Columnar microporous reactor

Abstract

Belonging to the technical field of reactors, the invention provides a columnar microporous reactor, which comprises a reactor shell and distribution reaction columns. The inner upper end of the reactor shell is divided by an upper distribution plate to form an upper feeding cavity; the lower end in the reactor shell is divided by a lower distribution plate to form a lower feeding cavity; a material reaction cavity is formed between the upper distribution plate and the lower distribution plate; an ammonia discharge pipe is arranged at the upper part of the material reaction cavity, and a reaction liquid discharge pipe is arranged at the lower part. The distribution reaction column comprises an upper distribution column, a lower reaction column and a liquid collection sleeve sleeving the outer side of the upper distribution column; an upper hollow cavity of the upper distribution column is communicated with the upper feeding cavity through upper distribution holes in the upper distribution plate, and a plug which is not communicated with the lower reaction column is arranged at the lower end of the upper distribution column; a lower hollow cavity of the lower reaction column is communicated with the lower feeding cavity through lower distribution holes in the lower distribution plate. The method has the characteristics that the reaction can be carried out step by step, backmixing is avoided, the reaction surface area is large and the like, and rapid escape of ammonia gas is facilitated.

Description

Technical Field

[0001] The present invention belongs to the technical field of chemical reactors, and particularly relates to a columnar microporous reactor. Background Art

[0002] EDTA (Ethylenediaminetetraacetic acid), abbreviated as (Ethylene Diamine Tetraacetic Acid), is a chelating agent with a wide range of uses. The reaction process using sodium cyanide, ethylenediamine, liquid alkali, and formaldehyde is an advanced production process, which has the characteristics of simple reaction and high yield.

[0003] During the EDTA condensation reaction, ammonia gas is released. If ammonia gas is not quickly removed, side reactions will occur to generate NTA (nitrilotriacetic acid), and at the same time, the consumption of raw materials will increase. In the currently disclosed production processes, most use reaction kettles as reactors. The surface area of the reaction kettle is small, and the backmixing phenomenon is serious, resulting in limited ammonia removal effect and being unfavorable for the diffusion and removal of ammonia gas. Summary of the Invention

[0004] An embodiment of the present invention provides a columnar microporous reactor, aiming to solve the problems that when using the existing reaction kettle for EDTA condensation reaction, the surface area is small, the backmixing phenomenon is serious, and it is unfavorable for the diffusion and removal of ammonia gas.

[0005] To achieve the above object, the technical solution adopted by the present invention is: to provide a columnar microporous reactor, including: a reactor housing and distributed reaction columns;

[0006] The upper end inside the reactor housing is separated by an upper distribution plate to form an upper feed chamber, and the upper feed port at the top of the reactor housing communicates with the upper feed chamber; the lower end inside the reactor housing is separated by a lower distribution plate to form a lower feed chamber, and the lower feed port at the bottom of the reactor housing communicates with the lower feed chamber; a material reaction chamber is formed between the upper distribution plate and the lower distribution plate; wherein, an ammonia discharge pipe is arranged at the upper part of the material reaction chamber, and a reaction liquid discharge pipe is arranged at the lower part.

[0007] The distributed reaction columns are arranged in the material reaction chamber; the distributed reaction columns include upper distribution columns, lower reaction columns connected to the lower ends of the upper distribution columns, and liquid collection sleeves sleeved outside the upper distribution columns; the upper hollow cavities of the upper distribution columns communicate with the upper feed chamber through upper distribution holes on the upper distribution plate, and the lower ends of the upper distribution columns are provided with plugs that do not communicate with the lower reaction columns; the lower hollow cavities of the lower reaction columns communicate with the lower feed chamber through lower distribution holes on the lower distribution plate.

[0008] The material A added through the upper feed port enters the upper hollow cavity through the upper distribution holes, and under pressure, penetrates through the upper micropores distributed on the wall surface of the upper distribution column to the outer wall surface of the upper distribution column. The formed microjet flows downward along the outer wall surface of the upper distribution column under the blockage of the liquid collection sleeve to form a liquid film.

[0009] The material B added through the lower feed port enters the lower hollow cavity through the lower distribution holes, and under pressure, penetrates through the lower micropores distributed on the wall surface of the lower reaction column to the outer wall surface of the lower reaction column, enters the liquid film in the form of a microjet, and laterally contacts the downward-flowing material A to achieve step-by-step reaction.

[0010] In an implementable manner, the upper end of the liquid collection sleeve is fixed on the lower surface of the upper distribution plate; the length of the liquid collection sleeve does not exceed the length of the upper distribution column, and there is a gap for the formation of a microjet of material A between the inner wall of the liquid collection sleeve and the outer wall surface of the upper distribution column.

[0011] In an implementable manner, the upper micropores are uniformly arranged on the wall surface of the upper distribution column, and the aperture of the upper micropores is 0.2 - 5 μm.

[0012] In an implementable manner, a plurality of the upper distribution holes are arrayed on the upper distribution plate, upper distribution pipes are arranged in each of the upper distribution holes, and the upper distribution columns are connected to the upper distribution pipes in a one-to-one correspondence.

[0013] In an implementable manner, the distribution reaction column further includes an upper connecting pipe connected between the upper distribution column and the lower reaction column, and the upper connecting pipe is not communicated with the upper distribution column and the lower reaction column.

[0014] In an implementable manner, the lower reaction column includes a plurality of short reaction columns, the lengths of the short reaction columns are either completely the same or at least the length of one short reaction column is different from the lengths of the other short reaction columns; wherein, two adjacent short reaction columns are communicated through a lower connecting pipe.

[0015] In an implementable manner, the lower micropores are uniformly arranged on the wall surface of the lower reaction column; the aperture of the lower micropores is 0.2 - 5 μm.

[0016] In an implementable manner, the aperture of the lower micropores gradually increases upward from the lower end of the lower reaction column.

[0017] In an implementable manner, a plurality of the lower distribution holes are arrayed on the lower distribution plate, the lower distribution holes correspond to the upper distribution holes in a one-to-one correspondence; lower distribution pipes are arranged in each of the lower distribution holes, and the lower reaction columns are connected to the lower distribution pipes in a one-to-one correspondence.

[0018] In an implementable manner, a heater is provided in the lower feed cavity to heat the material B entering the lower feed cavity.

[0019] Compared with the prior art, the columnar microporous reactor provided by the present invention has the following beneficial effects: (1) It improves the quality of the reaction liquid, which is beneficial to the rapid discharge of ammonia gas, avoids the problem of low ammonia removal effect caused by backmixing, and can also reduce the problem of impurities generated by the reaction of ammonia gas with sodium cyanide and formaldehyde, and reduce side reactions.

[0020] The material A added through the upper feed port enters the upper hollow cavity through the upper distribution holes, and under pressure, penetrates through the upper micropores distributed on the wall surface of the upper distribution column to the outer wall surface of the upper distribution column. The formed microjet flows downward along the outer wall surface of the upper distribution column under the blockage of the liquid collection sleeve to form a material liquid film.

[0021] The material B added through the lower feed port enters the lower hollow cavity from bottom to top through the lower distribution holes, and under pressure, penetrates through the lower micropores distributed on the wall surface of the lower reaction column to the outer wall surface of the lower reaction column, enters the liquid film in the form of a microjet, and is blocked by the downward flowing liquid film, and laterally contacts the downward flowing material A on the outer wall surface of the lower reaction column to achieve step-by-step reaction, without causing backmixing. The ammonia gas generated by the reaction escapes upward through the ammonia exhaust pipe, enabling the ammonia gas to be quickly discharged from the material reaction cavity, and improving the ammonia removal effect.

[0022] Since the material A flows from top to bottom, the material B in the lower hollow cavity is blocked by the blockage at the lower end of the upper distribution column and will not enter the upper hollow cavity, but can only penetrate through the lower micropores of the lower reaction column. The downward flowing liquid film can react with the material B penetrating outside, and the ammonia gas generated by the reaction escapes at any time; the unreacted material A, material B and the reaction liquid generated by the reaction will continue to flow downward under their own weight and form a liquid film wrapped around the outside of the lower reaction column. On the one hand, it blocks the material B away from the outer wall surface of the lower reaction column, avoiding waste of the material B, and on the other hand, it continues to react with the penetrated material B, which also ensures that the entire reaction process proceeds step by step from top to bottom on the outer wall surface of the lower reaction column, improving the reaction effect, not causing backmixing, improving the ammonia removal effect, reducing side reactions, and improving the production quality.

[0023] The penetrated material B forms a microjet state on the outer wall surface of the lower reaction column, strengthening the mixing with the material A in the transverse direction, being more conducive to the reaction, improving the reaction effect, and reducing the generation of by-product ammonia gas. The entire reaction process is gradually completed from top to bottom, without backmixing, and the materials form a film on the outer wall surface of the lower reaction column, with a large surface area and a thin material layer, which is beneficial to the rapid escape of ammonia gas.

[0024] The plug provided at the lower end of the upper distribution column makes the upper hollow cavity of the upper distribution column not communicate with the lower hollow cavity of the lower reaction column, avoiding the situation where the two materials meet and react in the hollow cavity, and ensuring that the materials form a film on the outer wall surface of the lower reaction column.

[0025] Therefore, by using the columnar microporous reactor provided by the present invention, the characteristics of step-by-step reaction, no backmixing, and large reaction surface area can be achieved, which is suitable for the EDTA chelating agent reaction process with a fast reaction rate and by-product gas generation, and is conducive to the escape of ammonia gas.

[0026] (2) The liquid collecting sleeve on the upper distribution column can collect the material A that penetrates through the upper hollow cavity of the upper distribution column, so that the material A flows down along the outer wall surface of the upper distribution column, preventing the material A from shooting away from the upper distribution column in the formed micro-jet. In this way, the material A that penetrates on the outer wall surface of the upper distribution column is wrapped on the outer wall surface of the upper distribution column under the block of the liquid collecting sleeve and flows downward under its own weight, forming a liquid film that wraps the upper distribution column. When there is no liquid collecting sleeve at the lower end of the upper distribution column, due to the continuous wrapping of the liquid film flowing from top to bottom on the upper distribution column, it also blocks the material A that penetrates to the outside at the lower end of the upper distribution column, making the material A that penetrates from the inside of the upper distribution column to the outside form a continuously wrapped liquid film on the upper distribution column and flow downward, all participating in the reaction with the material B, without causing waste of the material A and improving the utilization efficiency of the material A. And the unreacted material A and the generated reaction liquid flowing from top to bottom continue to form a liquid film on the outer wall surface of the lower reaction column, wrapping the lower reaction column, also avoiding the escape and waste of the material B, ensuring that all materials participate in the reaction process, and the rapid discharge of ammonia gas is also conducive to reducing side reactions and improving the quality of the reaction liquid. Description of the Drawings

[0027] Figure 1 It is a schematic structural diagram of the columnar microporous reactor provided by the embodiment of the present invention;

[0028] Figure 2 It is a sectional structure diagram of the upper distribution column provided by the embodiment of the present invention, a schematic diagram of the flow direction of the material A in the upper distribution column (downward arrow), and a schematic diagram of the principle of liquid collection in the upper distribution column (horizontal arrow);

[0029] Figure 3 It is a schematic diagram of the principle of action of the lower reaction column provided by the embodiment of the present invention, a schematic diagram of the flow direction of the material B (upward arrow), a schematic diagram of the escape of ammonia gas (diagonally upward arrow), and a schematic diagram of the overall flow direction of the reaction liquid (downward arrow shown);

[0030] Figure 4 It is a schematic top view structure diagram of the columnar microporous reactor provided by the embodiment of the present invention;

[0031] Description of the Reference Numerals:

[0032] 1. Upper feed inlet; 2. Upper distribution plate; 3. Upper feed cavity; 4. Ammonia discharge pipe; 5. Upper distribution column; 6. Liquid collecting sleeve; 7. Upper connecting pipe; 8. Reactor shell; 9. Short reaction column; 10. Lower connecting pipe; 11. Reaction liquid discharge pipe; 12. Lower feed inlet; 13. Lower feed cavity; 14. Jacket layer; 15. Lower distribution plate; 16. Lower distribution holes; 17. Upper distribution holes; 18. Upper micro holes; 19. Material liquid film; 20. Lower reaction column; 21. Lower micro holes; 22. Reaction liquid film; 23. Plugging. Specific embodiments

[0033] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention more clearly understood, the present invention 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 invention and are not used to limit the present invention.

[0034] Please refer to Figures 1 to Figure 4 , and now the columnar microporous reactor provided by the present invention will be described. The columnar microporous reactor includes: a reactor shell 8 and a distributed reaction column; the upper end inside the reactor shell 8 is separated by an upper distribution plate 2 to form an upper feed cavity 3, and the upper feed inlet 1 at the top of the reactor shell 8 communicates with the upper feed cavity 3; the lower end inside the reactor shell 8 is separated by a lower distribution plate 15 to form a lower feed cavity 13, and the lower feed inlet 12 at the bottom of the reactor shell 8 communicates with the lower feed cavity 13; a material reaction cavity is formed between the upper distribution plate 2 and the lower distribution plate 15; wherein, an ammonia discharge pipe 4 is arranged at the upper part of the material reaction cavity, and a reaction liquid discharge pipe 11 is arranged at the lower part.

[0035] The distributed reaction column is arranged in the material reaction cavity; the distributed reaction column includes an upper distribution column 5, a lower reaction column 20 connected to the lower end of the upper distribution column 5, and a liquid collecting sleeve 6 sleeved outside the upper distribution column 5; the upper hollow cavity of the upper distribution column 5 communicates with the upper feed cavity 3 through the upper distribution holes 17 on the upper distribution plate 2, and a plugging 23 that does not communicate with the lower reaction column 20 is arranged at the lower end of the upper distribution column 5; the lower hollow cavity of the lower reaction column 20 communicates with the lower feed cavity 13 through the lower distribution holes 16 on the lower distribution plate 15.

[0036] The reaction process using the columnar microporous reactor provided by the present invention is as follows: The material A added through the upper feed inlet 1 enters the upper hollow cavity through the upper distribution holes 17, and under pressure, penetrates through the upper micro holes 18 distributed on the wall surface of the upper distribution column 5 to the outer wall surface of the upper distribution column 5. The formed micro jet flows downward along the outer wall surface of the upper distribution column 5 under the block of the liquid collecting sleeve 6 to form a material liquid film 19 (the micro jet is shown in Figure 2The arrow e) pointing outwards from the middle; the material B added through the lower feed inlet 12 enters the lower hollow cavity through the lower distribution holes 16, and under pressure, penetrates through the lower micropores 21 distributed on the wall of the lower reaction column 20 to the outer wall surface of the lower reaction column 20, and forms a micro-jet (the micro-jet is shown by the arrow f) pointing outwards from the middle in Figure 3 enters the material liquid film 19, makes a lateral contact with the downward flowing material A, realizes step-by-step reaction, the generated ammonia gas escapes upwards, is discharged through the ammonia gas discharge pipe at the upper part of the material reaction cavity, and the generated reaction liquid is discharged from the reaction liquid discharge pipe 11 at the bottom of the material reaction cavity.

[0037] The columnar microporous reactor provided by the present invention, compared with the prior art, has the beneficial effects that:

[0038] (1) It can realize the rapid removal of ammonia gas C, avoid the problem of low ammonia removal effect caused by backmixing, reduce side reactions, and improve the quality of the reaction liquid.

[0039] Combined with Figures 1 to 3 Understand that the material A added through the upper feed inlet 1 enters the upper hollow cavity through the upper distribution holes 17, and under pressure, penetrates through the upper micropores 18 distributed on the wall of the upper distribution column 5 to the outer wall surface of the upper distribution column 5. The formed micro-jet, blocked by the liquid collecting sleeve 6, flows downwards along the outer wall surface of the upper distribution column 5 to form a liquid film.

[0040] The material B added through the lower feed inlet 12 enters the lower hollow cavity from bottom to top through the lower distribution holes 16, and under pressure, penetrates through the lower micropores 21 distributed on the wall of the lower reaction column 20 to the outer wall surface of the lower reaction column 20, forms a micro-jet and enters the liquid film, and is blocked by the downward flowing liquid film, and makes a lateral contact with the downward flowing material A on the outer wall surface of the lower reaction column 20 to realize step-by-step reaction, without causing backmixing phenomenon. The generated ammonia gas escapes upwards and is quickly discharged through the ammonia gas exhaust pipe, improving the ammonia removal effect.

[0041] Since the material A flows from top to bottom, the material B in the lower hollow cavity is blocked by the plug 23 at the lower end of the upper distribution column 5 and will not enter the upper hollow cavity, but can only penetrate through the lower micropores 21 of the lower reaction column 20. The downward flowing liquid film can react when encountering the material B permeating outside, and the generated ammonia gas escapes at any time; the unreacted material A, material B and the generated reaction liquid will continue to flow downwards under their own weight and form a reaction liquid film 22 wrapping outside the lower reaction column 20. On the one hand, it blocks the material B away from the outer wall surface of the lower reaction column 20, avoiding waste of the material B, and on the other hand, continues to react with the permeated material B, which also ensures that the whole reaction process proceeds step by step from top to bottom on the outer wall surface of the lower reaction column 20, improving the reaction effect, and will not occur backmixing situation, improving the ammonia removal effect, and thus also reducing the occurrence of side reactions.

[0042] The infiltrated material B forms a micro-jet state on the outer wall surface of the lower reaction column 20, strengthening the mixing with material A in the transverse direction, being more conducive to the reaction, improving the reaction effect, and reducing the generation of by-product ammonia. The entire reaction process is gradually completed from top to bottom, without backmixing, and the materials form a film on the outer wall surface of the lower reaction column 20. With a large surface area and a thin material layer, it is conducive to the rapid escape of ammonia C.

[0043] The plug 23 provided at the lower end of the upper distribution column 5 makes the upper hollow cavity of the upper distribution column 5 not communicate with the lower hollow cavity of the lower reaction column 20, avoiding the situation where the two materials meet and react in the hollow cavity, and ensuring that the materials form a film on the outer wall surface of the lower reaction column 20.

[0044] Therefore, by using the columnar microporous reactor provided by the present invention, characteristics such as step-by-step reaction progress, no backmixing, and a large reaction surface area can be achieved, which is suitable for the EDTA chelating agent reaction process with a fast reaction rate and by-product gas generation, and is conducive to the rapid escape of ammonia C.

[0045] It should be explained that the above-mentioned material liquid film 19 and reaction liquid film 22 are only named according to some of the materials therein in order to distinguish two different component liquid films. Among them, the material liquid film 19 formed on the outer wall surface of the upper distribution column 5 does not have the mixing of material B; while the reaction liquid film 22 wrapped on the outer wall surface of the lower reaction column 20 includes some unreacted material A, material B, and the reaction liquid generated by the reaction of the two. Therefore, it is named the reaction liquid film 22.

[0046] (2) The liquid collection sleeve 6 on the upper distribution column 5 can collect the material A that penetrates through the upper hollow cavity of the upper distribution column 5, making the material A flow down along the outer wall surface of the upper distribution column 5, so that the material A in the formed micro-jet does not shoot in a direction away from the upper distribution column 5. In this way, the material A infiltrated on the outer wall surface of the upper distribution column 5 is wrapped on the outer wall surface of the upper distribution column 5 under the blocking of the liquid collection sleeve 6 and flows downward under its own weight, forming a liquid film wrapping the upper distribution column 5. When there is no liquid collection sleeve 6 at the lower end of the upper distribution column 5, due to the liquid film flowing from top to bottom always wrapping the upper distribution column 5, it also blocks the material A that penetrates to the outside at the lower end of the upper distribution column 5, making the material A that penetrates from the inside of the upper distribution column 5 to the outside form a continuous material liquid film 19 wrapping the upper distribution column 5 and flow downward, all participating in the reaction with material B, without causing waste of material A and improving the utilization efficiency of material A. The unreacted material A flowing from top to bottom and the generated reaction liquid continue to form a material liquid film 19 on the outer wall surface of the lower reaction column 20, wrapping the lower reaction column 20, also avoiding the escape and waste of material B, ensuring that all materials participate in the reaction process, and also being conducive to reducing side reactions and improving the quality of the reaction liquid.

[0047] (3) The liquid film on the outer wall of the lower reaction column 20 flows downward evenly under its own weight, enabling continuous production reaction and improving the reaction effect, thereby achieving the purpose of reducing side reactions and improving the quality of the reaction solution.

[0048] Among them, both material A and material B are liquid materials, and each can be a single material or a mixed material. By pressurization, material A is added into the upper feed chamber 3 through the upper feed port 1 and can only enter the upper distribution column 5 through the upper distribution holes 17. Material A can only penetrate through the outer wall of the upper distribution column 5 under a certain pressure; similarly, by pressurization, material B is added into the lower feed chamber 13 through the lower feed port 12 and can only enter the lower reaction column 20 through the lower distribution holes 16. Material B also needs to flow upward under pressure and penetrate through the lower reaction column 20 to reach the outer wall of the lower reaction column 20.

[0049] It should be noted that using a pressure pump to pressurize the liquid is an easily achievable and conventional technical means. Adjusting to an appropriate pressure can achieve the penetration of the liquid, which can be done by those skilled in the art through conventional means. Pressurization and pressure adjustment are not the inventive points of the present invention, so they will not be elaborated in this article.

[0050] In some embodiments, as shown in Figure 1 the upper end of the liquid collection sleeve 6 is fixed on the lower surface of the upper distribution plate 2; the length of the liquid collection sleeve 6 does not exceed the length of the upper distribution column 5, and there is a gap for material A to form a microjet between the inner wall of the liquid collection sleeve 6 and the outer wall of the upper distribution column 5.

[0051] Under the action of pressure, material A penetrates to the outer wall of the upper distribution column 5 and forms a microjet. Without obstruction, some of material A will be ejected outside the upper distribution column 5 and cannot participate in the reaction well. Therefore, the liquid collection sleeve 6 at the top of the upper distribution column 5 will make material A flow down evenly along the outer wall of the upper distribution column 5. The length of the liquid collection sleeve 6 can be the same as the length of the upper distribution column 5 or shorter than the upper distribution column 5. In the part of the upper distribution column 5 without the liquid collection sleeve 6 at the lower part, a liquid film will be formed due to the flowing down of the liquid, blocking material A from being ejected outside the upper distribution column 5.

[0052] As shown in Figure 2 a gap needs to be reserved between the inner wall of the liquid collection sleeve 6 and the outer wall of the upper distribution column 5 for the penetrated material A. This gap d is between 1 - 5 mm, preferably 2 - 3 mm.

[0053] Optionally, the length of the liquid collection sleeve 6 is between 50 - 300 mm, preferably 100 - 200 mm; the length of the upper distribution column 5 is 200 - 500 mm, and the lower end is sealed to prevent material A from entering the lower reaction column 20 below.

[0054] The outer diameter of the upper distribution column 5 is 25 - 57 mm, preferably 32 - 47 mm. The outer diameter of the lower reaction column 20 is the same as that of the upper distribution column 5.

[0055] In some embodiments, as shown in Fig. 2, the upper micropores 18 are uniformly arranged on the wall surface of the upper distribution column 5. The pore diameter of the upper micropores 18 is 0.2 - 5 μm, preferably 0.45 - 3 μm. Under the condition that the pore diameter of the upper micropores 18 is constant, the permeation rate is proportional to the pressure in the upper feed chamber 3.

[0056] In some embodiments, referring to Figure 1 , a number of upper distribution holes 17 are arranged in an array on the upper distribution plate 2. Upper distribution pipes are provided in each of the upper distribution holes 17, and the upper distribution columns 5 are connected to the upper distribution pipes in a one-to-one correspondence. In the present invention, the upper distribution holes 17 are arranged in an array on the upper distribution plate 2, and each upper distribution pipe is connected to an upper distribution column 5. The material A entering the upper feed chamber 3 can uniformly enter each of the upper distribution columns 5, ensuring that the pressures in the inner cavities of the upper distribution columns 5 are the same, which also ensures that the material outflow rates of the upper distribution columns 5 are the same, enabling the uniform distribution of the material A, thus facilitating the full reaction of the material and improving the reaction quality while reducing side reactions. Among them, the upper distribution column 5 and the upper distribution pipe can be connected by threads. The upper distribution pipe and the upper distribution hole 17 are connected by threads.

[0057] Among them, the upper distribution column 5 can be directly thread-connected to the upper distribution hole 17, in which case the upper distribution pipe does not need to be provided; of course, since the upper distribution column 5 is connected by threads, providing an upper distribution pipe in the upper distribution hole 17 facilitates the setting of internal threads in the upper distribution pipe. When the threads on the upper distribution pipe are damaged, only the upper distribution pipe needs to be replaced, rather than the more valuable and more difficult-to-dismantle upper distribution plate 2. It should be noted that the upper distribution pipe is not shown in the drawings, so it is not labeled either. This design is also applicable to the structure with a lower distribution pipe provided on the lower distribution plate 15. Therefore, the lower distribution pipe is not shown in the drawings either.

[0058] In some embodiments, referring to Figure 1 , the distributed reaction column further includes an upper connecting pipe 7 connected between the upper distribution column 5 and the lower reaction column 20. The upper connecting pipe 7 is not communicated with the upper distribution column 5 and the lower reaction column 20. The upper connecting pipe 7 is made of a stainless steel pipe with external threads at both ends. The upper connecting pipe 7 is thread-connected to both the upper distribution column 5 and the lower reaction column 20, and the outer diameter of the upper connecting pipe 7 is the same as that of the upper distribution column 5 and the lower reaction column 20 to keep the outer diameter of the overall distributed reaction column consistent up and down, ensuring the uniform downward flow of the liquid film.

[0059] The length of the upper connecting pipe 7 is between 100 mm and 500 mm, preferably between 150 mm and 300 mm. The upper connecting pipe 7 made of stainless steel not only has a connecting function, but also has the function of accelerating the material A. In this way, when the material A reaches the top of the lower reaction column 20, it has a certain speed, which is more conducive to mixing and reaction.

[0060] In some embodiments, referring to Figure 1 , the lower reaction column 20 includes multiple short reaction columns 9. The lengths of the short reaction columns 9 are either exactly the same or at least the length of one short reaction column 9 is different from that of other short reaction columns 9; among them, two adjacent short reaction columns 9 are connected through a lower connecting pipe 10. According to this embodiment, it can be seen that the lower reaction column 20 can be composed of multiple short reaction columns 9 with different lengths connected in series by the lower connecting pipe 10. The overall length of the lower reaction column 20 can be greater than the length of the upper distribution column 5 to ensure the sufficiency of the reaction, improve the reaction quality, and reduce side reactions.

[0061] As for how many short reaction columns 9 need to be connected in series and the overall length of the lower reaction column 20 after series connection, the feeding gradient and technology of the reaction can be flexibly changed according to needs, and it can adapt to various reaction conditions.

[0062] The lower connecting pipe 10 is also a stainless steel pipe, and both ends are threadedly connected to the short reaction column 9. Similarly, the lower connecting pipe 10 not only has a connecting function, but also has the function of accelerating the material A, material B, and the reaction solution. The length of the lower connecting pipe 10 can be flexibly adjusted, so that the feeding gradient and technology of the reaction can be flexibly changed according to needs, and it can adapt to various reaction conditions.

[0063] The outer diameter of the lower connecting pipe 10 is also the same as the outer diameter of the lower reaction column 20.

[0064] Of course, there may also be a situation where the outer diameter of the lower connecting pipe 10 is not the same as the outer diameter of the short reaction column 9 to meet the design requirements of variable speed such as accelerating and decelerating the liquid film downward, so as to adjust the reaction rate of the material. However, a conical smooth outer wall needs to be formed at the connection position of the two to ensure the smooth downward flow of the liquid film; in this regard, the outer diameters of the upper distribution column 5 and the upper connecting pipe 7 do not necessarily have to be the same, and similarly, the outer diameters of the upper distribution column 5 and the lower reaction column 20 do not necessarily have to be the same.

[0065] Of course, according to production needs, it is also possible to set only one lower reaction column 20; similarly, the number of upper distribution columns 5 can also be one or more. It can also be decomposed into multiple short distribution columns according to the different lengths of the upper distribution column 5 monomers and then connected in series by connecting pipes.

[0066] Optionally, the length of the short reaction column 9 is between 100 - 500 mm, preferably 200 - 350 mm, and the length of the lower connecting pipe 10 between the short reaction columns 9 is between 50 - 300 mm, preferably 100 - 200 mm.

[0067] In some embodiments, referring to Figure 3 , the lower micropores 21 are uniformly arranged on the wall surface of the lower reaction column 20; the pore diameter of the lower micropores 21 is 0.2 - 5 μm, preferably 0.3 - 1.0 μm.

[0068] In some embodiments, the pore diameter of the lower micropores 21 gradually increases from the lower end to the upper end of the lower reaction column 20.

[0069] Material B enters the lower reaction column 20 from the lower feed chamber 13. Under the action of pressure, it penetrates from the inner cavity to the outer wall surface of the lower reaction column 20. Due to the different pore diameters of the lower micropores 21 on the lower reaction column 20, the penetration rates are different, so the feeding rate of material B gradually decreases, achieving the purpose of gradient feeding. At the same time, due to the existence of pressure, the penetration of material B forms a micro - jet state on the surface of the lower reaction column 20, strengthening the mixing with material A in the transverse direction and being more conducive to the reaction. The entire reaction process is gradually completed from top to bottom, without back - mixing, and the reaction proceeds in a film - like manner on the surface of the lower reaction column 20, with a large surface area and a thin material layer, which is conducive to the escape of ammonia.

[0070] Based on the gradually changing pore diameter of the lower micropores 21, when multiple or multiple segments of short reaction columns 9 are set, a multi - stage reaction is formed. The pore diameters of the lower micropores 21 of the short reaction columns 9 in different stages can be selected differently, and the pore diameters of the lower micropores 21 on the same segment of the short reaction column 9 can be the same. In this way, under the same pressure, the permeation rate of the material can be changed, thereby controlling the size of the feeding amount and being more conducive to reaction adjustment.

[0071] In some embodiments, referring to Figure 1 , a number of lower distribution holes 16 are array - distributed on the lower distribution plate 15, and the lower distribution holes 16 correspond one - to - one with the upper distribution holes 17; lower distribution pipes are arranged in each of the lower distribution holes 16, and the lower reaction columns 20 are connected to the lower distribution pipes one - to - one. Among them, the lower reaction column 20 is thread - connected to the lower distribution pipe.

[0072] In some embodiments, referring to Figure 1 , a heater is arranged in the lower feed chamber 13 to heat material B entering the lower feed chamber 13, so that material B has a certain temperature, which can compensate for a part of the heat required for gas - phase evaporation and better maintain the reaction temperature. Among them, the heater is a jacket heater. For example, the outer shell of the lower feed chamber 13 is provided with a jacket layer 14, and hot water or steam is introduced into the jacket layer 14 to realize the heating of material B, constituting a jacket heater.

[0073] The reaction solution uniformly flows from different lower reaction columns 20 to the bottom of the material reaction chamber, and then flows out from the reaction solution discharge pipe 11. The reaction solution stays at the bottom of the material reaction chamber for a short time, forming a thin layer state, which is also conducive to the outward escape of ammonia gas, thereby reducing the side reaction between ammonia gas and sodium cyanide and formaldehyde, and improving the quality of the product.

[0074] In order to quickly remove the generated ammonia gas, four ammonia gas discharge pipes 4 are uniformly arranged around the upper part of the material reaction chamber (see Figure 4 ), which is conducive to the escape of the generated ammonia gas under negative pressure conditions and will not affect the uniformity of the reaction material film due to the flow rate; the reaction solution discharge pipe 11 at the lower part of the material reaction chamber is at the lowest end of the material reaction chamber (see Figure 4 ), which is conducive to the reaction solution flowing out directly after reaching the bottom of the material reaction chamber, and also has a film-like flow form at the bottom of the material reaction chamber. The high-temperature material B also makes the reaction solution have a relatively high temperature, which is conducive to the volatilization of residual ammonia.

[0075] The working principle of the columnar microporous reactor involved in the present invention is as follows: The material enters the outside of the columnar lower reaction column 20 through the columnar lower reaction column 20 and reacts with the material A flowing down from the upper part. The gas generated during the reaction overflows into the gas phase; the lower reaction column 20 can be connected by multiple short reaction columns 9. At the same time, by continuously changing the outer diameter of different short reaction columns 9, it can be ensured that under the condition of increasing the reaction system material, the thickness of the reaction material film is maintained within a certain range, and the micropore diameter and pressure on different short reaction columns 9 can be changed to ensure that the material addition rate changes continuously according to requirements, and finally achieve the advantages of uniform distribution, fast reaction rate, no backmixing, conducive to gas overflow, and controllable reaction rate. It can be applied to various reactions such as reactions with gas release, reactions with solid formation, reactions with gas participation, and reactions with a large amount of heat release.

[0076] Generally speaking, the reaction process of the present invention is as follows: The material A enters the upper distribution column 5 with micropores from the upper feed chamber 3 at the top, uniformly distributes to the outside of the upper distribution column 5 after passing through the upper micropores 18, and then flows downward from the top under the action of gravity; the material B enters the inside of the columnar lower reaction column 20 with micropores from the lower feed chamber 13 at the bottom, and then passes through the micropores of the lower reaction column 20 and uniformly distributes to the outer wall surface of the lower reaction column 20; the material A and the material B uniformly contact and react outside the lower reaction column 20. The reaction material flows along the lower reaction column 20 to the bottom of the material reaction chamber under the action of gravity, and then is taken out.

[0077] There is no backmixing phenomenon in the whole reaction process. Gas is generated during the reaction of material A and material B. Due to the large reaction surface area, the generated gas can be quickly transferred to the gas phase, resulting in a very low concentration of dissolved gas in the reaction liquid and effectively reducing side reactions. If solids are generated in the reaction system, the solids will be washed to the bottom of the lower reaction column 20 along with the reaction liquid, and the interface of the lower reaction column 20 is continuously updated, which can prevent solid materials from adhering to the lower reaction column 20. For reactions involving gases, gases are introduced into the lower reaction column 20, and the gases can be well distributed, providing a large contact area.

[0078] Multiple distributed reaction columns in the reactor are combined in parallel, greatly improving the space utilization rate and increasing the throughput. The form of multiple reactors in series can also be adopted to ensure that the reaction proceeds completely and sufficiently. The reactor shell 8 can be used as a cooling or heating device to ensure that the temperature of the reaction system is within a certain range. For example, a sandwich or jacket is provided inside the bottom of the reactor shell, and the reaction temperature can be adjusted by introducing water at different temperatures.

[0079] In the above embodiments, the descriptions of each embodiment have their own emphases. For parts not detailed or recorded in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.

[0080] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, and improvements made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A columnar microporous reactor, characterized in that, Comprising: A reactor housing (8) and distributed reaction columns; The upper end inside the reactor housing (8) is separated by an upper distribution plate (2) to form an upper feed chamber (3), and the upper feed port (1) at the top of the reactor housing (8) communicates with the upper feed chamber (3); the lower end inside the reactor housing (8) is separated by a lower distribution plate (15) to form a lower feed chamber (13), and the lower feed port (12) at the bottom of the reactor housing (8) communicates with the lower feed chamber (13); a material reaction chamber is formed between the upper distribution plate (2) and the lower distribution plate (15); wherein, an ammonia discharge pipe (4) is provided at the upper part of the material reaction chamber, and a reaction liquid discharge pipe (11) is provided at the lower part; The distributed reaction columns are arranged in the material reaction chamber; the distributed reaction columns include an upper distribution column (5), a lower reaction column (20) connected to the lower end of the upper distribution column (5), and a liquid collection sleeve (6) sleeved outside the upper distribution column (5); the upper hollow cavity of the upper distribution column (5) communicates with the upper feed chamber (3) through an upper distribution hole (17) on the upper distribution plate (2), and a plug (23) that does not communicate with the lower reaction column (20) is provided at the lower end of the upper distribution column (5); the lower hollow cavity of the lower reaction column (20) communicates with the lower feed chamber (13) through a lower distribution hole (16) on the lower distribution plate (15); The material A added through the upper feed port (1) enters the upper hollow cavity through the upper distribution hole (17), and under pressure, penetrates through the upper micro-holes (18) distributed on the wall surface of the upper distribution column (5) to the outer wall surface of the upper distribution column (5), and the formed micro-jet flows downward along the outer wall surface of the upper distribution column (5) under the blockage of the liquid collection sleeve (6) to form a liquid film; The material B added through the lower feed port (12) enters the lower hollow cavity through the lower distribution hole (16), and under pressure, penetrates through the lower micro-holes (21) distributed on the wall surface of the lower reaction column (20) to the outer wall surface of the lower reaction column (20), enters the liquid film as a micro-jet, and makes a lateral contact with the downward-flowing material A to achieve step-by-step reaction.

2. The columnar microporous reactor according to claim 1, wherein The upper end of the liquid collection sleeve (6) is fixed on the lower surface of the upper distribution plate (2); the length of the liquid collection sleeve (6) does not exceed the length of the upper distribution column (5), and there is a gap for the formation of a micro-jet of material A between the inner wall of the liquid collection sleeve (6) and the outer wall surface of the upper distribution column (5).

3. The columnar microporous reactor according to claim 2, wherein The upper micro-holes (18) are uniformly arranged on the wall surface of the upper distribution column (5), and the aperture of the upper micro-holes (18) is 0.2 - 5 μm.

4. The columnar microporous reactor according to claim 1, wherein A plurality of the upper distribution holes (17) are arrayed and distributed on the upper distribution plate (2), and upper distribution pipes are provided in each of the upper distribution holes (17), and the upper distribution columns (5) are connected to the upper distribution pipes in a one-to-one correspondence.

5. The columnar microporous reactor according to claim 1, characterized in that, The distribution reaction column further includes an upper connecting pipe (7) connected between the upper distribution column (5) and the lower reaction column (20), and the upper connecting pipe (7) is not communicated with the upper distribution column (5) and the lower reaction column (20).

6. The columnar microporous reactor according to claim 1, wherein The lower reaction column (20) includes multiple short reaction columns (9), and the lengths of the short reaction columns (9) are either completely the same or at least the length of one of the short reaction columns (9) is different from the lengths of the other short reaction columns (9); wherein, two adjacent short reaction columns (9) are communicated through a lower connecting pipe (10).

7. The columnar microporous reactor according to claim 1, characterized in that, The lower micropores (21) are uniformly arranged on the wall surface of the lower reaction column (20); the pore diameter of the lower micropores (21) is 0.2 - 5 μm.

8. The columnar microporous reactor according to claim 1, wherein The pore diameter of the lower micropores (21) gradually increases upward from the lower end of the lower reaction column (20).

9. The columnar microporous reactor according to claim 1, wherein A number of the lower distribution holes (16) are arranged in an array on the lower distribution plate (15), and the lower distribution holes (16) correspond to the upper distribution holes (17) one by one; a lower distribution pipe is arranged in each of the lower distribution holes (16), and the lower reaction columns (20) are connected to the lower distribution pipes one by one.

10. The columnar microporous reactor according to claim 1, characterized in that, A heater is arranged in the lower feed chamber (13) to heat the material B entering the lower feed chamber (13).

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