A phosphorus trichloride vapor preparation reactor

By installing an annular gas distribution hood and a stirring paddle at the bottom of the reactor, the problem of uneven contact between chlorine gas and the mixed solution was solved, thereby improving the reaction efficiency and production efficiency of phosphorus trichloride steam preparation.

CN224486014UActive Publication Date: 2026-07-14NANTONG UNIPHOS CHEM CO LTD

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
NANTONG UNIPHOS CHEM CO LTD
Filing Date
2025-07-11
Publication Date
2026-07-14

AI Technical Summary

Technical Problem

In existing phosphorus trichloride vapor preparation reactors, the chlorine gas does not contact the mixed solution evenly, resulting in low reaction efficiency.

Method used

An annular gas distribution hood is installed at the bottom of the reactor body. The hood is densely covered with gas outlet holes and is uniformly stirred by a stirring paddle. Combined with jacket cooling, the reaction efficiency is improved.

Benefits of technology

This method achieves uniform contact between chlorine gas, yellow phosphorus, and phosphorus trichloride mother liquor, improving reaction efficiency and production efficiency while preventing solution accumulation.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses a phosphorus trichloride vapor preparation reation kettle, the kettle body top is provided with the kettle cover, the central position of kettle cover upper surface is provided with motor through motor base, and the output shaft of motor is connected with the stirring shaft top end through the shaft coupling, and the stirring shaft bottom is set up in the kettle body inside and is equipped with the stirring oar, the kettle cover upper surface still is provided with the steam export, and the central position of kettle body bottom is provided with the discharge gate, and the bottom surface of kettle body inside is provided with the air distribution cover, and the central hole is seted up in the air distribution cover central position, and the discharge gate is located in the central hole of air distribution cover, and the air distribution cover is densely covered with the air outlet, and a plurality of liquid outlet holes are seted up in the air distribution cover inboard, and the air inlet is connected with the air inlet connection pipe bottom end on one side of kettle body bottom, and the utility model discloses reasonable structure, and through the air distribution cover makes dry chlorine and yellow phosphorus and the mixed solution of phosphorus trichloride mother liquor even contact, and the reaction efficiency and effect between chlorine and yellow phosphorus and the mixed solution of phosphorus trichloride mother liquor are improved greatly, thereby improve the production efficiency.
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Description

Technical Field

[0001] This utility model relates to the field of reaction vessel technology, specifically to a reaction vessel for preparing phosphorus trichloride vapor. Background Technology

[0002] In the production process of 1-hydroxyethylidene-1,1-diphosphonic acid, the first step is to obtain phosphorus trichloride vapor, then distill the phosphorus trichloride vapor, then add water and acetic acid, and add phosphorus trichloride dropwise and mix them together to react. Finally, hydrolysis is performed to obtain a mixed solution of 1-hydroxyethylidene-1,1-diphosphonic acid and acetic acid. After recovering the acetic acid, crude 1-hydroxyethylidene-1,1-diphosphonic acid is obtained.

[0003] The preparation of phosphorus trichloride vapor generally involves passing dry chlorine gas into a mixed solution of yellow phosphorus and phosphorus trichloride, and producing phosphorus trichloride vapor through an exothermic reaction. Currently, the chlorine gas in the reaction vessel for preparing phosphorus trichloride vapor is generally introduced through an inlet pipe inside the vessel body that extends to the bottom. This structure of introducing chlorine gas results in uneven contact between the chlorine gas and the mixed solution, leading to a need to improve the reaction efficiency and effect. Therefore, an improved technology is urgently needed to solve this problem existing in the current technology. Utility Model Content

[0004] The purpose of this invention is to provide a phosphorus trichloride vapor preparation reactor to solve the problems mentioned in the background art.

[0005] To achieve the above objectives, this utility model provides the following technical solution: a phosphorus trichloride steam preparation reactor, comprising a reactor body, a reactor cover, and a gas distribution hood. The reactor body is topped with a reactor cover, and a motor is mounted on the center of the upper surface of the reactor cover via a motor mount. The output shaft of the motor is connected to the top of a stirring shaft via a coupling. The bottom end of the stirring shaft is located inside the reactor body and is fitted with a stirring paddle, which rotates within the reactor body. A steam outlet is also provided on the upper surface of the reactor cover. A discharge port is located at the center of the bottom of the reactor body. A gas distribution hood is located on the bottom surface of the reactor body. A central hole is formed at the center of the gas distribution hood, and the discharge port is located within the central hole of the gas distribution hood. A cavity is formed between the gas distribution hood and the inner wall of the reactor body. The gas distribution hood is densely covered with gas outlet holes, and several liquid drainage holes are formed on the inner side of the gas distribution hood. An air inlet is provided on one side of the bottom of the reactor body. The air inlet is interconnected with the cavity of the gas distribution hood and is connected to the bottom end of an air inlet connecting pipe.

[0006] Preferably, the present invention provides a phosphorus trichloride steam preparation reactor, wherein the reactor body is surrounded by a jacket, the jacket is provided with a cooling medium inlet and a cooling medium outlet, and the jacket is provided with several supports around its periphery.

[0007] Preferably, the present invention provides a phosphorus trichloride steam preparation reactor, wherein the upper surface of the reactor cover is further provided with a first feed inlet, a second feed inlet, a level gauge port, a manhole, a thermometer port, and a pressure gauge port.

[0008] Preferably, the present invention provides a phosphorus trichloride steam preparation reactor, wherein the stirring paddle includes a connecting sleeve, a U-shaped paddle and an orifice plate, the bottom of the connecting sleeve is connected to the middle position of the U-shaped paddle, and an orifice plate is provided between the U-shaped paddle and the connecting sleeve.

[0009] Preferably, in the phosphorus trichloride steam preparation reactor provided by this utility model, the horizontal height of the top end of the gas inlet connecting pipe is greater than the horizontal height of the top end of the reactor body, and one side of the gas inlet connecting pipe is connected to the side wall of the reactor body through a connecting rod.

[0010] Compared with the prior art, the beneficial effects of this utility model are:

[0011] The bottom of the reactor body is equipped with a ring-shaped gas distribution hood, which is densely covered with gas outlet holes. The gas distribution hood allows the dry chlorine gas to come into uniform contact with the mixture of yellow phosphorus and phosphorus trichloride mother liquor, which greatly improves the reaction efficiency and effect between the mixture of chlorine gas and yellow phosphorus and phosphorus trichloride mother liquor, thereby improving production efficiency. In addition, the gas distribution hood is equipped with a drain hole on the inside to prevent the solution from accumulating inside the gas distribution hood. Attached Figure Description

[0012] Figure 1 This is a schematic diagram of the structure of this utility model;

[0013] Figure 2 For the appendix Figure 1 Enlarged structural diagram of point A in the middle;

[0014] Figure 3 This is a top view of the internal structure of the vessel.

[0015] Figure 4 This is a schematic diagram of the appearance and structure of this utility model.

[0016] In the diagram: 1. Vessel body; 2. Vessel cover; 3. Gas distribution hood; 4. Motor base; 5. Motor; 6. Stirring shaft; 7. Stirring paddle; 8. Steam outlet; 9. Discharge port; 10. Center hole; 11. Gas outlet; 12. Liquid drain hole; 13. Air inlet; 14. Air inlet connecting pipe; 15. Jacket; 16. Cooling medium inlet; 17. Cooling medium outlet; 18. Support; 19. First feed inlet; 20. Second feed inlet; 21. Liquid level gauge port; 22. Manhole; 23. Thermometer port; 24. Pressure gauge port; 25. Connecting rod; 701. Connecting sleeve; 702. U-shaped paddle; 703. Orifice plate. Detailed Implementation

[0017] The technical solution of this utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. 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.

[0018] It should be noted that in the description of this utility model, the terms "inner", "outer", "upper", "lower", "both sides", "one end", "the other end", "left", "right", 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.

[0019] Please see Figure 1-4This utility model provides a technical solution: a phosphorus trichloride steam preparation reactor, including a reactor body 1, a reactor cover 2, and a gas distribution hood 3. The reactor cover 2 is provided at the top of the reactor body 1. A motor 5 is provided at the center of the upper surface of the reactor cover 2 via a motor base 4. The output shaft of the motor 5 is connected to the top of a stirring shaft 6 via a coupling. The bottom end of the stirring shaft 6 is located inside the reactor body 1 and is equipped with a stirring paddle 7. The stirring paddle 7 is rotatably located inside the reactor body 1. A steam outlet 8 is also provided on the upper surface of the reactor cover 2. A first feed inlet 19 and a second feed inlet 2 are also provided on the upper surface of the reactor cover 2. 0. Level gauge port 21, manhole 22, thermometer port 23, and pressure gauge port 24; first feed port 19 and second feed port 20 are used for feeding the mixture of yellow phosphorus and water and the mother liquor of phosphorus trichloride, respectively; level gauge port 21 is used to install a level gauge for level monitoring; thermometer port 23 and pressure gauge port 24 are used to install a thermometer and a pressure gauge, respectively, to monitor the temperature and pressure inside the vessel 1; a discharge port 9 is provided at the center of the bottom of the vessel 1; a gas distribution hood 3 is provided on the bottom surface inside the vessel 1; and a central opening is provided at the center of the gas distribution hood 3. Hole 10 and outlet 9 are located inside the center hole 10 of the gas distribution hood 3. A cavity is formed between the gas distribution hood 3 and the inner wall of the vessel body 1. The gas distribution hood 3 is densely covered with air outlet holes 11. Several drainage holes 12 are opened on the inner side of the gas distribution hood 3. An air inlet 13 is provided on one side of the bottom of the vessel body 1. The air inlet 13 is interconnected with the cavity of the gas distribution hood 3. The air inlet 13 is connected to the bottom end of the air inlet connecting pipe 14. The horizontal height of the top end of the air inlet connecting pipe 14 is greater than the horizontal height of the top end of the vessel body 1. Although the outer end of the air inlet connecting pipe 14 is connected to a one-way valve, raising the top of the air inlet connecting pipe 14... The height of the part is designed to ensure that the mixture inside the vessel 1 will not flow back from the top of the inlet connection pipe 14 when the one-way valve is damaged. One side of the inlet connection pipe 14 is connected to the side wall of the vessel 1 through the connecting rod 25 to ensure the stability of the inlet connection pipe 14. The vessel 1 is surrounded by a jacket 15, which is provided with a cooling medium inlet 16 and a cooling medium outlet 17. Several supports 18 are provided around the jacket 15. The jacket 15 is used to cool the inside of the vessel 1 during the reaction of the mixture of chlorine gas, yellow phosphorus and phosphorus trichloride mother liquor.

[0020] The stirring paddle 7 includes a connecting sleeve 701, a U-shaped paddle 702, and an orifice plate 703. The bottom of the connecting sleeve 701 is connected to the middle of the U-shaped paddle 702. An orifice plate 703 is provided between the U-shaped paddle 702 and the connecting sleeve 701. Stirring is carried out through the orifice plate 703 with dense holes to improve reaction efficiency.

[0021] Installation method and operating principle: Connect the stirring paddle 7 to the bottom end of the stirring shaft 6 via the connecting sleeve 701 and secure it with bolts. Weld the gas distribution hood 3 to the bottom of the vessel body 1, ensuring that the center hole 10 of the gas distribution hood 3 aligns with the outlet 9. Place the stirring paddle 7 inside the vessel body 1 and connect the vessel cover 2 to the top of the vessel body 1 to complete the installation. During operation, the mixture of yellow phosphorus and water and the mother liquor of phosphorus trichloride are fed into the reactor body 1 through the first feed port 19 and the second feed port 20, respectively. The motor 5 is started, and the motor 5 drives the stirring paddle 7 to rotate through the stirring shaft 6, thereby achieving the mixing of yellow phosphorus and the mother liquor of phosphorus trichloride. At the same time, dry chlorine gas is introduced into the gas distribution hood 3 through the gas inlet connection pipe 14 from the gas inlet port 13. The chlorine gas comes into contact with the mixed solution through the various gas outlets 11 of the gas distribution hood 3. During the process, phosphorus trichloride vapor is generated and discharged from the steam outlet 8 of the reactor cover 2. The reaction is exothermic, and cooling water enters the jacket 15 from the cooling medium inlet 16 to cool the side wall of the reactor body 1. This utility model has a reasonable structure. The bottom of the vessel body 1 is provided with an annular gas distribution hood 3. The gas distribution hood 3 is densely covered with gas outlet holes 11. The gas distribution hood 3 allows the dry chlorine gas and the mixture of yellow phosphorus and phosphorus trichloride mother liquor to come into uniform contact, which greatly improves the reaction efficiency and effect between the mixture of chlorine gas and yellow phosphorus and phosphorus trichloride mother liquor, thereby improving production efficiency. In addition, the gas distribution hood 3 is provided with a drain hole 12 on the inner side to prevent the solution from accumulating in the gas distribution hood 3.

[0022] Any aspects of this utility model not described in detail are well-known technologies to those skilled in the art.

[0023] Finally, it should be noted that the above specific embodiments are only used to illustrate the technical solution of this utility model and not to limit it. Although this utility model has been described in detail with reference to the embodiments, those skilled in the art should understand that modifications and equivalent substitutions can be made to the technical solution of this utility model without departing from the spirit and scope of the technical solution of this utility model, and all such modifications and substitutions should be covered within the scope of the claims of this utility model.

Claims

1. A reaction vessel for preparing phosphorus trichloride vapor, characterized in that: The vessel includes a vessel body (1), a vessel lid (2), and a gas distribution hood (3). The vessel body (1) is topped with a vessel lid (2). A motor (5) is mounted on the center of the upper surface of the vessel lid (2) via a motor mount (4). The output shaft of the motor (5) is connected to the top of a stirring shaft (6) via a coupling. The bottom of the stirring shaft (6) is located inside the vessel body (1) and is fitted with a stirring paddle (7). The stirring paddle (7) is rotatably mounted inside the vessel body (1). A steam outlet (8) is also provided on the upper surface of the vessel lid (2). A discharge port (9) is located at the center of the bottom of the vessel body (1). The bottom surface inside the vessel is provided with a gas distribution hood (3). The gas distribution hood (3) has a central hole (10) at its center. The discharge port (9) is located inside the central hole (10) of the gas distribution hood (3). A cavity is formed between the gas distribution hood (3) and the inner wall of the vessel body (1). The gas distribution hood (3) is densely covered with air outlet holes (11). Several drain holes (12) are opened on the inner side of the gas distribution hood (3). An air inlet (13) is provided on one side of the bottom of the vessel body (1). The air inlet (13) is connected to the cavity of the gas distribution hood (3). The air inlet (13) is connected to the bottom end of the air inlet connecting pipe (14).

2. The phosphorus trichloride steam preparation reactor according to claim 1, characterized in that: The vessel body (1) is surrounded by a jacket (15), which has a cooling medium inlet (16) and a cooling medium outlet (17). Several supports (18) are provided around the jacket (15).

3. The phosphorus trichloride steam preparation reactor according to claim 1, characterized in that: The upper surface of the vessel lid (2) is also provided with a first feed inlet (19), a second feed inlet (20), a level gauge inlet (21), a manhole (22), a thermometer inlet (23), and a pressure gauge inlet (24).

4. The phosphorus trichloride steam preparation reactor according to claim 1, characterized in that: The stirring paddle (7) includes a connecting sleeve (701), a U-shaped paddle (702) and a perforated plate (703). The bottom of the connecting sleeve (701) is connected to the middle position of the U-shaped paddle (702), and a perforated plate (703) is provided between the U-shaped paddle (702) and the connecting sleeve (701).

5. The phosphorus trichloride steam preparation reactor according to claim 1, characterized in that: The horizontal height of the top end of the air inlet connecting pipe (14) is greater than the horizontal height of the top end of the vessel body (1), and one side of the air inlet connecting pipe (14) is connected to the side wall of the vessel body (1) through a connecting rod (25).