Amination reaction device for producing N, N-dimethylacrylamide
By setting multiple through holes on the bottom plate or side wall of the dropping tube of the amination reaction device, the dropping process of chloropropylene is controlled, and the problems of unstable reaction temperature and many by-products are solved, and the amination content and yield are improved.
Patent Information
- Application Number
- CN202421105231.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-20
- Publication Date
- 2025-01-07
- Estimated Expiration
- 2034-05-20
AI Technical Summary
In the prior art, chloropropylene is difficult to control during the dropwise addition reaction, resulting in unstable reaction temperature, many by-products, low amination content and low yield.
A kind of amination reaction device is designed, with a bottom plate at the bottom of the dropper tube, and multiple through holes are provided on the bottom plate or side wall to form through holes in which chloropropylene flows to the reactor, reducing the reaction concentration and contact area, and controlling the reaction rate.
Through this device, the reaction temperature can be better controlled, side reactions can be reduced, amination content and yield can be increased, and the residue of N,N-dimethacrylate can be reduced.
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Figure CN222305806U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of chemical production, in particular to an amination reaction device for producing N,N-dimethylpropyleneamine. Background Art
[0002] Insecticide is a chemical agent or medicine used to kill pests. N,N-dimethylpropyleneamine is an important intermediate in the production of insecticide. The quality of N,N-dimethylpropyleneamine directly affects the production of the chlorination section.
[0003] In the prior art, the insecticide monoamination process uses allyl chloride as the main raw material to react with dimethylamine to generate N,N-dimethylallylamine. In the process of dripping allyl chloride into dimethylamine, the following methods are usually used: Figure 7 The straight-through valve dripping tube shown in the figure is used to drip into the kettle. The bottom of the dripping tube of this structure is open, and the dripping amount is controlled by a valve. However, in the actual production process, the dripping amount of propylene chloride is difficult to control using the dripping tube of this structure, resulting in difficulty in controlling the reaction temperature, violent local reactions, and more by-products. As a result, the content of the amination is not high, the yield is low, and the quality is unstable. Utility Model Content
[0004] The technical problem to be solved by the utility model is to overcome the deficiencies of the prior art and provide an amination reaction device for producing N,N-dimethylpropyleneamine, which is convenient for controlling the dripping amount of allyl chloride.
[0005] In order to solve the above technical problems, the utility model adopts the following technical solutions:
[0006] An amination reaction device comprises a chloropropylene metering tank and an amination reaction kettle. The chloropropylene metering tank is provided with a dripping tube for dripping chloropropylene into the reaction kettle, a bottom plate is provided at the bottom of the dripping tube, and a plurality of through holes are provided on the dripping tube for allowing the chloropropylene in the dripping tube to flow into the amination reaction kettle.
[0007] As a further improvement of the above solution:
[0008] The through hole is arranged on the bottom plate.
[0009] The through holes are distributed circumferentially on the side wall of the drip tube.
[0010] The through hole includes a first through hole and a second through hole, and the diameter of the first through hole is larger than that of the second through hole.
[0011] The first through holes and the second through holes are staggeredly distributed along the length direction of the drip tube.
[0012] The first through holes and the second through holes are staggeredly distributed along the circumference of the drip tube.
[0013] The diameter of the first through hole is 50 mm, and the diameter of the second through hole is 25 mm.
[0014] Compared with the prior art, the advantages of the utility model are:
[0015] The utility model provides an amination reaction device for producing N,N-dimethylpropyleneamine. By arranging a bottom plate at the bottom of a dropping tube and arranging a plurality of through holes on the bottom plate or the side wall of the dropping tube, the reaction concentration and the reaction contact area in the dropping process of allyl chloride are reduced on the basis of unchanged existing process parameters, so as to slow down the reaction rate, help to better control the reaction process, avoid severe reaction conditions, facilitate control of the reaction temperature, reduce the occurrence of side reactions, increase the content of amination products, reduce the residual N,N-dimethylpropyleneamine, and improve the average yield. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 It is a schematic structural diagram of the amination reaction device for producing N,N-dimethylpropyleneamine in Example 1.
[0017] Figure 2 It is a schematic diagram of the structure of the dripping tube in Example 1.
[0018] Figure 3 1 is a schematic top view of the structure of the dripping tube in Example 1.
[0019] Figure 4 It is a schematic diagram of the structure of the dripping tube in the second embodiment.
[0020] Figure 5 It is a schematic top view of the structure of the dripping tube in the second embodiment.
[0021] Figure 6 It is a schematic diagram of the structure of the dripping tube in the third embodiment.
[0022] Figure 7 It is a structural schematic diagram of an existing straight-through dripping tube.
[0023] The symbols in the figure represent:
[0024] 1. Allyl chloride metering tank; 2. Amination reaction kettle; 3. Dropping tube; 4. Bottom plate; 5. Through hole; 6. First through hole; 7. Second through hole. DETAILED DESCRIPTION
[0025] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.
[0026] Embodiment 1:
[0027] Figures 1 to 3An embodiment of an amination reaction device for producing N,N-dimethylpropyleneamine of the utility model is shown, comprising a chloropropylene metering tank 1 and an amination reaction kettle 2, a dripping tube 3 for dripping chloropropylene into the reaction kettle is provided at the end of the chloropropylene metering tank 1, a bottom plate 4 is provided at the bottom of the dripping tube 3, and a plurality of through holes 5 are provided on the dripping tube 3 to enable the chloropropylene inside the dripping tube 3 to flow to the amination reaction kettle 2. The through holes 5 are provided on the bottom plate 4. In this structure, by providing the bottom plate 4 at the bottom of the dripping tube 3, the chloropropylene cannot directly enter the reaction kettle, and by providing the through holes 5 on the bottom plate 4, the chloropropylene in the dripping tube 3 is dripped into the reaction kettle through the through holes 5 for reaction, so as to reduce the reaction concentration and the reaction contact area in the dripping process of chloropropylene on the basis of the existing process parameters being unchanged, so as to slow down the reaction rate, help better control the reaction process, avoid severe reaction conditions, facilitate control of the reaction temperature, reduce the occurrence of side reactions, increase the content of aminations, reduce the residual N,N-dimethylpropyleneamine, and improve the average yield.
[0028] Embodiment 2:
[0029] Figure 4 and Figure 5 The second embodiment of the amination reaction device of the utility model for producing N,N-dimethylpropyleneamine is shown. The structure of the amination reaction device of this embodiment is basically the same as that of the first embodiment, except that:
[0030] In this embodiment, the through holes 5 are distributed around the side wall of the dripping tube 3. In this structure, by setting a plurality of through holes 5 on the side wall of the dripping tube 3, the allyl chloride can be distributed in a larger height range during the dripping process, and further by setting the distribution of each through hole 5, the dripping speed and the dispersion of the droplets can be more easily controlled, and the sputtering or bubbles generated by direct impact on the bottom can be reduced, which is convenient for further reducing the reaction concentration and reaction contact area during the dripping process of allyl chloride; it helps to avoid local overheating or uneven distribution of reaction heat, so as to reduce the occurrence of side reactions, increase the content of amination, reduce the residual N,N-dimethylpropyleneamine, and improve the average yield.
[0031] Embodiment three:
[0032] Figure 6 The second embodiment of the amination reaction device of the utility model for producing N,N-dimethylpropyleneamine is shown. The structure of the amination reaction device of this embodiment is basically the same as that of the second embodiment, except that:
[0033] In this embodiment, the through hole 5 includes a first through hole 6 and a second through hole 7, the diameter of the first through hole 6 is larger than that of the second through hole 7, and the first through hole 6 and the first through hole 6 are staggered along the circumferential direction and the length direction of the drip tube 3. Specifically, the aperture of the first through hole 6 is 50 mm, and the diameter of the second through hole 7 is 25 mm. In this structure, by setting the first through hole 6 and the second through hole 7, through holes of different apertures can form droplets or flow rates of different sizes in the reactor, which helps to improve the mixing efficiency of the liquid. The staggered layout of the first through hole 6 and the second through hole 7 further enhances this mixing, thereby promoting a more uniform distribution of chloropropylene. At the same time, the reaction temperature and concentration gradient are also more effectively controlled, further reducing local overheating or areas of excessive concentration, further improving the stability of the reaction and reducing the occurrence of side reactions. By accurately controlling the dripping of different through holes, the reaction conditions can be adjusted more accurately.
[0034] Comparative Example:
[0035] By using a conventional valve to control the straight-through dripping tube and the bottom-sealed dripping tube in Examples 1 to 3, allyl chloride and dimethylamine were dripped into the reactor to react and generate N,N-dimethylpropyleneamine. 200 batches were collected for each group, and the production data statistics are as follows:
[0036] The structure of the drip tube Amine content Residual dimethylamine Average yield Existing straight-through drip tube 85%-88% 6%-8% 80%-90% The dripping tube in the embodiment 1 90%-91% 4%-6% 90%-92% The dripping tube in the second embodiment 91%-95% 3%-5% 91%-95% The dripping tube in the third embodiment 95%-98% 1%-2% 95%-98%
[0037] It can be seen from the statistical structure that the bottom-sealed dripping tube of the utility model can effectively improve the content of aminated products and the average yield, and reduce the residual dimethylamine, and the dripping tube in Example 3 has the best performance.
[0038] Although the present invention has been disclosed as a preferred embodiment as above, it is not intended to limit the present invention. Any technician familiar with the art can use the above disclosed technical content to make many possible changes and modifications to the technical solution of the present invention without departing from the scope of the technical solution of the present invention, or modify it into an equivalent embodiment of equivalent changes. Therefore, any simple modification, equivalent change and modification made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention should fall within the scope of protection of the technical solution of the present invention.
Claims
1. An amination reaction device for producing N,N-dimethylpropyleneamine, comprising a chloropropylene metering tank (1) and an amination reaction kettle (2), wherein the chloropropylene metering tank (1) is provided with a dripping tube (3) for dripping chloropropylene into the reaction kettle, characterized in that: A bottom plate (4) is provided at the bottom of the dripping tube (3), and a plurality of through holes (5) are provided on the dripping tube (3) for enabling the propylene chloride inside the dripping tube (3) to flow to the amination reaction kettle (2).
2. The amination reaction device for producing N,N-dimethylpropyleneamine according to claim 1, characterized in that: The through hole (5) is arranged on the bottom plate (4).
3. The amination reaction device for producing N,N-dimethylpropyleneamine according to claim 1, characterized in that: The through holes are distributed circumferentially on the side wall of the drip tube (3).
4. The amination reaction device for producing N,N-dimethylpropyleneamine according to claim 3, characterized in that: The through holes comprise a first through hole (6) and a second through hole (7), and the diameter of the first through hole (6) is larger than that of the second through hole (7).
5. The amination reaction device for producing N,N-dimethylpropyleneamine according to claim 4, characterized in that: The first through holes (6) and the second through holes (7) are distributed alternately along the length direction of the drip tube (3).
6. The amination reaction device for producing N,N-dimethylpropyleneamine according to claim 4, characterized in that: The first through holes (6) and the second through holes (7) are distributed alternately along the circumference of the drip tube (3).
7. The amination reaction device for producing N,N-dimethylpropyleneamine according to any one of claims 4 to 6, characterized in that: The diameter of the first through hole (6) is 50 mm, and the diameter of the second through hole (7) is 25 mm.