A phosphorus oxychloride synthesis oxidation kettle
Patent Information
- Application Number
- CN202522114960.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-30
- Publication Date
- 2026-09-11
- Estimated Expiration
- 2035-09-30
AI Technical Summary
现有三氯氧磷合成氧化釜在实际应用中存在以下不足:传统氧化釜多采用单一桨叶搅拌,三氯化磷液体与氧气气体难以充分接触,易出现局部反应不完全的问题,导致产品收率降低,且未反应的氧气可能与产物混合形成安全隐患;反应释放的大量热量若无法及时导出,易导致釜内局部温度过高,引发副反应,影响产品纯度;现有换热结构多为外部夹套,换热面积有限,无法满足强放热需求;氧气通入方式多为单管直吹,气泡易团聚且分布范围窄,仅能在釜底局部区域与三氯化磷接触,导致气液传质效率低,进一步降低反应速率
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Figure CN224736288U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of chemical reaction equipment technology, specifically to a phosphorus oxychloride synthesis oxidation reactor. Background Technology
[0002] Phosphorus oxychloride is an important chemical raw material widely used in pesticides, pharmaceuticals, dyes, and electronic materials. Its synthesis typically involves an oxidation reaction of phosphorus trichloride and oxygen in an oxidation reactor. Existing phosphorus oxychloride synthesis oxidation reactors have the following shortcomings in practical applications: traditional reactors often use a single paddle stirrer, making it difficult for liquid phosphorus trichloride and gaseous oxygen to fully contact, leading to incomplete local reactions, reduced product yield, and the potential for unreacted oxygen to mix with the product, posing a safety hazard; if the large amount of heat released during the reaction cannot be dissipated in time, it can easily cause excessively high local temperatures within the reactor, triggering side reactions and affecting product purity; existing heat exchange structures are mostly external jackets with limited heat exchange area, unable to meet the demands of strong exothermic reactions; oxygen is often introduced via a single-pipe direct blowing method, resulting in bubble aggregation and a narrow distribution range, allowing contact with phosphorus trichloride only in a localized area at the bottom of the reactor, leading to low gas-liquid mass transfer efficiency and further reducing the reaction rate. Utility Model Content
[0003] In view of the above situation and to overcome the defects of the prior art, this utility model provides a phosphorus oxychloride synthesis oxidation kettle with efficient stirring, sufficient heat exchange, uniform gas distribution, convenient disassembly and assembly, and real-time temperature control.
[0004] The technical solution adopted by this utility model is as follows: This utility model provides a phosphorus oxychloride synthesis oxidation reactor, including a reactor body and a reactor cover detachably mounted on the top of the reactor body via flange bolts. The bottom of the reactor body is provided with support legs for support, and a discharge pipe is also provided. The discharge pipe is provided with a discharge valve. The reactor cover is provided with a feeding pipe, a tail gas discharge pipe, and a nitrogen replacement pipe. Each of the feeding pipe, tail gas discharge pipe, and nitrogen replacement pipe is provided with a corresponding control valve. It also includes a combined stirring mechanism, a composite heat exchange mechanism, and a gas distribution mechanism. The combined stirring mechanism is located on the reactor cover, the composite heat exchange mechanism is located on the reactor body, and the gas distribution mechanism is located at the bottom of the reactor body. The combined stirring mechanism includes a stirring motor, a stirring shaft, a semi-pipe open turbine propeller, and a sawtooth disc turbine propeller. The stirring motor is located on the reactor cover, the stirring shaft is located on the output shaft of the stirring motor and extends rotatably into the reactor body, the semi-pipe open turbine propeller is located on the stirring shaft, and the sawtooth disc turbine propeller is located at the bottom of the stirring shaft.
[0005] Preferably, the composite heat exchange mechanism includes an outer half-pipe jacket and an inner serpentine coil. The outer half-pipe jacket is wound around the outer wall of the vessel body. The cooling medium enters through the first input pipe end of the outer half-pipe jacket and exits through the first output pipe end of the outer half-pipe jacket. The inner serpentine coil is disposed inside the vessel body. The cooling medium enters through the second input pipe end of the inner serpentine coil and exits through the second output pipe end of the inner serpentine coil.
[0006] Preferably, the gas distribution mechanism includes an air inlet pipe and a gas distribution disk. The gas distribution disk is located at the bottom of the vessel and extends into the vessel body. The air inlet pipe of the gas distribution disk is detachably mounted on the air inlet pipe via a quick-release connector. The gas distribution disk is located below the serrated disc turbine propeller.
[0007] More preferably, the serrated disc turbine propeller is provided with a circular hole.
[0008] More preferably, the bottom wall inside the vessel is provided with a mounting column, and the gas distribution plate is provided with a mounting seat, which is detachably mounted on the mounting column by fixing bolts.
[0009] Preferably, the vessel lid is equipped with a temperature sensor, and the temperature measuring end of the temperature sensor is inserted into the reactants.
[0010] More preferably, the semi-pipe-type open turbine propellers are arranged in several groups at equal intervals along the axial direction of the stirring shaft.
[0011] The beneficial effects of this utility model by adopting the above structure are as follows:
[0012] Highly efficient stirring and uniform material mixing: The combined stirring mechanism adopts a layered design of "semi-tube open turbine propeller and serrated disc turbine propeller". The semi-tube open turbine propeller provides a strong radial flow while its semi-tube structure can effectively entrain and disperse gas, so that the fine oxygen bubbles are evenly distributed in the liquid phase and the residence time is extended. The serrated blades cut the bubbles and promote gas-liquid diffusion, achieving efficient gas-liquid mixing, greatly improving the reaction rate and product yield, and avoiding incomplete local reactions.
[0013] Sufficient heat exchange and precise temperature control: The composite heat exchange mechanism uses an external half-tube jacket and an internal serpentine coil for dual heat exchange, resulting in a significantly larger heat exchange area than the traditional single-jacket structure. This allows for the rapid removal of heat generated by strong exothermic reactions. Combined with real-time monitoring by temperature sensors, the temperature inside the reactor can be controlled within the optimal reaction range, reducing side reactions and improving product purity.
[0014] Uniform gas distribution and high mass transfer efficiency: The gas distribution disk can evenly distribute oxygen at the bottom of the vessel. Combined with the bubble cutting action of the serrated disc turbine, the oxygen forms tiny bubbles, which greatly increases the gas-liquid contact area. The bubbles diffuse upward under the stirring action, avoiding local enrichment, improving the gas-liquid mass transfer efficiency, and further promoting the complete reaction.
[0015] Easy to assemble and disassemble, and low maintenance cost: The gas distribution mechanism is detachably connected by quick-release connectors and fixing bolts. If the gas holes become blocked after long-term use, it can be quickly removed for cleaning or replacement without disassembling the entire vessel body. The vessel cover is detachable by flange bolts, which facilitates the maintenance and repair of the internal components and reduces downtime. Attached Figure Description
[0016] The accompanying drawings are provided to further illustrate the present invention and form part of the specification. They are used together with the embodiments of the present invention to explain the present invention, but do not constitute a limitation thereof. In the drawings:
[0017] Figure 1 This is a perspective view of an embodiment of the present utility model;
[0018] Figure 2 This is an exploded view of an embodiment of the present utility model;
[0019] Figure 3 This is a front view of an embodiment of the present utility model;
[0020] Figure 4 This is a left view of an embodiment of the present utility model;
[0021] Figure 5 This is a top view of an embodiment of the present utility model;
[0022] Figure 6 for Figure 4 A sectional view along section AA;
[0023] Figure 7 for Figure 6 A sectional view along section BB.
[0024] Figure 8 for Figure 2 Enlarged view of part A in the middle.
[0025] The components include: 1. vessel body; 2. vessel cover; 3. combined stirring mechanism; 4. composite heat exchange mechanism; 5. gas distribution mechanism; 11. support leg; 12. mounting column; 13. discharge pipe; 14. discharge valve; 21. feeding pipe; 22. exhaust gas discharge pipe; 23. nitrogen replacement pipe; 24. flange bolt; 25. temperature sensor; 31. stirring motor; 32. stirring shaft; 33. semi-pipe open turbine propeller; 34. serrated disc turbine propeller; 41. external semi-pipe jacket; 42. internal serrated coil; 51. air inlet pipe; 52. gas distribution disc; 53. quick-release connector; 54. mounting base; 55. fixing bolt; 341. round hole; 411. first input pipe; 412. first output pipe; 421. second input pipe; 422. second output pipe. Detailed Implementation
[0026] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present utility model. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present utility model without creative effort are within the protection scope of the present utility model.
[0027] In the description of this utility model, it should be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.
[0028] like Figures 1-8 As shown, this utility model discloses a phosphorus oxychloride synthesis oxidation reactor, including a reactor body 1 and a reactor cover 2 detachably mounted on the top of the reactor body 1 via flange bolts 24. The bottom of the reactor body 1 is provided with support legs 11 for supporting it, and a discharge pipe 13 is also provided. The discharge pipe 13 is provided with a discharge valve 14. The reactor cover 2 is provided with a feeding pipe 21, a tail gas discharge pipe 22, and a nitrogen replacement pipe 23. Each of the feeding pipe 21, the tail gas discharge pipe 22, and the nitrogen replacement pipe 23 is provided with a corresponding control valve. It also includes a combined stirring mechanism 3, a composite heat exchange mechanism 4, and a gas distribution mechanism 5. The combined stirring mechanism 3 is located on the reactor cover 2, the composite heat exchange mechanism 4 is located on the reactor body 1, and the gas distribution mechanism 5 is located at the bottom of the reactor body 1. The reactor cover 2 is provided with a temperature sensor 25, and the temperature measuring end of the temperature sensor 25 is inserted into the reactants.
[0029] The combined stirring mechanism 3 includes a stirring motor 31, a stirring shaft 32, a semi-pipe open turbine blade 33, and a serrated disc turbine blade 34. The stirring motor 31 is mounted on the vessel cover 2. The stirring shaft 32 is mounted on the output shaft of the stirring motor 31 and extends rotatably into the vessel body 1. The semi-pipe open turbine blade 33 is mounted on the stirring shaft 32, and the serrated disc turbine blade 34 is mounted at the bottom of the stirring shaft 32. Several sets of semi-pipe open turbine blades 33 are equidistantly arranged along the axial direction of the stirring shaft 32. The serrated disc turbine blade 34 is provided with a circular hole 341.
[0030] The composite heat exchange mechanism 4 includes an outer half-pipe jacket 41 and an inner serpentine coil 42. The outer half-pipe jacket 41 is wound around the outer wall of the vessel body 1. The cooling medium enters through the first input pipe 411 end of the outer half-pipe jacket 41 and exits through the first output pipe 412 end of the outer half-pipe jacket 41. The inner serpentine coil 42 is located inside the vessel body 1. The cooling medium enters through the second input pipe 421 end of the inner serpentine coil 42 and exits through the second output pipe 422 end of the inner serpentine coil 42.
[0031] The gas distribution mechanism 5 includes an inlet pipe 51 and a gas distribution plate 52. The gas distribution plate 52 is located at the bottom of the vessel body 1 and extends into the vessel body 1. The inlet pipe 51 of the gas distribution plate 52 is detachably mounted on the inlet pipe 51 via a quick-release connector 53. The gas distribution plate 52 is located below the serrated disc turbine propeller 34. An installation column 12 is provided on the bottom wall inside the vessel body 1. An installation seat 54 is provided on the gas distribution plate 52. The installation seat 54 is detachably mounted on the installation column 12 via fixing bolts 55.
[0032] In practical use, close the discharge valve 14, introduce nitrogen into the reactor body through the nitrogen replacement pipe 23 to replace the internal air, close the control valve on it after replacement, start the composite heat exchange mechanism 4, introduce cooling medium into the outer half-pipe jacket 41 and the internal serpentine coil 42 to pre-cool the reactor body; monitor the temperature inside the reactor through the temperature sensor 25, and prepare to add material after the temperature stabilizes.
[0033] A measured amount of phosphorus trichloride is added to the reactor through the feeding pipe 21. The stirring motor 31 is started, driving the stirring shaft 32, the semi-pipe turbine 33, and the serrated disc turbine 34 to rotate. Dry oxygen is introduced into the gas distribution plate 52 through the air inlet pipe 51. The oxygen is evenly discharged through the gas holes and cut into tiny bubbles by the serrated disc turbine 34, which then mix thoroughly with the phosphorus trichloride. The heat released during the reaction is discharged through the composite heat exchange mechanism 4, and the temperature sensor 25 monitors the temperature in real time. The temperature is controlled at 60-80℃ by adjusting the flow rate of the cooling medium or the oxygen introduction rate. The exhaust gas generated by the reaction is discharged to the exhaust gas treatment system through the exhaust gas discharge pipe 22. After the reaction is completed, the oxygen supply and stirring motor 31 are stopped, and the discharge valve 14 is opened. The reaction product, phosphorus oxychloride, is discharged through the discharge pipe 13 to the subsequent refining process. After discharge, cleaning liquid can be added through the feeding pipe 21, and stirring is started to clean the inside of the reactor. The cleaning wastewater is discharged through the discharge pipe 13. If the gas distribution plate 52 is clogged, after shutting down the equipment, unscrew the fixing bolts 55 and disassemble the quick-release connector 53 to remove the gas distribution plate 52 for cleaning.
[0034] In summary, the combined stirring mechanism 3 adopts a layered design of "semi-tube open turbine propeller 33 and serrated disc turbine propeller 34". The semi-tube open turbine propeller 33 provides strong radial flow while its semi-tube structure effectively entrains and disperses gas, ensuring uniform distribution of fine oxygen bubbles in the liquid phase and extending their residence time. The serrated blades cut the bubbles and promote gas-liquid diffusion, achieving efficient gas-liquid mixing, significantly improving the reaction rate and product yield, and avoiding incomplete local reactions. The composite heat exchange mechanism 4 uses a dual heat exchange system of an external semi-tube jacket 41 and an internal serpentine coil 42, resulting in a significantly larger heat exchange area than a traditional single-jacket structure. This allows for rapid heat removal from the strongly exothermic reaction. Combined with real-time monitoring by the temperature sensor 25, the temperature inside the reactor can be controlled within the optimal reaction range, reducing side reactions and improving product purity. The gas distribution disk 52 evenly distributes oxygen at the bottom of the vessel. Combined with the bubble-cutting action of the serrated disc turbine propeller 34, the oxygen forms tiny bubbles, significantly increasing the gas-liquid contact area. The bubbles diffuse upwards under stirring, preventing localized enrichment, improving gas-liquid mass transfer efficiency, and further promoting complete reaction. The gas distribution mechanism 5 is detachably connected to the fixing bolts 55 via quick-release connectors 53. If the gas vents become clogged after long-term use, it can be quickly removed for cleaning or replacement without disassembling the entire vessel. The vessel cover 2 is detachable via flange bolts 24, facilitating maintenance and repair of internal components and reducing downtime.
[0035] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.
[0036] The foregoing has shown and described the basic principles, main features, and advantages of this utility model. It will be apparent to those skilled in the art that this utility model is not limited to the details of the exemplary embodiments described above, and that it can be implemented in other specific forms without departing from the spirit or basic characteristics of this utility model. Therefore, the embodiments should be considered exemplary and non-limiting in all respects. The scope of this utility model is defined by the appended claims rather than the foregoing description, and thus all variations falling within the meaning and scope of equivalents of the claims are intended to be included within this utility model. No reference numerals in the claims should be construed as limiting the scope of the claims.
[0037] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. A phosphorus oxychloride synthesis oxidation reactor, comprising a reactor body (1) and a reactor cover (2) detachably mounted on the top of the reactor body (1) via flange bolts (24), wherein the bottom of the reactor body (1) is provided with support legs (11) for supporting it, and a discharge pipe (13) is also provided, wherein a discharge valve (14) is provided on the discharge pipe (13), and the reactor cover (2) is provided with a feeding pipe (21), a tail gas discharge pipe (22) and a nitrogen replacement pipe (23), wherein each of the feeding pipe (21), the tail gas discharge pipe (22) and the nitrogen replacement pipe (23) is provided with a corresponding control valve, characterized in that: It also includes a combined stirring mechanism (3), a composite heat exchange mechanism (4), and a gas distribution mechanism (5). The combined stirring mechanism (3) is located on the lid (2), the composite heat exchange mechanism (4) is located on the body (1), and the gas distribution mechanism (5) is located at the bottom of the body (1). The combined stirring mechanism (3) includes a stirring motor (31), a stirring shaft (32), a semi-pipe open turbine propeller (33), and a sawtooth disc turbine propeller (34). The stirring motor (31) is located on the lid (2), the stirring shaft (32) is located on the output shaft of the stirring motor (31) and extends rotatably into the body (1), the semi-pipe open turbine propeller (33) is located on the stirring shaft (32), and the sawtooth disc turbine propeller (34) is located at the bottom of the stirring shaft (32).
2. The phosphorus oxychloride synthesis oxidation kettle according to claim 1, characterized in that: The composite heat exchange mechanism (4) includes an outer half-pipe jacket (41) and an inner serpentine coil (42). The outer half-pipe jacket (41) is wrapped around the outer wall of the vessel body (1). The cooling medium enters through the first input pipe (411) end of the outer half-pipe jacket (41) and exits through the first output pipe (412) end of the outer half-pipe jacket (41). The inner serpentine coil (42) is located inside the vessel body (1). The cooling medium enters through the second input pipe (421) end of the inner serpentine coil (42) and exits through the second output pipe (422) end of the inner serpentine coil (42).
3. The phosphorus oxychloride synthesis oxidation kettle according to claim 1, characterized in that: The gas distribution mechanism (5) includes an air inlet pipe (51) and a gas distribution disk (52). The gas distribution disk (52) is located at the bottom of the vessel body (1) and extends into the vessel body (1). The air inlet pipe (51) of the gas distribution disk (52) is detachably mounted on the air inlet pipe (51) via a quick-release connector (53). The gas distribution disk (52) is located below the sawtooth disc turbine propeller (34).
4. The phosphorus oxychloride synthesis oxidation kettle according to claim 1, characterized in that: The sawtooth disc turbine propeller (34) is provided with a circular hole (341).
5. The phosphorus oxychloride synthesis oxidation kettle according to claim 3, wherein: The bottom wall inside the vessel body (1) is provided with a mounting column (12), and the gas distribution plate (52) is provided with a mounting seat (54). The mounting seat (54) is detachably mounted on the mounting column (12) by fixing bolts (55).
6. The phosphorus oxychloride synthesis oxidation kettle according to claim 1, wherein: The reactor lid (2) is equipped with a temperature sensor (25), and the temperature measuring end of the temperature sensor (25) is inserted into the reactants.
7. The phosphorus oxychloride synthesis oxidation kettle according to claim 1, wherein: The semi-pipe type open turbine propeller (33) is arranged in several groups at equal intervals along the axial direction of the stirring shaft (32).