Phosphorus pentachloride production equipment and production process thereof

Abstract

The invention discloses phosphorus pentachloride production equipment and a production process thereof, and relates to the technical field of phosphorus pentachloride production.The phosphorus pentachloride production equipment comprises a reaction kettle, an air supply device and a liquid storage tank are arranged on the outer side of the reaction kettle, a motor is fixedly connected to the bottom of the reaction kettle, and an output shaft of the motor is fixedly connected with a stirrer; according to the device, phosphorus trichloride introduced into the reaction kettle is uniformly distributed through the four nozzles which are annularly distributed, phosphorus trichloride liquid is introduced by utilizing the nozzles annularly distributed on the side wall of the inner cavity of the reaction kettle, and in the process of introducing phosphorus trichloride, the nozzles are periodically oriented in cooperation with pushing and extruding of a triggering rod on an inclined plate, so that the phosphorus trichloride is uniformly introduced into the reaction kettle; the phosphorus trichloride falls into the reaction kettle from four points, compared with single-point pipeline conveying, the problem that the concentration of the phosphorus trichloride is enriched near a conveying pipeline due to long-time single-point conveying of the phosphorus trichloride can be avoided, distribution of the phosphorus trichloride can be further enhanced in cooperation with synchronous operation of a stirrer, and the subsequent mixing effect of the phosphorus trichloride and chlorine is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of phosphorus pentachloride production, and more specifically, to a phosphorus pentachloride production device and its production process. Background Art

[0002] A phosphorus pentachloride production device is a device that uses chlorine gas and phosphorus trichloride to mix inside a reaction kettle, and then reacts to produce phosphorus pentachloride; The existing production equipment usually adopts the method of single-point pipeline transportation of liquid phosphorus trichloride. When transporting phosphorus trichloride in this way, it is easy to cause a relatively high concentration of phosphorus trichloride near the pipeline. And during single-point transportation, the speed and direction of phosphorus trichloride entering the reaction kettle cause the liquid to form a strong flow in a specific area, further expanding the uneven concentration situation. The uneven concentration distribution will reduce the subsequent mixing effect with chlorine gas; Moreover, the existing production equipment usually adopts the method of continuously introducing chlorine gas into the liquid phosphorus trichloride. If chlorine gas is continuously transported, it is easy to form a local high-concentration chlorine gas area inside the liquid. This high-concentration area will cause the local reaction rate to be too fast, which will not only cause overheating, but also generate by-products, thus reducing the quality of the produced phosphorus pentachloride; To solve the above problems, the inventor has proposed a phosphorus pentachloride production device and its production process. Summary of the Invention

[0003] To solve the above technical problems, a phosphorus pentachloride production device and its production process are provided. This technical solution solves the problems raised in the above background art; To achieve the above objectives, the present invention can adopt the following technical solutions: The present invention provides a phosphorus pentachloride production device, including a reaction kettle. A gas supply device and a liquid storage tank are arranged outside the reaction kettle. Chlorine gas is stored in the gas supply device, and liquid phosphorus trichloride is stored in the liquid storage tank. A water pump is arranged inside the liquid storage tank. An outlet pipe is installed on the outer surface of the reaction kettle. A motor is fixedly connected to the bottom of the reaction kettle, and an output shaft of the motor is fixedly connected to a stirrer, and the stirrer is rotationally connected to the inner cavity of the reaction kettle; A mixing assembly is arranged above the stirrer. The mixing assembly includes a reciprocating lead screw fixedly connected to the stirrer. A pressing plate is threadedly connected to the reciprocating lead screw. A guide rod is fixedly connected to the inner cavity of the reaction kettle. A ratchet wheel is rotationally connected to the top of the reaction kettle. A support plate is fixedly connected to the top of the reaction kettle. A linkage disk is rotationally connected to the support plate. One side of the linkage disk close to the ratchet wheel is rotationally connected to a pawl. There are two pawls, and a compression spring is fixedly connected to the outside of the pawl.

[0004] Preferably, the mixing assembly further includes a limiting disk fixedly connected to the upper surface of the linkage disk. One side of the limiting disk close to the support plate is fixedly connected with a connecting rod. One side of the connecting rod away from the limiting disk is inserted with a pushing column. The top of the reaction kettle is rotatably connected with a dividing disk. Inner grooves are annularly and equidistantly formed on the surface of the dividing disk. There are four inner grooves. An infrared sensor is fixedly connected to the upper surface of the dividing disk. A protective cover is fixedly connected to the top of the reaction kettle. An induction strip is fixedly connected to the inner cavity of the protective cover. An air inlet pipe is communicated with the inner cavity of the reaction kettle. A vertical rod is fixedly connected to the bottom of the pressing disk. There are four vertical rods arranged annularly and equidistantly.

[0005] Preferably, the reciprocating lead screw is rotatably connected to the inner cavity of the reaction kettle. The pressing disk is adapted to the inner cavity of the reaction kettle. The pressing disk is slidably connected to the guide rod.

[0006] Preferably, the ratchet is fixedly connected to the reciprocating lead screw. The ratchet is slidably connected to the pawl. The compression spring is fixedly connected to the linkage disk.

[0007] Preferably, the limiting disk is slidably connected to the dividing disk. The pushing column is adapted to the inner groove. The shape of the induction strip is a quarter circle. The air inlet pipe is communicated with the air supply device. An electromagnetic valve is arranged inside the air inlet pipe, and the electromagnetic valve is electrically controlled and connected to the infrared sensor.

[0008] Preferably, a liquid inlet assembly is arranged in the inner cavity of the reaction kettle. The liquid inlet assembly includes fixing blocks fixedly connected to the inner cavity of the reaction kettle. There are four fixing blocks arranged annularly and equidistantly. A support frame is fixedly connected to the fixing block. A nozzle is rotatably connected to the support frame. A spring is fixedly connected to one side of the fixing block close to the nozzle. An inclined plate is fixedly connected to one side of the nozzle away from the fixing block. A connecting pipe is communicated with the inside of the nozzle. A cavity ring is fixedly connected to the outer surface of the reaction kettle. A liquid inlet pipe is communicated with the inside of the cavity ring. A trigger rod is fixedly connected to the bottom of the pressing disk. There are four trigger rods arranged annularly and equidistantly.

[0009] Preferably, the spring is fixedly connected to the nozzle. All four inclined plates are inclined.

[0010] Preferably, all four connecting pipes are communicated with the cavity ring. The liquid inlet pipe is communicated with the liquid storage tank.

[0011] Preferably, a phosphorus pentachloride production process includes the following steps: Step 1, raw material preparation: Store high-purity chlorine gas in the air supply device as the gaseous raw material for the reaction. Store the measured liquid phosphorus trichloride in the liquid storage tank as the liquid raw material for the reaction; Step 2, perform the reaction: Introduce the measured liquid phosphorus trichloride into the reaction kettle, then introduce high-purity chlorine gas into the liquid phosphorus trichloride, and stir and mix them. Step 3, product collection: Phosphorus pentachloride is the main product of the reaction and precipitates in solid form after the reaction is completed. The cooled phosphorus pentachloride is transferred from the reaction kettle to a special container for storage through the discharge port. Step 4, tail gas treatment: The unreacted chlorine gas and volatiles during the reaction process need to be purified through a special tail gas treatment system to meet the environmental protection standards for discharge.

[0012] Preferably, performing the reaction includes: using the stirrer in the reaction kettle to maintain good mixing of the liquid, enhancing the contact area between the gas and liquid, and promoting the full occurrence of the chemical reaction between chlorine gas and phosphorus trichloride.

[0013] As described above, the advantages of the present invention are: Through the four nozzles arranged in a ring, the phosphorus trichloride introduced into the reaction kettle is evenly distributed. Compared with the prior art of opening a conveying pipeline on the outer surface of the reaction kettle and adopting a single-point conveying method, this device uses the nozzles annularly distributed on the inner cavity side wall of the reaction kettle to introduce the liquid phosphorus trichloride. During the process of introducing phosphorus trichloride, the nozzle cooperates with the pushing of the trigger rod on the inclined plate, causing the orientation of the nozzle to change periodically, so that the action range of each nozzle will continuously change, and the phosphorus trichloride falls into the interior of the reaction kettle from four points, thus being evenly distributed inside the reaction kettle. Compared with the single-point pipeline conveying, it can avoid the problem of concentration enrichment of phosphorus trichloride near the conveying pipeline caused by long-term single-point conveying of phosphorus trichloride. The synchronous operation of the stirrer can further enhance the distribution of phosphorus trichloride and improve the subsequent mixing effect with chlorine gas.

[0014] By periodically opening and closing the solenoid valve, periodic segmented chlorine gas conveying is realized. Compared with the prior art of continuously introducing chlorine gas into the liquid phosphorus trichloride, in the process of the stirrer rotating four circles in this device, a part of the running track of the infrared sensor coincides with the induction strip. When the infrared sensor is below the induction strip, the solenoid valve in the air inlet pipe opens, and when the infrared sensor leaves below the induction strip, the solenoid valve in the air inlet pipe closes. Whenever the solenoid valve opens, chlorine gas is introduced into the liquid phosphorus trichloride. The disturbance of the stirrer can make the newly added chlorine gas as evenly distributed as possible in the liquid phase. Periodic ventilation combined with appropriate stirring can realize the continuous update of the gas-liquid interface and improve the mixing efficiency of chlorine gas and liquid phosphorus trichloride. Compared with the continuous ventilation method, periodic addition can synchronously optimize the flow of the liquid in the reaction kettle and the reaction process, reducing the possibility of uneven mixing of chlorine gas and liquid phosphorus trichloride.

[0015] By the reciprocating vertical movement of the vertical rod, the generation of bubbles during the introduction of chlorine gas is effectively reduced. Compared with the prior art where only a stirrer is used for mixing and stirring, in this device, while the stirrer rotates, it drives the vertical rod to perform reciprocating vertical movement. The vertical rod inserts into and disengages from the phosphorus trichloride liquid, causing the liquid at the top to sink. In this way, the limitation of the traditional single stirring method, which cannot effectively stir the phosphorus trichloride liquid at the bottom of the reaction kettle, can be avoided. Moreover, the periodic up and down movement of the vertical rod can effectively break the bubbles generated by introducing chlorine gas into the phosphorus trichloride liquid and redistribute them, increasing the mixing contact area of the gas-liquid interface, thereby improving the reaction rate. Description of the Drawings

[0016] Figure 1 Front three-dimensional schematic diagram of the overall structure shown in the present invention; Figure 2 Internal sectional three-dimensional schematic diagram of the reaction kettle shown in the present invention; Figure 3 Three-dimensional schematic diagram of the reciprocating lead screw, pressure plate and related components shown in the present invention; Figure 4 Three-dimensional schematic diagram of the connection between the reciprocating lead screw and the ratchet shown in the present invention; Figure 5 Three-dimensional schematic diagram of the linkage disk, ratchet pawl and related components shown in the present invention; Figure 6 Internal sectional three-dimensional schematic diagram of the protective cover shown in the present invention; Figure 7 Exploded three-dimensional schematic diagram of the linkage disk and the limit disk shown in the present invention; Figure 8 Planar schematic diagram of the operating trajectory of the infrared sensor shown in the present invention; Figure 9 Partial three-dimensional schematic diagram of the liquid inlet assembly shown in the present invention; Figure 10 Three-dimensional schematic diagram of the inclined plate, trigger rod and related components shown in the present invention; Figure 11 Process flow schematic diagram of the phosphorus pentachloride production process in the present invention.

[0017] Among them, the reference numerals in the present invention are: 1. Reaction kettle; 2. Gas supply device; 3. Liquid storage tank; 4. Motor; 41. Stirrer; Mixing assembly: 51. Reciprocating lead screw; 52. Pressure plate; 53. Guide rod; 54. Ratchet; 55. Support plate; 56. Linkage disk; 57. Ratchet pawl; 58. Compression spring; 59. Limit disk; 510. Connecting rod; 511. Pushing column; 512. Dividing disk; 513. Inner groove; 514. Infrared sensor; 515. Protective cover; 516. Induction strip; 517. Inlet pipe; 518. Vertical rod; Liquid inlet assembly: 61, fixed block; 62, support frame; 63, nozzle; 64, spring; 65, inclined plate; 66, connecting pipe; 67, cavity ring; 68, liquid inlet pipe; 69, trigger rod. Detailed implementation

[0018] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present invention.

[0019] The embodiments provided by the present invention will be elaborated in detail below: Embodiment:

[0020] A phosphorus pentachloride production device, as Figure 1 and Figure 2 shown, includes a reaction kettle 1. A gas supply device 2 and a liquid storage tank 3 are arranged on the outer side of the reaction kettle 1. The gas supply device 2 and the liquid storage tank 3 are respectively located on the left and right sides of the reaction kettle 1. Chlorine is stored in the gas supply device 2, and phosphorus trichloride liquid is stored in the liquid storage tank 3. A water pump is arranged in the liquid storage tank 3, and the water pump can transport the phosphorus trichloride liquid into the reaction kettle 1. An outlet pipe is installed on the outer surface of the reaction kettle 1, and a valve is arranged on the outlet pipe. The prepared phosphorus pentachloride can be discharged from the inside of the reaction kettle 1 by opening the valve on the outlet pipe. The bottom surface of the reaction kettle 1 is fixedly connected with a motor 4, and the output shaft of the motor 4 is fixedly connected with a stirrer 41. The stirrer 41 is rotatably connected to the bottom surface of the inner cavity of the reaction kettle 1; As Figures 2 to 5 shown, a mixing assembly is arranged above the stirrer 41. The mixing assembly includes a reciprocating lead screw 51 fixedly connected to the stirrer 41. The reciprocating lead screw 51 is located at one end of the stirrer 41 away from the motor 4. A pressure plate 52 is threadedly connected to the outer surface of the reciprocating lead screw 51. A guide rod 53 is fixedly connected to the top surface of the inner cavity of the reaction kettle 1. A ratchet wheel 54 is rotatably connected to the top surface of the reaction kettle 1. A support plate 55 is fixedly connected to the top surface of the reaction kettle 1. The support plate 55 is located above the ratchet wheel 54. A linkage disk 56 is rotatably connected to the support plate 55. A pawl 57 is rotatably connected to one side of the linkage disk 56 close to the ratchet wheel 54. There are two pawls 57. A compression spring 58 is fixedly connected to the side of the pawl 57 away from the ratchet wheel 54. The compression spring 58 is in a compressed state.

[0021] Further, as Figures 6 to 8As shown, the mixing component further includes a limit disk 59 fixedly connected to the linkage disk 56. One side of the limit disk 59 close to the support plate 55 is fixedly connected with a connecting rod 510. One side of the connecting rod 510 away from the center of the limit disk 59 is inserted with a push column 511. One side of the reaction kettle 1 close to the limit disk 59 is rotatably connected with a dividing disk 512. Inner grooves 513 are annularly and equidistantly arranged on the surface of the dividing disk 512. There are four inner grooves 513. An infrared sensor 514 is fixedly connected to the upper surface of the dividing disk 512. A protective cover 515 is fixedly connected to the top of the reaction kettle 1. An induction strip 516 is fixedly connected to the inner cavity of the protective cover 515. The induction strip 516 is located above the infrared sensor 514. An air inlet pipe 517 is communicated with the inner cavity of the reaction kettle 1. A vertical rod 518 is fixedly connected to the bottom of the pressing disk 52. Four vertical rods 518 are annularly and equidistantly arranged.

[0022] Further, as Figure 3 and Figure 4 shown, one end of the reciprocating lead screw 51 away from the stirrer 41 is rotatably connected to the top surface of the inner cavity of the reaction kettle 1. The pressing disk 52 is adapted to the inner cavity of the reaction kettle 1. The pressing disk 52 is slidably connected to the outer surface of the guide rod 53.

[0023] Further, as Figure 4 and Figure 5 shown, the ratchet wheel 54 is fixedly connected to the bottom surface of the reciprocating lead screw 51. The outer surface of the ratchet wheel 54 is in interference fit with the pawl 57. One end of the compression spring 58 away from the pawl 57 is fixedly connected to the linkage disk 56.

[0024] Further, as Figures 6 to 8 shown, the outer arc surface of the limit disk 59 is in fitting contact with the outer surface of the dividing disk 512. The push column 511 is adapted to the inner groove 513. The shape of the induction strip 516 is a quarter circle. The induction strip 516 is located on the running track of the infrared sensor 514. The air inlet pipe 517 is communicated with the gas supply device 2. An electromagnetic valve is arranged inside the air inlet pipe 517. And the electromagnetic valve is electrically controlled and connected to the infrared sensor 514 through an external controller. When the infrared sensor 514 is located below the induction strip 516, the electromagnetic valve inside the air inlet pipe 517 is opened. When the infrared sensor 514 moves out from below the induction strip 516, the electromagnetic valve inside the air inlet pipe 517 is closed.

[0025] Further, as Figure 9 and Figure 10As shown in the figure, a liquid inlet assembly is provided inside the inner cavity of the reactor 1. The liquid inlet assembly includes a fixing block 61 fixedly connected to the side wall of the inner cavity of the reactor 1. Four fixing blocks 61 are arranged equidistantly in a ring shape. On one side of the fixing block 61 close to the reciprocating lead screw 51, a support frame 62 is fixedly connected. On the side of the support frame 62 away from the fixing block 61, a nozzle 63 is rotatably connected. The liquid outlet of the nozzle 63 faces downward. On one side of the fixing block 61 close to the nozzle 63, a spring 64 is fixedly connected. The spring 64 is located directly below the support frame 62. On the side of the nozzle 63 away from the fixing block 61, an inclined plate 65 is fixedly connected. A connecting pipe 66 is communicated inside the nozzle 63. The connecting pipe 66 is located above the nozzle 63. The outer surface of the reactor 1 is fixedly connected with a cavity ring 67. The inside of the cavity ring 67 is communicated with a liquid inlet pipe 68. The bottom of the pressing disc 52 is fixedly connected with a trigger rod 69. Four trigger rods 69 are arranged equidistantly in a ring shape. All four trigger rods 69 are directly above the four inclined plates 65 and correspond one by one.

[0026] Further, as Figure 9 and Figure 10 shown in the figure, one end of the spring 64 away from the fixing block 61 is fixedly connected to the nozzle 63. All four inclined plates 65 are inclined. When the trigger rod 69 moves downward and pushes the inclined plate 65, the nozzle 63 can be rotated through the inclined plate 65.

[0027] Further, as Figure 9 and Figure 10 shown in the figure, one ends of the four connecting pipes 66 away from the nozzle 63 are all communicated with the inside of the cavity ring 67. One end of the liquid inlet pipe 68 away from the cavity ring 67 is communicated with the inside of the liquid storage tank 3. The phosphorus trichloride liquid in the nozzle 63 can be transported to the cavity ring 67 through the liquid inlet pipe 68 and then be respectively transported to the nozzle 63 through the connecting pipes 66.

[0028] As Figure 11 shown in the figure, a production process of phosphorus pentachloride includes the following steps: Step 1, raw material preparation: Store high-purity chlorine gas in the gas supply device 2 as the gaseous raw material for the reaction, and store the measured phosphorus trichloride liquid in the liquid storage tank 3 as the liquid-phase raw material for the reaction; Step 2, carry out the reaction: Introduce the measured phosphorus trichloride liquid into the reactor 1, then introduce high-purity chlorine gas into the phosphorus trichloride liquid and stir and mix them; Step 3, product collection: Phosphorus pentachloride is the main product of the reaction and precipitates in solid form after the reaction is completed. The cooled phosphorus pentachloride is transferred from the reactor 1 to a special container for storage through the discharge port; Step 4, tail gas treatment: The unreacted chlorine gas and volatiles during the reaction process need to be purified through a special tail gas treatment system and discharged to meet the environmental protection standards.

[0029] Further, asFigure 11 As shown, the reaction steps include: using the stirrer 41 in the reaction kettle 1 to maintain good mixing of the liquid, enhancing the contact area between gas and liquid, and promoting the full occurrence of the chemical reaction between chlorine gas and phosphorus trichloride.

[0030] During operation: This device can be transported by multi-point nozzles 63, and the phosphorus trichloride liquid is sent into the interior of the reaction kettle 1 to avoid the problem of concentration enrichment caused by single-point transportation. The detailed steps are as follows: When preparing phosphorus pentachloride, the staff simultaneously starts the water pump and the motor 4 provided inside the liquid storage tank 3 through the controller. When the water pump provided inside the liquid storage tank 3 is started, the water pump pumps the phosphorus trichloride liquid stored inside the liquid storage tank 3 to the liquid inlet pipe 68, transports it through the liquid inlet pipe 68 to the inside of the cavity ring 67, and then through four connecting pipes 66, the phosphorus trichloride liquid inside the cavity ring 67 is respectively transported to the four nozzles 63, and the phosphorus trichloride is introduced into the interior of the reaction kettle 1 through the four nozzles 63 arranged in an equidistant ring inside the reaction kettle 1; When the motor 4 is started, the output shaft of the motor 4 rotates forward, driving the stirrer 41 to rotate forward. The stirrer 41 causes the reciprocating lead screw 51 to rotate forward together with the stirrer 41, and the reciprocating lead screw 51 further drives the ratchet wheel 54 to rotate clockwise, so that Figure 5 For reference, during the clockwise rotation of the ratchet wheel 54, the one-way teeth outside the ratchet wheel 54 slide past the inside of the pawl 57 one by one and squeeze the pawl 57, causing the pawl 57 to rotate in the direction close to the compression spring 58 with the rotation connection point with the linkage disk 56 as the axis. At this time, the compression spring 58 is compressed. As the ratchet wheel 54 rotates, the compression spring 58 extends and pushes the pawl 57 into the angle between the next one-way teeth. In this way, the ratchet wheel 54 will not be hindered by the pawl 57 and the compression spring 58 during the clockwise rotation, so that the linkage disk 56 will not rotate together with the ratchet wheel 54 and the reciprocating lead screw 51.

[0031] During the forward rotation of the reciprocating lead screw 51, the double-thread on the surface of the reciprocating lead screw 51 causes the pressure plate 52 to move vertically back and forth along the guide rod 53. During this process, when the pressure plate 52 moves vertically downward and the trigger rod 69 at the bottom of the pressure plate 52 contacts the inclined plate 65, as the pressure plate 52 continues to move vertically downward, the trigger rod 69 pushes the inclined plate 65, causing the nozzle 63 to rotate around the rotational connection with the support frame 62 in the direction towards the spring 64 side, further changing the orientation angle of the nozzle 63. At this time, the spring 64 is compressed. When the pressure plate 52 starts to move vertically upward, as the spring 64 expands, the nozzle 63 gradually rotates back to the initial position, once again changing the orientation angle of the nozzle 63. When the nozzle 63 rotates back to the initial position, the trigger rod 69 disengages from the inclined plate 65. In this way, through the change in the orientation angle of the nozzle 63, the introduced phosphorus trichloride liquid can be evenly distributed inside the reaction kettle 1.

[0032] During the above process, through the four nozzles 63 arranged in a ring, the phosphorus trichloride introduced into the reaction kettle 1 is evenly distributed. Compared with the prior art of opening a conveying pipeline on the outer surface of the reaction kettle 1 and adopting a single-point conveying method, this device uses the nozzles 63 annularly distributed on the inner cavity side wall of the reaction kettle 1 to introduce the phosphorus trichloride liquid. During the introduction of phosphorus trichloride by the nozzle 63, with the cooperation of the trigger rod 69 pushing the inclined plate 65, the orientation of the nozzle 63 changes periodically, so that the action range of each nozzle 63 will continuously change, causing the phosphorus trichloride to fall into the reaction kettle 1 from four points, thereby being evenly distributed inside the reaction kettle 1. Compared with single-point pipeline conveying, it can avoid the problem of phosphorus trichloride concentration enrichment near the conveying pipeline caused by long-term single-point conveying of phosphorus trichloride. The synchronous operation of the agitator 41 can further enhance the distribution of phosphorus trichloride and improve the subsequent mixing effect with chlorine.

[0033] This device can feed chlorine in periodic segments, and the detailed steps are as follows: After all the phosphorus trichloride liquid stored in the liquid storage tank 3 is introduced into the reaction kettle 1, the staff closes the water pump arranged inside the liquid storage tank 3 through the controller, and makes the output shaft of the motor 4 change from forward rotation to reverse rotation through the controller. When the output shaft of the motor 4 rotates in reverse, the ratchet 54 fixedly connected to the reciprocating lead screw 51 has a tendency to rotate counterclockwise, Figure 5 Taking this as a reference, the compression spring 58 in the compressed state at this time will cause the pawl 57 to be stuck in the angle between the external single teeth of the ratchet 54, so that the linkage disk 56 rotates counterclockwise together with the ratchet 54, and further makes the limit disk 59 rotate together with the linkage disk 56.

[0034] During the process of the limiting disk 59 rotating one full circle, the pushing column 511 rotates in a circular motion at an eccentric position of the limiting disk 59. During this process, the limiting disk 59 gradually enters the inner groove 513 formed on the surface of the dividing disk 512 according to the rotation angle. When the pushing column 511 enters the inner groove 513 formed on the surface of the dividing disk 512, the outer ring surface of the dividing disk 512 disengages from the contact with the outer arc surface of the limiting disk 59. After the pushing column 511 enters the inner groove 513, the pushing column 511 pushes the dividing disk 512 to rotate. At this time, after the inner groove 513 near the pushing column 511 is pushed to the position of the previous inner groove 513, the limiting disk 59 has not completed one full rotation. As the limiting disk 59 continues to rotate, it drives the pushing column 511 to rotate so that the pushing column 511 disengages from the inner groove 513. At this time, the limiting disk 59 continues to rotate until the pushing column 511 is driven by the limiting disk 59 to complete one full rotation. At this time, the dividing disk 512 rotates ninety degrees, and the arc surface of the dividing disk 512 fits with the outer surface of the limiting disk 59, making the dividing disk 512 remain stationary after rotation.

[0035] Taking Figure 8 as a reference, when the limiting disk 59 rotates one full circle, the infrared sensor 514 rotates counterclockwise ninety degrees. Therefore, when the limiting disk 59 rotates four full circles, the infrared sensor 514 rotates one full circle. During the process of the infrared sensor 514 rotating counterclockwise one full circle, the running track of the infrared sensor 514 coincides with the induction strip 516. When the infrared sensor 514 rotates to the lower part of the induction strip 516, the electromagnetic valve arranged in the air inlet pipe 517 is opened, enabling the chlorine gas stored in the gas supply device 2 to enter the phosphorus trichloride liquid in the reaction kettle 1 through the air inlet pipe 517. When the infrared sensor 514 leaves the lower part of the induction strip 516, the electromagnetic valve arranged in the air inlet pipe 517 is closed, but the stirrer 41 is still running for stirring.

[0036] During the process of the reciprocating lead screw 51 rotating counterclockwise, the pressing disk 52 will move vertically back and forth along the guide rod 53. The pressing disk 52 drives the vertical rod 518 to move together. When the pressing disk 52 moves vertically downward, the vertical rod 518 will insert into the interior of the phosphorus trichloride liquid inside the reaction kettle 1. When the pressing disk 52 moves vertically upward, the vertical rod 518 will gradually leave the interior of the phosphorus trichloride liquid. In this way, by periodically inserting and disengaging from the phosphorus trichloride liquid through the vertical rod 518, the vertical rod 518 drives the phosphorus trichloride liquid to form a periodic up-and-down circulating flow, so as to better mix and contact with the chlorine gas and further improve the mixing efficiency.

[0037] In the above process, by periodically opening and closing the solenoid valve, periodic segmented chlorine delivery is achieved. Compared with the prior art method of continuously introducing chlorine into the phosphorus trichloride liquid, in the present device, during the process of the stirrer 41 rotating four times, a part of the running track of the infrared sensor 514 coincides with the induction strip 516. When the infrared sensor 514 is located below the induction strip 516, the solenoid valve in the air inlet pipe 517 opens. When the infrared sensor 514 leaves below the induction strip 516, the solenoid valve in the air inlet pipe 517 closes. Each time the solenoid valve opens, chlorine is introduced into the phosphorus trichloride liquid. With the disturbance of the stirrer 41, the newly added chlorine can be distributed as evenly as possible in the liquid phase. Periodic gas injection combined with appropriate stirring can continuously update the gas-liquid interface and improve the mixing efficiency of chlorine and the phosphorus trichloride liquid. Compared with the continuous gas injection method, periodic addition allows the flow of the liquid in the reaction kettle 1 and the reaction process to be optimized synchronously, reducing the possibility of uneven mixing of chlorine and the phosphorus trichloride liquid.

[0038] In the above process, through the reciprocating vertical movement of the vertical rod 518, the generation of bubbles during chlorine injection is effectively reduced. Compared with the prior art method of only using the stirrer 41 for mixing and stirring, in the present device, while the stirrer 41 rotates, it drives the vertical rod 518 to perform reciprocating vertical movement. The vertical rod 518 inserts into and disengages from the phosphorus trichloride liquid, causing the top liquid to sink. In this way, the limitation of the traditional single stirring method, which cannot effectively stir the phosphorus trichloride liquid at the bottom of the reaction kettle 1, can be avoided. Moreover, the periodic up and down movement of the vertical rod 518 can effectively break the bubbles generated by introducing chlorine into the phosphorus trichloride liquid and redistribute them, increasing the mixing contact area of the gas-liquid interface and thus improving the reaction rate.

[0039] The above are only embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included within the protection scope of the present invention.

Claims

1. A phosphorus pentachloride production device, including a reaction kettle (1), characterized in that, A gas supply device (2) and a liquid storage tank (3) are arranged outside the reactor (1). Chlorine is stored in the gas supply device (2), and phosphorus trichloride liquid is stored in the liquid storage tank (3). A water pump is arranged in the liquid storage tank (3). An outlet pipe is installed on the outer surface of the reactor (1). A motor (4) is fixedly connected to the bottom of the reactor (1), and an output shaft of the motor (4) is fixedly connected to a stirrer (41). The stirrer (41) is rotationally connected to the inner cavity of the reactor (1). Above the stirrer (41), there is a mixing assembly. The mixing assembly includes a reciprocating lead screw (51) fixedly connected to the stirrer (41). A pressing plate (52) is threadedly connected to the reciprocating lead screw (51). A guide rod (53) is fixedly connected to the inner cavity of the reactor (1). A ratchet wheel (54) is rotationally connected to the top of the reactor (1). A support plate (55) is fixedly connected to the top of the reactor (1). A linkage disk (56) is rotationally connected inside the support plate (55). A pawl (57) is rotationally connected to one side of the linkage disk (56) close to the ratchet wheel (54). There are two pawls (57), and a compression spring (58) is fixedly connected to the outer side of the pawl (57). An air inlet pipe (517) communicates with the inner cavity of the reactor (1), and the air inlet pipe (517) is connected to the gas supply device (2). An electromagnetic valve is arranged inside the air inlet pipe (517), and the electromagnetic valve is electrically controlled and connected through an infrared sensor (514). Four nozzles (63) are annularly arranged on the inner cavity side wall of the reactor (1).

2. The phosphorus pentachloride production equipment according to claim 1, characterized in that, The mixing assembly further includes a limit disk (59) fixedly connected to the upper surface of the linkage disk (56). A connecting rod (510) is fixedly connected to one side of the limit disk (59) close to the support plate (55). A push rod (511) is inserted into the side of the connecting rod (510) away from the limit disk (59). A dividing disk (512) is rotationally connected to the top of the reactor (1). Inner grooves (513) are annularly and equidistantly arranged on the surface of the dividing disk (512). There are four inner grooves (513). The upper surface of the dividing disk (512) is fixedly connected to the infrared sensor (514). A protective cover (515) is fixedly connected to the top of the reactor (1). An induction strip (516) is fixedly connected to the inner cavity of the protective cover (515). A vertical rod (518) is fixedly connected to the bottom of the pressing plate (52). The vertical rods (518) are annularly and equidistantly arranged with four.

3. The phosphorus pentachloride production equipment according to claim 1, characterized in that, The reciprocating lead screw (51) is rotationally connected to the inner cavity of the reactor (1). The pressing plate (52) is adapted to the inner cavity of the reactor (1), and the pressing plate (52) is slidably connected to the guide rod (53).

4. A phosphorus pentachloride production device according to claim 1, characterized in that, The ratchet wheel (54) is fixedly connected to the reciprocating lead screw (51). The ratchet wheel (54) is slidably connected to the pawl (57). The compression spring (58) is fixedly connected to the linkage disk (56).

5. A phosphorus pentachloride production device according to claim 2, characterized in that, The limiting disk (59) is slidably connected to the dividing disk (512). The pushing column (511) is adapted to the inner groove (513). The sensing strip (516) is in the shape of a quarter ring.

6. The phosphorus pentachloride production equipment according to claim 1, characterized in that, An inlet liquid assembly is arranged in the inner cavity of the reactor (1). The inlet liquid assembly includes a fixed block (61) fixedly connected to the inner cavity of the reactor (1). Four fixed blocks (61) are arranged annularly and equidistantly. A support frame (62) is fixedly connected to the fixed block (61). The support frame (62) is rotatably connected to a nozzle (63). A spring (64) is fixedly connected to one side of the fixed block (61) close to the nozzle (63). An inclined plate (65) is fixedly connected to the side of the nozzle (63) away from the fixed block (61). A connecting pipe (66) is communicated inside the nozzle (63). An air cavity ring (67) is fixedly connected to the outer surface of the reactor (1). An inlet liquid pipe (68) is communicated inside the air cavity ring (67). A trigger rod (69) is fixedly connected to the bottom of the pressing disk (52). Four trigger rods (69) are arranged annularly and equidistantly.

7. A phosphorus pentachloride production device according to claim 6, characterized in that, The spring (64) is fixedly connected to the nozzle (63). The four inclined plates (65) are all inclined.

8. A phosphorus pentachloride production device according to claim 6, characterized in that, The four connecting pipes (66) are all communicated with the air cavity ring (67). The inlet liquid pipe (68) is communicated with the liquid storage tank (3).

9. A phosphorus pentachloride production process is now proposed for a phosphorus pentachloride production device according to any one of claims 1-8, characterized in that, It includes the following steps: Step 1, raw material preparation: Store high-purity chlorine gas in the gas supply device (2) as the gas-phase raw material for the reaction. Store the measured phosphorus trichloride liquid in the liquid storage tank (3) as the liquid-phase raw material for the reaction. Step 2, carry out the reaction: Introduce the measured phosphorus trichloride liquid into the reactor (1), then introduce high-purity chlorine gas into the phosphorus trichloride liquid, and stir and mix them. Step 3, product collection: Phosphorus pentachloride is the main product of the reaction. After the reaction is completed, it precipitates in solid form, and the cooled phosphorus pentachloride is transferred from the reactor (1) to a special container for storage through the discharge port. Step 4, tail gas treatment: The unconsumed chlorine gas and volatiles during the reaction process need to be purified through a special tail gas treatment system, and the emissions meet the environmental protection standards.

10. A phosphorus pentachloride production process according to claim 9, characterized in that, Carrying out the reaction includes: Using the stirrer (41) in the reactor (1) to maintain good mixing of the liquid, enhance the contact area between the gas and the liquid, and promote the full occurrence of the chemical reaction between chlorine gas and phosphorus trichloride.

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