Vertical multi-section nitrification device
Through the design of a vertical multi-stage nitrification device, the problem of concentrated heat release in the nitrification reactor is solved by using a continuous tube reactor and an independent cooling system, which improves safety and efficiency and reduces the risk of explosion.
Patent Information
- Application Number
- CN202422343200.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-25
- Publication Date
- 2025-07-11
- Estimated Expiration
- 2034-09-25
AI Technical Summary
During the current nitration reaction, the concentrated release of heat in the reactor can easily cause safety hazards, especially for large-equivalent reactors that may cause explosions.
Vertical multi-stage nitrification device is adopted, including a first stirring tube, a first lifting tube, a second stirring tube and a second lifting tube. Each pipe body is equipped with a cooling jacket and driving component. It replaces the traditional kettle reactor through a continuous tube reactor, dispersing heat with multi-stage stirring and lifting structures, and accurately controls the temperature through an independent cooling water system.
It improves the safety and efficiency of nitration reaction, reduces the equivalent of the reactor, enhances heat dispersion and heat exchange efficiency, and reduces safety risks.
Smart Images
Figure CN223082787U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of nitrification devices, in particular to a vertical multi-stage nitrification device. Background Art
[0002] With the continuous expansion of the scope of hydrogen energy utilization, the market has a huge demand for the quantity of new hydrogen storage materials. At present, the storage methods of hydrogen include high-pressure gaseous hydrogen storage, cryogenic liquid hydrogen storage, organic liquid hydrogen storage and solid hydrogen storage. Among them, organic liquid hydrogen storage has the advantages of high storage efficiency, convenient transportation and recyclability. Therefore, carbazole-based organic liquid hydrogen storage materials will usher in a rapid development. In the production process of the carbazole-based organic liquid hydrogen storage material N-ethylcarbazole, after the alkylation reaction kettle reaction is completed, the upper organic phase is directly put into the crystallization kettle for crystallization, and then discharged, centrifugally washed, spun dry and refined to obtain high-purity N-ethylcarbazole. The N-ethylcarbazole with a content that does not reach high purity after refining goes to the next nitrification workshop for nitrification, and 3-nitro-N-ethylcarbazole is obtained after nitrification, which is used as an intermediate for the high-grade organic pigment permanent violet RL.
[0003] In the prior art, the nitrification reaction is generally carried out in an intermittent reaction kettle. The material to be nitrified is all put into the reaction kettle at one time, then stirring is started, and circulating cooling water is used for cooling, and nitric acid is added dropwise under temperature control. However, a large amount of heat will be released intensively in the reaction kettle during this nitrification reaction process. If the cooling and temperature reduction are insufficient, resulting in the large amount of heat released in the reaction kettle not being taken away in time, there is an easy potential safety hazard. Especially for a reaction kettle with a larger processing equivalent, it may even cause an explosion. Summary of the Utility Model
[0004] In order to solve the technical problems existing in the prior art that a large amount of heat will be released intensively in the reaction kettle during the nitrification reaction process, there is an easy potential safety hazard, and for a reaction kettle with a larger processing equivalent, it may even cause an explosion, the utility model provides the following technical solutions.
[0005] A vertical multi-stage nitrification device of the utility model includes a first stirring pipe, a first lifting pipe, a second stirring pipe and a second lifting pipe which are sequentially arranged and supported by a support frame and are both provided with cooling jackets and driving components. A first communication pipe is connected to the lower ends of the first stirring pipe and the first lifting pipe, a second communication pipe is connected to the upper ends of the first lifting pipe and the second stirring pipe, a third communication pipe is connected to the lower ends of the second stirring pipe and the second lifting pipe. A first feeding port and a second feeding port are arranged at the upper end of the first stirring pipe, and a discharge port is arranged at the upper end of the second lifting pipe. Stirring blades connected to the output end of the driving component are rotatably connected to the inner cavities of the first stirring pipe and the second stirring pipe, and lifting blades connected to the output end of the driving component are rotatably connected to the inner cavities of the first lifting pipe and the second lifting pipe.
[0006] As a further technical solution, the cooling jackets of the first stirring tube, the first lifting tube, the second stirring tube and the second lifting tube are respectively connected to different circulating cooling water systems, and a cold water inlet and a cooling outlet are respectively connected to the lower end and the upper end of the cooling jacket.
[0007] As a further technical solution, external metering pumps are connected to both the first feeding port and the second feeding port to facilitate the control of the feeding speed and flow rate of raw materials.
[0008] As a further technical solution, the diameter of the lifting paddle is larger than that of the stirring paddle, and the lifting paddle abuts against the inner walls of the first lifting tube and the second lifting tube.
[0009] As a further technical solution, the rotational speed of the lifting paddle is greater than that of the stirring paddle.
[0010] As a further technical solution, the lower ends of the stirring paddle and the lifting paddle are not lower than the lower wall surfaces of the first connecting pipe and the third connecting pipe in the horizontal direction.
[0011] The beneficial effects of the present utility model: The vertical multi-stage nitrification device of the present utility model adopts a continuous tube reactor composed of a first stirring tube, a first lifting tube, a second stirring tube and a second lifting tube to replace the traditional kettle reactor, thereby greatly improving the safety. Moreover, the vertical multi-stage tube structure can make the solution fully and repeatedly stirred evenly in the tube, improving the efficiency of the nitrification reaction. This vertical multi-stage tube structure reduces the reaction equivalent of the nitrification reaction compared with the traditional reaction kettle, and the heat in the tube is dispersed for heat exchange, improving the heat exchange efficiency and the safety during the nitrification reaction process. Description of the Drawings
[0012] Figure 1 is the external structure schematic diagram of the vertical multi-stage nitrification device of the present utility model;
[0013] Figure 2 is the partial structure sectional view of the vertical multi-stage nitrification device of the present utility model;
[0014] Figure 3 is the connection schematic diagram of the second connecting pipe of the vertical multi-stage nitrification device of the present utility model;
[0015] In the figure: 1 - support frame; 2 - first stirring tube; 201 - first feeding port; 202 - second feeding port; 3 - first lifting tube; 4 - second stirring tube; 5 - second lifting tube; 501 - discharge port; 6 - driving component; 7 - cooling jacket; 701 - cold water inlet; 702 - cold water outlet; 8 - stirring paddle; 9 - lifting paddle; 10 - first connecting pipe; 11 - second connecting pipe; 12 - third connecting pipe. Detailed implementation manners
[0016] In order to make the objectives, technical solutions and advantages of the present utility model clearer and more understandable, the present utility model will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present utility model and are not used to limit the present utility model. It should be noted that, without conflict, the embodiments in the present utility model and the features in the embodiments can be combined with each other.
[0017] In the description of the present utility model, it should be understood that the terms "upper", "lower", and "both sides" are based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation to the present utility model. In addition, the terms "first", "second", etc. are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features.
[0018] As Figure 1 and Figure 2 shown, a vertical multi-stage nitrification device of the present utility model includes a first stirring tube 2, a first lifting tube 3, a second stirring tube 4, and a second lifting tube 5 arranged in sequence. The first stirring tube 2, the first lifting tube 3, the second stirring tube 4, and the second lifting tube 5 are all supported by a support frame 1. That is, the support frame 1 has at least two layers with different heights. The lower parts of the first stirring tube 2, the first lifting tube 3, the second stirring tube 4, and the second lifting tube 5 are connected or welded to the lower layer of the support frame 1 by bolts, and the upper parts of the first stirring tube 2, the first lifting tube 3, the second stirring tube 4, and the second lifting tube 5 are connected or welded to the upper layer of the support frame 1 by bolts.
[0019] In a preferred embodiment, the first stirring tube 2, the first lifting tube 3, the second stirring tube 4, and the second lifting tube 5 are respectively connected end to end, so that the nitrification raw materials are fed into the first stirring tube 2 and discharged from the second lifting tube 5 after sufficient stirring and reaction. Specifically, a first connecting pipe 10 is connected to the lower ends of the first stirring tube 2 and the first lifting tube 3, a second connecting pipe 11 is connected to the upper ends of the first lifting tube 3 and the second stirring tube 4, and a third connecting pipe 12 is connected to the lower ends of the second stirring tube 4 and the second lifting tube 5. A first feeding port 201 and a second feeding port 202 are provided at the upper end of the first stirring tube 2, and a discharging port 501 is provided at the upper end of the second lifting tube 5. The nitrification raw materials enter the inner cavity of the first stirring tube 2 from the first feeding port 201 and the second feeding port 202. After stirring and reacting in the inner cavity of the first stirring tube 2, the solution is lifted by the first lifting tube 3 from the first connecting pipe 10. The solution lifted by the first lifting tube 3 enters the inner cavity of the second stirring tube 4 through the second connecting pipe 11 to continue stirring and reacting. Then the solution is lifted by the second lifting tube 5 from the third connecting pipe 12 and is discharged from the discharging port 501 after the reaction is completed and is discharged into a quenching crystallization kettle for quenching crystallization.
[0020] External metering pumps are connected to both the first feeding port 201 and the second feeding port 202 to facilitate controlling the feeding speed and flow rate of the N-ethylcarbazole mixture and the nitric acid material.
[0021] As Figure 2 and Figure 3 shown, in a preferred embodiment, the first stirring tube 2, the first lifting tube 3, the second stirring tube 4, and the second lifting tube 5 are all provided with cooling jackets 7 and driving components 6. The driving components 6 at the upper ends of each tube body have the same structure, the cooling jackets 7 in each tube have the same structure, and cold water inlets 701 and cooling outlets 702 are separately provided at the lower and upper ends of the cooling jackets 7 in each tube body. Each cooling jacket 7 is separately connected to circulating cooling water to facilitate supplying cooling water with different temperatures to the first stirring tube 2, the first lifting tube 3, the second stirring tube 4, and the second lifting tube 5 respectively for precise temperature control inside the tubes.
[0022] In a preferred embodiment, stirring blades 8 connected to the output ends of the driving components 6 are rotatably connected to the inner cavities of the first stirring tube 2 and the second stirring tube 4, and lifting blades 9 connected to the output ends of the driving components 6 are rotatably connected to the inner cavities of the first lifting tube 3 and the second lifting tube 5. Both the stirring blades 8 and the lifting blades 9 are in a spiral shape, which is convenient for uniformly stirring and lifting the solution.
[0023] In a preferred embodiment, the diameter of the lifting blade 9 is greater than that of the stirring blade 8, and the lifting blade 9 abuts against the inner wall of the first lifting tube 3 and the second lifting tube 5. The rotation speed of the lifting blade 9 is greater than that of the stirring blade 8, so that the lifting blade 9 can smoothly lift the solution. At the same time, the lower ends of the stirring blade 8 and the lifting blade 9 are not lower than the lower wall surface of the first connecting tube 10 and the third connecting tube 12 in the horizontal direction, and the solution after edge stirring is completely lifted upward by the lifting blade 9.
[0024] When the utility model is used, chlorobenzene and N-ethylcarbazole are firstly put into a dissolving kettle and mixed into a mixed solution, and the solution is kept at a temperature of 28-32° C. under stirring and then put into use; dilute nitric acid is prepared in a nitric acid kettle, and 38% of nitric acid is prepared and the temperature is kept at 28-32° C. for use; the circulating cooling temperature of each cooling jacket 7 in a first stirring tube 2, a first lifting tube 3, a second stirring tube 4 and a second lifting tube 5 is adjusted, the mixed solution is added into the first stirring tube 2 from a first feeding port 201, and the dilute nitric acid is added into the second feeding port 202, and each driving component 6 is turned on at the same time, so that the stirring blade 8 and the lifting blade 9 start to rotate, and stirring and lifting are started for multiple times until the reaction is finished. After the reaction is finished, the material flows into the quenching crystallization kettle from a discharge port 501 to perform quenching crystallization.
[0025] The preferred specific implementation modes and embodiments of the utility model are described in detail above in conjunction with the accompanying drawings, but the utility model is not limited to the above implementation modes and embodiments, and various changes or equivalent substitutions can be made within the knowledge scope of those skilled in the art without departing from the concept of the utility model. Therefore, the utility model is not limited to the specific embodiments disclosed herein, and all embodiments falling within the scope of the claims of this application belong to the scope protected by the utility model.
Claims
1. A vertical multi-stage nitrification device, characterized in that: It includes a first stirring pipe (2), a first lifting pipe (3), a second stirring pipe (4) and a second lifting pipe (5) which are successively arranged and supported by a support frame (1), and are all provided with a cooling jacket (7) and a driving component (6). A first connecting pipe (10) is connected to the lower ends of the first stirring pipe (2) and the first lifting pipe (3). A second connecting pipe (11) is connected to the upper ends of the first lifting pipe (3) and the second stirring pipe (4). A third connecting pipe (12) is connected to the lower ends of the second stirring pipe (4) and the second lifting pipe (5). A first feeding port (201) and a second feeding port (202) are provided at the upper end of the first stirring pipe (2). A discharge port (501) is provided at the upper end of the second lifting pipe (5). Stirring blades (8) connected to the output end of the driving component (6) are rotatably connected to the inner cavities of the first stirring pipe (2) and the second stirring pipe (4). Lifting blades (9) connected to the output end of the driving component (6) are rotatably connected to the inner cavities of the first lifting pipe (3) and the second lifting pipe (5).
2. The vertical multi-stage nitrification device according to claim 1, wherein: The cooling jackets (7) of the first stirring pipe (2), the first lifting pipe (3), the second stirring pipe (4) and the second lifting pipe (5) are respectively communicated with different circulating cooling water systems. A cold water inlet (701) and a cooling outlet (702) are respectively connected to the lower end and the upper end of the cooling jacket (7).
3. The vertical multi-stage nitrification device according to claim 1, characterized in that: External metering pumps are connected to both the first feeding port (201) and the second feeding port (202) to facilitate the control of the feeding speed and flow rate of raw materials.
4. The vertical multi-stage nitrification device according to claim 1, characterized in that: The diameter of the lifting blade (9) is larger than that of the stirring blade (8), and the lifting blade (9) abuts against the inner walls of the first lifting pipe (3) and the second lifting pipe (5).
5. The vertical multi-stage nitrification device according to claim 1, characterized in that: The rotation speed of the lifting blade (9) is greater than that of the stirring blade (8).
6. The vertical multi-stage nitrification device according to claim 1, characterized in that: The lower ends of the stirring blade (8) and the lifting blade (9) are not lower than the lower wall surfaces of the first connecting pipe (10) and the third connecting pipe (12) in the horizontal direction.