Continuous hydrogenation reaction device
By incorporating a Venturi reactor and a circulation and cooling mechanism within the batch reactor, the problems of long reaction time and low conversion efficiency in batch reactors are solved, enabling rapid mixing and temperature control, and improving the production efficiency of the batch reactor.
Patent Information
- Application Number
- CN202520343468.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-28
- Publication Date
- 2026-02-06
- Estimated Expiration
- 2035-02-28
AI Technical Summary
When producing 4-fluoro-N-isopropylaniline, batch reactors suffer from problems such as long reaction time, low conversion efficiency, difficulty in temperature control, and poor mixing effect, especially for catalysts with high density such as platinum-carbon.
A Venturi reactor is installed inside the vessel, and a circulation and cooling mechanism is installed on the outside. The circulation mechanism achieves rapid mixing of materials through a circulation pump and circulation pipe, while the cooling mechanism uses coolant to reduce the temperature of the circulation pipe to control the material temperature, thereby improving mixing efficiency and cooling effect.
It significantly shortened the reaction time, improved the material mixing efficiency, reduced the material temperature, and increased the production efficiency of the batch reactor. The single batch occupancy time was reduced from 39 hours to 20 hours, and the monthly production capacity doubled.
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Figure CN223875057U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to the field of kettle type reactor, concretely to a continuous hydrogenation reaction device. BACKGROUND
[0002] 4-fluoro-N-isopropyl aniline as the intermediate of herbicide flufenacet can be obtained by hydrogenation reaction of 4-fluoro nitrobenzene, acetone and hydrogen in the presence of active catalyst. Specifically, 1 equivalent of 4-fluoro nitrobenzene and 1-5 times molar equivalent of compound (such as acetone, etc.) are added in the reactor, and 0.2%-5% of total mass percentage of transition metal catalyst (such as supported noble metal catalyst, etc.) and 0.1%-10% of total mass percentage of sulfonic acid or carboxylic acid are added, and then the reaction is carried out at 30-130℃ in an organic solvent (such as ethanol, methanol, etc.) and hydrogen environment. After the reaction is completed, 4-fluoro-N-isopropyl aniline is obtained by conventional separation and purification methods such as distillation and extraction.
[0003] The reactor used in the above operation is mostly a kettle type reactor, and there are many types of kettle type reactors. For example, a reaction kettle disclosed in a Chinese patent with publication number CN103480319B includes a kettle body, a stirring shaft arranged in the kettle body along the axis direction of the kettle body, stirring blades mounted on the stirring shaft, and an output end of a driving device connected to one end of the stirring shaft. The driving device is fixed on the upper part of the kettle body, and a manhole is arranged on the upper part of the kettle body. The stirring blades are spiral blades, and two spiral blades are symmetrically arranged on the stirring shaft in a spiral manner. The surface of the spiral blades faces the axis direction of the kettle body, and the spiral directions of the two spiral blades are opposite. When the reaction kettle works, the materials in the kettle body can be uniformly mixed by the working of the stirring shaft and the stirring blades, and the product quality is improved.
[0004] Similarly, when producing 4-fluoro-N-isopropyl aniline by using the reaction kettle provided by the above patent, paddle stirring is used to promote the reaction, but there are problems such as long reaction time and low conversion efficiency. First, it is difficult to control the reaction temperature in the kettle type reaction, and the temperature rises rapidly in the early stage. The existing cooling method of the reaction kettle cannot quickly remove the reaction heat. In order to control the reaction temperature, the hydrogenation rate needs to be reduced, which further prolongs the reaction time. Second, the mixing effect of paddle stirring for platinum-carbon catalyst with high density is poor, and the reaction conversion efficiency is low, which leads to long reaction time, especially the conversion rate decreases significantly in the later stage of the reaction, and a long time is needed to react qualified. UTILITY MODEL CONTENTS
[0005] The utility model aims at providing a continuous hydrogenation reaction device to improve the problem of low production efficiency of the kettle type reactor.
[0006] The utility model discloses a continuous hydrogenation reaction device, including the kettle body, is provided with venturi reactor on the inside of kettle body, the top of venturi reactor is set up and is passed through the top cover of kettle body, and the bottom is inserted into the bottom of kettle body, is provided with circulating mechanism on the outside of kettle body, and circulating mechanism includes circulating pipe and circulating pump, and circulating pump is connected with circulating pipe, and the both ends of circulating pipe are connected with the top of venturi reactor and the bottom valve of kettle body bottom respectively, still is provided with cooling mechanism on the outside of kettle body, and one section of cooling mechanism is set up on circulating pipe and forms the flow passage, and cooling mechanism includes cooling liquid, and cooling liquid flows into the flow passage.
[0007] As an embodiment of the utility model, two circles of second flange plates are fixedly arranged on the top of the venturi reactor, and the two circles of second flange plates are arranged in an upper and lower distribution manner; a first flange plate is connected to the lower side of the second flange plate through bolts, and the first flange plate is installed on the top cover of the kettle body.
[0008] As an embodiment of the utility model, the circulating pipe comprises a first pipe body, a second pipe body, and a third pipe body, the first pipe body and the third pipe body are both arranged in an L-shaped structure, and are both arranged at the two ends of the second pipe body, respectively, one end of the first pipe body away from the second pipe body is connected to the top of the venturi reactor, and one end of the third pipe body away from the second pipe body is connected to the bottom valve.
[0009] As an embodiment of the utility model, the circulating pump is arranged on the third pipe body, a double-valve sampling pipe is arranged on the side of the third pipe body or the first pipe body, and two control valves are arranged on the double-valve sampling pipe.
[0010] As an embodiment of the utility model, the cooling mechanism comprises a condenser, a pump body, a conveying pipe, and a cooling bin, the pump body is arranged at one end of the condenser, the conveying pipe is arranged at the other end of the condenser, the pump body and the conveying pipe are both connected to the cooling bin, and the cooling liquid flows among the pump body, the cooling bin, and the condenser.
[0011] As an embodiment of the utility model, the cooling bin comprises a first shell and a second shell, the central angles of the first shell and the second shell are arranged as 180°, the first shell and the second shell are connected in a sealed splicing manner and are arranged on the second pipe body, a liquid pipe is arranged on the first shell or the second shell, and the liquid pipe is connected to the pump body and the conveying pipe.
[0012] As an embodiment of the utility model, the length of the second pipe body is greater than the length of the cooling bin, a conductive rod is arranged on the side wall of the second pipe body, and the conductive rods are arranged on the inside of the cooling bin in a uniform distribution manner.
[0013] As an embodiment of the utility model, the cooling mechanism further comprises an expansion valve, and the expansion valve is arranged on the side of the condenser.
[0014] As an embodiment of the utility model, the circulating mechanism further comprises a buffer tank, which is arranged on the circulating pipe.
[0015] The utility model brings the beneficial effect that:
[0016] 1. The utility model discloses a venturi reactor is arranged on the inside of cauldron body, and circulating mechanism is arranged on the outside of cauldron body, can move the material of cauldron body bottom to the top of venturi reactor under the action of circulating mechanism, then falls in cauldron body from the bottom output of venturi reactor, realizes the full reaction of material, and correspondingly improves material mixing efficiency.
[0017] 2. The utility model discloses cooling mechanism, and a section of cooling mechanism is set on circulating pipe, therefore, can reduce the temperature of circulating pipe under the action of cooling mechanism, and then reduce the temperature of material flowing into circulating pipe, realizes the cooling treatment of material.
[0018] 3. The utility model discloses cooling bin includes first shell and second shell, and first shell and second shell are spliced and set on second pipe body, in addition, a plurality of conducting rods are arranged on second pipe body, increase the contact area of cooling liquid and second pipe body, improve the efficiency of material cooling. DRAWINGS
[0019] The drawings that form a part of the utility model are used to provide further understanding of the utility model, so that other features, purposes and characteristics of the utility model become more obvious. The illustrative embodiment drawing of the utility model and its explanation are used to explain the utility model, and do not constitute undue limitation to the utility model.
[0020] Figure 1 It is the structure schematic drawing of the whole of the utility model;
[0021] Figure 2 It is the structure schematic drawing of the venturi reactor of the utility model;
[0022] Figure 3 It is the first structure schematic drawing of cooling mechanism, circulating mechanism of the utility model;
[0023] Figure 4 It is the structure schematic drawing of second pipe body of the utility model;
[0024] Figure 5 It is the structure schematic drawing of cooling bin of the utility model;
[0025] Figure 6 It is the second structure schematic drawing of cooling mechanism, circulating mechanism of the utility model.
[0026] In the figure: vessel body 1; first flange 11; bottom valve 12; buffer tank 13; venturi reactor 2; second flange 21; cooling mechanism 3; condenser 31; pump body 32; delivery pipe 33; cooling chamber 34; first shell 341; second shell 342; liquid pipe 343; expansion valve 35; circulation mechanism 4; first pipe body 41; second pipe body 42; third pipe body 43; circulation pump 44; double valve sampling pipe 45; conduction rod 46. Detailed Implementation
[0027] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.
[0028] It should be noted that all directional indicators (such as up, down, left, right, front, back, etc.) in this utility model embodiment are only used to explain the relative positional relationship and movement of each component in a certain specific posture (as shown in the figure). If the specific posture changes, the directional indicator will also change accordingly.
[0029] Example 1
[0030] like Figure 1 As shown, in order to improve the mixing efficiency of materials in the reactor, this embodiment provides a new reaction device. The reaction device includes a reactor body 1 and a top cover set on the top of the reactor body 1. The top cover is sealed above the reactor body 1. A feed inlet is provided on the top cover, and thermometers, pressure gauges, safety valves and other devices can also be installed on the top cover. The specific devices are set according to actual needs. A discharge outlet is provided at the bottom of the reactor body 1.
[0031] like Figure 1 , Figure 2 , Figure 3As shown, to achieve faster material mixing, a Venturi reactor 2 is installed inside the vessel body 1. The top of the Venturi reactor 2 penetrates the top cover of the vessel body 1, and the bottom extends into the bottom of the vessel body 1. Simultaneously, a circulation mechanism 4 is installed on the outside of the vessel body 1. One end of the circulation mechanism 4 is connected to a bottom valve 12 installed at the discharge port at the bottom of the vessel body 1, and the other end is connected to the top of the Venturi reactor 2. Therefore, under the action of the circulation mechanism 4, the material in the vessel body 1 can be controlled to move along the circulation mechanism 4 to the top of the Venturi reactor 2, then circulate inside the Venturi reactor 2, and finally be discharged from the bottom of the Venturi reactor 2 back into the vessel body 1. Repeating the above operation significantly improves the mixing effect and greatly shortens the reaction time. For example, the single-batch occupancy time of existing batch reactors is as long as 39 hours, while the single-batch occupancy time of this invention is only 20 hours, doubling the monthly production capacity of a single device.
[0032] like Figure 2 As shown, to ensure the stable installation of the Venturi reactor 2 within the space formed by the vessel body 1 and the top cover, two rings of second flanges 21 are fixedly installed on the top of the Venturi reactor 2, arranged vertically. The upper second flange 21 is connected to the circulation mechanism 4, and a first flange 11 is bolted to the lower part of the lower second flange 21. The first flange 11 is installed on the top cover of the vessel body 1. Therefore, the stable installation of the Venturi reactor 2 is achieved through the cooperation of the first flange 11 and the second flange 21.
[0033] like Figure 3 As shown, to achieve material circulation, the circulation mechanism 4 includes a circulation pipe and a circulation pump 44. The circulation pipe includes a first pipe body 41, a second pipe body 42, and a third pipe body 43. Both the first pipe body 41 and the third pipe body 43 are L-shaped and connected to both ends of the second pipe body 42, forming a U-shaped circulation pipe. The end of the first pipe body 41 furthest from the second pipe body 42 is connected to the top of the Venturi reactor 2, and the end of the third pipe body 43 furthest from the second pipe body 42 is connected to the bottom valve 12. The circulation pump 44 is connected to the third pipe body 43. Therefore, under the action of the circulation pump 44, material at the bottom of the vessel 1 can be pumped along the circulation pipe to the top of the Venturi reactor 2 and output from the bottom of the Venturi reactor 2, falling back to the bottom of the vessel 1. Repeating the above operation achieves material circulation, conveying, and mixing, improving mixing efficiency.
[0034] The circulation mechanism 4 also includes a buffer tank 13, which is installed on the circulation pipe. The buffer tank 13 can buffer the pressure fluctuations of the circulation pipeline system, eliminate water hammer, and play a role in stabilizing pressure and unloading. When the water pressure in the circulation pipe changes slightly, the automatic expansion and contraction of the air bladder of the buffer tank will have a certain buffering effect on the water pressure change, and can ensure the stability of the water pressure in the circulation pipe.
[0035] likeFigure 3 As shown, in order to extract the material inside the vessel 1 and determine whether the material has reacted sufficiently, a double-valve sampling pipe 45 is provided on the side of the third pipe 43 or the first pipe 41. Two control valves are provided on the double-valve sampling pipe 45. When sampling is required, the control valve of the adjacent circulation pipe is opened to allow the material to flow into the double-valve sampling pipe 45, and then the control valve of the adjacent circulation pipe is closed. Finally, the control valve of the pipe far from the circulation pipe is opened and closed according to the sampling requirements, which facilitates the material sampling.
[0036] Example 2
[0037] like Figure 3 As shown, based on Example 1, in order to effectively reduce the temperature of the material, a cooling mechanism 3 is also provided on the outside of the vessel body 1. One section of the cooling mechanism 3 is sleeved on the circulation pipe to form a flow channel, and the cooling mechanism 3 includes a coolant. The coolant flows into the flow channel, so the temperature of the circulation pipe can be reduced under the action of the coolant, thereby reducing the temperature of the material flowing in the circulation pipe.
[0038] like Figure 3 As shown, specifically, the cooling mechanism 3 includes a condenser 31, a pump body 32, a delivery pipe 33, and a cooling chamber 34. The pump body 32 is connected to one end of the condenser 31, and the delivery pipe 33 is connected to the other end of the condenser 31. Both the pump body 32 (which can be a positive displacement pump) and the delivery pipe 33 are connected to the cooling chamber 34. Simultaneously, under the action of the pump body 32, the coolant flows between the cooling chamber 34 and the condenser 31. Furthermore, the condenser 31 is equipped with a fan, i.e., it is a wind-cooled condenser. The fan blows air, reducing the temperature of the liquid flowing into the condenser 31, thus allowing low-temperature coolant to be delivered into the cooling chamber 34. Because the cooling chamber 34 is fitted onto the second pipe 42, the coolant comes into contact with the second pipe 42, absorbing the temperature of the second pipe 42 and the material, achieving material cooling. This further enables the material to circulate and cool. The position of the pump body 32 relative to the condenser 31 and the cooling chamber 34 is determined according to the actual situation.
[0039] like Figure 5 As shown, in order to install the cooling chamber 34 on the second pipe body 42, the length of the second pipe body 42 is greater than the length of the cooling chamber 34. The cooling chamber 34 includes a first shell 341 and a second shell 342. The central angle of the first shell 341 and the second shell 342 is set to 180°, and they are connected by bolts and sealed together on the second pipe body 42. A liquid pipe 343 is provided in communication with the first shell 341 or the second shell 342. The liquid pipe 343 is connected in communication with the pump body 32 and the delivery pipe 33.
[0040] like Figure 4As shown, to accelerate material cooling, conductive rods 46 are installed on the side wall of the second pipe 42. These rods 46 are evenly distributed inside the cooling chamber 34, ensuring full contact between the rods 46 and the coolant. This increases the contact area between the second pipe 42 and the coolant, further improving the material cooling efficiency. Additionally, sensors can be installed on the circulation pipe to monitor the material temperature.
[0041] Example 3
[0042] like Figure 6 As shown, based on Example 2, in order to further reduce the temperature of the coolant, the cooling mechanism 3 also includes an expansion valve 35. The expansion valve 35 is connected between the condenser 31 and the cooling chamber 34. That is, the coolant output from the condenser 31 is further reduced in temperature after being processed by the expansion valve 35, and then flows into the cooling chamber 34 to achieve the cooling treatment of the material.
[0043] Furthermore, the technical solutions of the various embodiments of this utility model can be combined with each other, but only if they are based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such combination of technical solutions does not exist and is not within the scope of protection claimed by this utility model.
[0044] The above-described embodiments are merely illustrative of several implementations of this utility model, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of this utility model patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this utility model, and these all fall within the protection scope of this utility model. Therefore, the protection scope of this utility model should be determined by the appended claims.
Claims
1. A continuous hydrogenation reaction apparatus characterized by comprising: The utility model provides a kind of venturi reactor and cooling mechanism, including kettle body (1), venturi reactor (2) is provided in the inside of the kettle body (1), the top of the venturi reactor (2) is arranged through the top cover of kettle body (1), and bottom extends into the bottom of kettle body (1);Recycling mechanism (4) is provided in the outside of the kettle body (1), and the recycling mechanism (4) includes circulation pipe and circulation pump (44), the circulation pump (44) is connected with circulation pipe, and the two ends of circulation pipe are respectively connected with the top of venturi reactor (2) and the bottom valve (12) of kettle body (1) bottom, cooling mechanism (3) is further provided in the outside of the kettle body (1), and a section of cooling mechanism (3) is sleeved on circulation pipe to form flow channel, and the cooling mechanism (3) includes cooling liquid, and cooling liquid flows into flow channel.
2. The continuous hydrogenation reactor of claim 1, wherein, Two circles of second flange plate (21) are fixedly provided on the top of the venturi reactor (2), and the two circles of second flange plate (21) are arranged in an upper and lower distribution manner;A first flange plate (11) is connected by bolts below the lower second flange plate (21), and the first flange plate (11) is installed on the top cover of the kettle body (1).
3. The continuous hydrogenation reactor of claim 1, wherein, The circulation pipe includes a first pipe body (41), a second pipe body (42) and a third pipe body (43), the first pipe body (41) and the third pipe body (43) are both arranged in an L-shaped structure, and are respectively arranged at two ends of the second pipe body (42), one end of the first pipe body (41) away from the second pipe body (42) is connected with the top of the venturi reactor (2), and one end of the third pipe body (43) away from the second pipe body (42) is connected with the bottom valve (12).
4. The continuous hydrogenation reactor of claim 3, wherein The circulation pump (44) is arranged on the third pipe body (43), and a double-valve sampling pipe (45) is arranged on the side of the third pipe body (43) or the first pipe body (41), and two control valves are arranged on the double-valve sampling pipe (45).
5. The continuous hydrogenation reactor of claim 3, wherein The cooling mechanism (3) includes a condenser (31), a pump body (32), a delivery pipe (33) and a cooling bin (34), the pump body (32) is arranged on one end of the condenser (31), the delivery pipe (33) is arranged on the other end of the condenser (31), and the pump body (32) and the delivery pipe (33) are both connected with the cooling bin (34), and the cooling liquid flows among the pump body (32), the cooling bin (34) and the condenser (31).
6. The continuous hydrogenation reactor of claim 5, wherein, The cooling bin (34) includes a first shell (341) and a second shell (342), the central angles of the first shell (341) and the second shell (342) are 180°, and the first shell (341) and the second shell (342) are sealingly connected and sleeved on the second pipe body (42), a liquid pipe (343) is arranged on the first shell (341) or the second shell (342), and the liquid pipe (343) is connected with the pump body (32) and the delivery pipe (33).
7. The continuous hydrogenation reactor of claim 6, wherein, The length of the second pipe body (42) is greater than the length of the cooling bin (34), and a conductive rod (46) is arranged on the side wall of the second pipe body (42), and the conductive rods (46) are evenly arranged on the inside of the cooling bin (34).
8. The continuous hydrogenation reactor of claim 5, wherein, The cooling mechanism (3) further comprises an expansion valve (35) which is in communication with the side of the condenser (31).
9. The continuous hydrogenation reactor of claim 1, wherein, The circulating mechanism (4) further comprises a buffer tank (13) which is arranged on the circulating pipe.
Citation Information
Patent Citations
Reactor
CN103480319B