Phosphorus pentachloride production equipment and production process

Abstract

The invention discloses phosphorus pentachloride production equipment and a production process thereof, relating to the technical field of phosphorus pentachloride production. The equipment comprises a reactor, wherein an air supply device and a liquid storage tank are provided on the outside of the reactor, a motor is fixedly connected to the bottom of the reactor, and an agitator is fixedly connected to the output shaft of the motor. Four nozzles arranged in an annular manner ensure that the phosphorus trichloride introduced into the reactor is evenly distributed. The device introduces phosphorus trichloride liquid by using the nozzles annularly distributed on the side wall of the inner cavity of the reactor. During the process of introducing the phosphorus trichloride, the nozzles cooperate with a trigger rod to push an inclined plate, so that the directions of the nozzles are periodically changed, so that the phosphorus trichloride falls into the interior of the reactor from four points. Compared with single-point pipeline transportation, the device can avoid the problem of phosphorus trichloride concentration enrichment near the transportation pipeline caused by long-term single-point transportation of phosphorus trichloride. Synchronous operation of the agitator can further enhance the distribution of the phosphorus trichloride and improve the subsequent mixing effect with chlorine.

Description

Technical Field

[0001] The present invention relates to the technical field of phosphorus pentachloride production, in particular to phosphorus pentachloride production equipment and a production process thereof. Background Art

[0002] Phosphorus pentachloride production equipment is a device that uses chlorine and phosphorus trichloride to mix inside a reactor to react and produce phosphorus pentachloride;

[0003] Existing production equipment typically uses a single-point pipeline to transport phosphorus trichloride liquid. This method easily leads to high phosphorus trichloride concentrations near the pipeline when transporting phosphorus trichloride. In addition, during single-point delivery, the speed and direction of phosphorus trichloride entering the reactor cause the liquid to form a strong flow in a specific area, further amplifying the uneven concentration distribution and reducing the subsequent mixing effect with chlorine.

[0004] Furthermore, existing production equipment typically uses a method of continuously introducing chlorine gas into the phosphorus trichloride liquid. Continuous chlorine delivery can easily lead to the formation of localized high-concentration chlorine areas within the liquid. These high-concentration areas can cause localized excessive reaction rates, leading to overheating and the generation of by-products, thereby reducing the quality of the phosphorus pentachloride produced.

[0005] In order to solve the above problems, the inventors proposed a phosphorus pentachloride production device and a production process thereof. Summary of the Invention

[0006] In order to solve the above technical problems, a phosphorus pentachloride production device and a production process thereof are provided. This technical solution solves the problems raised in the above background technology;

[0007] To achieve the above objectives, the present invention can be implemented by adopting the following technical solutions:

[0008] The present invention provides phosphorus pentachloride production equipment, comprising a reactor, an air supply device and a liquid storage tank are provided on the outside of the reactor, chlorine gas is stored in the air supply device, phosphorus trichloride liquid is stored in the liquid storage tank, a water pump is provided in the liquid storage tank, a discharge pipe is installed on the outer surface of the reactor, a motor is fixedly connected to the bottom of the reactor, an agitator is fixedly connected to the output shaft of the motor, and the agitator is rotatably connected to the inner cavity of the reactor;

[0009] A mixing assembly is provided above the agitator, and the mixing assembly includes a reciprocating screw fixedly connected to the agitator, a pressure plate is threadedly connected to the reciprocating screw, a guide rod is fixedly connected to the inner cavity of the reactor, a ratchet is rotatably connected to the top of the reactor, a support plate is fixedly connected to the top of the reactor, a linkage disk is rotatably connected in the support plate, a pawl is rotatably connected to the side of the linkage disk close to the ratchet, two pawls are provided, and a compression spring is fixedly connected to the outer side of the pawl.

[0010] Preferably, the mixing assembly also includes a limit plate fixedly connected to the upper surface of the linkage plate, the limit plate is fixedly connected to a connecting rod on the side close to the support plate, and a push column is inserted into the side of the connecting rod away from the limit plate, the top of the reactor is rotatably connected to a partition plate, the surface of the partition plate is provided with inner grooves at equal intervals in an annular shape, and four inner grooves are provided, the upper surface of the partition plate is fixedly connected to an infrared sensor, the top of the reactor is fixedly connected to a protective cover, the inner cavity of the protective cover is fixedly connected to a sensor strip, the inner cavity of the reactor is connected to an air inlet pipe, and the bottom of the pressure plate is fixedly connected to a vertical rod, and four vertical rods are provided at equal intervals in an annular shape.

[0011] Preferably, the reciprocating screw is rotatably connected to the inner cavity of the reactor, the pressure plate is adapted to the inner cavity of the reactor, and the pressure plate is slidably connected to the guide rod.

[0012] Preferably, the ratchet is fixedly connected to the reciprocating screw, the ratchet is slidingly connected to the pawl, and the compression spring is fixedly connected to the linkage disk.

[0013] Preferably, the limit plate is slidably connected to the dividing plate, the push column is adapted to the inner groove, the sensor strip is shaped like a quarter ring, the air intake pipe is connected to the air supply device, an electromagnetic valve is provided inside the air intake pipe, and the electromagnetic valve is electrically controlled and connected to the infrared sensor.

[0014] Preferably, the inner cavity of the reactor is provided with a liquid inlet assembly, which includes a fixed block fixedly connected to the inner cavity of the reactor, four fixed blocks are equidistantly arranged in a ring, a support frame is fixedly connected to the fixed block, a nozzle is rotatably connected to the support frame, a spring is fixedly connected to the side of the fixed block close to the nozzle, an inclined plate is fixedly connected to the side of the nozzle away from the fixed block, a connecting pipe is connected to the interior of the nozzle, a cavity ring is fixedly connected to the outer surface of the reactor, the interior of the cavity ring is connected to the liquid inlet pipe, a trigger rod is fixedly connected to the bottom of the pressure plate, and four trigger rods are equidistantly arranged in a ring.

[0015] Preferably, the spring is fixedly connected to the nozzle, and the four inclined plates are all arranged at an angle.

[0016] Preferably, the four connecting pipes are all connected to the cavity ring, and the liquid inlet pipe is connected to the liquid storage tank.

[0017] Preferably, a process for producing phosphorus pentachloride comprises the following steps:

[0018] Step 1, raw material preparation: high-purity chlorine is stored in the gas supply device as the gaseous raw material for the reaction, and measured phosphorus trichloride liquid is stored in the liquid storage tank as the liquid raw material for the reaction;

[0019] Step 2, reacting: introducing a measured amount of phosphorus trichloride liquid into a reactor, then passing high-purity chlorine gas into the phosphorus trichloride liquid, and stirring and mixing the liquid;

[0020] Step 3, product collection: Phosphorus pentachloride is the main product of the reaction and precipitates as a solid after the reaction is completed. The cooled phosphorus pentachloride is transferred from the reactor through the discharge port to a dedicated container for storage;

[0021] Step 4: Tail gas treatment: The chlorine and volatiles not used up during the reaction process need to be purified through a dedicated tail gas treatment system to meet environmental standards.

[0022] Preferably, carrying out the reaction includes: utilizing an agitator in the reactor to maintain good mixing of the liquid, increasing the contact area between the gas and the liquid, and promoting a sufficient chemical reaction between the chlorine gas and the phosphorus trichloride.

[0023] From the above, the advantages of the present invention are:

[0024] The four nozzles arranged in a ring ensure that the phosphorus trichloride introduced into the reactor is evenly distributed. Compared to the prior art method of providing a delivery pipeline on the outer surface of the reactor and adopting a single-point delivery method, the present device introduces phosphorus trichloride liquid using nozzles arranged in a ring on the side wall of the reactor cavity. During the process of introducing phosphorus trichloride, the nozzles cooperate with the trigger rod to push the inclined plate, causing the direction of the nozzles to rotate periodically. The effective range of each nozzle is continuously changed, causing phosphorus trichloride to fall into the interior of the reactor from four points and thus be evenly distributed inside the reactor. Compared with single-point pipeline delivery, this device can avoid the problem of phosphorus trichloride concentration enrichment near the delivery pipeline due to long-term single-point delivery of phosphorus trichloride. The synchronous operation of the agitator can further enhance the distribution of phosphorus trichloride and improve the subsequent mixing effect with chlorine gas.

[0025] By periodically opening and closing the solenoid valve, chlorine is delivered in stages. Compared to the prior art method of continuously introducing chlorine into the phosphorus trichloride liquid, this device utilizes a stirrer that rotates four times, during which a portion of the infrared sensor's trajectory overlaps with the sensing strip. When the infrared sensor is below the sensing strip, the solenoid valve in the air intake pipe opens; when the infrared sensor leaves the sensing strip, the solenoid valve in the air intake pipe closes. Each time the solenoid valve opens, chlorine is introduced into the phosphorus trichloride liquid. Combined with the agitation of the stirrer, the newly added chlorine is distributed as evenly as possible in the liquid phase. Periodic ventilation combined with appropriate stirring can continuously update the gas-liquid interface, improving the efficiency of mixing of chlorine and phosphorus trichloride liquid. Compared to continuous ventilation, periodic addition allows the flow of liquid in the reactor to be optimized synchronously with the reaction process, reducing the possibility of uneven mixing of chlorine and phosphorus trichloride liquid.

[0026] The reciprocating vertical movement of the vertical rod effectively reduces the generation of bubbles when chlorine gas is introduced. Compared to the prior art method of using only an agitator for mixing and stirring, the present device utilizes the rotation of the agitator while driving the vertical rod to move back and forth vertically. The vertical rod is inserted into and out of the phosphorus trichloride liquid, causing the top liquid to sink. This avoids the limitation of using a traditional single stirring method, which results in the inability to effectively stir the phosphorus trichloride liquid at the bottom of the reactor. In addition, the periodic up and down movement of the vertical rod can effectively break up and redistribute bubbles generated by the introduction of chlorine gas into the phosphorus trichloride liquid, thereby increasing the mixing contact area at the gas-liquid interface and thereby improving the reaction rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a front perspective schematic diagram of the overall structure shown in the present invention;

[0028] Figure 2 It is a schematic diagram of the interior of the reactor of the present invention;

[0029] Figure 3 It is a three-dimensional schematic diagram of the reciprocating screw and the pressure plate related components shown in the present invention;

[0030] Figure 4 It is a three-dimensional schematic diagram of the connection between the reciprocating screw rod and the ratchet wheel shown in the present invention;

[0031] Figure 5 It is a three-dimensional schematic diagram of the linkage disk and pawl related components shown in the present invention;

[0032] Figure 6 This is a schematic cutaway perspective view of the interior of the protective cover shown in the present invention;

[0033] Figure 7 This is an exploded perspective diagram of the linkage disk and the limit disk shown in the present invention;

[0034] Figure 8 This is a schematic plan view of the infrared sensor's operating trajectory shown in the present invention;

[0035] Figure 9 It is a partial three-dimensional schematic diagram of the liquid inlet component shown in the present invention;

[0036] Figure 10 It is a three-dimensional schematic diagram of the inclined plate and trigger rod related components shown in the present invention;

[0037] Figure 11 The figure is a schematic flow diagram of the phosphorus pentachloride production process of the present invention.

[0038] Wherein, the accompanying drawings in the present invention are:

[0039] 1. Reactor; 2. Air supply device; 3. Liquid storage tank; 4. Motor; 41. Agitator;

[0040] Mixing assembly: 51, reciprocating screw; 52, pressure plate; 53, guide rod; 54, ratchet; 55, support plate; 56, linkage plate; 57, pawl; 58, compression spring; 59, limit plate; 510, connecting rod; 511, push column; 512, dividing plate; 513, inner groove; 514, infrared sensor; 515, protective cover; 516, sensor strip; 517, intake pipe; 518, vertical rod;

[0041] 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 DESCRIPTION

[0042] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only 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 ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0043] The embodiments provided by the present invention will be described in detail below:

[0044] Example:

[0045] A phosphorus pentachloride production device, such as Figure 1 and Figure 2As shown, it includes a reactor 1, an air supply device 2 and a liquid storage tank 3 are provided on the outside of the reactor 1, the air supply device 2 and the liquid storage tank 3 are respectively located on the left and right sides of the reactor 1, chlorine is stored in the air supply device 2, and phosphorus trichloride liquid is stored in the liquid storage tank 3. A water pump is provided in the liquid storage tank 3, and the water pump can transport the phosphorus trichloride liquid into the reactor 1. A discharge pipe is installed on the outer surface of the reactor 1, and a valve is provided on the discharge pipe. The prepared phosphorus pentachloride can be discharged from the interior of the reactor 1 by opening the valve on the discharge pipe. The bottom surface of the reactor 1 is fixedly connected to a motor 4, and the output shaft of the motor 4 is fixedly connected to a stirrer 41, and the stirrer 41 is rotatably connected to the bottom surface of the inner cavity of the reactor 1;

[0046] like Figures 2 to 5 As shown, a mixing assembly is provided above the agitator 41, and the mixing assembly includes a reciprocating screw 51 fixedly connected to the agitator 41, the reciprocating screw 51 is located at the end of the agitator 41 away from the motor 4, the outer surface of the reciprocating screw 51 is threadedly connected to a pressure plate 52, the top surface of the inner cavity of the reactor 1 is fixedly connected to a guide rod 53, the top surface of the reactor 1 is rotatably connected to a ratchet 54, the top surface of the reactor 1 is fixedly connected to a support plate 55, the support plate 55 is located above the ratchet 54, and a linkage disk 56 is rotatably connected in the support plate 55, and a pawl 57 is rotatably connected to the side of the linkage disk 56 close to the ratchet 54, and two pawls 57 are provided, and a compression spring 58 is fixedly connected to the side of the pawl 57 away from the ratchet 54, and the compression spring 58 is in a compressed state.

[0047] Further, such as Figures 6 to 8 As shown, the mixing assembly also includes a limit plate 59 fixedly connected to the linkage plate 56, and a connecting rod 510 is fixedly connected to the side of the limit plate 59 close to the support plate 55, and a pushing column 511 is inserted into the side of the connecting rod 510 away from the center of the limit plate 59. A partition plate 512 is rotatably connected to the side of the reactor 1 close to the limit plate 59, and an inner groove 513 is equidistantly provided on the surface of the partition plate 512. There are four inner grooves 513. An infrared sensor 514 is fixedly connected to the upper surface of the partition plate 512. A protective cover 515 is fixedly connected to the top of the reactor 1. The inner cavity of the protective cover 515 is fixedly connected to the induction strip 516. The induction strip 516 is located above the infrared sensor 514. The inner cavity of the reactor 1 is connected to the air inlet pipe 517. The bottom of the pressure plate 52 is fixedly connected to a vertical rod 518, and four vertical rods 518 are equidistantly provided in a ring.

[0048] Further, such as Figure 3 and Figure 4 As shown, the end of the reciprocating screw 51 away from the stirrer 41 is rotatably connected to the top surface of the inner cavity of the reactor 1, the pressure plate 52 is adapted to the inner cavity of the reactor 1, and the pressure plate 52 is slidably connected to the outer surface of the guide rod 53.

[0049] Further, such as Figure 4 and Figure 5 As shown, the ratchet 54 is fixedly connected to the bottom surface of the reciprocating screw 51 , the outer surface of the ratchet 54 is in contact with the pawl 57 , and the end of the compression spring 58 away from the pawl 57 is fixedly connected to the linkage disk 56 .

[0050] Further, such as Figures 6 to 8 As shown, the outer arc surface of the limit plate 59 fits snugly with the outer surface of the dividing plate 512, the push column 511 fits with the inner groove 513, the shape of the sensing strip 516 is a quarter ring, the sensing strip 516 is located on the running track of the infrared sensor 514, the air intake pipe 517 is connected to the air supply device 2, and an electromagnetic valve is provided inside the air intake 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 sensing strip 516, the electromagnetic valve inside the air intake pipe 517 is opened, and when the infrared sensor 514 moves out from under the sensing strip 516, the electromagnetic valve inside the air intake pipe 517 is closed.

[0051] Further, such as Figure 9 and Figure 10 As shown, the inner cavity of the reactor 1 is provided with a liquid inlet assembly, which includes a fixed block 61 fixedly connected to the side wall of the inner cavity of the reactor 1, and four fixed blocks 61 are arranged in an annular shape at equal intervals. The side of the fixed block 61 close to the reciprocating screw 51 is fixedly connected to a support frame 62, and the side of the support frame 62 away from the fixed block 61 is rotatably connected to a nozzle 63, and the liquid outlet of the nozzle 63 faces downward. The side of the fixed block 61 close to the nozzle 63 is fixedly connected to a spring 64, and the spring 64 is located directly below the support frame 62. The side of the nozzle 63 away from the fixed block 61 is fixedly connected to an inclined plate 65, and the interior of the nozzle 63 is connected to a connecting pipe 66, which is located above the nozzle 63. The outer surface of the reactor 1 is fixedly connected to a cavity ring 67, and the interior of the cavity ring 67 is connected to a liquid inlet pipe 68. The bottom of the pressure plate 52 is fixedly connected to a trigger rod 69, and four trigger rods 69 are arranged in an annular shape at equal intervals. The four trigger rods 69 are all located directly above the four inclined plates 65 and correspond one to one.

[0052] Further, such as Figure 9 and Figure 10 As shown, one end of the spring 64 away from the fixed block 61 is fixedly connected to the nozzle 63, and the four inclined plates 65 are all inclined. When the trigger rod 69 moves downward and pushes the inclined plates 65, the nozzle 63 can be rotated through the inclined plates 65.

[0053] Further, such as Figure 9 and Figure 10As shown, one end of the four connecting pipes 66 away from the nozzle 63 is connected to the interior of the cavity ring 67, and one end of the liquid inlet pipe 68 away from the cavity ring 67 is connected to the interior 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 transported to the nozzle 63 through the connecting pipe 66.

[0054] like Figure 11 As shown, a phosphorus pentachloride production process comprises the following steps:

[0055] Step 1, raw material preparation: high-purity chlorine gas is stored in the gas supply device 2 as the gaseous raw material for the reaction, and a measured phosphorus trichloride liquid is stored in the liquid storage tank 3 as the liquid raw material for the reaction;

[0056] Step 2, reacting: introducing a measured amount of phosphorus trichloride liquid into the reactor 1, then passing high-purity chlorine gas into the phosphorus trichloride liquid, and stirring and mixing the liquid;

[0057] 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 through the discharge port to a dedicated container for storage;

[0058] Step 4: Tail gas treatment: The chlorine and volatiles not used up during the reaction process need to be purified through a dedicated tail gas treatment system to meet environmental standards.

[0059] Further, such as Figure 11 As shown, the reaction steps include: utilizing the stirrer 41 in the reactor 1 to maintain good mixing of the liquid, increase the contact area between the gas and the liquid, and promote the chemical reaction between the chlorine gas and the phosphorus trichloride to fully occur.

[0060] While working:

[0061] This device can deliver phosphorus trichloride liquid into the interior of the reactor 1 through multiple nozzles 63, avoiding the problem of concentration enrichment caused by single-point delivery. The detailed steps are as follows:

[0062] When phosphorus pentachloride needs to be produced, 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, and then transports it to the inside of the cavity ring 67 through the liquid inlet pipe 68. Then, the phosphorus trichloride liquid inside the cavity ring 67 is transported to the four nozzles 63 through four connecting pipes 66. The phosphorus trichloride is introduced into the interior of the reactor 1 through the four nozzles 63 arranged equidistantly in an annular manner inside the reactor 1.

[0063] When the motor 4 is started, the output shaft of the motor 4 rotates forward, driving the stirrer 41 to rotate forward, and the stirrer 41 causes the reciprocating screw 51 to rotate forward together with the stirrer 41, and the reciprocating screw 51 further drives the ratchet 54 to rotate clockwise. Figure 5 For reference, during the clockwise rotation of the ratchet 54, the one-way teeth on the outside of the ratchet 54 slide over the inner side of the pawl 57 one by one and squeeze the pawl 57, so that the pawl 57 rotates toward the side close to the compression spring 58 with the rotating connection with the linkage disk 56 as the axis. At this time, the compression spring 58 is compressed. As the ratchet 54 rotates, the compression spring 58 stretches, pushing the pawl 57 into the angle between the next one-way teeth. In this way, the ratchet 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 54 and the reciprocating screw 51.

[0064] During the forward rotation of the reciprocating screw 51, the bidirectional thread on the surface of the reciprocating screw 51 causes the pressure plate 52 to move back and forth vertically 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 in the direction close to the spring 64 with the rotation connection with the support frame 62 as the axis, 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, causing the orientation angle of the nozzle 63 to change again. 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 reactor 1.

[0065] In the above process, the phosphorus trichloride introduced into the reactor 1 is evenly distributed by the four nozzles 63 arranged in an annular manner. Compared with the prior art in which a delivery pipe is opened on the outer surface of the reactor 1 and a single-point delivery method is adopted, the present device uses nozzles 63 distributed in an annular manner on the side wall of the inner cavity of the reactor 1 to introduce phosphorus trichloride liquid. In the process of introducing phosphorus trichloride, the nozzle 63 cooperates with the trigger rod 69 to push the inclined plate 65, so that the direction of the nozzle 63 rotates and changes periodically, so that the range of action of each nozzle 63 changes continuously, so that phosphorus trichloride falls into the interior of the reactor 1 from four points, thereby being evenly distributed inside the reactor 1. Compared with single-point pipeline delivery, it can avoid long-term single-point delivery of phosphorus trichloride, which leads to the problem of concentration enrichment of phosphorus trichloride near the delivery pipe. The synchronous operation of the agitator 41 can further enhance the distribution of phosphorus trichloride and improve the subsequent mixing effect with chlorine.

[0066] This device can periodically feed chlorine in sections. The detailed steps are as follows:

[0067] When all the phosphorus trichloride liquid stored in the liquid storage tank 3 is introduced into the interior of the reactor 1, the staff turns off the water pump provided in the liquid storage tank 3 through the controller, and changes the output shaft of the motor 4 from forward to reverse through the controller. When the output shaft of the motor 4 reverses, the ratchet 54 fixedly connected to the reciprocating screw 51 tends to rotate counterclockwise, so that Figure 5 For 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 one-way teeth of the ratchet 54, so that the linkage disk 56 rotates counterclockwise with the ratchet 54, and further causes the limit disk 59 to rotate with the linkage disk 56.

[0068] When the limit plate 59 rotates one circle, the push post 511 is located at the eccentric position of the limit plate 59 and rotates in a circle. During this process, the limit plate 59 gradually enters the inner groove 513 opened on the surface of the dividing plate 512 according to the rotation angle. When the push post 511 enters the inner groove 513 opened on the surface of the dividing plate 512, the outer ring surface of the dividing plate 512 is separated from the contact with the outer arc surface of the limit plate 59, so that after the push post 511 enters the inner groove 513, the dividing plate 512 is pushed by the push post 511 to rotate. After the inner groove 513 of the near pushing post 511 is pushed to the position of the previous inner groove 513, the limit plate 59 has not yet rotated a full circle. As the limit plate 59 continues to rotate, the pushing post 511 is driven to rotate so that the pushing post 511 is disengaged from the inner groove 513. At this time, the limit plate 59 continues to rotate until the pushing post 511 is driven by the limit plate 59 to rotate a full circle. At this time, the dividing plate 512 rotates ninety degrees, and the arc surface of the dividing plate 512 fits with the outer surface of the limit plate 59, so that the dividing plate 512 remains stationary after the rotation.

[0069] by Figure 8 For reference, when the limit plate 59 rotates one circle, the infrared sensor 514 rotates ninety degrees counterclockwise, so when the limit plate 59 rotates four circles, the infrared sensor 514 rotates one circle. During the process of the infrared sensor 514 rotating one circle counterclockwise, the running trajectory of the infrared sensor 514 coincides with the sensing bar 516. When the infrared sensor 514 rotates to the bottom of the sensing bar 516, the solenoid valve provided in the air inlet pipe 517 is opened, so that the chlorine gas stored in the gas supply device 2 enters the phosphorus trichloride liquid in the reactor 1 through the air inlet pipe 517. When the infrared sensor 514 leaves the bottom of the sensing bar 516, the solenoid valve provided in the air inlet pipe 517 is closed, but the agitator 41 is still running for stirring.

[0070] During the counterclockwise rotation of the reciprocating screw 51, the pressure plate 52 will move back and forth vertically along the guide rod 53, and the pressure plate 52 will drive the vertical rod 518 to move together. When the pressure plate 52 moves vertically downward, the vertical rod 518 will be inserted into the phosphorus trichloride liquid inside the reactor 1. When the pressure plate 52 moves vertically upward, the vertical rod 518 will gradually leave the phosphorus trichloride liquid. In this way, the vertical rod 518 periodically inserts into and out of the phosphorus trichloride liquid, so that the vertical rod 518 drives the phosphorus trichloride liquid to form a periodic up and down circulation flow, thereby better mixing and contacting with the chlorine gas, and further improving the mixing efficiency.

[0071] In the above process, the periodic segmented delivery of chlorine is achieved by periodically opening and closing the solenoid valve. Compared with the method of continuously introducing chlorine into the phosphorus trichloride liquid in the prior art, in the present device, during the four rotations of the stirrer 41, a portion of the running trajectory of the infrared sensor 514 coincides with the sensing bar 516. When the infrared sensor 514 is below the sensing bar 516, the solenoid valve in the air inlet pipe 517 is opened. When the infrared sensor 514 leaves the bottom of the sensing bar 516, the solenoid valve in the air inlet pipe 517 is closed. Whenever the solenoid valve is opened, chlorine is introduced into the phosphorus trichloride liquid. The disturbance of the stirrer 41 can make the newly added chlorine as evenly distributed as possible in the liquid phase. Periodic ventilation combined with appropriate stirring can achieve continuous updating of the gas-liquid interface, thereby improving the efficiency of mixing of chlorine and phosphorus trichloride liquid. Compared with the continuous ventilation method, periodic addition allows the flow of liquid in the reactor 1 to be optimized synchronously with the reaction process, reducing the possibility of uneven mixing of chlorine and phosphorus trichloride liquid.

[0072] During the above process, the reciprocating vertical movement of the vertical rod 518 effectively reduces the generation of bubbles when chlorine is introduced. Compared with the method of only using the agitator 41 for mixing and stirring in the prior art, the present device uses the agitator 41 to rotate while driving the vertical rod 518 to move back and forth vertically. The vertical rod 518 is inserted into and out of the phosphorus trichloride liquid, causing the top liquid to sink. This avoids the limitation of using a traditional single stirring method, which leads to the inability to effectively stir the phosphorus trichloride liquid at the bottom of the reactor 1. In addition, the periodic up and down movement of the vertical rod 518 can effectively break up the bubbles generated by the introduction of chlorine into the phosphorus trichloride liquid and redistribute them, thereby increasing the mixing contact area of ​​the gas-liquid interface and thus improving the reaction rate.

[0073] The above descriptions are merely embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A phosphorus pentachloride production equipment, comprising a reactor, characterized in that: An air supply device and a liquid storage tank are provided on the outside of the reactor. Chlorine gas is stored in the air supply device, phosphorus trichloride liquid is stored in the liquid storage tank, a water pump is provided in the liquid storage tank, a discharge pipe is installed on the outer surface of the reactor, a motor is fixedly connected to the bottom of the reactor, an agitator is fixedly connected to the output shaft of the motor, and the agitator is rotatably connected to the inner cavity of the reactor; A mixing assembly is provided above the agitator, and the mixing assembly includes a reciprocating screw fixedly connected to the agitator, a pressure plate threadedly connected to the reciprocating screw, a guide rod fixedly connected to the inner cavity of the reactor, a ratchet rotatably connected to the top of the reactor, a support plate fixedly connected to the top of the reactor, a linkage disk rotatably connected in the support plate, a pawl rotatably connected to the side of the linkage disk close to the ratchet, two pawls are provided, and a compression spring is fixedly connected to the outer side of the pawl; the inner cavity of the reactor is connected to an air inlet pipe, the air inlet pipe is connected to the air supply device, a solenoid valve is provided inside the air inlet pipe, and the solenoid valve is electrically controlled and connected by setting an infrared sensor; four nozzles are arranged in an annular manner on the side wall of the inner cavity of the reactor; The mixing assembly also includes a limit plate fixedly connected to the upper surface of the linkage plate, the limit plate is fixedly connected to a connecting rod on one side close to the support plate, and a push column is inserted into the side of the connecting rod away from the limit plate. The top of the reactor is rotatably connected to the partition plate, and the surface of the partition plate is equidistantly provided with inner grooves, and the inner grooves are provided with four. The upper surface of the partition plate is fixedly connected to the infrared sensor, the top of the reactor is fixedly connected to a protective cover, the inner cavity of the protective cover is fixedly connected to a sensor strip, and the bottom of the pressure plate is fixedly connected to a vertical rod, and four vertical rods are equidistantly provided in a ring; The limiting plate is slidably connected to the dividing plate, the pushing column is adapted to the inner groove, and the shape of the sensing strip is a quarter of a circle.

2. A phosphorus pentachloride production equipment according to claim 1, characterized in that, The reciprocating screw is rotatably connected to the inner cavity of the reactor, the pressure plate is adapted to the inner cavity of the reactor, and the pressure plate is slidably connected to the guide rod.

3. A phosphorus pentachloride production equipment according to claim 1, characterized in that, The ratchet is fixedly connected to the reciprocating screw rod, the ratchet is slidingly connected to the pawl, and the compression spring is fixedly connected to the linkage disk.

4. A phosphorus pentachloride production equipment according to claim 1, characterized in that, The inner cavity of the reactor is provided with a liquid inlet assembly, which includes a fixed block fixedly connected to the inner cavity of the reactor, four fixed blocks are equidistantly arranged in a ring, a support frame is fixedly connected to the fixed block, and the support frame is rotatably connected to the nozzle, a spring is fixedly connected to the side of the fixed block close to the nozzle, an inclined plate is fixedly connected to the side of the nozzle away from the fixed block, a connecting pipe is connected to the interior of the nozzle, a cavity ring is fixedly connected to the outer surface of the reactor, the interior of the cavity ring is connected to the liquid inlet pipe, and a trigger rod is fixedly connected to the bottom of the pressure plate, and four trigger rods are equidistantly arranged in a ring.

5. A phosphorus pentachloride production equipment according to claim 4, characterized in that, The spring is fixedly connected to the nozzle, and the four inclined plates are all arranged obliquely.

6. A phosphorus pentachloride production equipment according to claim 4, characterized in that, The four connecting pipes are all connected to the cavity ring, and the liquid inlet pipe is connected to the liquid storage tank.

7. A process for producing phosphorus pentachloride, characterized in that: The phosphorus pentachloride production equipment according to any one of claims 1 to 6 comprises the following steps: Step 1, raw material preparation: high-purity chlorine is stored in the gas supply device as the gaseous raw material for the reaction, and measured phosphorus trichloride liquid is stored in the liquid storage tank as the liquid raw material for the reaction; Step 2, reacting: introducing a measured amount of phosphorus trichloride liquid into a reactor, then passing high-purity chlorine gas into the phosphorus trichloride liquid, and stirring and mixing the liquid; Step 3, product collection: Phosphorus pentachloride is the main product of the reaction and precipitates as a solid after the reaction is completed. The cooled phosphorus pentachloride is transferred from the reactor through the discharge port to a dedicated container for storage; Step 4: Tail gas treatment: The chlorine and volatiles not used up during the reaction process need to be purified through a dedicated tail gas treatment system to meet environmental standards.

8. A process for producing phosphorus pentachloride according to claim 7, characterized in that: The reaction includes: utilizing an agitator in the reactor to maintain good mixing of the liquid, increasing the contact area between the gas and the liquid, and promoting the chemical reaction between the chlorine gas and the phosphorus trichloride to fully occur.

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