A continuous synthesis apparatus and method for hexachlorocyclotriphosphazene

Abstract

This invention belongs to the field of hexachlorocyclotriphosphazene synthesis technology, specifically a continuous synthesis apparatus and method for hexachlorocyclotriphosphazene. The continuous synthesis apparatus includes a three-necked flask, inside which are installed a thermometer, a stirrer, and a water separator. A condenser is located at the upper end of the water separator. An alcohol lamp is located below the three-necked flask, positioned above an iron stand. A fixing rod is located at the upper end of the iron stand near the alcohol lamp. The three-necked flask is fixedly connected to the arc surface of the fixing rod. An adjustment device is located at the upper surface of the iron stand away from the three-necked flask. The adjustment device includes a first fixing arm, one end of which is connected to the water separator, and the other end of which slides on the surface of the fixing rod. By changing the connection method between the water separator, the condenser, and the iron stand, the water separator and the condenser can move automatically, while increasing the accuracy of subsequent insertion of the condenser into the three-necked flask.

Description

Technical Field

[0001] This invention belongs to the field of hexachlorocyclotriphosphazene synthesis, specifically a continuous synthesis apparatus and method for hexachlorocyclotriphosphazene. Background Technology

[0002] Hexachlorocyclotriphosphazene is an important chemical intermediate, mainly used in the synthesis of chlorine-containing specialty monomers and copolymers, such as high-performance chloroplastics like polytetrachloroethylene and polyvinyl chloride propylene. In addition, it can also be used to synthesize fine chemicals containing phosphorus and nitrogen elements, such as flame retardants, crosslinking agents, and photoinitiators.

[0003] The existing process for synthesizing hexachlorocyclotriphosphazene involves adding tetrachloroethane and ammonium chloride to a three-necked flask, then fixing the flask to a support rod on the surface of an iron stand. A thermometer, a water separator, and a stirrer are then inserted into the flask. An alcohol lamp is placed at the bottom of the flask, and after the flask is secured, the lamp is lit to heat and evaporate some of the solvent, carrying away water from the system, until the solvent in the flask is no longer cloudy. Once the solvent inside the flask is clear, the water separator is removed, and phosphorus pentachloride and a small amount of pyridine are quickly added. The condenser tube on the water separator is directly connected to the three-necked flask; heating under reflux continues.

[0004] However, in the above operation, since the three-necked flask is at a high temperature, the operator can only move the position of the water distributor and the condenser. Before this operation, phosphorus pentachloride and a small amount of pyridine must be added to the three-necked flask, and the condenser must be quickly moved into the interior of the three-necked flask. Since the traditional way of placing the water distributor and the condenser is to fix them to a certain point on the surface of the fixing rod on the iron stand, if it is necessary to move the position of the water distributor and the condenser, the connection between the water distributor and the iron stand must be disconnected first, and then the position of the water distributor must be adjusted. After adjusting the water distributor to the designated position, the water distributor is fixed. Then the condenser must be operated in the same way. This operation is very cumbersome and time-consuming.

[0005] Therefore, the present invention provides a continuous synthesis apparatus and synthesis method for hexachlorocyclotriphosphazene. Summary of the Invention

[0006] In order to overcome the shortcomings of the prior art, at least one technical problem raised in the background art is solved.

[0007] The technical solution adopted by this invention to solve its technical problem is: a continuous synthesis equipment and method for hexachlorocyclotriphosphazene, comprising the following steps:

[0008] Step 1: Add tetrachloroethane and ammonium chloride to a three-necked flask, then insert a thermometer, a water separator, and a stirrer. A condenser is connected above the water separator. Heat the mixture to evaporate some of the solvent, while also removing water from the system, until the solvent is no longer cloudy.

[0009] Step 2: Separate the water separator from the three-necked flask, quickly add phosphorus pentachloride and a small amount of pyridine to the three-necked flask, connect the condenser on the water separator directly to the three-necked flask, continue heating the three-necked flask until the solvent in the condenser refluxes, control the temperature at 135°C, and react for 20 hours.

[0010] Step 3: Filter to remove excess ammonium chloride from the three-necked flask, remove the solvent by vacuum distillation of the three-necked flask to obtain a yellow crystalline crude product, dissolve the crude product in benzene, and then evaporate the solvent under vacuum to obtain white crystals;

[0011] Step 4: Place the white crystals in a round-bottom flask, add petroleum ether, and heat to 60°C to dissolve them. Since the filamentous structures inside the white crystals are insoluble, they can be separated out. Add 98% concentrated sulfuric acid to the round-bottom flask to prepare a petroleum ether solution. Extract the hexachlorocyclotriphosphazene from the petroleum ether solution multiple times. Combine the hexachlorocyclotriphosphazene with the sulfuric acid extract, and then dilute with water to prepare a 60% sulfuric acid solution. The hexachlorocyclotriphosphazene precipitates out again. Dissolve the precipitated product in hot heptane and decolorize with activated carbon to obtain a white solid, which is hexachlorocyclotriphosphazene.

[0012] A continuous synthesis apparatus for hexachlorocyclotriphosphazene, applicable to the aforementioned synthesis method of hexachlorocyclotriphosphazene, includes a three-necked flask. Inside the three-necked flask are a thermometer, a stirrer, and a water separator. A condenser is located at the upper end of the water separator. An alcohol lamp is positioned below the three-necked flask and above an iron stand. A fixing rod is located at the upper end of the iron stand near the alcohol lamp. The three-necked flask is fixedly connected to the arc surface of the fixing rod. An adjustment device is located at the upper surface of the iron stand away from the three-necked flask. The adjustment device includes: a first fixing... The first fixed arm has one end connected to the water distributor and the other end sliding on the surface of the fixed rod, and can rotate on the arc surface of the fixed rod; a connecting frame has one end sliding on the arc surface of the fixed rod; a second fixed arm has one end connected to the condenser pipe and slides inside the connecting frame, with its initial position located at the rightmost side of the connecting frame; and a limiting ring is located on the arc surface of the fixed rod, between the first fixed arm and the connecting frame, and is engaged with the first fixed arm.

[0013] Preferably, the adjusting device further includes: a drive screw, which is rotatably connected to the upper surface of the iron frame near the fixed rod; a transition frame, which slides on the arc surface of the fixed rod, and a first fixed arm is fixedly connected to one end of the transition frame; a first connecting arm, one end of which engages with the surface of the drive screw; a limiting strip, which is fixedly connected to the two sides of the first connecting arm away from the drive screw; a transition arm, one end of which is fixedly connected to the transition frame; and a moving groove, wherein the two sides of the transition arm away from the fixed rod are provided with a moving groove, the limiting strip slides on the inner wall of the moving groove, and the limiting strip engages with the moving rod. The moving grooves are interlocked; rubber pillars are provided at the upper end of the adapter frame; an arc-shaped track is provided inside the limiting ring, and the rubber pillars are interlocked with the arc-shaped track; a second connecting arm is provided, one end of which engages with the surface of the driving screw, and the other end of which is fixedly connected to the connecting frame; an auxiliary turntable is fixedly connected to the upper end of the driving screw; a drive motor is provided on the side wall of the iron frame near the auxiliary turntable; and a drive track is provided, one end of which is rotatably connected to the arc surface of the auxiliary turntable, and the other end of which is rotatably connected to the drive motor.

[0014] Preferably, the trajectory of the arc-shaped track is arc-shaped, and the rubber column is in a compressed state on the inner wall of the arc-shaped track.

[0015] Preferably, the upper surface of the adapter frame is connected to a universal ball, which is in pairs, with one universal ball connected to the upper surface of the adapter frame and the other universal ball connected to the lower surface of the rubber column.

[0016] Preferably, the side wall of the iron frame is provided with a sliding rail, and an auxiliary roller is fixedly connected to the side of the first connecting arm away from the adapter arm, and the auxiliary roller slides on the inner wall of the sliding rail.

[0017] Preferably, an infrared ray is provided at the upper end of the iron stand near the three-necked flask, and the infrared ray is at the same horizontal level as the three-necked flask. An infrared receiver is provided on the arc surface of the fixing rod, and the infrared receiver is at the same horizontal level as the infrared ray. The infrared receiver is connected to the drive motor.

[0018] Preferably, a first auxiliary gear is fixedly connected to the end of the active screw near the auxiliary turntable. A sliding frame is provided on the upper side wall of the iron frame. A sliding rack is slidably connected inside the sliding frame. A fixing ring is fixedly connected to one side of the sliding rack. A sliding rod is fixedly connected inside the sliding frame, and a fixing ring is slidably connected to the arc surface of the sliding rod. A compression spring is sleeved on the arc surface of the sliding rod. One end of the compression spring is fixedly connected to the sliding frame, and the other end of the compression spring is fixedly connected to the fixing ring. A second auxiliary gear is meshed with one end of the sliding rack, and the second auxiliary gear meshes with the first auxiliary gear. The sliding rack has a fixed plate fixedly connected to one end away from the second auxiliary gear. A fixed shaft is fixedly connected inside the fixed plate. A connecting ring is rotatably connected to the arc surface of the fixed shaft. A return spring is sleeved on the arc surface of the fixed shaft. An abutment plate is fixedly connected to one end of the connecting ring. An arc-shaped groove is formed on the surface of the abutment plate. A one-way abutment plate is provided on one side of the fixed plate. The one-way abutment plate abuts against the rear of the abutment plate. A slot is formed on the upper surface of the connecting frame. An abutment rod is slidably connected to the inner wall of the slot on the upper surface of the connecting frame. The abutment rod is fixedly connected to the upper surface of the second fixed arm and contacts the arc-shaped groove.

[0019] Preferably, the inner wall of the groove on the upper surface of the connecting frame is provided with a limiting buckle, and the abutment rod is engaged with the inner wall of the limiting buckle.

[0020] Preferably, a rotating plate is rotatably connected to the upper interior of the adapter arm, one end of the rotating plate is fixedly connected to a limiting plate, and the initial position of the limiting plate is located above the moving groove. Both ends of the rotating plate are fixedly connected to coil springs.

[0021] The beneficial effects of this invention are as follows:

[0022] 1. The continuous synthesis equipment and method for hexachlorocyclotriphosphazene described in this invention, by changing the connection method between the water separator and the condenser and the iron stand, allows the water separator and the condenser to move automatically, while increasing the accuracy of the subsequent insertion of the condenser into the three-necked flask.

[0023] 2. The continuous synthesis equipment and method for hexachlorocyclotriphosphazene described in this invention, by setting up infrared rays and infrared receivers, can determine whether to start the adjustment device by detecting the turbidity of the solvent inside the three-necked flask. This not only reduces the number of operational tasks, but also automatically shuts off the adjustment device when the condenser is subsequently inserted into the three-necked flask.

[0024] 3. The continuous synthesis equipment and method for hexachlorocyclotriphosphazene described in this invention, by setting a second auxiliary gear, can automatically move the sliding rack when the active screw rotates, thereby automatically moving the condenser tube to the top of the three-necked flask. After the condenser tube is inserted into the three-necked flask, it can also be automatically reset. Attached Figure Description

[0025] The invention will now be further described with reference to the accompanying drawings.

[0026] Figure 1 This is a perspective view of Embodiment 2 of the present invention;

[0027] Figure 2 This is a flowchart of Embodiment 1 of the present invention;

[0028] Figure 3 This is a side view of Embodiment 2 of the present invention;

[0029] Figure 4 This is a partial view of the active screw of the present invention;

[0030] Figure 5 This is an internal view of the sliding frame of the present invention;

[0031] Figure 6 yes Figure 5 Enlarged view of a portion of point A in the middle;

[0032] Figure 7 This is a top view of the active screw of the present invention;

[0033] Figure 8 This is a rear view of the abutment plate of the present invention;

[0034] Figure 9 This is a perspective view of the first connecting arm of the present invention;

[0035] Figure 10 yes Figure 9 Enlarged view of a section at point B in the middle;

[0036] Figure 11 This is a cross-sectional view of the limiting ring of the present invention;

[0037] Figure 12 This is a perspective view of the infrared receiver of the present invention;

[0038] In the diagram: 1. Base frame; 2. Fixing rod; 3. Three-necked flask; 4. Water distributor; 5. Condenser; 6. Adjusting device; 601. Drive screw; 602. First connecting arm; 603. First fixing arm; 604. Second fixing arm; 605. Drive motor; 606. Drive track; 607. Auxiliary turntable; 608. First auxiliary gear; 609. Sliding rail; 610. Connecting frame; 611. Sliding frame; 612. Second auxiliary gear; 613. Sliding rack; 614. Fixing ring; 615. Sliding rod; 616. Compression spring; 617. Fixing plate; 618. Abutment plate; 619. Arc-shaped groove; 620. Fixed shaft; 621. Return spring; 622. Connecting ring; 623. Adapter arm; 624. Limiting ring; 625. Moving groove; 626. Limiting strip; 627. Coil spring; 628. Rotating plate; 629. Limiting plate; 630. Adapter frame; 631. Universal ball; 632. Rubber column; 633. Arc-shaped track; 634. Infrared ray; 635. Infrared receiver; 636. Auxiliary roller; 637. Second connecting arm; 638. Abutment rod; 639. Limiting buckle; 640. One-way abutment plate. Detailed Implementation

[0039] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments. Example

[0040] like Figure 2 As shown in the figure, a continuous synthesis apparatus and method for hexachlorocyclotriphosphazene according to an embodiment of the present invention includes the following steps:

[0041] Step 1: Add tetrachloroethane and ammonium chloride to the three-necked flask 3, then insert a thermometer, a water separator 4 and a stirrer. A condenser 5 is connected above the water separator 4. Heat the mixture to evaporate some of the solvent, while also removing water from the system, until the solvent is no longer cloudy.

[0042] Step 2: Separate the water separator 4 from the three-necked flask 3, quickly add phosphorus pentachloride and a small amount of pyridine to the three-necked flask 3, connect the condenser 5 on the water separator 4 directly to the three-necked flask 3, continue heating the three-necked flask 3 until the solvent in the condenser 5 refluxes, control the temperature at 135°C, and react for 20 hours.

[0043] Step 3: Filter to remove excess ammonium chloride from three-necked flask 3, remove solvent by vacuum distillation of three-necked flask 3 to obtain yellow crystalline crude product, dissolve the crude product in benzene, and then evaporate the solvent under vacuum to obtain white crystals;

[0044] Step 4: Place the white crystals in a round-bottom flask, add petroleum ether, and heat to 60°C to dissolve them. Since the filamentous structures inside the white crystals are insoluble, they can be separated out. Add 98% concentrated sulfuric acid to the round-bottom flask to prepare a petroleum ether solution. Extract the hexachlorocyclotriphosphazene from the petroleum ether solution multiple times. Combine the hexachlorocyclotriphosphazene with the sulfuric acid extract, and then dilute with water to prepare a 60% sulfuric acid solution. The hexachlorocyclotriphosphazene precipitates out again. Dissolve the precipitated product in hot heptane and decolorize with activated carbon to obtain a white solid, which is hexachlorocyclotriphosphazene. Example

[0045] like Figures 1 to 11 As shown, a continuous synthesis apparatus for hexachlorocyclotriphosphazene is described. This apparatus is suitable for the aforementioned synthesis method of hexachlorocyclotriphosphazene. It includes a three-necked flask 3, inside which a thermometer, a stirrer, and a water separator 4 are installed. A condenser 5 is located at the upper end of the water separator 4. An alcohol lamp 7 is located below the three-necked flask 3, positioned above an iron stand 1. A fixing rod 2 is located at the upper end of the iron stand 1 near the alcohol lamp 7. The three-necked flask 3 is fixedly connected to the arc surface of the fixing rod 2. An adjusting device 6 is located at the upper surface of the iron stand 1 away from the three-necked flask 3. The adjusting device 6 includes a first fixing arm 603, one end of which is connected to the water separator 4. The other end of a fixed arm 603 slides on the surface of a fixed rod 2, and the first fixed arm 603 can rotate on the arc surface of the fixed rod 2; a connecting frame 610, one end of which slides on the arc surface of the fixed rod 2; a second fixed arm 604, one end of which is connected to the condenser pipe 5, and the second fixed arm 604 slides inside the connecting frame 610, with the initial position of the second fixed arm 604 located at the rightmost side of the connecting frame 610; a limiting ring 624, which is located on the arc surface of the fixed rod 2, between the first fixed arm 603 and the connecting frame 610, and is engaged with the first fixed arm 603.

[0046] Specifically, when continuously synthesizing hexachlorocyclotriphosphazene, tetrachloroethane and ammonium chloride are added to the inside of a three-necked flask 3. The flask 3 is then fixed to a fixing rod on the upper surface of an iron stand 1. A thermometer, a water separator 4, and a stirrer are then inserted into the flask 3. An alcohol lamp 7 is placed at the bottom of the flask 3. After the flask 3 is fixed, the alcohol lamp 7 is lit to heat and evaporate some of the solvent in the flask 3, simultaneously removing water from the system. This continues until the solvent in the flask 3 is no longer cloudy. When the solvent inside the flask 3 is no longer cloudy, the water separator 4 is removed, and phosphorus pentachloride and a small amount of pyridine are quickly added. The condenser 5 on the water separator 4 is then directly connected to the three-necked flask 3. On flask 3; continue heating under reflux. When the solvent inside the three-necked flask 3 is observed to be clear, activate the first fixed arm 603 and the connecting frame 610, causing them to move upwards along the inner wall of the fixed rod 2. The second fixed arm 604, connected to the connecting frame 610, will also be moved. As the first fixed arm 603 moves upwards, the water separator 4 will also be moved upwards, thus separating the pipe of the water separator 4 from the three-necked flask 3. Simultaneously, the connecting frame 610 will also move the condenser tube 5 upwards via the second fixed arm 604, with the condenser tube 5 moving synchronously with the water separator 4. After the pipe detaches from the three-necked flask 3, phosphorus pentachloride and a small amount of pyridine can be added to the three-necked flask 3. At this time, the first fixing arm 603 will engage with the limiting ring 624. Then, the limiting ring 624 is rotated, causing the limiting ring 624 to rotate along with the water distributor 4 via the first fixing arm 603. This prevents the pipe of the water distributor 4 from being directly above the three-necked flask 3. At the same time as the first fixing arm 603 engages with the limiting ring 624, the connecting frame 610 continues to move upward along the fixing rod 2, causing the pipe of the condenser tube 5 to detach from the water distributor 4. Since the three-necked flask 3 is no longer obstructing the water distributor 4, the water distributor 4 can be rotated by the limiting ring 624. When the flask is rotated to a position where it is no longer directly above the three-necked flask 3, the connecting frame 610 is closed, causing it to stop sliding on the surface of the fixing rod 2. Then, the second fixing arm 604 is activated, sliding along the inner wall of the connecting frame 610. The second fixing arm 604 will move the condenser tube 5 towards the top of the three-necked flask 3. When the condenser tube 5 reaches the top of the three-necked flask 3, the second fixing arm 604 stops, and the connecting frame 610 is activated again. The connecting frame 610 will move the condenser tube 5 along with the second fixing arm 604 until the pipe below the condenser tube 5 is inserted into the interior of the three-necked flask 3. Then, the connecting frame 610 is closed and stops moving.By installing a first fixing arm 603 between the water separator 4 and the fixing rod 2, and a second fixing arm 604 and a connecting frame 610 between the condenser tube 5 and the fixing rod 2, the water separator 4 and the condenser tube 5 can be moved synchronously when the solvent inside the three-necked flask 3 is not turbid. This allows for the simultaneous removal of the water separator 4 and the direct connection of the condenser tube 5 from the water separator 4 to the three-necked flask 3 when the operator adds phosphorus pentachloride and a small amount of pyridine to the three-necked flask 3, reducing time and personnel costs.

[0047] like Figures 1 to 11 As shown, the adjusting device 6 further includes: a drive screw 601, which is rotatably connected to the upper surface of the iron frame 1 near the fixed rod 2; a transition frame 630, which slides on the arc surface of the fixed rod 2, and one end of the transition frame 630 is fixedly connected to a first fixed arm 603; a first connecting arm 602, one end of which engages with the surface of the drive screw 601; a limiting strip 626, which is fixedly connected to the two sides of the first connecting arm 602 away from the drive screw 601; a transition arm 623, one end of which is fixedly connected to the transition frame 630; and a moving groove 625, which is provided on the two sides of the transition arm 623 away from the fixed rod 2, and the limiting strip 626 slides on the inner wall of the moving groove 625, and the limiting strip 626 engages with the moving groove. 625 are interlocked; rubber pillars 632, several rubber pillars 632 are provided at the upper end of the adapter frame 630; arc-shaped track 633, an arc-shaped track 633 is provided inside the limiting ring 624, the rubber pillars 632 are interlocked with the arc-shaped track 633; ​​second connecting arm 637, one end of the second connecting arm 637 is engaged with the surface of the driving screw 601, and the other end of the second connecting arm 637 is fixedly connected to the connecting frame 610; auxiliary turntable 607, the auxiliary turntable 607 is fixedly connected to the upper end of the driving screw 601; drive motor 605, the drive motor 605 is provided on the side wall of the iron frame 1 near the end of the auxiliary turntable 607; drive track 606, one end of the drive track 606 is rotatably connected to the arc surface of the auxiliary turntable 607, and the other end of the drive track 606 is fixed to the drive motor 605.

[0048] Specifically, when the solvent inside the three-necked flask 3 is not turbid, the drive motor 605 is started. At this time, the drive track 606 will be driven to rotate. The auxiliary turntable 607 connected to the drive track 606 will also drive the drive screw 601 to rotate. Due to the rotation of the drive screw 601, the first connecting arm 602, which meshes with the drive screw 601, cannot rotate due to the constraint of the adapter arm 623, and can only move upward. Since the limit strip 626 is engaged with the inner wall of the moving groove 625, the first connecting arm 602 will move with the adapter arm 623. The adapter arm 623 will drive the water distributor 4 to move through the adapter frame 630. During the movement of the adapter frame 630, when the rubber post 632 on the upper surface of the adapter frame 630 engages with the arc-shaped track 633 inside the limiting ring 624, the adapter arm 623, which is fixed to the adapter frame 630, can no longer move due to the fixation of the rubber post 632. The limiting strip 626 will also move upward along the moving groove 625, realizing the separation of the first connecting arm 602 and the adapter arm 623. At this time, the pipe of the water distributor 4 also leaves the interior of the three-necked flask 3. At this time, the limiting ring 624 is started to rotate, and the limiting ring 624 will rotate with the water distributor 4, so that the pipe of the water distributor 4 is no longer directly above the three-necked flask 3; in the active screw When the first connecting arm 602 separates from the adapter arm 623, the second connecting arm 637, which meshes with the drive screw 601, will also move upward due to the constraint of the connecting frame 610. When the first connecting arm 602 separates from the adapter arm 623, the second connecting arm 637, still carrying the condenser tube 5, will continue to move upward, causing the pipe below the condenser tube 5 to disengage from the interior of the water distributor 4. After disengagement, the second fixing arm 604 is activated, causing the second fixing arm 604 to slide along the inner wall of the connecting frame 610. The second fixing arm 604 will then move the condenser tube 5 directly upwards towards the three-necked flask 3. At this time, the drive motor 605 is adjusted to drive the drive screw. Reversing step 601 causes the second connecting arm 637 to move downwards with the condenser tube 5 until it extends into the interior of the three-necked flask 3. Finally, the drive motor 605 is turned off, causing the active screw 601 to stop rotating. By setting the active screw 601, the initial upward movement speed of the first connecting arm 602 and the second connecting arm 637, which mesh with the active screw 601, can be synchronized, avoiding collisions with the condenser tube 5 due to the excessively fast movement of the water distributor 4. Furthermore, by setting the limiting strip 626 and the moving groove 625, the separation of the first connecting arm 602 and the transition arm 623 can be made smoother when the adapter frame 630 and the limiting ring 624 are fixed.

[0049] The trajectory of the arc track 633 is arc-shaped, and the rubber column 632 is in a compressed state on the inner wall of the arc track 633.

[0050] Specifically, although the rubber post 632 is located directly below the arc-shaped track 633, misalignment can still easily occur when the adapter frame 630 contacts the limiting ring 624, causing the adapter frame 630 to fail to be fixed below the limiting ring 624. To address this, the rubber post 632 is made of rubber, and the trajectory of the arc-shaped track 633 is made arc-shaped. This not only makes the connection between the rubber post 632 and the arc-shaped track 633 smoother, but also allows the arc-shaped track 633 to completely fix the rubber post 632.

[0051] The upper surface of the adapter frame 630 is connected to a universal ball 631. The universal balls 631 are in pairs, with one universal ball 631 connected to the upper surface of the adapter frame 630 and the other universal ball 631 connected to the lower surface of the rubber post 632.

[0052] Specifically, in order to make the rubber column 632 move more smoothly inside the limiting ring 624, a universal ball 631 is provided on the lower surface of the rubber column 632. This allows the rubber column 632 to change its position freely according to the trajectory of the arc track 633 when it is inserted into the limiting ring 624, without affecting the stable placement of the adapter frame 630.

[0053] like Figures 1 to 12 As shown, a sliding rail 609 is provided on the side wall of the iron frame 1. An auxiliary roller 636 is fixedly connected to the side of the first connecting arm 602 away from the adapter arm 623. The auxiliary roller 636 slides on the inner wall of the sliding rail 609.

[0054] Specifically, when the adapter frame 630 is fixed to the limiting ring 624, the first connecting arm 602 needs to be separated from the adapter arm 623. However, at this time, the first connecting arm 602 is not restrained by the adapter arm 623 and is easily rotated by the active screw 601, which may damage the instrument on the upper end of the iron frame 1. Therefore, an auxiliary roller 636 is set at one end of the first connecting arm 602, and the auxiliary roller 636 moves on the sliding rail 609 on the side wall of the iron frame 1. Even if the first connecting arm 602 is separated from the adapter arm 623, the first connecting arm 602 will move upward along the active screw 601 and move synchronously with the second connecting arm 637.

[0055] An infrared ray 634 is installed at the upper end of the iron stand 1 near the three-necked flask 3, and the infrared ray 634 and the three-necked flask 3 are on the same horizontal line. An infrared receiver 635 is installed on the arc surface of the fixing rod 2, and the infrared receiver 635 and the infrared ray 634 are on the same horizontal line. The infrared receiver 635 is connected to the drive motor 605.

[0056] Specifically, since the drive motor 605 will start when the solvent inside the three-necked flask 3 is clear, an infrared ray 634 is placed at the same horizontal level as the three-necked flask 3. Then, tetrachloroethane and ammonium chloride are added inside the three-necked flask 3, and the infrared ray 634 is activated to irradiate the three-necked flask 3. At this time, the infrared ray 634 cannot be captured by the infrared receiver 635 opposite the three-necked flask 3. The alcohol lamp 7 is lit to heat the three-necked flask 3. When the gas inside the three-necked flask 3 is no longer clear, the infrared receiver 635 will capture the infrared ray 634, thereby transmitting a signal to the drive motor 605, causing the drive motor 605 to start, thereby driving the active screw 601 to rotate. When the pipe below the condenser tube 5 is inserted into the three-necked flask 3, the pipe below the condenser tube 5 will also block the infrared rays, so that the infrared receiver 635 cannot receive the signal, causing the drive motor 605 to automatically shut down. Example

[0057] like Figures 1 to 8 As shown in Comparative Embodiment 2, another embodiment of the present invention is as follows: A first auxiliary gear 608 is fixedly connected to one end of the surface of the active screw 601 near the auxiliary turntable 607. A sliding frame 611 is provided on the upper side wall of the iron frame 1. A sliding rack 613 is slidably connected inside the sliding frame 611. A fixing ring 614 is fixedly connected to one side of the sliding rack 613. A sliding rod 615 is fixedly connected inside the sliding frame 611, and the fixing ring 614 is slidably connected to the arc surface of the sliding rod 615. A compression spring 616 is sleeved on the arc surface of the sliding rod 615. One end of the compression spring 616 is fixedly connected to the sliding frame 611, and the other end of the compression spring 616 is fixedly connected to the fixing ring 614. A second auxiliary gear 612 is meshed with one end of the sliding rack 613. The second auxiliary gear 612 and the first… The auxiliary gear 608 meshes with the sliding rack 613. A fixed plate 617 is fixedly connected to the end of the sliding rack 613 away from the second auxiliary gear 612. A fixed shaft 620 is fixedly connected inside the fixed plate 617. A connecting ring 622 is rotatably connected to the arc surface of the fixed shaft 620. A return spring 621 is sleeved on the arc surface of the fixed shaft 620. An abutment plate 618 is fixedly connected to one end of the connecting ring 622. An arc-shaped groove 619 is opened on the surface of the abutment plate 618. A one-way abutment plate 640 is provided on one side of the fixed plate 617. The one-way abutment plate 640 abuts against the rear of the abutment plate 618. A slot is opened on the upper surface of the connecting frame 610. An abutment rod 638 is slidably connected to the inner wall of the slot on the upper surface of the connecting frame 610. The abutment rod 638 is fixedly connected to the upper surface of the second fixed arm 604, and the abutment rod 638 is in contact with the arc-shaped groove 619.

[0058] Specifically, when the drive screw 601 rotates, the first auxiliary gear 608 located above the drive screw 601 will also be driven to rotate, and the sliding rack 613 can be moved through the second auxiliary gear 612. The fixed plate 617 located on one side of the sliding rack 613 will also move towards the direction of the second auxiliary gear 612, and the abutment plate 618 connected to the fixed plate 617 will also be driven. Since the drive screw 601 is rotating at this time, the second connecting arm 637 will also drive the condenser tube 5 to move upward through the second fixed arm 604. When it moves to a certain position, the arc-shaped groove 619 opened on the surface of the abutment plate 618 will contact the abutment rod 638 on the upper surface of the second fixed arm 604, thereby carrying the abutment rod 638 towards Moving in the direction of the fixed rod 2, the second fixed arm 604, which is fixed to the abutment rod 638, will also move along with the condenser tube 5 to directly above the three-necked flask 3. Then, the drive motor 605 reverses, and the second auxiliary gear 612 will also reset the sliding rack 613. At this time, the compression spring 616 will also release its elasticity to facilitate the reset of the sliding rack 613. During the reset process of the sliding rack 613, when the abutment plate 618 contacts the condenser tube 5, the abutment plate 618 will also automatically bend, so as not to interfere with the movement track of the condenser tube 5. The reset spring 621 will also drive the connecting ring 622 to automatically reset. Then, when the pipe below the condenser tube 5 is inserted into the three-necked flask 3, the sliding rack 613 also completes the reset.

[0059] like Figures 1 to 7 As shown, the inner wall of the slot on the upper surface of the connecting frame 610 is provided with a limiting buckle 639, and the abutment rod 638 is engaged with the inner wall of the limiting buckle 639.

[0060] Specifically, when the arc-shaped groove 619 on the surface of the abutment plate 618 pushes the abutment rod 638 to move, the abutment rod 638 can be fixed at a certain position on the upper surface groove of the connecting frame 610 by setting the limit buckle 639. At this time, the pipe below the condenser tube 5 is exactly above the three-necked flask 3. At this time, simply reverse the active screw 601 to allow the condenser tube 5 to be inserted into the interior of the three-necked flask 3.

[0061] like Figure 10 As shown, a rotating plate 628 is rotatably connected to the upper interior of the adapter arm 623. One end of the rotating plate 628 is fixedly connected to a limiting plate 629, and the initial position of the limiting plate 629 is located above the moving groove 625. Both ends of the rotating plate 628 are fixedly connected to coil springs 627.

[0062] Specifically, since the first connecting arm 602 needs to move along with the adapter arm 623 during the movement process, in order to prevent the limiting strip 626 from prematurely detaching from the inner wall of the moving groove 625, a limiting plate 629 is set inside the adapter arm 623, and coil springs 627 are set on both sides of the rotating plate 628. When the limiting strip 626 prematurely detaches from the inner wall of the moving groove 625, the limiting strip 626 will abut against the lower surface of the limiting plate 629, thus preventing the limiting strip 626 from prematurely detaching from the inner wall of the moving groove 625. When the first connecting arm 602 and the adapter arm 623 separate, the rotating plate 628 will also rotate through the deformation of the coil spring 627, so that the first connecting arm 602 and the adapter arm 623 can be separated normally. After the separation is completed, the coil spring 627 will release its elasticity, causing the limiting plate 629 to reset.

[0063] Working principle: When continuously synthesizing hexachlorocyclotriphosphazene, tetrachloroethane and ammonium chloride are added to the three-necked flask 3. The flask 3 is then fixed to a fixing rod on the upper surface of the iron stand 1. A thermometer, water separator, and stirrer 4 are then inserted into the flask 3. An alcohol lamp 7 is placed at the bottom of the flask 3. After the flask 3 is fixed, the alcohol lamp 7 is lit, heating and distilling off some of the solvent in the flask 3, while also removing water from the system. When the solvent inside the flask 3 is no longer turbid, the infrared receiver 635 will capture infrared rays 634, thereby transmitting a signal to the drive motor 605, causing the drive motor 605 to start. At this time, the drive track 606 will be... This rotation causes the auxiliary turntable 607, connected to the drive track 606, to rotate the drive screw 601. Due to the rotation of the drive screw 601, the first connecting arm 602, meshing with the drive screw 601, cannot rotate due to the constraint of the adapter arm 623, and can only move upwards. Since the limiting strip 626 is engaged with the inner wall of the moving groove 625, the first connecting arm 602 will move with the adapter arm 623. The adapter arm 623 will drive the water distributor 4 to move through the adapter frame 630. During the movement of the adapter frame 630, when the rubber post 632 on the upper surface of the adapter frame 630 engages with the arc-shaped track 633 inside the limiting ring 624, it is fixed to the adapter frame 630. The fixed adapter arm 623 is immobilized by the rubber column 632, and the limiting strip 626 will move upward along the moving groove 625, separating the first connecting arm 602 from the adapter arm 623. At this time, the pipe of the water distributor 4 also leaves the interior of the three-necked flask 3. Then, the limiting ring 624 is activated to rotate, which will cause the water distributor 4 to rotate, so that the pipe of the water distributor 4 is no longer directly above the three-necked flask 3. When the drive screw 601 is activated, the second connecting arm 637, which meshes with the drive screw 601, will also move upward due to the restraint of the connecting frame 610. When the first connecting arm 602 separates from the adapter arm 623, the second connecting arm 637 still carries the condensate. The tube 5 will continue to move upward, causing the pipe below the condenser tube 5 to detach from the interior of the distributor 4. After detachment, the arc-shaped groove 619 on the surface of the abutment plate 618 will contact the abutment rod 638 on the upper surface of the second fixed arm 604, thereby moving the abutment rod 638 towards the fixed rod 2. The second fixed arm 604, which is fixed to the abutment rod 638, will also move together with the condenser tube 5 to the top of the three-necked flask 3. At this time, the drive motor 605 is adjusted to drive the active screw 601 to reverse, thereby causing the second connecting arm 637 to move downward with the condenser tube 5 until it extends into the interior of the three-necked flask 3. Finally, the drive motor 605 is turned off so that the active screw 601 stops rotating.By setting the active screw 601, the initial upward movement speeds of the first connecting arm 602 and the second connecting arm 637, which mesh with the active screw 601, can be synchronized, preventing collisions between the water distributor 4 and the condenser tube 5 due to excessively rapid movement. Furthermore, by setting the limiting strip 626 and the moving groove 625, the separation of the first connecting arm 602 and the connecting arm 623 is smoother when the adapter frame 630 and the limiting ring 624 are fixed.

[0064] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A continuous synthesis apparatus for hexachlorocyclotriphosphazene, characterized in that: The device includes a three-necked flask (3), inside which a thermometer, a stirrer and a water separator (4) are installed respectively. The upper end of the water separator (4) is provided with a condenser (5). An alcohol lamp (7) is provided below the three-necked flask (3). The alcohol lamp (7) is located above an iron stand (1). A fixing rod (2) is provided at the upper end of the iron stand (1) near the alcohol lamp (7). The three-necked flask (3) is fixedly connected to the arc surface of the fixing rod (2). An adjustment device (6) is provided at the upper surface of the iron stand (1) away from the three-necked flask (3). The regulating device (6) includes: The first fixed arm (603) has one end connected to the water distributor (4), and the other end slides on the surface of the fixed rod (2). The first fixed arm (603) can rotate on the arc surface of the fixed rod (2). A connecting frame (610) is provided, one end of which slides on the arc surface of the fixed rod (2); The second fixed arm (604) has one end connected to the condenser (5) and slides inside the connecting frame (610). The initial position of the second fixed arm (604) is located at the rightmost side of the connecting frame (610). A limiting ring (624) is provided on the arc surface of the fixing rod (2). The limiting ring (624) is located between the first fixing arm (603) and the connecting frame (610), and the limiting ring (624) is engaged with the first fixing arm (603). The regulating device (6) further includes: An active screw (601) is rotatably connected to the upper surface of the iron frame (1) near the fixed rod (2); The adapter frame (630) slides on the arc surface of the fixed rod (2), and one end of the adapter frame (630) is fixedly connected to the first fixed arm (603). A first connecting arm (602) has one end engaged with the surface of the driving screw (601); Limiting strip (626), the limiting strip (626) is fixedly connected to one end of the first connecting arm (602) away from the active screw (601); An adapter arm (623) is fixedly connected at one end to an adapter frame (630); The movable groove (625) is provided at one end of the two sides of the adapter arm (623) away from the fixed rod (2). The limiting strip (626) slides on the inner wall of the movable groove (625) and the limiting strip (626) and the movable groove (625) are engaged with each other. Rubber posts (632), a plurality of rubber posts (632) are provided at the upper end of the adapter frame (630). The arc-shaped track (633) is provided inside the limiting ring (624), and the rubber column (632) is engaged with the arc-shaped track (633); The second connecting arm (637) has one end engaged with the surface of the active screw (601), and the other end of the second connecting arm (637) is fixedly connected to the connecting frame (610); An auxiliary turntable (607) is fixedly connected to the upper end of the active screw (601); A drive motor (605) is located on the side wall of the iron frame (1) near the auxiliary turntable (607); A drive track (606) is provided, one end of which is rotatably connected to the arc surface of an auxiliary turntable (607), and the other end of which is rotatably connected to a drive motor (605).

2. The continuous synthesis equipment for hexachlorocyclotriphosphazene according to claim 1, characterized in that: The trajectory of the arc track (633) is arc-shaped, and the rubber column (632) is in a compressed state on the inner wall of the arc track (633).

3. The continuous synthesis equipment for hexachlorocyclotriphosphazene according to claim 2, characterized in that: The upper surface of the adapter frame (630) is connected to a universal ball (631). The universal balls (631) are in pairs. One universal ball (631) is connected to the upper surface of the adapter frame (630), and the other universal ball (631) is connected to the lower surface of the rubber column (632).

4. The continuous synthesis equipment for hexachlorocyclotriphosphazene according to claim 1, characterized in that: The side wall of the iron frame (1) is provided with a sliding rail (609), and an auxiliary roller (636) is fixedly connected to the side of the first connecting arm (602) away from the adapter arm (623). The auxiliary roller (636) slides on the inner wall of the sliding rail (609).

5. The continuous synthesis apparatus for hexachlorocyclotriphosphazene according to claim 1, characterized in that: An infrared ray (634) is provided at the upper end of the iron stand (1) near the three-necked flask (3), and the infrared ray (634) and the three-necked flask (3) are on the same horizontal line. An infrared receiver (635) is provided on the arc surface of the fixing rod (2), and the infrared receiver (635) and the infrared ray (634) are on the same horizontal line. The infrared receiver (635) is connected to the drive motor (605).

6. The continuous synthesis apparatus for hexachlorocyclotriphosphazene according to claim 1, characterized in that: The surface of the active screw (601) near the auxiliary turntable (607) is fixedly connected to the first auxiliary gear (608). A sliding frame (611) is provided on the upper side wall of the iron frame (1). A sliding rack (613) is slidably connected inside the sliding frame (611). A fixing ring (614) is fixedly connected to one side of the sliding rack (613). A sliding rod (615) is fixedly connected inside the sliding frame (611), and the fixing ring (614) is slidably connected to the arc surface of the sliding rod (615). A compression spring (616) is sleeved on the arc surface of the sliding rod (615). One end of the compression spring (616) is fixedly connected to the sliding frame (611), and the other end of the compression spring (616) is fixedly connected to the fixing ring (614). One end of the sliding rack (613) is meshed with a second auxiliary gear (612). The second auxiliary gear (612) meshes with the first auxiliary gear (608). A fixing plate (617) is fixedly connected to one end of the strip (613) away from the second auxiliary gear (612). A fixing shaft (620) is fixedly connected inside the fixing plate (617). A connecting ring (622) is rotatably connected to the arc surface of the fixing shaft (620). A return spring (621) is sleeved on the arc surface of the fixing shaft (620). An abutment plate (618) is fixedly connected to one end of the connecting ring (622). An arc-shaped groove is formed on the surface of the abutment plate (618). (619) A one-way abutment plate (640) is provided on one side of the fixing plate (617). The one-way abutment plate (640) abuts against the back of the abutment plate (618). A slot is provided on the upper surface of the connecting frame (610). An abutment rod (638) is slidably connected to the inner wall of the slot on the upper surface of the connecting frame (610). The abutment rod (638) is fixedly connected to the upper surface of the second fixing arm (604), and the abutment rod (638) contacts the arc-shaped slot (619).

7. The continuous synthesis apparatus for hexachlorocyclotriphosphazene according to claim 6, characterized in that: The upper surface of the connecting frame (610) has a groove inner wall with a limiting buckle (639), and the abutment rod (638) is engaged with the inner wall of the limiting buckle (639).

8. The continuous synthesis apparatus for hexachlorocyclotriphosphazene according to claim 1, characterized in that: A rotating plate (628) is rotatably connected to the upper part of the adapter arm (623). One end of the rotating plate (628) is fixedly connected to a limiting plate (629), and the initial position of the limiting plate (629) is located above the moving groove (625). Both ends of the rotating plate (628) are fixedly connected to coil springs (627).

9. A method for synthesizing hexachlorocyclotriphosphazene, characterized in that: The synthesis is carried out using the continuous synthesis equipment for hexachlorocyclotriphosphazene according to any one of claims 1-8, comprising the following steps: Step 1: Add tetrachloroethane and ammonium chloride to a three-necked flask (3), then insert a thermometer, a water separator (4) and a stirrer. A condenser (5) is connected above the water separator (4). Heat the flask to evaporate some of the solvent, while carrying away the water in the system, until the solvent is no longer cloudy. Step 2: Separate the water separator (4) from the three-necked flask (3), quickly add phosphorus pentachloride and a small amount of pyridine to the three-necked flask (3), connect the condenser (5) on the water separator (4) directly to the three-necked flask (3), continue heating the three-necked flask (3) until the solvent in the condenser (5) refluxes, control the temperature at 135°C, and react for 20 hours; Step 3: Filter to remove excess ammonium chloride from the three-necked flask (3), remove the solvent by vacuum distillation of the three-necked flask (3) to obtain a yellow crystalline crude product, dissolve the crude product in benzene, and then evaporate the solvent under vacuum to obtain white crystals; Step 4: Place the white crystals in a round-bottom flask, add petroleum ether, and heat to 60°C to dissolve them. Since the filamentous structures inside the white crystals are insoluble, they can be separated out. Add 98% concentrated sulfuric acid to the round-bottom flask to prepare a petroleum ether solution. Extract the hexachlorocyclotriphosphazene from the petroleum ether solution multiple times. Combine the hexachlorocyclotriphosphazene with the sulfuric acid extract, and then dilute with water to prepare a 60% sulfuric acid solution. The hexachlorocyclotriphosphazene precipitates out again. Dissolve the precipitated product in hot heptane and decolorize with activated carbon to obtain a white solid, which is hexachlorocyclotriphosphazene.

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