A reaction kettle for synthesizing ammonium dihydrogen phosphate
Patent Information
- Application Number
- CN202522520632.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-27
- Publication Date
- 2026-10-23
- Estimated Expiration
- 2035-11-27
AI Technical Summary
[0004]目前,常规反应釜所采用的气体分布器在该特定应用场景下暴露出如下缺陷:1)其出气方式往往难以确保氨气与磷酸溶液的充分、均匀接触,导致吸收效率不高,存在氨气逸散风险;2)更为棘手的是,生成的大量磷酸二氢铵固体颗粒极易在气体分布器的出气口及内部流道沉积、附着,迅速引发堵塞
[0022]本实用新型用于合成磷酸二氢铵的反应釜,其工作原理如下:
Smart Images

Figure CN224878011U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of reaction vessel technology, and in particular to a reaction vessel for synthesizing ammonium dihydrogen phosphate. Background Technology
[0002] Tris(trimethylsilyl)phosphate, a key additive in lithium-ion battery electrolytes, produces a large amount of ammonia gas as a byproduct during its synthesis. Current technologies typically treat this ammonia-containing waste gas by absorbing large amounts of water. While simple to operate, this method consumes significant water resources and generates ammonia nitrogen wastewater requiring further treatment, increasing environmental pressure and treatment costs, and failing to achieve effective recovery and utilization of ammonia resources.
[0003] To promote cleaner production and resource recycling, the industry is actively exploring the introduction of ammonia gas from the aforementioned synthesis tail gas into a phosphoric acid solution to produce economically valuable ammonium dihydrogen phosphate (MDH). However, in this gas-liquid reaction process, the generated MDH is prone to supersaturation in the solution, leading to crystallization and precipitation of solid particles. This characteristic places extremely stringent requirements on the reactors used for synthesizing MDH, especially its core component—the gas distributor.
[0004] Currently, the gas distributors used in conventional reactors exhibit the following drawbacks in this specific application scenario: 1) Their gas outlet methods often fail to ensure sufficient and uniform contact between ammonia and phosphoric acid solution, resulting in low absorption efficiency and a risk of ammonia escape; 2) More problematic is that the large amount of solid ammonium dihydrogen phosphate generated easily deposits and adheres to the gas distributor's outlet and internal flow channels, rapidly causing blockages. This not only severely hinders the normal distribution of gas and disrupts the continuity of the reaction, but also leads to low production efficiency due to frequent shutdowns for cleaning; 3) Traditional distributor structures are often quite complex, making cleaning and maintenance extremely inconvenient.
[0005] Based on this, a novel reaction vessel for synthesizing ammonium dihydrogen phosphate was developed in this invention to solve the above problems. Utility Model Content
[0006] The purpose of this invention is to provide a reactor for synthesizing ammonium dihydrogen phosphate. This reactor, in conjunction with an L-shaped pipe and a stirrer, achieves efficient ammonia absorption and enhanced gas-liquid mass transfer. It also utilizes mechanical cleaning and airflow flushing to actively prevent clogging and ensure continuous and stable production.
[0007] This utility model adopts the following technical solution: a reaction vessel for synthesizing ammonium dihydrogen phosphate, comprising:
[0008] Reactor body;
[0009] A stirrer is disposed within the reactor body;
[0010] A gas distributor, which is an L-shaped pipe, is detachably installed inside the reactor body and located next to the agitator; the L-shaped pipe has an outlet near the agitator.
[0011] Furthermore, the L-shaped pipe has an air inlet end and an air outlet end;
[0012] The inlet end of the L-shaped pipe extends to the outside of the reactor body, and the outlet end of the L-shaped pipe is located at the bottom of the reactor body.
[0013] Furthermore, the diameter of the L-shaped pipe decreases gradually from the inlet end to the outlet end.
[0014] Furthermore, the L-shaped pipe is composed of multiple pipe sections with successively decreasing diameters, which are nested together to form a sleeve-type structure.
[0015] Furthermore, the L-shaped pipe is a one-piece molded structure, and its diameter changes smoothly through arc-shaped rounded corners.
[0016] Furthermore, the vent is shaped like a volcano, narrow at the top and wide at the bottom.
[0017] Furthermore, the L-shaped pipe is made of polytetrafluoroethylene (PTFE).
[0018] Furthermore, the reactor body is made of enamel material.
[0019] Furthermore, the agitator is an anchor-type agitator.
[0020] Furthermore, the frame of the stirrer is made of enamel material.
[0021] Compared with related technologies, the beneficial effects of this utility model are as follows:
[0022] This invention relates to a reaction vessel for synthesizing ammonium dihydrogen phosphate, and its working principle is as follows:
[0023] During operation, a measured amount of phosphoric acid solution is first injected into the reactor body, the stirrer is started and it is run at a preset speed to form a uniform stirring flow field without obvious dead corners in the phosphoric acid solution; then, the synthesis tail gas containing ammonia is introduced into the reactor body through the gas distributor with an L-shaped pipe structure and released from the gas outlet near the stirrer.
[0024] The stirrer creates strong forced convection inside the reactor: on the one hand, the shear force generated by the rotating blades breaks up ammonia bubbles, increasing the gas-liquid contact area; on the other hand, it continuously refreshes the liquid surface near the gas outlet, removes saturated liquid and replenishes fresh phosphoric acid solution, maintaining a high-efficiency reaction concentration difference, ensuring that ammonia and phosphoric acid fully undergo a neutralization reaction (NH3 + H3PO4 → NH4H2PO4), which not only improves the reaction rate and synthesis efficiency, but also minimizes ammonia escape, meeting environmental protection requirements.
[0025] Meanwhile, the layout design of the gas outlet being close to the stirrer can continuously sweep the surface of the gas outlet by means of the shearing force and scouring effect of the rotating blades. This actively prevents the growth of ammonium dihydrogen phosphate crystals at the outlet through mechanical action, replacing the traditional passive anti-clogging method. This significantly reduces the risk of production interruption caused by solid accumulation and ensures the continuity and stability of the synthesis process.
[0026] In addition, the gas distributor adopts a simple L-shaped pipe with low manufacturing cost; and makes the most of the internal space of the reactor body with a stirrer to ensure the uniformity of gas output and prevent gas from escaping due to ammonia not being absorbed in time; it adopts a detachable installation design, which makes it easy to remove from the reactor body for cleaning or maintenance, making maintenance convenient. Attached Figure Description
[0027] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0028] Figure 1 This is a schematic diagram of the reaction vessel used for synthesizing ammonium dihydrogen phosphate in a specific embodiment of this utility model;
[0029] Figure 2 for Figure 1 A schematic diagram illustrating the principle of the L-shaped pipe as a sleeve structure;
[0030] Figure 3 for Figure 1 Enlarged view of a portion of the image;
[0031] In the figure: reactor body 1; stirrer 2, frame 20, stirring blade 21, drive mechanism 22; gas distributor 3, gas outlet 30, first gas outlet 301, second gas outlet 302, gas inlet 31, gas outlet 32, pipe section 33. Detailed Implementation
[0032] The technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model.
[0033] The following is in conjunction with the appendix Figure 1 The appendix Figure 3 The present invention will be described in detail with specific embodiments:
[0034] like Figures 1 to 3 As shown, this utility model provides a reaction vessel for synthesizing ammonium dihydrogen phosphate, which includes:
[0035] Reactor body 1;
[0036] Stirrer 2, wherein the stirrer 2 is disposed inside the reaction vessel body 1;
[0037] Gas distributor 3, which is an L-shaped pipe, is detachably installed inside the reactor body 1 and located next to the stirrer 2; the L-shaped pipe has an outlet 30 near the stirrer 2; preferably, the outlet 30 of the L-shaped pipe is located near the blades of the stirrer 2, which can further improve the gas-liquid mixing efficiency.
[0038] In this embodiment, the L-shaped pipe is made of polytetrafluoroethylene (PTFE). Using PTFE to fabricate the L-shaped pipe provides it with stable chemical properties and excellent non-stick properties. This material effectively resists corrosion from reaction media (such as phosphoric acid and ammonia), ensuring the long-term reliability of the equipment. Simultaneously, its smooth and hydrophobic surface greatly inhibits the adhesion of ammonium dihydrogen phosphate crystals generated during the reaction to the inner wall of the pipe and the gas outlet 30, further enhancing the anti-clogging capability of the entire gas distribution system from a material perspective.
[0039] This invention relates to a reaction vessel for synthesizing ammonium dihydrogen phosphate, and its working principle is as follows:
[0040] During operation, a measured amount of phosphoric acid solution is first injected into the reactor body 1, and the stirrer 2 is started and operated at a preset speed to form a uniform stirring flow field without obvious dead corners in the phosphoric acid solution. Subsequently, the synthesis tail gas containing ammonia is introduced into the reactor body 1 through the gas distributor 3 with an L-shaped pipe structure and released from the gas outlet 30 near the stirrer 2.
[0041] Stirrer 2 creates strong forced convection inside the reactor: on the one hand, the shear force generated by the rotation of the blades breaks up ammonia bubbles, increasing the gas-liquid contact area; on the other hand, it continuously refreshes the liquid surface near the gas outlet 30, removes saturated liquid and replenishes fresh phosphoric acid solution, maintains a high-efficiency reaction concentration difference, and ensures that ammonia and phosphoric acid fully undergo a neutralization reaction (NH3+H3PO4→NH4H2PO4), which not only improves the reaction rate and synthesis efficiency, but also minimizes ammonia escape and meets environmental protection requirements.
[0042] Meanwhile, the layout of the outlet 30 close to the stirrer 2 allows the shearing force and scouring effect of the rotating blades to continuously sweep the surface of the outlet 30. This mechanical action actively prevents ammonium dihydrogen phosphate crystals from adhering and growing at the outlet, replacing the traditional passive anti-blocking method. This significantly reduces the risk of production interruption caused by solid accumulation and ensures the continuity and stability of the synthesis process.
[0043] In addition, the gas distributor adopts a simple L-shaped pipe with low manufacturing cost; and makes the maximum use of the internal space of the reactor body 1 with stirrer 2 to ensure the uniformity of gas output and prevent gas from escaping due to ammonia not being absorbed in time; it adopts a detachable installation design, which makes it easy to remove from the reactor body 1 for cleaning or maintenance, and is convenient to maintain.
[0044] Furthermore, the L-shaped pipe has an air inlet end 31 and an air outlet end 32.
[0045] The air inlet 31 of the L-shaped pipe extends to the outside of the reactor body 1, facilitating the connection between the air inlet 31 of the L-shaped pipe and an external air source. It should be noted that this invention does not specifically limit how to ensure the sealing of the connection between the air inlet 31 of the L-shaped pipe and the reactor body 1; for example, a sealing ring or similar design can be used to ensure a tight seal.
[0046] The outlet 32 of the L-shaped pipe is located at the bottom of the reactor body 1 and below the stirrer 2.
[0047] The gas outlet 32 is located at the bottom of the reactor body 1, allowing ammonia gas to be directly delivered to the bottom layer of the liquid inside the reactor and released. After escaping in the form of tiny bubbles, the gas rises from bottom to top through the entire liquid layer under the action of buoyancy, significantly extending the contact time between the gas and liquid phases and ensuring the full reaction of ammonia and phosphoric acid.
[0048] Meanwhile, the bottom of the reactor body 1 is the area with the strongest shear force and the most intense turbulence of the stirrer 2. After the ammonia bubbles are released from the bottom, they are immediately broken into smaller bubbles by the high-speed rotating stirring blades and quickly dispersed to the entire reactor by the liquid flow, which significantly increases the total gas-liquid contact area and thus effectively improves the gas absorption rate and reaction efficiency.
[0049] Furthermore, the diameter of the L-shaped pipe gradually decreases from the inlet end 31 to the outlet end 32. By gradually decreasing the pipe diameter from the inlet end 31 to the outlet end 32, the gas velocity is continuously increased using the Venturi effect, ultimately forming a high-speed airflow at the outlet 30. This provides continuous flushing of the outlet 30, effectively preventing blockage by the solid products generated in the reaction; on the other hand, it allows for pressure accumulation and self-clearing in the event of minor blockage, significantly improving the equipment's anti-clogging capability and operational continuity, ensuring the stability and efficiency of the synthesis process. In addition, compared to a pipe with a constant diameter, the gradually decreasing pipe diameter design reduces the flow resistance loss of gas within the pipe, reducing the external gas supply pressure requirement while ensuring the flow velocity at the outlet end 32 meets the anti-clogging requirements, thereby reducing power consumption.
[0050] Specifically, the L-shaped pipe can be formed by interlocking multiple pipe sections 33 with progressively smaller diameters to create a sleeve-like structure. This "sleeve-like structure" design, by interlocking multiple pipe sections 33 with progressively smaller diameters, achieves a gradual decrease in pipe diameter. This not only realizes the aforementioned gas acceleration and anti-clogging functions but also brings the advantage of modularity, making manufacturing, installation, and disassembly simpler. When a section of the pipe becomes clogged or damaged due to long-term use, it can be replaced or cleaned individually, greatly reducing maintenance costs and time, and improving the convenience and economy of equipment maintenance. It should be noted that the specific design of the multiple pipe sections 33, and how adjacent pipe sections 33 are connected and how sealing is ensured, are not specifically limited in this invention; those skilled in the art can design and select according to the actual situation.
[0051] Specifically, the L-shaped pipe can also be a one-piece molded structure, with smooth transitions at pipe diameter changes via rounded corners. This one-piece molded structure, through seamless design and optimized arc-shaped flow channels, eliminates potential leaks at the source while effectively reducing gas flow resistance. Its smooth inner wall significantly reduces the risk of solid particle adhesion and media corrosion, thereby improving equipment reliability, enhancing anti-clogging performance, and extending pipe service life.
[0052] Furthermore, the outlet 30 is shaped like a crater, narrower at the top and wider at the bottom, with the larger end of the outlet 30 close to the L-shaped pipe. The crater shape of the outlet 30 serves two purposes: firstly, its sloping sidewalls reduce the space for solid particles to adhere and remain, making it difficult for the generated ammonium dihydrogen phosphate solid particles to accumulate at the outlet 30, thus forming a physical flow guide and preventing blockage. Secondly, the narrow-top-wide-bottom contraction-diffusion structure creates a converging and accelerating effect on the airflow, increasing the impact force of the exhaust and actively dispersing initial blockages; simultaneously, the diffused airflow prevents bubble aggregation, and combined with stirring, increases the gas-liquid contact area. The arc-shaped transition reduces liquid film resistance, improving absorption efficiency and reducing ammonia escape. It should be noted that the crater shape, with its narrow-top-wide-bottom and arc-shaped sidewall design, resembles a figure-eight shape.
[0053] Specifically, the air outlet 30 includes a first air outlet 301 located on one side of the L-shaped pipe and a second air outlet 302 located on the other side of the L-shaped pipe. The first air outlet 301 and the second air outlet 302 are staggered. This staggered arrangement of the first air outlet 301 and the second air outlet 302 can effectively expand the gas distribution range and eliminate the stirring dead zone. At the same time, the staggered arrangement can ensure the strength of the L-shaped pipe.
[0054] Furthermore, the reactor body 1 is made of enamel material to prevent corrosion by phosphoric acid.
[0055] Furthermore, the stirrer 2 is an anchor-type stirrer, which rotates at a speed of 10 rpm to 60 rpm in actual use. It should be noted that this anchor-type stirrer is not specifically limited in this invention; it may include a frame portion 20, stirring blades 21, and a drive mechanism 22. The frame portion 20 of the stirrer 2 is made of enamel to prevent corrosion by phosphoric acid, and its shape matches the inner wall contour of the reactor body 1. The stirring blades 21 are arranged along the frame portion 20 and configured in an anchor-type structure. The drive mechanism 22 is connected to the frame portion 20 and is used to drive the frame portion 20 to rotate.
[0056] The drive mechanism 22 may include a drive motor and a reducer that is connected to the drive motor. The output end of the reducer is connected to the frame part 20 to drive the frame part 20 to rotate.
[0057] The anchor-type agitator, with its frame section 20 designed to closely match the shape of the inner wall of the reactor body 1, can continuously scrape the entire inner wall of the reactor during rotation, effectively preventing solid materials from adhering and forming scale on the inner wall. The strong macroscopic circulating flow it generates eliminates reaction dead zones and breaks up and evenly disperses the bubbles released by the bottom gas distributor 3, greatly enhancing gas-liquid mass transfer and reaction efficiency. At the same time, it ensures that the solid particles generated by the reaction are always in a suspended state, thereby enhancing the system's anti-clogging ability and operational stability from a mixing perspective.
[0058] The present invention has been further described above with reference to specific embodiments. However, it should be understood that the specific description herein should not be construed as limiting the substance and scope of the present invention. Various modifications made by those skilled in the art to the above embodiments after reading this specification are all within the scope of protection of the present invention.
Claims
1. A reaction vessel for synthesizing ammonium dihydrogen phosphate, characterized in that: It includes: Reactor body; A stirrer is disposed within the reactor body; A gas distributor, which is an L-shaped pipe, is detachably installed inside the reactor body and located next to the agitator; the L-shaped pipe has an outlet near the agitator.
2. The reaction vessel for synthesizing ammonium dihydrogen phosphate according to claim 1, characterized in that: The L-shaped pipe has an air inlet and an air outlet; The inlet end of the L-shaped pipe extends to the outside of the reactor body, and the outlet end of the L-shaped pipe is located at the bottom of the reactor body.
3. The reaction vessel for synthesizing ammonium dihydrogen phosphate according to claim 2, characterized in that: The diameter of the L-shaped pipe decreases gradually from the inlet end to the outlet end.
4. The reaction vessel for synthesizing ammonium dihydrogen phosphate according to claim 3, characterized in that: The L-shaped pipe is composed of multiple pipe sections with successively decreasing diameters, which are nested together to form a sleeve-type structure.
5. The reaction vessel for synthesizing ammonium dihydrogen phosphate according to claim 3, characterized in that: The L-shaped pipe is a one-piece molded structure, and its diameter changes are smoothly transitioned by arc-shaped rounded corners.
6. The reaction vessel for synthesizing ammonium dihydrogen phosphate according to claim 1, characterized in that: The vent is shaped like a volcano, narrow at the top and wide at the bottom.
7. The reaction vessel for synthesizing ammonium dihydrogen phosphate according to claim 1, characterized in that: The L-shaped pipe is made of polytetrafluoroethylene.
8. The reaction vessel for synthesizing ammonium dihydrogen phosphate according to claim 1, characterized in that: The reactor body is made of enamel.
9. The reaction vessel for synthesizing ammonium dihydrogen phosphate according to claim 1, characterized in that: The agitator is an anchor-type agitator.
10. The reaction vessel for synthesizing ammonium dihydrogen phosphate according to claim 1, characterized in that: The frame of the stirrer is made of enamel.