradually increased, and the reaction liquid is sent to the subsequent process section through a pipeline with an overflow valve (21).

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