Production device for continuously synthesizing tributyl phosphate

Abstract

The utility model discloses a production device for continuously synthesizing tributyl phosphate, and relates to the technical field of preparation of tributyl phosphate. The phosphorus oxychloride and butanol mixed reaction device comprises a base, two supporting plates are fixedly installed at the top of the base, a first reaction tank and a second reaction tank are fixedly arranged between the two supporting plates in a penetrating mode, the first reaction tank is located above the second reaction tank, and the first reaction tank is used for storage and mixed reaction of phosphorus oxychloride and butanol. According to the utility model, the production efficiency and the stability of the tributyl phosphate are obviously improved through the continuous production design; the synchronous stirring of the stirring assembly ensures the sufficient mixing of the solution, and the reaction efficiency and uniformity are improved; air and by-products are effectively exhausted by the air exhaust assembly, so that the vacuum state of the reaction environment is guaranteed, and the product quality is optimized; a stable temperature environment is provided for the reaction through the synergistic effect of the temperature adjusting pipe and the heat preservation shell; and the overall design ensures the uniformity and stability of the reaction, and the use effect is good.

Description

Technical Field

[0001] This invention belongs to the field of tributyl phosphate preparation technology, and in particular relates to a production apparatus for continuous synthesis of tributyl phosphate. Background Technology

[0002] Tributyl phosphate, as an important organic compound, has wide applications in many fields, such as as an extractant, solvent, and flame retardant. Tributyl phosphate is generally synthesized by direct esterification of butanol and phosphorus oxychloride. During the synthesis of tributyl phosphate, the generated hydrogen chloride will continue to react with n-butanol in a side reaction, producing dibutyl ether and chlorobutane, which reduces the utilization rate of n-butanol and results in a low product yield.

[0003] Therefore, existing tributyl phosphate production equipment often suffers from the following problems during use:

[0004] Traditional methods for synthesizing tributyl phosphate typically employ a batch production approach, where all reaction steps are completed in a single reactor. This approach suffers from poor production continuity, low production efficiency, high energy consumption, and long reaction times.

[0005] Meanwhile, in continuous production, the continuous addition of reactants and the continuous discharge of products are key to achieving high-efficiency production. However, some existing continuous production equipment cannot effectively mix reactants during the reaction process, resulting in incomplete reactions. Some equipment cannot effectively extract air and by-product gases during the reaction process, affecting reaction efficiency and product quality. Some equipment also has deficiencies in temperature control, failing to provide a suitable temperature environment for the reaction. Utility Model Content

[0006] The purpose of this invention is to provide a production apparatus for the continuous synthesis of tributyl phosphate. In this invention, the continuous production design significantly improves the production efficiency and stability of tributyl phosphate; the synchronous stirring of the stirring assembly ensures thorough mixing of the solution, improving reaction efficiency and uniformity; the vacuum assembly effectively removes air and byproducts, ensuring a vacuum environment for the reaction and optimizing product quality; the synergistic effect of the temperature control tube and the insulation shell provides a stable temperature environment for the reaction; the design of the first and second infusion pipes and their branch pipes enables the uniform addition of reactants, further enhancing the uniformity and stability of the reaction and solving existing technical problems.

[0007] To solve the above-mentioned technical problems, this utility model is achieved through the following technical solution:

[0008] A production apparatus for the continuous synthesis of tributyl phosphate, comprising:

[0009] The base has two support plates fixedly installed on its top. A first reaction vessel and a second reaction vessel are fixedly connected between the two support plates. The first reaction vessel is located above the second reaction vessel. The first reaction vessel is used to store and mix phosphorus oxychloride and butanol to complete the preliminary preparation of tributyl phosphate. The second reaction vessel is used to perform a secondary reaction and extraction on the solution after the preliminary reaction.

[0010] It also includes a first liquid addition connector and a second liquid addition connector. The first liquid addition connector is fixedly installed on the outer wall of the first reaction vessel, and the second liquid addition connector is fixedly installed on the outer wall of the second reaction vessel. Both the first liquid addition connector and the second liquid addition connector are used to connect to external pipelines for adding reaction solution.

[0011] It also includes a stirring assembly, which is used to simultaneously stir the solutions inside the first reaction vessel and the second reaction vessel to ensure that they are fully mixed;

[0012] It also includes a vacuum pumping assembly, which works in conjunction with the first reaction vessel to extract air and reaction byproduct gases from the first reaction vessel, ensuring that the interior of the first reaction vessel is in a vacuum state.

[0013] Optionally, the stirring assembly includes two rotating shafts, which respectively seal and rotate through the first reaction vessel and the second reaction vessel. Multiple stirring rods are fixedly installed on the outer walls of both rotating shafts. The multiple stirring rods are used to stir the corresponding solutions inside the first reaction vessel and the second reaction vessel. A first synchronous pulley and a second synchronous pulley are fixedly installed on one end of the two rotating shafts on the same side, and the first synchronous pulley and the second synchronous pulley are connected by a synchronous belt drive. A motor is fixedly installed on one end of the second reaction vessel by a fixed bracket, and one end of the output shaft of the motor is fixedly connected to one end of the adjacent rotating shaft.

[0014] Optionally, the extraction assembly includes a fixed plate fixedly installed on the top of one of the support plates, an extraction pump fixedly installed on the top of the fixed plate, an extraction connector fixedly passing through the outer wall of the first reaction vessel, one end of the extraction connector being fixedly connected to the air inlet of the extraction pump via a pipe, and one end of the air outlet of the extraction pump being fixedly connected to an exhaust pipe for connecting to an external collection device to ensure that the discharged by-product gas is fully collected.

[0015] Optionally, the first reaction vessel and the second reaction vessel are respectively provided with a first infusion pipe and a second infusion pipe on their exteriors. The outer walls of the first infusion pipe and the second infusion pipe are connected to multiple diversion pipes. One end of each of the multiple diversion pipes passes through the adjacent first reaction vessel and the second reaction vessel, and is used to uniformly add reaction containers to the interior of the first reaction vessel and the second reaction vessel.

[0016] Optionally, a first connecting joint is fixedly connected to one end of the first reaction vessel, and a second connecting joint is fixedly connected to one end of the second reaction vessel. The first connecting joint and the second connecting joint cooperate and are fixedly connected by the same connecting pipe to complete the transfer of liquid in the first reaction vessel. A regulating valve is provided on the connecting pipe to control the start and stop of liquid delivery.

[0017] Optionally, a temperature regulating tube is spirally sleeved on the outer wall of the first reaction vessel. The two ends of the temperature regulating tube pass through adjacent support plates and are connected to external circulation equipment. The temperature regulating tube is used to control the temperature inside the first reaction vessel to improve the efficiency of the internal solution reaction. A heat insulation shell is fixedly sleeved on the outer wall of the first reaction vessel. The temperature regulating tube is located between the first reaction vessel and the heat insulation shell. The heat insulation shell is used to reduce the temperature change of the temperature regulating tube and the inside of the first reaction vessel.

[0018] Optionally, a drain port is fixedly installed at one end of the second reaction vessel. The drain port is equipped with a corresponding valve and is connected to an external drain pipe for discharging the mixed liquid after the reaction in the second reaction vessel.

[0019] The embodiments of this utility model have the following beneficial effects:

[0020] In this invention, continuous production of tributyl phosphate is achieved by setting up a first reaction tank and a second reaction tank. The first reaction tank is used for storing and initially mixing phosphorus oxychloride and butanol, while the second reaction tank is used for secondary reaction and extraction of the solution after the initial reaction. This design not only improves production efficiency but also makes the reaction process more stable and controllable.

[0021] In this invention, the stirring assembly enables simultaneous stirring of the solutions inside the first and second reaction vessels, ensuring thorough mixing of the solutions and thus improving reaction efficiency. Furthermore, the synchronous belt drive connection of the stirring assembly ensures that the stirring speeds of the two reaction vessels remain consistent, further enhancing the uniformity of the reaction.

[0022] In this invention, by setting up the air extraction component, the air and reaction by-product gas in the first reaction tank can be effectively extracted, ensuring that the inside of the first reaction tank is in a vacuum state. This not only prevents air from interfering with the reaction process, but also improves the reaction efficiency and product quality.

[0023] In this invention, by setting a temperature regulating pipe and a heat insulation shell, the internal temperature of the first reaction vessel can be effectively controlled; the temperature regulating pipe is connected to an external circulation device to provide a suitable temperature environment for the reaction; the heat insulation shell is used to reduce the magnitude of temperature changes and improve the stability of temperature control.

[0024] In this invention, by setting up a first infusion pipe and a second infusion pipe and a branch pipe thereon, uniform addition of reactants to the internal reaction vessels of the first and second reaction vessels is achieved. This design not only improves the utilization rate of reactants, but also makes the reaction process more uniform and stable.

[0025] Of course, any product implementing this utility model does not necessarily need to achieve all of the advantages described above at the same time. Attached Figure Description

[0026] To more clearly illustrate the technical solutions of the embodiments of this utility model, the accompanying drawings used in the description of the embodiments 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.

[0027] Figure 1 This is a three-dimensional structural diagram of an embodiment of the present invention;

[0028] Figure 2 This is a cross-sectional structural diagram of an embodiment of the present invention;

[0029] Figure 3 This is a schematic diagram of the disassembled structure of a reaction vessel according to an embodiment of the present invention;

[0030] Figure 4 This is a schematic diagram of the air extraction component structure according to an embodiment of the present invention;

[0031] Figure 5 This is a schematic diagram of the motor connection structure according to an embodiment of the present invention.

[0032] In the diagram: 1. Base; 2. Support plate; 3. First reaction vessel; 4. Second reaction vessel; 5. Rotating shaft; 6. Stirring rod; 7. First connecting joint; 8. Second connecting joint; 9. Connecting pipe; 10. Adjusting valve; 11. Drainage port; 12. First infusion pipe; 13. First liquid filling joint; 14. Vacuum fitting joint; 15. Second infusion pipe; 16. Second liquid filling joint; 17. Temperature control pipe; 18. Insulation shell; 19. Fixing plate; 20. Vacuum pump; 21. Exhaust pipe; 22. Motor; 23. First synchronous pulley; 24. Second synchronous pulley. Detailed Implementation

[0033] The technical solutions of the present 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 the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present utility model.

[0034] In the description of this utility model, it should be understood that the terms "opening", "upper", "middle", "length", "inner", etc., which indicate orientation or positional relationship, are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the components or elements referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model.

[0035] To keep the following description of the embodiments of this utility model clear and concise, detailed descriptions of known functions and known components are omitted.

[0036] Example 1: Please refer to Figure 1-5 As shown, this embodiment provides a production apparatus for tributyl phosphate, comprising:

[0037] A base 1 has two support plates 2 fixedly mounted on its top. A first reaction vessel 3 and a second reaction vessel 4 are fixedly connected between these two support plates 2, with the first reaction vessel 3 located above the second reaction vessel 4. The first reaction vessel 3 is used for storing and mixing phosphorus oxychloride and butanol to complete the initial preparation of tributyl phosphate. The second reaction vessel 4 is used for a secondary reaction and extraction of the solution after the initial reaction to obtain tributyl phosphate with higher purity.

[0038] To facilitate the addition of the reaction solution, in this embodiment, a first liquid addition connector 13 is fixedly installed on the outer wall of the first reaction vessel 3, and a second liquid addition connector 16 is fixedly installed on the outer wall of the second reaction vessel 4. Both liquid addition connectors are used to connect to external pipelines, facilitating the addition of the reaction solution into the reaction vessels.

[0039] To ensure thorough mixing of the reaction solution, this embodiment also includes a stirring assembly. The stirring assembly comprises two rotating shafts 5, which respectively and rotatably pass through the first reaction vessel 3 and the second reaction vessel 4. Simultaneously, multiple stirring rods 6 are fixedly installed on the outer wall of each rotating shaft 5 for stirring the solution within the reaction vessel. A first synchronous pulley 23 and a second synchronous pulley 24 are respectively fixedly installed at one end of the two rotating shafts 5 on the same side, and these two synchronous pulleys are connected by a synchronous belt drive. A motor 22 is also fixedly installed at one end of the second reaction vessel 4 via a fixed bracket, and one end of the output shaft of the motor 22 is fixedly connected to the adjacent rotating shaft 5. When the motor 22 starts, it drives the two rotating shafts 5 to rotate simultaneously via the synchronous belt, thereby achieving synchronous stirring of the solutions within the two reaction vessels.

[0040] To maintain a vacuum inside the first reaction vessel 3, this embodiment also includes a vacuum assembly. The vacuum assembly includes a fixed plate 19 fixedly mounted on the top of one of the support plates 2, and a vacuum pump 20 is fixedly mounted on the top of the fixed plate 19. A vacuum connector 14 is fixedly passed through the outer wall of the first reaction vessel 3, and one end of the vacuum connector 14 is fixedly connected to the air inlet of the vacuum pump 20 via a pipe. An exhaust pipe 21 is fixedly connected to the air outlet of the vacuum pump 20 for connection to an external collection device to fully collect the discharged by-product gases.

[0041] To ensure uniform addition of the reaction solution, this embodiment provides a first infusion pipe 12 and a second infusion pipe 15 on the outside of the first reaction vessel 3 and the second reaction vessel 4, respectively. Multiple branch pipes are connected to the outer walls of both infusion pipes, with one end of each branch pipe penetrating an adjacent reaction vessel to ensure uniform addition of the reaction solution into the reaction vessel.

[0042] This application can be used in the field of tributyl phosphate preparation technology, or in other fields applicable to this application.

[0043] Example 2: Reference Figure 2 , 3 An improvement based on Example 1: a production apparatus for the continuous synthesis of tributyl phosphate, which is applied to the field of tributyl phosphate preparation technology;

[0044] To control the temperature inside the first reaction vessel 3, a temperature regulating pipe 17 is spirally sleeved on the outer wall of the first reaction vessel 3 in this embodiment. Both ends of the temperature regulating pipe 17 pass through adjacent support plates 2 and are connected to external circulation equipment. By allowing fluids of different temperatures to flow through its interior, the temperature regulating pipe 17 can regulate the temperature inside the first reaction vessel 3, thereby improving the efficiency of the internal solution reaction.

[0045] To mitigate temperature fluctuations within the temperature control tube 17 and the first reaction vessel 3, this embodiment also includes a heat insulation shell 18 fixedly fitted onto the outer wall of the first reaction vessel 3. The temperature control tube 17 is located between the first reaction vessel 3 and the heat insulation shell 18, which effectively reduces temperature fluctuations.

[0046] To facilitate the transfer of liquid within the first reaction vessel 3, this embodiment includes a first connecting joint 7 fixedly connected to one end of the first reaction vessel 3 and a second connecting joint 8 fixedly connected to one end of the second reaction vessel 4. These two connecting joints mate and are connected by a common connecting pipe 9, which enables liquid transfer between the reaction vessels. A regulating valve 10 is installed on the connecting pipe 9 to control the start and stop of liquid transport.

[0047] Finally, in order to discharge the mixed liquid after reaction in the second reaction tank 4, a drain port 11 is fixedly installed at one end of the second reaction tank 4 in this embodiment. A corresponding valve is provided on the drain port 11 and it is connected to an external drain pipe. After the reaction is completed, the valve can be opened to discharge the mixed liquid for subsequent processing.

[0048] However, as is well known to those skilled in the art, the working principle and wiring method of motor 22 are commonplace and are all conventional methods or common knowledge, so they will not be described in detail here. Those skilled in the art can make any selections according to their needs or convenience.

[0049] The usage process and working principle of this utility model technical solution are as follows:

[0050] In use, the user can add butanol solution to the first reaction vessel 3 through the first liquid addition connector 13. Then, the user can use the first infusion pipe 12 to deliver external phosphorus oxychloride solution into the first reaction vessel 3. Because the outer wall of the first infusion pipe 12 is equipped with multiple branch pipes, the phosphorus oxychloride solution can be evenly dripped into the butanol solution in the first reaction vessel 3, which helps ensure that the phosphorus oxychloride is fully reacted. While the reaction is proceeding, the user can lower the temperature inside the first reaction vessel 3 by supplying coolant to the temperature control pipe 17. Simultaneously, the user can start the vacuum pump 20 to extract air and any possible byproduct hydrogen chloride gas from the first reaction vessel 3, ensuring a vacuum state inside the first reaction vessel 3. This low-temperature vacuum environment is conducive to efficient reaction. Afterwards, the user can open the regulating valve 10 and use the connecting pipe 9 to move the reacted solution to the second reaction vessel 4. The above operations can then be repeated to further improve the reaction process. Sodium butoxide is slowly added to the second reaction vessel 4 through the second infusion tube 15 for a secondary reaction. After a period of time, petroleum ether is added to the second reaction vessel 4 through the second liquid addition connector 16 to complete the extraction. The mixed solution after the reaction can then be discharged through the drain port 11 for the next operation. After the solution in the first reaction vessel 3 is transferred to the second reaction vessel 4, a new solution can be added to the first reaction vessel 3 to start a new batch of reaction. The first reaction vessel 3 and the second reaction vessel 4 work simultaneously, which helps to ensure the continuous production of tributyl phosphate and high processing efficiency. At the same time, the user can also start the motor 22 during the reaction. The motor 22 can drive the two rotating shafts 5 to rotate synchronously under the transmission of the first synchronous pulley 23 and the second synchronous pulley 24, thereby simultaneously stirring the liquids in the first reaction vessel 3 and the second reaction vessel 4, so as to ensure thorough mixing and ensure efficient reaction while ensuring good processing continuity.

[0051] It should be noted that in the description of this specification, descriptions such as "first" and "second" are only used to distinguish the features and do not have any actual order or directional meaning. This application is not limited to this.

[0052] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0053] The preferred embodiments of this utility model disclosed above are merely illustrative of the present utility model. These preferred embodiments do not exhaustively describe all details, nor do they limit the utility model to the specific implementations described. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of this utility model, thereby enabling those skilled in the art to better understand and utilize it. This utility model is limited only by the claims and their full scope and equivalents.

Claims

1. A production apparatus for the continuous synthesis of tributyl phosphate, characterized in that, include: The base (1) has two support plates (2) fixedly installed on its top. A first reaction tank (3) and a second reaction tank (4) are fixedly connected between the two support plates (2). The first reaction tank (3) is located above the second reaction tank (4). The first reaction tank (3) is used to store and mix phosphorus oxychloride and butanol to complete the preliminary preparation of tributyl phosphate. The second reaction tank (4) is used to perform a secondary reaction and extraction on the solution after the preliminary reaction. It also includes a first liquid addition connector (13) and a second liquid addition connector (16). The first liquid addition connector (13) is fixedly installed on the outer wall of the first reaction vessel (3), and the second liquid addition connector (16) is fixedly installed on the outer wall of the second reaction vessel (4). Both the first liquid addition connector (13) and the second liquid addition connector (16) are used to connect to external pipelines for adding reaction solution. It also includes a stirring assembly, which is used to simultaneously stir the solutions inside the first reaction vessel (3) and the second reaction vessel (4) to ensure that they are fully mixed; It also includes a vacuum pumping assembly, which works in conjunction with the first reaction vessel (3) to extract the air and reaction byproduct gas inside the first reaction vessel (3) to ensure that the inside of the first reaction vessel (3) is in a vacuum state.

2. The production apparatus for continuous synthesis of tributyl phosphate as described in claim 1, characterized in that, The stirring assembly includes two rotating shafts (5), which respectively seal and rotate through the first reaction vessel (3) and the second reaction vessel (4). Multiple stirring rods (6) are fixedly installed on the outer walls of the two rotating shafts (5). The multiple stirring rods (6) are used to stir the corresponding solutions inside the first reaction vessel (3) and the second reaction vessel (4). A first synchronous pulley (23) and a second synchronous pulley (24) are fixedly installed on one end of the two rotating shafts (5) on the same side, respectively. The first synchronous pulley (23) and the second synchronous pulley (24) are connected by a synchronous belt drive. A motor (22) is fixedly installed on one end of the second reaction vessel (4) through a fixed bracket. One end of the output shaft of the motor (22) is fixedly connected to one end of the adjacent rotating shaft (5).

3. The production apparatus for continuous synthesis of tributyl phosphate as described in claim 1, characterized in that, The extraction assembly includes a fixed plate (19) fixedly installed on the top of one of the support plates (2). An extraction pump (20) is fixedly installed on the top of the fixed plate (19). An extraction connector (14) is fixedly inserted through the outer wall of the first reaction tank (3). One end of the extraction connector (14) is fixedly connected to the air inlet of the extraction pump (20) through a pipe. An exhaust pipe (21) is fixedly connected to one end of the air outlet of the extraction pump (20) for connection to an external collection device to ensure that the discharged by-product gas is fully collected.

4. The production apparatus for continuous synthesis of tributyl phosphate as described in claim 1, characterized in that, The first reaction vessel (3) and the second reaction vessel (4) are respectively provided with a first infusion pipe (12) and a second infusion pipe (15). The outer walls of the first infusion pipe (12) and the second infusion pipe (15) are connected to multiple diversion pipes. One end of each of the multiple diversion pipes passes through the adjacent first reaction vessel (3) and second reaction vessel (4) for uniformly adding reaction containers to the inside of the first reaction vessel (3) and the second reaction vessel (4).

5. The production apparatus for continuous synthesis of tributyl phosphate as described in claim 4, characterized in that, One end of the first reaction vessel (3) is fixedly connected to a first connecting joint (7), and one end of the second reaction vessel (4) is fixedly connected to a second connecting joint (8). The first connecting joint (7) and the second connecting joint (8) cooperate with each other and are fixedly connected to the same connecting pipe (9) for transferring the liquid in the first reaction vessel (3). The connecting pipe (9) is equipped with a regulating valve (10) for controlling the start and stop of liquid delivery.

6. The production apparatus for continuous synthesis of tributyl phosphate as described in claim 1, characterized in that, The outer wall of the first reaction vessel (3) is spirally fitted with a temperature regulating tube (17). The two ends of the temperature regulating tube (17) pass through the adjacent support plate (2) and are connected to the external circulation equipment. The temperature regulating tube (17) is used to control the temperature inside the first reaction vessel (3) to improve the efficiency of the internal solution reaction. The outer wall of the first reaction vessel (3) is fixedly fitted with a heat insulation shell (18). The temperature regulating tube (17) is located between the first reaction vessel (3) and the heat insulation shell (18). The heat insulation shell (18) is used to slow down the temperature change of the temperature regulating tube (17) and the inside of the first reaction vessel (3).

7. The continuous synthesis apparatus for tributyl phosphate as described in claim 5, characterized in that, A drain port (11) is fixedly installed at one end of the second reaction vessel (4). The drain port (11) is equipped with a corresponding valve and is connected to an external drain pipe for discharging the mixed liquid after reaction in the second reaction vessel (4).

Images