A partitioned reaction ketone azine synthesis apparatus and methods of use thereof

Abstract

This invention belongs to the field of ketazine synthesis technology, and discloses a ketazine synthesis apparatus with partitioned reaction and its usage method. The apparatus includes a reactor, a washing tower, a first mixer, and a second mixer. The washing tower is located at the top of the reactor and is interconnected with the reactor. A fixedly connected partition is installed inside the reactor, which divides the reactor cavity into a first reaction zone and a second reaction zone. The output end of the first mixer is connected to the first reaction zone, and the output end of the second mixer is connected to the second reaction zone. Sodium hypochlorite is delivered in stages to control the reaction sequence and mixing intensity, suppress side reactions caused by excess sodium hypochlorite in strongly alkaline conditions, and improve the yield of ketazine. The washing tower connected to the reactor absorbs and recovers unreacted ketones and ammonia entrained in the rising gas phase, reducing gas phase loss, improving raw material utilization, and reducing production costs and floor space requirements.

Description

Technical Field

[0001] This invention belongs to the field of ketone azide synthesis technology, and relates to a partitioned reaction ketone azide synthesis apparatus and its usage method. Background Technology

[0002] Hydrazine hydrate, also known as hydrazine hydrate, is used in the production of foaming agents, insecticides, fungicides, and pharmaceuticals. Production methods for hydrazine hydrate include the Raschig process, urea process, ketazine process, and hydrogen peroxide process. The ketazine process is economically superior to the urea and Raschig processes and is safer than the hydrogen peroxide process. In the synthesis of ketazine, sodium hypochlorite solution is used as an oxidant, which reacts with ammonia and acetone to produce acetone hydrazine. The chemical reaction formula is: 2NH3 + 2CH3COCH3 + NaClO → (CH3)2C=NN=C(CH3)2 (acetone nitrogen azide) + NaCl + 3H2O When the chlorine content increases from 5% to 10%, the yield of ketazine decreases from 94% to 75%. In actual production, although the chlorine content of sodium hypochlorite is 10%, it needs to be diluted with by-product brine to ensure the yield of ketazine, which increases the overall energy consumption of the system. In addition, the yield of ketazine from sodium hypochlorite diluted with by-product brine is about 2% lower than that from sodium hypochlorite diluted with pure water due to the influence of impurities. Injecting sodium hypochlorite in two stages can reduce the sodium hypochlorite content in each reactor, but it requires two reactors and a scrubbing tower, resulting in high equipment investment and a large footprint. Summary of the Invention

[0003] To address the shortcomings of existing technologies, the present invention aims to provide a partitioned reaction apparatus for the synthesis of ketone azones and its method of use.

[0004] To achieve the above objectives, the present invention adopts the following technical solution: This invention provides a partitioned reaction apparatus for synthesizing ketadiazine, comprising a reactor, a washing tower, a first mixer, and a second mixer; the washing tower is disposed at the upper end of the reactor and is interconnected with the reactor; a fixedly connected partition is provided inside the reactor, the partition dividing the inner cavity of the reactor into a first reaction zone and a second reaction zone; the output end of the first mixer is connected to the first reaction zone, and the output end of the second mixer is connected to the second reaction zone.

[0005] Furthermore, the reactor has a first through hole, a second through hole, a third through hole, and a fourth through hole arranged sequentially from top to bottom. The first through hole is connected to a first mixer, the third through hole is connected to a washing tower, and the fourth through hole is connected to the input end of a second mixer. The second through hole is used to introduce recovered ketone and recovered ammonia, and the first mixer is used to mix sodium hypochlorite, fresh ketone, recovered ketone, and recovered ammonia.

[0006] Furthermore, the reactor has a fifth, sixth, seventh, and eighth through hole on its side wall; the fifth, sixth, seventh, and eighth through holes are arranged sequentially from top to bottom; the fifth through hole is connected to the output end of the second mixer, the seventh through hole is connected to the washing tower, the eighth through hole is connected to the separation section, and the sixth through hole is used to introduce recovered ketones and recovered ammonia.

[0007] Furthermore, the upper end of the reactor is provided with a through hole for introducing liquid ammonia into the first reaction zone and the second reaction zone.

[0008] Furthermore, a gas distributor is provided in the first reaction zone and the second reaction zone, and the gas distributor is fixedly connected to the reactor.

[0009] Furthermore, the washing tower is provided with a first packing material and a second packing material. Soft water at the top of the washing tower enters the second packing material through the first packing material, and the material output from the third and seventh through holes enters the washing tower through the second packing material; the first packing material and the second packing material fill the washing tower.

[0010] Furthermore, a liquid separator is provided at the bottom of the washing tower, which is rotatably connected to the washing tower. The liquid separator is used to control the proportion of washing liquid entering the first reaction zone and the second reaction zone.

[0011] Furthermore, the first mixer and the second mixer are sodium hypochlorite mixers.

[0012] Furthermore, the height of the partition is less than the height of the reactor.

[0013] The present invention also provides a method of using a partitioned reaction ketazine synthesis apparatus. Based on the above-mentioned partitioned reaction ketazine synthesis apparatus, the method includes the following steps: fresh ketone, recovered ketone, recovered ammonia, and sodium hypochlorite solution are fed into a first mixer and mixed to obtain a first mixture. The first mixture and liquid ammonia are fed into a first reaction zone in a reactor for a synthesis reaction. Sodium hypochlorite and the intermediate reaction material discharged from the first reaction zone are fed into a second mixer and mixed to obtain a second mixture. The second mixture and liquid ammonia are fed into a second reaction zone in a reactor for a synthesis reaction. The liquid phase material generated during the synthesis reaction in the first and second reaction zones is fed into a washing tower. After the gaseous material is washed by the washing tower, it re-enters the first and second reaction zones.

[0014] Compared with the prior art, the present invention has the following beneficial technical effects: This invention discloses a partitioned reaction apparatus for synthesizing ketazine. An internal partition divides the reactor cavity into a first reaction zone and a second reaction zone. The first reaction zone is connected to a first mixer, and the second reaction zone is connected to a second mixer. Sodium hypochlorite is transported in stages to control the reaction sequence and mixing intensity, suppressing side reactions caused by excess sodium hypochlorite in strongly alkaline conditions and improving the yield of ketazine. A washing tower connected to each other at the top of the reactor absorbs and recovers unreacted ketones and ammonia carried in the rising gas phase, reducing gas phase loss, improving raw material utilization, and lowering production costs and floor space requirements.

[0015] The first to fourth through holes are arranged sequentially from top to bottom on the left side wall of the reactor. The first through hole is connected to the first mixer, where sodium hypochlorite, fresh ketone and recovered materials are premixed. The second through hole independently allows the recovered ketone and ammonia to be introduced, facilitating flexible replenishment of ammonia and ketone. The third through hole is connected to the washing tower to reduce gas phase loss. The fourth through hole is connected to the input end of the second mixer, which leads out the reaction liquid and returns it to the second reaction zone after mixing in the second mixer, thereby improving the synthesis yield of ketone hydride and the utilization rate of raw materials.

[0016] Gas distributors are fixed in the first and second reaction zones to ensure that the recovered ammonia and ketones are uniformly dispersed in the form of bubbles, thereby increasing the gas-liquid contact area, promoting the mixing of reactants, prolonging the residence time of the gas in the reaction zone, ensuring that ammonia and ketones participate in the reaction, and improving the reaction efficiency.

[0017] The bottom of the washing tower is equipped with a rotating separator plate, which can flexibly adjust the distribution ratio of the washing and recovery liquid according to the actual reaction load, raw material ratio and working conditions of the first and second reaction zones, match the reaction consumption and avoid material imbalance in a single reaction zone.

[0018] The height of the baffle is less than the height of the reactor, and there is a gas connection zone between the top of the baffle and the top inner wall of the reactor, so that the upper gas phase space of the first reaction zone and the second reaction zone are interconnected.

[0019] The washing tower is equipped with a first packing and a second packing. The first packing is used for the absorption of gaseous ketones and ammonia by soft water. The material output from the third and seventh through holes is mixed with the effluent from the first packing and then enters the second packing to absorb gaseous ketones and ammonia. After the ketones and ammonia are absorbed, they are returned to the reactor to improve the recovery efficiency. The first and second packings are installed on the upper end face of the packing support device. The packing support device is detachably connected to the washing tower, which facilitates the replacement, cleaning and maintenance of the first and second packings.

[0020] A through hole is provided at the top of the reactor to simultaneously introduce liquid ammonia into the first and second reaction zones. On the one hand, it provides an ammonia source to ensure the ammonia requirement for the ketone-azo synthesis reaction. On the other hand, the liquid ammonia vaporizes and absorbs heat after entering the reactor, which regulates the reaction temperature and suppresses the occurrence of side reactions at high temperatures. In addition, the gas phase agitation formed by the vaporization of liquid ammonia can further enhance the mixing of the reactants. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the structure of a partitioned reaction ketone azo synthesis apparatus according to the present invention.

[0022] Figure label: 1-Reactor; 2-Scrubbing tower; 3-First mixer; 4-Second mixer; 5-Baffle; 6-First reaction zone; 7-Second reaction zone; 8-Gas distributor; 9-Separating plate. Detailed Implementation

[0023] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of the present invention.

[0024] Example 1 The present invention discloses a partitioned reaction apparatus for the synthesis of ketazine, comprising a reactor 1, a washing tower 2, a first mixer 3, and a second mixer 4; the washing tower 2 is disposed at the upper end of the reactor 1 and is interconnected with the reactor 1; a fixedly connected partition 5 is disposed inside the reactor 1, the partition 5 dividing the inner cavity of the reactor 1 into a first reaction zone 6 and a second reaction zone 7; the output end of the first mixer 3 is connected to the first reaction zone 6, and the output end of the second mixer 4 is connected to the second reaction zone 7.

[0025] like Figure 1As shown, the scrubbing tower 2 is fixedly installed at the upper end of the reactor 1, and the inner cavity of the scrubbing tower 2 is interconnected with the inner cavity of the reactor 1. The reactor 1 is cylindrical, and a baffle 5 is installed in its inner cavity. The sides and bottom of the baffle 5 are fixedly connected to the inner wall of the reactor 1, dividing the inner cavity of the reactor 1 into two independent reaction spaces, specifically a first reaction zone 6 and a second reaction zone 7. The height of the baffle 5 is less than the height of the inner cavity of the reactor 1, and a gas-connected passage is left between the top of the baffle 5 and the top inner wall of the reactor 1, allowing the upper gas phase spaces of the first reaction zone 6 and the second reaction zone 7 to be interconnected.

[0026] Integrating the two-stage series reaction process into a single reactor shell reduces costs and floor space; the air-connection space reserved at the top of the partition ensures dynamic equilibrium of the gas phase pressure between the first reaction zone 6 and the second reaction zone 7, preventing material cross-flow due to pressure differences.

[0027] The left sidewall of reactor 1 has a first through hole, a second through hole, a third through hole, and a fourth through hole arranged sequentially from top to bottom. The first through hole is connected to the output end of the first mixer 3. The input end of the first mixer 3 is connected to sodium hypochlorite, fresh ketone, recovered ammonia, and recovered ketone, respectively. Before entering the first reaction zone 6, each raw material is mixed in the first mixer 3 to avoid side reactions caused by excessively high local sodium hypochlorite concentration and to improve the yield of ketone azo. The first through hole is located at the top and flows from top to bottom under the action of gravity, prolonging the residence time in the first reaction zone 6 and making the reaction more complete.

[0028] The second through hole is located below the first through hole and is used to directly introduce the recovered ketone and recovered ammonia materials into the first reaction zone 6, so as to facilitate the adjustment of the replenishment amount of ammonia and recovered ketone, and control the material ratio and pH environment.

[0029] The third through hole is located below the second through hole and is connected to the upper liquid inlet of the washing tower 2. It is used to introduce the liquid phase material (ketone nitrogen, excess ammonia, ketone, sodium hypochlorite and the generated brine) in the first reaction zone into the washing tower 2.

[0030] The fourth through hole is located below the first reaction zone 6 and is connected to the input end of the second mixer 4. The intermediate material after the first stage of reaction in the first reaction zone 6 flows out of the reactor 1 through the fourth through hole and is sent into the second mixer 4 for secondary batching, maximizing the utilization of the reactor volume.

[0031] The right sidewall of reactor 1 has a fifth through hole, a sixth through hole, a seventh through hole, and an eighth through hole arranged sequentially from top to bottom. The fifth through hole is located on the same horizontal line as the first through hole and is connected to the output end of the second mixer 4. The second stage of reactants mixed by the second mixer 4 are sent into the second reaction zone 7 through the fifth through hole.

[0032] The sixth through-hole is located below the fifth through-hole, and is used to replenish the recovered ketone and recovered ammonia materials into the second reaction zone 7. The seventh through-hole is located below the sixth through-hole and is connected to the upper liquid inlet of the washing tower 2. It is used to transport the liquid phase materials (ketone nitrogen, excess ammonia, ketone, sodium hypochlorite, and generated brine) generated in the second reaction zone 7 to the washing tower 2. The eighth through-hole is located below the second reaction zone 7. The reaction liquid containing ketone nitrogen after the two-stage synthesis reaction is discharged from reactor 1 through the eighth through-hole and enters the separation section.

[0033] The first and fifth through holes are on the same horizontal line, as are the second and sixth, third and seventh, and fourth and eighth through holes. The through holes on both sides are set at the same height, ensuring that the liquid level, liquid residence path, gas rise path, and material self-flow pressure difference within the first reaction zone 6 and the second reaction zone 7 are completely equal. This facilitates the use of the same process control parameters for regulation and reduces the difficulty of process debugging. The symmetrical openings at the same height ensure uniform stress on the reactor 1 shell, avoiding stress concentration problems caused by concentrated openings on one side. The pipe lengths from the third and seventh through holes to the washing tower 2 are equal, preventing excessive liquid flow on one side and liquid accumulation on the other, ensuring liquid pressure balance in both reaction zones. The fourth and eighth through holes are on the same horizontal plane, resulting in uniform discharge liquid levels, enabling synchronous and stable material delivery and preventing material accumulation or abnormal liquid level rise in one reaction zone.

[0034] The top cover plate of reactor 1 has a through-hole for liquid ammonia feed, which is connected to the inner cavity of the first reaction zone 6 and the second reaction zone 7 respectively. The liquid ammonia feedstock is fed into the two reaction zones through the top through-hole. Gas distributors 8 are installed inside the first reaction zone 6 and the second reaction zone 7 respectively. The gas distributors 8 are annular porous structures and are fixedly connected to the inner wall of reactor 1 by a fixed support. The recovered gaseous ammonia and ketone fed into reactor 1 are evenly dispersed through the gas outlet of the gas distributor 8. Liquid ammonia enters from the top, vaporizes and absorbs heat to reduce the temperature in the upper part of the reaction zone, avoids excessive decomposition of sodium hypochlorite and generation of by-products due to insufficient local ammonia concentration, and improves the reaction yield of ketone azohydride.

[0035] The scrubbing tower 2 is fixedly installed at the top center of the reactor 1, and its bottom opening is directly connected to the top gas phase space of the reactor 1. Inside the scrubbing tower 2, from top to bottom, are a first packing layer and a second packing layer, stacked on the upper surface of a packing support device. The edge of the support device is detachably connected to the inner wall of the scrubbing tower 2 by bolts. Soft water is introduced into the top of the scrubbing tower 2 and sprayed evenly from the top, forming a countercurrent contact with the gas phase material. The first packing layer absorbs gas phase ketones and ammonia with the soft water. The material output from the third and seventh through holes mixes with the effluent from the first packing layer and enters the second packing layer to absorb gas phase ketones and ammonia. After absorption, the ketones and ammonia are returned to the reactor 1. The first and second packing layers can remove ketones and ammonia from the gas phase in stages, improving the scrubbing and recovery efficiency.

[0036] The packing support device is installed at the bottom of the packing layer to support the packing and the liquid-laden packing during operation. The packing support device should not only have sufficient strength and rigidity to support the weight of the packing layer, but also ensure a free-flow cross-sectional area to reduce the flow resistance between the gas and liquid phases. Types include grid-type and hump-type supports. Grid-type supports are welded from flat steel bars and flat steel rings; they have a simple structure, are easy to manufacture, and are often used for supporting structured packing. For smaller tower diameters, a single-piece grid can be used, while for larger tower diameters, a segmented grid can be used.

[0037] Hump ​​supports are assembled from several hump support beams (referred to as hump beams). A 10mm gap is maintained between each hump beam using spaced bosses for drainage. The humps have elongated or strip-shaped side holes. Hump supports are characterized by high gas throughput and high liquid load, making them suitable for large towers. For towers with a diameter greater than 3m, I-beam supports should be installed perpendicular to the hump axis in the middle to increase rigidity.

[0038] A separator plate 9 is installed at the bottom of the washing tower 2. The separator plate 9 is rotatably connected to the inner wall of the washing tower 2 via a rotating shaft. The separator plate 9 is located below the liquid outlet of the washing tower 2 and above the gas phase space at the top of the reactor 1. By rotating and adjusting the angle and opening of the separator plate 9, the flow area of ​​the washing liquid flowing to both sides is changed, thereby controlling the flow ratio of the washing liquid flowing out of the bottom of the washing tower 2 into the first reaction zone 6 and the second reaction zone 7 respectively. By setting a separator plate at the bottom of the washing tower 2, the distribution ratio of the washing recovery liquid can be flexibly adjusted according to the actual reaction load, raw material ratio and operating conditions of the first reaction zone 6 and the second reaction zone 7, matching the reaction consumption and avoiding material imbalance in a single reaction zone.

[0039] The first mixer 3 corresponds to the first reaction zone 6, and the second mixer 4 corresponds to the second reaction zone 7. The first mixer 3 mixes fresh ketone, sodium hypochlorite, recovered ketone, and recovered ammonia; the second mixer 4 mixes the intermediate material from the first reaction zone 6 with sodium hypochlorite.

[0040] The working process in the first reaction zone is as follows: Fresh ketone, sodium hypochlorite, and recovered ketone and ammonia are fed into the first mixer 3 to obtain a first mixture. This mixture is then fed into the upper part of the first reaction zone 6 through the first through-hole on the side wall of reactor 1. Liquid ammonia enters the first reaction zone 6 through the through-hole at the top of reactor 1, where a ketone-azo synthesis reaction occurs. During the reaction, the recovered gaseous ketone and ammonia are dispersed into bubbles by the distributor 8 through the second through-hole and rise to contact the liquid phase material flowing downwards countercurrently. Recovered ketone and recovered ammonia are then added. The liquid phase material produced by the reaction is fed into the washing tower 2 through the third through-hole for washing; the intermediate material flows out through the fourth through-hole at the bottom of the first reaction zone 6 and enters the second mixer 4.

[0041] The working process of the second reaction zone is as follows: the intermediate material from the first reaction zone 6 is mixed with sodium hypochlorite in the second mixer 4 to obtain a second mixture, which is then fed into the upper part of the second reaction zone 7 through the fifth through-hole. Liquid ammonia enters the second reaction zone 7 from the through-hole at the top of the reactor 1 to carry out the second-stage synthesis reaction, causing the remaining ketone to react with sodium hypochlorite to generate ketone hydride. During the reaction, the recovered gaseous ketone and ammonia are dispersed into bubbles by the distributor 8 through the sixth through-hole and rise to contact the liquid phase material flowing from top to bottom in a countercurrent manner, with the recovery of ketone and ammonia being added. The utilization rate of sodium hypochlorite is improved through two-stage injection, eliminating the need for dilution of high-concentration sodium hypochlorite. The liquid phase produced by the reaction is fed into the washing tower 2 through the seventh through-hole; the final solution is output from the eighth through-hole at the bottom of the second reaction zone 7.

[0042] The working process of the scrubbing tower is as follows: the liquid phase materials in the first reaction zone 6 and the second reaction zone 7 are fed into the scrubbing tower 2 through the third and seventh through holes, respectively; soft water is sprayed down from the top of the scrubbing tower 2, passing through the first packing layer and the second packing layer in sequence, and comes into countercurrent contact with the gas phase material to absorb the ketones and ammonia entrained in the gas phase. The scrubbing liquid that has absorbed the ketones and ammonia flows downward, passes through the liquid separator 9 at the bottom of the scrubbing tower 2, and flows into the first reaction zone 6 and the second reaction zone 7 respectively according to the preset ratio. The flow ratio between the first reaction zone 6 and the second reaction zone 7 can be flexibly adjusted by rotating the liquid separator 9.

[0043] In summary, by setting up vertical baffles inside the reactor to form two series-connected first reaction zones 6 and second reaction zones 7, and injecting sodium hypochlorite in stages, the yield of ketone nitrogen caused by high chlorine concentration is avoided without using brine to dilute the sodium hypochlorite, thus reducing the wastewater treatment load; at the same time, the footprint is reduced.

[0044] Example 2 The present invention discloses a method for using a partitioned reaction ketone-azo synthesis apparatus, comprising the following steps: fresh ketone, recovered ketone, recovered ammonia, and sodium hypochlorite solution are fed into a first mixer 3 for mixing to obtain a first mixture; the first mixture and liquid ammonia are fed into a first reaction zone 6 within a reactor 1 for a synthesis reaction; sodium hypochlorite and intermediate reaction materials discharged from the first reaction zone 6 are fed into a second mixer 4 for mixing to obtain a second mixed product; the second mixture and liquid ammonia are fed into a second reaction zone 7 within a reactor 1 for a synthesis reaction; the liquid phase material generated during the synthesis reaction in the first reaction zone 6 and the second reaction zone 7 is fed into a washing tower 2; the gaseous material washed by the washing tower 2 is then reintroduced into the first reaction zone 6 and the second reaction zone 7.

[0045] Fresh ketone, recycled ketone, recycled ammonia, and sodium hypochlorite solution are fed into the first mixer 3, where they are mixed to form a first mixture. This first mixture is then fed into the inner cavity of the first reaction zone 6 from the top through a first through-hole in the side wall of the reactor 1. Simultaneously, liquid ammonia enters the first reaction zone 6 through a through-hole at the top of the reactor 1, ensuring a sufficient ammonia supply. Through mixing in the first mixer 3, sodium hypochlorite is dispersed with the ketone and ammonia materials before entering the reaction system, avoiding side reactions caused by sudden spikes in local chlorine concentration. Furthermore, since only a portion of the sodium hypochlorite is injected into the first reaction zone 6, dilution is unnecessary, reducing the additional energy consumption and risk of impurity introduction associated with brine dilution.

[0046] The first stage of synthesis reaction takes place in the first reaction zone 6. The first mixture entering the first reaction zone 6 flows downward under gravity, undergoing a ketone-azo synthesis reaction. During the reaction, recovered ketones and recovered ammonia are added to the first reaction zone 6 through the second through-hole, dynamically adjusting the ammonia-ketone ratio. The liquid phase material produced by the reaction flows out of reactor 1 through the third through-hole and enters the washing tower 2 for washing and recovery of gaseous ammonia and ketones; the intermediate material from the first stage reaction collects at the bottom of the first reaction zone 6 and flows out of reactor 1 through the fourth through-hole, entering the second mixer 4.

[0047] The intermediate material flowing out from the bottom of the first reaction zone 6 enters the second mixer 4, while sodium hypochlorite solution is simultaneously added to the second mixer 4. After mixing in the second mixer 4, a second mixture is formed. The second mixture enters the second reaction zone 7 through the fifth through-hole on the right side wall of reactor 1; liquid ammonia enters through the through-hole at the top of reactor 1. The sodium hypochlorite is injected in stages to avoid a high-chlorine reaction environment, thus improving the product yield compared to traditional single-stage reactions.

[0048] The second mixture entering the upper part of the second reaction zone 7 also flows downwards under gravity, continuing the ketazine synthesis reaction, converting the remaining reactants from the first stage reaction and the added sodium hypochlorite into ketazine products. During the reaction, recovered ketones and recovered ammonia are added through the sixth through-hole on the side wall of reactor 1. The liquid phase produced by the reaction flows out of reactor 1 through the seventh through-hole and enters the washing tower 2; the final solution collects at the bottom of the second reaction zone 7, exits reactor 1 through the eighth through-hole, and then enters the separation section for purification. The first reaction zone 6 and the second reaction zone 7 are integrated into reactor 1, reducing the floor space and equipment investment, while also reducing the probability of side reactions occurring during the transportation of intermediate products.

[0049] The liquid phase from the first reaction zone 6 is fed into the washing tower 2 through the third through-hole, and the liquid phase from the second reaction zone 7 is fed into the washing tower 2 through the seventh through-hole. Soft water is introduced from the top spray nozzle of the washing tower 2, passing through the first packing and the second packing in sequence, forming a sufficient countercurrent contact with the rising gaseous material. The washing liquid, which has absorbed the ketone and ammonia components, continues to flow downwards and falls onto the distributor plate 9 at the bottom of the washing tower 2. By rotating the distributor plate 9 to adjust the opening and angle, the flow area of ​​the washing liquid flowing to both sides is changed, thereby controlling the flow ratio of the washing liquid flowing into the first reaction zone 6 and the second reaction zone 7 respectively.

[0050] It should be noted that the terms "first," "second," etc., in the specification, claims, and accompanying drawings of this invention are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of the invention described herein can be implemented in orders other than those illustrated or described herein. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover a non-exclusive inclusion; for example, a process, method, system, product, or apparatus that comprises a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or units not explicitly listed or inherent to such processes, methods, products, or apparatus.

Claims

1. A partitioned reaction apparatus for the synthesis of ketazine, characterized in that: It includes a reactor (1), a scrubbing tower (2), a first mixer (3), and a second mixer (4); The washing tower (2) is located at the top of the reactor (1) and is interconnected. The reactor (1) is provided with a fixedly connected partition (5). The partition (5) divides the inner cavity of the reactor (1) into a first reaction zone (6) and a second reaction zone (7). The output end of the first mixer (3) is connected to the first reaction zone (6), and the output end of the second mixer (4) is connected to the second reaction zone (7).

2. The ketone azo synthesis apparatus according to claim 1, characterized in that: The reactor (1) has a first through hole, a second through hole, a third through hole and a fourth through hole on its side wall, which are arranged sequentially from top to bottom; The first through-hole is connected to the first mixer (3), the third through-hole is connected to the washing tower (2), and the fourth through-hole is connected to the input end of the second mixer (4). The second through hole is used to pass in the recovered ketone and recovered ammonia, and the first mixer (3) is used to mix sodium hypochlorite, fresh ketone, recovered ketone and recovered ammonia.

3. The ketone azo synthesis apparatus for partitioned reactions according to claim 2, characterized in that: The reactor (1) has a fifth through hole, a sixth through hole, a seventh through hole and an eighth through hole on its side wall; the fifth through hole, the sixth through hole, the seventh through hole and the eighth through hole are arranged sequentially from top to bottom; The fifth through hole is connected to the output end of the second mixer (4), the seventh through hole is connected to the washing tower (2), the eighth through hole is connected to the separation section, and the sixth through hole is used to pass in recovered ketone and recovered ammonia.

4. The ketone azo synthesis apparatus according to claim 3, characterized in that: The upper end of the reactor (1) is provided with a through hole for introducing liquid ammonia into the first reaction zone (6) and the second reaction zone (7).

5. The ketone azide synthesis apparatus for partitioned reaction according to claim 1, characterized in that: Gas distributors (8) are provided in the first reaction zone (6) and the second reaction zone (7), and the gas distributors (8) are fixedly connected to the reactor (1).

6. The ketone azo synthesis apparatus according to claim 1, characterized in that: The washing tower (2) is provided with a first packing and a second packing. The soft water at the top of the washing tower enters the second packing through the first packing. The materials output from the third and seventh through holes enter the washing tower through the second packing. The first packing and the second packing are filled inside the scrubbing tower (2).

7. The ketone azo synthesis apparatus according to claim 6, characterized in that: The bottom of the washing tower (2) is provided with a liquid separator (9), which is rotatably connected to the washing tower (2); the liquid separator (9) is used to control the ratio of washing liquid entering the first reaction zone (6) and the second reaction zone (7).

8. The ketone azo synthesis apparatus according to claim 7, characterized in that: The first mixer (3) and the second mixer (4) are sodium hypochlorite mixers.

9. The ketone azo synthesis apparatus according to claim 8, characterized in that: The height of the partition (5) is less than the height of the reactor (1).

10. A method of using a partitioned reaction apparatus for the synthesis of ketazine, characterized in that, The ketone azo synthesis apparatus based on the partitioned reaction according to any one of claims 1-9 includes the following steps: Fresh ketone, recycled ketone, recycled ammonia and sodium hypochlorite solution are fed into the first mixer (3) and mixed to obtain the first mixture. The first mixture and liquid ammonia are fed into the first reaction zone (6) in the reactor (1) for synthesis reaction. Sodium hypochlorite and the intermediate reaction material discharged from the first reaction zone (6) are fed into the second mixer (4) for mixing to obtain the second mixed product. The second mixed material and liquid ammonia are then fed into the second reaction zone (7) inside the reactor (1) for a synthesis reaction. The liquid phase material generated during the synthesis reaction in the first reaction zone (6) and the second reaction zone (7) is fed into the washing tower (2). After the gas phase material is washed by the washing tower (2), it re-enters the first reaction zone (6) and the second reaction zone (7).

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