Reaction kettle with double heat exchange system for synthesis of organic amine

CN224749095UActive Publication Date: 2026-09-15江苏万盛大伟化学有限公司
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Patent Information

Application Number
CN202522648320.4
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-12-15
Publication Date
2026-09-15
Estimated Expiration
2035-12-15

AI Technical Summary

Technical Problem

[0007]通过采用上述技术方案,解决了二甲胺气体充入反应釜后易聚合形成较大的气泡导致与液体反应物无法充分接触反应的技术问题,当气体经过气体分布器充入反应釜内部后,多组高速旋转的破碎器会对气体聚合形成的气泡进行剪切破碎,使其形成细小的气泡,第一抽吸器和第二抽吸器通过负压块旋转产生的负压效果,使得第一抽吸器和第二抽吸器对反应釜顶部的气体进行抽吸,并再次充入至液体反应物中,从而增加气体与液态反应物之间的接触时间和接触面积,使得气体能够与反应物充分反应

Benefits of technology

本实用新型通过设置反应釜、伺服电机、转杆、吸气管、第一抽吸器和第二抽吸器,解决了二甲胺气体充入反应釜后易聚合形成较大的气泡导致与液体反应物无法充分接触反应的技术问题,当气体经过气体分布器充入反应釜内部后,多组高速旋转的破碎器会对气体聚合形成的气泡进行剪切破碎,使其形成细小的气泡,第一抽吸器和第二抽吸器通过负压块旋转产生的负压效果,使得第一抽吸器和第二抽吸器对反应釜顶部的气体进行抽吸,并再次充入至液体反应物中,从而增加气体与液态反应物之间的接触时间和接触面积,使得气体能够与反应物充分反应。

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Abstract

The utility model discloses a kind of reaction kettle with double heat exchange system for organic amine synthesis, it is related to double heat exchange system reaction kettle field, including reaction kettle, the top of the reaction kettle is equipped with servo motor, the one end of driving shaft is equipped with rotary rod, the outer wall of rotary rod is fixed with suction pipe, the outer wall of suction pipe is provided with first suction device and second suction device, the outer surface of suction pipe is fixedly installed with multiple groups of breaker. The utility model when gas is filled into the inside of reaction kettle after passing through gas distributor, multiple groups of high-speed rotating breaker can shear and break the bubble formed by gas polymerization to form small bubble, the negative pressure effect generated by the rotation of first suction device and second suction device through negative pressure block, so that first suction device and second suction device suck the gas on the top of reaction kettle, and then filled into liquid reactant, so as to increase the contact time and contact area between gas and liquid reactant, so that gas can fully react with reactant.
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Description

Technical Field

[0001] This utility model relates to the field of reactors with dual heat exchange systems, specifically a reactor with a dual heat exchange system for the synthesis of organic amines. Background Technology

[0002] Dual heat exchange system reactors are a type of chemical reaction equipment specifically designed for precise temperature control. Their core feature is the integration of two independent and synergistically controllable heat exchange loops, typically consisting of two sets of independent built-in coils. The two heat exchange loops can be supplied with heat transfer media of different temperatures and types, achieving dual temperature control targets through differentiated regulation. With its high heat exchange efficiency and flexible temperature control capabilities, this type of reactor can effectively avoid side reactions caused by temperature fluctuations in the reaction system.

[0003] As a high-end fine chemical raw material, the synthesis of high-purity C18-16 tertiary amines with low residual alcohol requires extremely high stability of reaction temperature and uniformity of the reaction system. Therefore, reactors with dual heat exchange systems have become the mainstream equipment for the large-scale preparation of this type of organic amine. In the preparation process, the raw material pretreatment is carried out first. C18-16 fatty alcohols are mixed with copper-nickel-aluminum composite catalysts at a specific mass ratio and preheated to 80-90℃ to form a homogeneous liquid mixture before being sent to the reactor. Then, the dual heat exchange system is activated to preheat the internal environment of the reactor. Dimethylamine gas is introduced into the reactor, and the reaction temperature is controlled at 180-230℃ and the pressure at 0.1-0.35MPa. The exothermic reaction is controlled in real time by the dual heat exchange system to maintain the system temperature stability. During the reaction, it is necessary to ensure sufficient gas-liquid contact to improve the conversion rate. After the reaction, the product is subjected to vacuum distillation to remove excess dimethylamine and residual alcohol, and finally, high-purity C18-16 tertiary amine product is obtained.

[0004] In existing double heat exchange system reactors for the synthesis of C18-16 tertiary amines, in order to improve the gas-liquid reaction efficiency, the industry generally installs a gas distributor at the bottom of the reactor. The purpose is to disperse dimethylamine gas into the reaction system through the microporous structure of the distributor, thereby increasing the contact area between the gas and the liquid raw materials. However, when dimethylamine gas is introduced through the distributor, it will quickly form discrete bubbles in the C18-16 fatty alcohol. These bubbles will rise rapidly due to buoyancy and have a short residence time in the liquid, resulting in insufficient contact between the reaction gas and the reaction liquid. Summary of the Invention

[0005] Based on this, the purpose of this utility model is to provide a reactor with a dual heat exchange system for the synthesis of organic amines, so as to solve the technical problems mentioned in the background art.

[0006] To achieve the above objectives, this utility model provides the following technical solution: a reactor with a dual heat exchange system for the synthesis of organic amines, comprising a reactor, a feed pipe and a discharge pipe respectively provided at the top and bottom of the reactor, a servo motor installed at the top of the reactor, a drive shaft connected to one end of the servo motor, a rotating rod installed at one end of the drive shaft, a suction pipe fixed to the outer wall of the rotating rod, a first suction device and a second suction device provided on the outer wall of the suction pipe, three sets of negative pressure blocks provided on the outer walls of both the first and second suction devices, a negative pressure chamber opened inside the negative pressure block, a first connecting pipe fixed to one end of the negative pressure block, and multiple sets of crushers fixedly installed on the outer surface of the suction pipe.

[0007] By adopting the above technical solution, the technical problem of dimethylamine gas easily polymerizing and forming large bubbles after being introduced into the reactor, thus preventing it from fully contacting and reacting with the liquid reactants, is solved. After the gas is introduced into the reactor through the gas distributor, multiple sets of high-speed rotating crushers will shear and break the bubbles formed by gas polymerization, turning them into small bubbles. The first and second suction devices, through the negative pressure effect generated by the rotation of the negative pressure block, allow the first and second suction devices to draw the gas from the top of the reactor and re-introduce it into the liquid reactants, thereby increasing the contact time and contact area between the gas and the liquid reactants, so that the gas can fully react with the reactants.

[0008] The present invention is further configured such that the first suction device and the second suction device are respectively provided with a first air chamber and a second air chamber, and the top of the suction pipe is provided with three sets of first suction holes and second suction holes, and the bottom of the first suction holes and the second suction holes are respectively connected to a first vent hole and a second vent hole.

[0009] Preferably, the first air intake port is connected to the first air chamber through the first vent, and the second air intake port is connected to the second air chamber through the second vent.

[0010] The present invention is further configured such that the wall surface of the negative pressure block rotating in the same direction is arc-shaped, and the port of the negative pressure chamber is located on the side opposite to the rotation direction of the rotating rod.

[0011] Preferably, since the negative pressure chamber port inside the negative pressure block is set in the opposite direction to the rotation direction of the negative pressure block, the fluid at the negative pressure chamber port will be quickly carried away due to the relative motion during the rotation of the negative pressure block, thereby making the negative pressure chamber port a negative pressure state.

[0012] The present invention is further configured such that three sets of crushing blades are fixedly provided on the outer wall of the crusher, and the wall surface of the crushing blades is provided with serrations.

[0013] Preferably, during the rotation of the rotating rod, two sets of crushers fixedly installed at the bottom of the rotating rod break the bubbles floating above the gas distributor through high-speed rotating crushing blades, breaking the bubbles into tiny bubbles at the μm level.

[0014] The present invention is further configured such that a mounting shaft is fixed to the top of the rotating rod, a support shaft is connected to the bottom of the rotating rod, a fixing rod is fixed to the outer wall of the support shaft, and the fixing rod is fixedly installed on the inner wall of the reactor.

[0015] Preferably, the rotating rod is fixedly connected to the drive shaft at the end of the servo motor via a mounting shaft at its end.

[0016] The present invention is further configured such that a baffle plate is fixed to the outer wall of the top end of the air inhalation pipe, and the top wall surface of the baffle plate is inclined.

[0017] Preferably, the baffle is located above the surface of the liquid reactants, and the baffle blocks the liquid reactants from being stirred, preventing a large amount of liquid from splashing onto the top of the suction pipe.

[0018] The present invention is further configured such that a shield is fixed to the top outer wall of the rotating rod, and the diameter of the shield is larger than the outer wall diameter of the suction pipe.

[0019] Preferably, the shield blocks the top of the suction pipe to prevent liquid reactants poured into the reactor through the feed pipe from dripping onto the first and second suction ports.

[0020] The present invention is further configured such that the reactor is provided with two sets of heat exchange tubes inside, a gas distributor is installed at the bottom of the reactor, and a gas supply pipe is connected to one side of the gas distributor, and a gas exchange pipe is installed at the top of the reactor.

[0021] Preferably, two sets of heat exchange tubes heat the liquid reactants inside the reactor, the reaction gas is transported to the reactor through a gas delivery pipe, and the gas inside the reactor is discharged through a gas exchange pipe. A gas control valve is installed at the end of the gas exchange pipe.

[0022] In summary, the present invention has the following main advantages: This invention solves the technical problem that dimethylamine gas easily polymerizes into large bubbles after being introduced into the reaction vessel, preventing sufficient contact and reaction with the liquid reactants. By incorporating a reaction vessel, servo motor, rotating rod, suction pipe, first suction device, and second suction device, the invention addresses this issue. After the gas is introduced into the reaction vessel via a gas distributor, multiple sets of high-speed rotating crushers shear and break the polymerized bubbles into smaller bubbles. The first and second suction devices, through the negative pressure effect generated by the rotating negative pressure block, draw gas from the top of the reaction vessel and re-introduce it into the liquid reactants. This increases the contact time and area between the gas and the liquid reactants, allowing for a more complete reaction.

[0023] This invention solves the technical problem of a large difference in the amount of gas ejected from the negative pressure block due to the different installation heights of the first and second suction devices by setting up a wind-facing block, a wind-facing chamber, a second connecting pipe, and a suction pipe. During the rotation of the suction pipe, the three sets of wind-facing blocks fixed at the top of the suction pipe rotate accordingly. During the high-speed rotation of the wind-facing blocks, the arc-shaped inner wall of the wind-facing chamber guides the gas around the port of the wind-facing chamber, so that the gas is sequentially introduced into the second suction hole through the wind-facing chamber and the second connecting pipe, thereby reducing the difference in the amount of gas ejected by the second suction device compared to the first suction device caused by the compression of the gas ejected by the liquid reactants. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the reaction vessel of this utility model; Figure 2 This is a diagram of the internal structure of the reaction vessel of this utility model; Figure 3 This is a schematic diagram of the suction tube installation of this utility model; Figure 4 This is an overall structural diagram of the suction tube of this utility model; Figure 5 This is a schematic diagram of the first vent of the present invention; Figure 6 This is a schematic diagram of the second vent of this utility model; Figure 7 For the present utility model Figure 6 Enlarged view of Figure A; Figure 8 This is a structural diagram of the crusher of this utility model; Figure 9 This is a schematic diagram of the installation of the windward block of this utility model; Figure 10 This is a structural diagram of the windward block of this utility model. Explanation of reference numerals in the attached figures: 1. Reactor; 101. Feed pipe; 102. Discharge pipe; 103. Ventilation pipe; 104. Heat exchanger; 105. Gas distributor; 106. Gas delivery pipe; 2. Servo motor; 201. Drive shaft; 3. Rotating rod; 301. Shield; 302. Support shaft; 303. Fixing rod; 304. Mounting shaft; 4. Suction pipe; 401. Shielding plate; 5. Crusher; 501. Crusher blade; 6. First suction device; 601. Second suction device; 602. First connecting pipe; 603. Negative pressure block; 604. Negative pressure chamber; 605. First suction port; 606. First vent; 607. First gas chamber; 608. Second suction port; 609. Second vent; 610. Second gas chamber; 7. Wind-facing block; 701. Wind-facing chamber; 702. Second connecting pipe. Detailed Implementation

[0025] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention.

[0026] The embodiments of this utility model will be described below based on its overall structure.

[0027] First embodiment: Please refer to Figure 1 — Figure 8 The reactor includes a reaction vessel 1. A feed pipe 101 and a discharge pipe 102 are respectively installed on the top of the reaction vessel 1. A servo motor 2 is installed on the top of the reaction vessel 1. One end of the servo motor 2 is connected to a drive shaft 201. A rotating rod 3 is installed on one end of the drive shaft 201. A suction pipe 4 is fixed to the outer wall of the rotating rod 3. A first suction device 6 and a second suction device 601 are installed on the outer wall of the suction pipe 4. Three sets of negative pressure blocks 603 are installed on the outer walls of both the first suction device 6 and the second suction device 601. A negative pressure chamber 604 is opened inside the negative pressure block 603. A first connecting pipe 602 is fixed to one end of the negative pressure block 603. Multiple sets of crushers 5 are fixedly installed on the outer surface of the suction pipe 4, solving the problem of two The technical problem is that methylamine gas easily polymerizes into large bubbles after being introduced into the reactor, preventing it from fully contacting and reacting with the liquid reactants. After the gas is introduced into the reactor 1 through the gas distributor 105, multiple sets of high-speed rotating crushers 5 shear and break the bubbles formed by gas polymerization, turning them into smaller bubbles. The first suction device 6 and the second suction device 601, through the negative pressure effect generated by the rotation of the negative pressure block 603, allow the first suction device 6 and the second suction device 601 to draw the gas from the top of the reactor 1 and re-introduce it into the liquid reactants, thereby increasing the contact time and contact area between the gas and the liquid reactants, so that the gas can fully react with the reactants.

[0028] For details regarding the above embodiments, please refer to [link / reference]. Figure 5 , Figure 6 and Figure 7 The first suction device 6 and the second suction device 601 are respectively provided with a first air chamber 607 and a second air chamber 610. The top of the suction pipe 4 is provided with three sets of first suction holes 605 and second suction holes 608. The bottom of the first suction holes 605 and the second suction holes 608 are respectively connected to a first vent hole 606 and a second vent hole 609. The first suction hole 605 is connected to the first air chamber 607 through the first vent hole 606, and the second suction hole 609 is connected to the second air chamber 610 through the second vent hole 609.

[0029] For details regarding the above embodiments, please refer to [link / reference]. Figure 5 The wall surface of the negative pressure block 603 with the same rotation direction is set as an arc, and the port of the negative pressure chamber 604 is set on the side opposite to the rotation direction of the rotating rod 3. Since the port of the negative pressure chamber 604 inside the negative pressure block 603 is set in the opposite direction to the rotation direction of the negative pressure block 603, during the rotation of the negative pressure block 603, the fluid at the port of the negative pressure chamber 604 will be quickly carried away due to the relative motion, so that the port of the negative pressure chamber 604 is in a negative pressure state.

[0030] For details regarding the above embodiments, please refer to [link / reference]. Figure 8 Three sets of crushing blades 501 are fixedly installed on the outer wall of the crusher 5, and the wall surface of the crushing blades 501 is provided with serrations. During the rotation of the rotating rod 3, the two sets of crushers 5 fixedly installed at the bottom of the rotating rod 3 crush the bubbles floating above the gas distributor 105 through the high-speed rotating crushing blades 501, so that the bubbles are broken into tiny bubbles at the μm level.

[0031] For details regarding the above embodiments, please refer to [link / reference]. Figure 2 and Figure 3 The top of the rotating rod 3 is fixed with a mounting shaft 304, and the bottom of the rotating rod 3 is connected with a support shaft 302. A fixing rod 303 is fixed on the outer wall of the support shaft 302, and the fixing rod 303 is fixedly set on the inner wall of the reactor 1. The rotating rod 3 is fixedly connected to the drive shaft 201 at the end of the servo motor 2 through the mounting shaft 304 at the end.

[0032] For details regarding the above embodiments, please refer to [link / reference]. Figure 2 A baffle plate 401 is fixed to the outer wall of the top end of the suction pipe 4, and the top wall of the baffle plate 401 is inclined. The baffle plate 401 is located above the liquid surface of the liquid reactant. The baffle plate 401 blocks the liquid reactant of the stirring reaction and prevents a large amount of liquid from splashing to the top of the suction pipe 4.

[0033] For details regarding the above embodiments, please refer to [link / reference]. Figure 2A shield 301 is fixed to the top outer wall of the rotating rod 3, and the diameter of the shield 301 is larger than the outer wall diameter of the suction pipe 4. The shield 301 blocks the top of the suction pipe 4 to prevent the liquid reactants poured into the reactor 1 through the feed pipe 101 from dripping onto the first suction hole 605 and the second suction hole 609.

[0034] For details regarding the above embodiments, please refer to [link / reference]. Figure 1 and Figure 2 The reactor 1 is equipped with two sets of heat exchange tubes 104. A gas distributor 105 is installed at the bottom of the reactor 1, and a gas supply pipe 106 is connected to one side of the gas distributor 105. A gas exchange pipe 103 is installed at the top of the reactor 1. The two sets of heat exchange tubes 104 heat the liquid reactants inside the reactor 1. The reaction gas is transported to the reactor 1 through the gas supply pipe 106. The gas inside the reactor 1 is discharged through the gas exchange pipe 103. A gas control valve is installed at the end of the gas exchange pipe 103.

[0035] Second embodiment: Please refer to Figure 9 and Figure 10 Three sets of wind-facing blocks 7 are fixedly installed at the top of the suction pipe 4. A second connecting pipe 702 is fixed at one end of the wind-facing block 7, and the connecting pipe 702 is fixedly installed at the top of the second suction hole 608. A wind-facing chamber 701 is opened inside the wind-facing block 7. The inner wall of the wind-facing chamber 701 is set in an arc shape, and the direction of the port of the wind-facing chamber 701 is the same as the rotation direction of the suction pipe 4. When the suction pipe 4 rotates, the three sets of wind-facing blocks 7 fixedly installed at the top of the suction pipe 4 rotate accordingly. During the high-speed rotation of the wind-facing blocks 7, the arc-shaped inner wall of the wind-facing chamber 701 will guide the gas around the port of the wind-facing chamber 701, so that the gas is sequentially introduced into the second suction hole 608 through the wind-facing chamber 701 and the second connecting pipe 702, thereby reducing the difference in the amount of gas ejected by the second suction device 601 and the first suction device 6 due to the compression of the gas ejected by the liquid reactant on the second suction device 601.

[0036] In practical operation, the pretreated raw materials are injected into the reactor 1 through the feed pipe 101. Then, the reaction gas is transported into the reactor 1 through the gas delivery pipe 106, so that the pressure inside the reactor 1 is controlled at 0.1-0.35MPa. The liquid reactants are heated by two sets of heat exchange tubes 104 installed inside the reactor 1, so that the temperature of the reactants is controlled and maintained at 180-230℃. As the reaction gas is injected into the liquid reactants from the gas distributor 105, the reaction gas and the liquid reactants undergo a chemical reaction. As the reaction gas is continuously fed into the reactor 1, the servo motor 2 drives the rotating rod 3 to rotate synchronously via its drive shaft 201. During the rotation of the rotating rod 3, two sets of crushers 5 fixedly installed at the bottom of the rotating rod 3 crush the bubbles floating above the gas distributor 105 with high-speed rotating breaking blades 501, breaking the bubbles into tiny bubbles at the μm level. Since the suction pipe 4 is fixedly installed with the rotating rod 3, it rotates along with the rotating rod 3, causing the suction pipe 4 to drive the first suction device 6, the second suction device 601, and the multiple sets of crushers 5 fixedly installed on its outer wall to rotate synchronously. During the high-speed rotation of the first suction device 6 and the second suction device 601, the negative pressure blocks 603 fixedly installed on the outer walls of the first suction device 6 and the second suction device 601 rotate at a constant speed. As the pressure block 603 rotates clockwise, the fluid at the port of the negative pressure chamber 604 inside the negative pressure block 603 is rapidly carried away due to the relative motion during the rotation of the negative pressure block 603, thus creating a negative pressure state at the port of the negative pressure chamber 604. The negative pressure blocks 603 on the first suction device 6 and the second suction device 601 respectively draw gas from the top of the reactor 1 through the first suction port 605 and the second suction port 608, so that the drawn gas is again injected into the liquid reactants through the first suction device 6 and the second suction device 601 for mixing and reaction. The crusher 5 set above the first suction device 6 and the second suction device 601 shears and breaks the bubbles generated by the gas ejected from the negative pressure block 603, thereby increasing the full mixing and reaction between the reaction gas and the liquid reactants.

Claims

1. A reactor with a dual heat exchange system for the synthesis of organic amines, comprising a reactor (1), characterized in that: The reactor (1) is provided with a feed pipe (101) and a discharge pipe (102) at the top and bottom respectively. A servo motor (2) is installed at the top of the reactor (1). One end of the servo motor (2) is connected to a drive shaft (201). A rotating rod (3) is installed at one end of the drive shaft (201). A suction pipe (4) is fixed on the outer wall of the rotating rod (3). A first suction device (6) and a second suction device (601) are provided on the outer wall of the suction pipe (4). Three sets of negative pressure blocks (603) are provided on the outer walls of the first suction device (6) and the second suction device (601). A negative pressure chamber (604) is opened inside the negative pressure block (603). A first connecting pipe (602) is fixed at one end of the negative pressure block (603). Multiple sets of crushers (5) are fixedly installed on the outer surface of the suction pipe (4).

2. The reactor with a dual heat exchange system for the synthesis of organic amines according to claim 1, characterized in that: The first suction device (6) and the second suction device (601) are respectively provided with a first air chamber (607) and a second air chamber (610). The top of the suction pipe (4) is provided with three sets of first suction holes (605) and second suction holes (608). The bottom of the first suction hole (605) and the second suction hole (608) are respectively connected to a first vent hole (606) and a second vent hole (609).

3. The reactor with a dual heat exchange system for the synthesis of organic amines according to claim 1, characterized in that: The wall surface of the negative pressure block (603) with the same rotation direction is set in an arc shape, and the port of the negative pressure chamber (604) is set on the side opposite to the rotation direction of the rotating rod (3).

4. The reactor with a dual heat exchange system for the synthesis of organic amines according to claim 1, characterized in that: The outer wall of the crusher (5) is fixedly provided with three sets of crushing blades (501), and the wall surface of the crushing blades (501) is provided with serrations.

5. The reactor with a dual heat exchange system for the synthesis of organic amines according to claim 1, characterized in that: The top of the rotating rod (3) is fixed with an installation shaft (304), and the bottom of the rotating rod (3) is connected with a support shaft (302). The outer wall of the support shaft (302) is fixed with a fixing rod (303), and the fixing rod (303) is fixedly installed on the inner wall of the reactor (1).

6. The reactor with a dual heat exchange system for the synthesis of organic amines according to claim 1, characterized in that: The top outer wall of the air intake pipe (4) is fixed with a baffle plate (401), and the top wall of the baffle plate (401) is inclined.

7. The reactor with a dual heat exchange system for the synthesis of organic amines according to claim 1, characterized in that: The top outer wall of the rotating rod (3) is fixed with a shield (301), and the diameter of the shield (301) is larger than the outer wall diameter of the suction pipe (4).

8. The reactor with a dual heat exchange system for the synthesis of organic amines according to claim 1, characterized in that: The reactor (1) is equipped with two sets of heat exchange tubes (104), a gas distributor (105) is installed at the bottom of the reactor (1), and a gas supply pipe (106) is connected to one side of the gas distributor (105). A gas exchange pipe (103) is installed at the top of the reactor (1).

9. A reaction vessel with a dual heat exchange system for the synthesis of organic amines according to claim 1, characterized in that: Three sets of wind-facing blocks (7) are fixedly installed on the top of the air intake pipe (4). A second connecting pipe (702) is fixed at one end of the wind-facing block (7), and the connecting pipe (702) is fixedly installed on the top of the second air intake hole (608). A wind-facing chamber (701) is opened inside the wind-facing block (7).

10. A reaction vessel with a dual heat exchange system for the synthesis of organic amines according to claim 9, characterized in that: The inner wall of the wind chamber (701) is set in an arc shape, and the direction of the port of the wind chamber (701) is the same as the rotation direction of the air intake pipe (4).