A reaction kettle for producing aminotri(methylphosphonic acid)

Abstract

The utility model discloses a reaction kettle for amino trimethyl phosphonic acid production, the top of cauldron body is provided with upper seal plate, the bottom of cauldron body is provided with lower seal plate, and the outside of cauldron body and lower seal plate is provided with the clamping sleeve, one side of cauldron body is provided with the vacuumizing mouth, and dropwise adding jar is connected with upper seal plate, the top of dropwise adding jar is provided with the apron, the central position of apron upper surface is provided with the cylinder, and the piston rod of cylinder passes apron and is connected with the top of valve stem through the connecting sleeve, and the bottom of valve stem is provided with the valve plug, the bottom of dropwise adding jar is conical and is provided with dropwise adding pipe, and the top of dropwise adding pipe extends and is provided with flow control guide bush, and the lateral wall of flow control guide bush is provided with the through groove along the axial direction, and the valve plug is movably arranged in flow control guide bush, and the lateral wall of dropwise adding jar and below upper seal plate is provided with the vent hole, the utility model discloses reasonable structure, and the structure does not need to set up vacuum dropwise adding jar additionally, and does not need to carry out reflux again, saves the cost and improves production efficiency, and can realize vacuum dropwise adding formaldehyde simultaneously.

Description

Technical Field

[0001] This utility model relates to the field of reaction vessel technology, specifically to a reaction vessel for the production of aminotrimethylphosphonic acid. Background Technology

[0002] Aminotrimethylphosphonic acid generally refers to aminotrimethylenephosphonic acid. Solid aminotrimethylenephosphonic acid is readily soluble in water, with a melting point above 195℃ and a decomposition temperature of 200–212℃. Liquid products are also readily soluble in water. It is one of the commonly used organophosphonic acids, and it has a good scale inhibition effect on calcium carbonate.

[0003] Currently, the production of aminotrimethylphosphonic acid (ATMP) generally involves first vacuum-feeding metered liquid phosphoric acid, then adding solid ammonium chloride into the reactor through the manhole, and finally metering reverse osmosis water into the reactor via a flow meter. The mixture is heated to 80°C and stirred, then heated to 95°C and stabilized. The material is then transferred to a dropping vessel, where formaldehyde is introduced under vacuum and added dropwise at 95°C. After addition, the mixture is refluxed back into the reactor and kept at 100–105°C for 8 hours with stirring to ensure complete reaction. The generated hydrogen chloride, excess formaldehyde, and water are removed by evaporation. The crude ATMP product is then collected in a filter press, decolorized with activated carbon, filtered using a plate and frame filter press to remove impurities, and finally diluted with a specified amount of water to obtain the final product.

[0004] The existing process requires a separate dripping kettle for formaldehyde addition, which increases costs and reduces production efficiency. Therefore, there is an urgent need for an improved technology to solve this problem in the existing technology. Utility Model Content

[0005] The purpose of this invention is to provide a reaction vessel for the production of aminotrimethylphosphonic acid, so as to solve the problems mentioned in the background art.

[0006] To achieve the above objectives, this utility model provides the following technical solution: a reaction vessel for the production of aminotrimethylphosphonic acid, comprising a vessel body and a dripping mechanism;

[0007] The top of the vessel body is provided with an upper sealing plate, and the bottom of the vessel body is provided with a lower sealing plate. A motor is provided at the center of the upper surface of the upper sealing plate via a motor base. The output shaft of the motor is connected to the top of the stirring shaft via a coupling. A stirring paddle is provided at the bottom of the stirring shaft. The stirring paddle is rotatably mounted inside the vessel body. A jacket is provided outside the vessel body and the lower sealing plate. A vacuum port is provided on one side of the vessel body, and a discharge port is provided at the bottom of the lower sealing plate.

[0008] The dripping mechanism includes a dripping tank connected to an upper sealing plate. A cover plate is provided at the top of the dripping tank. A cylinder is provided at the center of the upper surface of the cover plate. The piston rod of the cylinder passes through the cover plate and is connected to the top of a valve rod through a connecting sleeve. A valve plug is provided at the bottom of the valve rod. The bottom of the dripping tank is conical and is provided with a dripping tube. A flow control guide sleeve extends from the top of the dripping tube. A through groove is provided on the side wall of the flow control guide sleeve along the axial direction. The valve plug is movably disposed in the flow control guide sleeve. A vent hole is provided on the side wall of the dripping tank below the upper sealing plate.

[0009] Preferably, the present invention provides a reaction vessel for the production of aminotrimethylphosphonic acid, wherein the upper sealing plate is further provided with a manhole, a thermometer port, a pressure gauge port, a level gauge port, a liquid phosphorous acid feed port and a reverse osmosis water feed port on its upper surface.

[0010] Preferably, the present invention provides a reaction vessel for the production of aminotrimethylphosphonic acid, wherein a formaldehyde inlet is provided on the upper surface of the cover plate.

[0011] Preferably, the present invention provides a reaction vessel for the production of aminotrimethylphosphonic acid, wherein a heat exchange medium inlet is provided at the bottom of the jacket, and a heat exchange medium outlet is provided on one side of the upper part of the jacket.

[0012] Preferably, the present invention provides a reaction vessel for the production of aminotrimethylphosphonic acid, wherein the jacket is provided with several support seats.

[0013] Preferably, the reaction vessel for the production of aminotrimethylphosphonic acid provided by this utility model is provided with sealing elements at the joint between the upper sealing plate and the stirring shaft, and at the joint between the cover plate and the piston rod of the cylinder.

[0014] Preferably, the present invention provides a reaction vessel for the production of aminotrimethylphosphonic acid, wherein the manhole is provided with a sealing cover.

[0015] Compared with the prior art, the beneficial effects of this utility model are:

[0016] The upper sealing plate is connected to a dripping tank. A cylinder is installed on the upper surface of the cover plate of the dripping tank. A flow control guide sleeve is installed at the top of the dripping tube at the bottom of the dripping tank. The piston rod of the cylinder is connected to the valve rod. A valve plug is installed at the bottom of the valve rod, which cooperates with the through groove on the side of the flow control guide sleeve, thereby controlling the formaldehyde dripping rate. A vent is opened on the side wall of the dripping tank to ensure that there is no pressure difference between the dripping tank and the vessel body when under vacuum, thus realizing the dripping of formaldehyde. This structure eliminates the need for a separate vacuum dripping tank and reflux, saving costs and improving production efficiency, while also enabling vacuum dripping of formaldehyde. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the structure of this utility model;

[0018] Figure 2 This is a schematic cross-sectional view of the present invention.

[0019] Figure 3 This is a schematic diagram of the dropping tank structure;

[0020] Figure 4 This is an enlarged structural diagram of the dripping tank located at the flow control guide sleeve.

[0021] In the diagram: 1. Reactor body; 2. Upper sealing plate; 3. Lower sealing plate; 4. Motor; 5. Stirring shaft; 6. Stirring paddle; 7. Jacket; 8. Vacuum port; 9. Discharge port; 10. Dropping tank; 11. Cover plate; 12. Cylinder; 13. Valve stem; 14. Valve plug; 15. Dropping tube; 16. Flow control guide sleeve; 17. Through groove; 18. Vent hole; 19. Manhole; 20. Thermometer port; 21. Pressure gauge port; 22. Liquid level gauge port; 23. Liquid phosphorous acid inlet; 24. Reverse osmosis water inlet; 25. Formaldehyde inlet; 26. Heat exchange medium inlet; 27. Heat exchange medium outlet; 28. Support base; 29. ​​Sealing cover. Detailed Implementation

[0022] 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.

[0023] 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.

[0024] Please see Figure 1-4 This utility model provides a technical solution: a reaction vessel for the production of aminotrimethylphosphonic acid, including a vessel body 1 and a dripping mechanism;

[0025] The upper sealing plate 2 is provided at the top of the vessel body 1, and the lower sealing plate 3 is provided at the bottom of the vessel body 1. A motor 4 is provided at the center of the upper surface of the upper sealing plate 2 through a motor base. The output shaft of the motor 4 is connected to the top of the stirring shaft 5 through a coupling. A stirring paddle 6 is provided at the bottom of the stirring shaft 5. The stirring paddle 6 is rotatably installed inside the vessel body 1. A jacket 7 is provided outside the vessel body 1 and the lower sealing plate 3. A heat exchange medium inlet 26 is provided at the bottom of the jacket 7, and a heat exchange medium outlet 27 is provided on one side of the upper part of the jacket 7. The heat exchange medium enters or leaves the jacket 7 through the heat exchange medium inlet 26 and the heat exchange medium outlet 27, thereby controlling the internal temperature of the vessel body 1. Several support seats 28 are provided outside the jacket 7 to support and fix the reactor. A vacuum port 8 is provided on one side of the vessel body 1, and a discharge port 9 is provided at the bottom of the lower sealing plate 3.

[0026] The upper surface of the upper sealing plate 2 is also provided with a manhole 19, a thermometer port 20, a pressure gauge port 21, a level gauge port 22, a liquid phosphoric acid inlet 23, and a reverse osmosis water inlet 24. The manhole 19 is used to check the working condition inside the vessel 1 and to add solid ammonium chloride. The thermometer port 20 is used to install a thermometer to monitor the temperature inside the vessel 1. The pressure gauge port 21 is used to install a pressure gauge to monitor the pressure inside the vessel 1. The level gauge port 22 is used to install a level gauge to monitor the liquid level inside the vessel 1. The liquid phosphoric acid inlet 23 is used to add liquid phosphoric acid. The reverse osmosis water inlet 24 is used to add reverse osmosis water. The manhole 19 is provided with a sealing cover 29 to ensure the sealing of the inside of the vessel 1 after the addition of solid ammonium chloride is completed.

[0027] The dripping mechanism includes a dripping tank 10, which is connected to an upper sealing plate 2. A cover plate 11 is located at the top of the dripping tank 10. A cylinder 12 is positioned at the center of the upper surface of the cover plate 11. A formaldehyde inlet 25 is located on the upper surface of the cover plate 11 for adding formaldehyde. The piston rod of the cylinder 12 passes through the cover plate 11 and is connected to the top of a valve rod 13 via a connecting sleeve. Sealing elements are provided at the junctions of the upper sealing plate 2 and the stirring shaft 5, and at the junctions of the cover plate 11 and the piston rod of the cylinder 12, to ensure... The sealing plate 2 and the stirring shaft 5 are designed to prevent air leakage at their joints, and the cover plate 11 and the piston rod of the cylinder 12 are designed to prevent air leakage at their joints. A valve plug 14 is provided at the bottom of the valve rod 13. The bottom of the dripping tank 10 is conical and is provided with a dripping tube 15. A flow control guide sleeve 16 is provided at the top of the dripping tube 15. A through groove 17 is provided on the side wall of the flow control guide sleeve 16 along the axial direction. The valve plug 14 is movably disposed in the flow control guide sleeve 16. A vent hole 18 is provided on the side wall of the dripping tank 10 and below the upper sealing plate 2.

[0028] Installation method and operating principle: Pass the dripping tank 10 through the upper sealing plate 2 and weld it to the upper sealing plate 2. Install the cylinder 12 on the cover plate 11 and pass the piston rod of the cylinder 12 through the cover plate 11. Connect the top of the valve rod 13 to the piston rod of the cylinder 12 through the connecting sleeve. Install the valve plug 14 at the bottom of the valve rod 13 and insert the valve plug 14 into the flow control guide sleeve 16 to complete the installation of the dripping tank 10. Before use, install the thermometer inlet 20 and seal it. Install the pressure gauge inlet 21 and seal it. Install the level gauge inlet 22 and seal it. Connect the liquid phosphoric acid inlet 23 to the liquid phosphoric acid storage tank through a valve. Connect the reverse osmosis water inlet 24 to the reverse osmosis water storage tank through a valve. Connect the formaldehyde inlet 25 to the formaldehyde storage tank through a valve. Connect the vacuum port 8 to the vacuum device through a pipe. During operation, liquid phosphoric acid is added into the reactor body 1 through the liquid phosphoric acid inlet 23 and the corresponding valve is closed. Reverse osmosis water is added into the reactor body 1 through the reverse osmosis water inlet 24 and the corresponding valve is closed. Solid ammonium chloride is added into the reactor body 1 through the manhole 19, and then the sealing cap 29 is covered and locked. Steam is introduced into the jacket 7 to heat to 80°C. The motor 4 is started, and the motor 4 drives the stirring paddle 6 through the stirring shaft 5 to start stirring. After the temperature rises to 95°C, formaldehyde is first added into the dripping tank 10 through the formaldehyde inlet 25 and the corresponding valve is closed. Vacuum is drawn into the reactor body 1 through the vacuum port 8. After stabilization, the piston rod of the cylinder 12 moves upward, and the valve plug 14 moves upward along the flow control guide sleeve 16 until the lower part of the through groove 17 opens. Formaldehyde passes through the through groove 17 and drips into the reactor body 1 through the dripping pipe 15. Formaldehyde is added at 95°C for 3.5 to 4 hours. Next, the temperature is raised to 100-105℃ through jacket 7, and maintained at this temperature while stirring for 8 hours to allow the materials to react fully, resulting in a mixed liquid of aminotrimethylphosphonic acid. After being discharged from the outlet 9 at the bottom of the reactor body 1, impurities such as hydrogen chloride, excess formaldehyde, and water are removed by steam rinsing. The crude aminotrimethylphosphonic acid is then collected in a filter press, where activated carbon is added for decolorization, and the mixture is filtered using a plate and frame filter press to remove impurities. Finally, it is diluted with a specified amount of water to obtain the finished product. This utility model has a reasonable structure. The upper sealing plate 2 is connected to the dripping tank 10. The upper surface of the cover plate 11 of the dripping tank 10 is provided with a cylinder 12. The top of the dripping tube 15 at the bottom of the dripping tank 10 is provided with a flow control guide sleeve 16. The piston rod of the cylinder 12 is connected to the valve rod 13. The bottom end of the valve rod 13 is provided with a valve plug 14, which cooperates with the through groove 17 on the side of the flow control guide sleeve 16, thereby realizing the control of the formaldehyde dripping rate. The side wall of the dripping tank 10 is opened with a vent hole 18 to ensure that there is no pressure difference between the dripping tank 10 and the vessel body 1 when under vacuum, thereby realizing the dripping of formaldehyde. This structure does not require the separate vacuum dripping tank 10, nor does it require reflux, saving costs and improving production efficiency, while realizing vacuum dripping of formaldehyde.

[0029] Any aspects of this utility model not described in detail are well-known technologies to those skilled in the art.

[0030] 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 the production of aminotrimethylphosphonic acid, characterized in that: Includes the vessel body (1) and the dripping mechanism; The top of the vessel body (1) is provided with an upper sealing plate (2), the bottom of the vessel body (1) is provided with a lower sealing plate (3), a motor (4) is provided at the center of the upper surface of the upper sealing plate (2) through a motor seat, the output shaft of the motor (4) is connected to the top of the stirring shaft (5) through a coupling, a stirring paddle (6) is provided at the bottom of the stirring shaft (5), the stirring paddle (6) is rotatably disposed inside the vessel body (1), a jacket (7) is provided outside the vessel body (1) and the lower sealing plate (3), a vacuum port (8) is provided on one side of the vessel body (1), and a discharge port (9) is provided at the bottom of the lower sealing plate (3); The dripping mechanism includes a dripping tank (10), which is connected to an upper sealing plate (2). A cover plate (11) is provided at the top of the dripping tank (10). A cylinder (12) is provided at the center of the upper surface of the cover plate (11). The piston rod of the cylinder (12) passes through the cover plate (11) and is connected to the top of the valve rod (13) through a connecting sleeve. A valve plug (14) is provided at the bottom of the valve rod (13). The bottom of the dripping tank (10) is conical and is provided with a dripping tube (15). A flow control guide sleeve (16) extends from the top of the dripping tube (15). A through groove (17) is provided on the side wall of the flow control guide sleeve (16) along the axial direction. The valve plug (14) is movably disposed in the flow control guide sleeve (16). A vent hole (18) is provided on the side wall of the dripping tank (10) and below the upper sealing plate (2).

2. The reaction vessel for producing aminotrimethylphosphonic acid according to claim 1, characterized in that: The upper surface of the upper sealing plate (2) is also provided with a manhole (19), a thermometer port (20), a pressure gauge port (21), a level gauge port (22), a liquid phosphorous acid feed port (23), and a reverse osmosis water feed port (24).

3. The reaction vessel for producing aminotrimethylphosphonic acid according to claim 1, characterized in that: The upper surface of the cover plate (11) is provided with a formaldehyde inlet (25).

4. The reaction vessel for producing aminotrimethylphosphonic acid according to claim 1, characterized in that: The jacket (7) is provided with a heat exchange medium inlet (26) at the bottom and a heat exchange medium outlet (27) on one side of the upper part of the jacket (7).

5. The reaction vessel for producing aminotrimethylphosphonic acid according to claim 1, characterized in that: The jacket (7) is provided with several support seats (28) on its outside.

6. The reaction vessel for producing aminotrimethylphosphonic acid according to claim 1, characterized in that: Sealing elements are provided at the joint between the upper sealing plate (2) and the stirring shaft (5), and at the joint between the cover plate (11) and the piston rod of the cylinder (12).

7. The reaction vessel for producing aminotrimethylphosphonic acid according to claim 2, characterized in that: The manhole (19) is provided with a sealing cover (29).

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