A phosphorous trichloride automatic adding triisocresyl phosphate synthesis esterification reactor and a method for using the same

Abstract

The present application relates to a kind of esterification reaction kettle, specifically, a kind of automatic addition phosphorus trichloride's tris (m-cresyl) phosphate synthesis esterification reaction kettle and its using method, including kettle body and cover;Cover is also equipped with temperature control module;Still include the dropping tube installed on the cover, and the transition tank is connected by valve pipe;Valve pipe is provided with on-off member and adjusting member, and the on-off member includes multiple groups of on-off plate, which is rotatably installed on the valve pipe;Cover is provided with stirring member, and stirring member can perform stirring action;And after the action of stirring member, on-off member can be communicated valve pipe, to perform drop action;Temperature control module can drive adjusting member action, to adjust the conduction area of valve pipe, by the cooperation of stirring member and on-off member, on-off member only in the action of stirring member valve pipe is completely communicated;To avoid the fatal hidden danger of not stirring first drop, stop stirring still drop, effectively avoid the local overheating, carbonization even the risk of material rush caused by phosphorus trichloride accumulation in kettle.

Description

Technical Field

[0001] This invention relates to an esterification reactor, specifically an esterification reactor for the synthesis of tri-m-toluene phosphite with automatic addition of phosphorus trichloride and its usage method. Background Technology

[0002] Tri-m-toluene phosphite, an important organophosphorus antioxidant and auxiliary stabilizer for polyvinyl chloride, is widely used in the processing of plastics, rubber, and synthetic fibers. Its industrial synthesis typically involves the esterification condensation reaction of m-cresol and phosphorus trichloride. Because this reaction is highly exothermic, and the raw material phosphorus trichloride is highly toxic, corrosive, and reacts violently with water, the reactor, as the core equipment in this synthesis process, directly determines the product quality, yield, and production safety through its design and operational reliability.

[0003] Common reaction vessels include mechanical stirring devices, temperature control systems, and dropping devices. The dropping devices typically use metering pumps to deliver phosphorus trichloride and regulate the flow rate automatically based on the reaction intensity signal within the vessel using a regulating valve.

[0004] Because there is no direct connection between the existing dripping device and the stirring device, it is easy for the stirring to fail to start during dripping, or for the stirring to stop unexpectedly due to a malfunction during dripping, and the dripping system to fail to shut off synchronously. This makes it impossible to physically control the dripping behavior by stirring. Once the operator is negligent or the electrical control interlock fails, phosphorus trichloride will rapidly accumulate in the unstirred vessel and undergo a violent exothermic reaction, causing a sudden surge in local temperature, which may lead to material spillage, carbonization, or even explosion, posing a serious safety hazard. Summary of the Invention

[0005] The purpose of this invention is to provide an esterification reactor for the synthesis of tri-m-toluene phosphite with automatic addition of phosphorus trichloride and its usage method, so as to solve the problems mentioned in the background art.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] An esterification reactor for the synthesis of trimethyl-m-toluene phosphite with automatic phosphorus trichloride addition includes a reactor body and a cover body; an upper rotating shaft and a lower rotating shaft are rotatably mounted on the cover body, and the upper rotating shaft and the lower rotating shaft are sleeved together, and multiple sets of upper blades and lower blades are respectively mounted on the two shafts; a temperature control module is also installed on the cover body.

[0008] It also includes a drip tube installed on the cover, the drip tube being connected via a valve tube to a transition tank for connection to a metering pump;

[0009] The valve tube is provided with an opening and closing element and an adjusting element. The opening and closing element includes multiple sets of opening and closing plates rotatably mounted on the valve tube. The multiple sets of opening and closing plates can rotate to move away from or towards the valve tube.

[0010] The cover is provided with a stirring element, which can drive the upper rotating shaft and the lower rotating shaft to rotate synchronously, thereby driving multiple sets of upper and lower blades to rotate, thus performing a stirring action; and after the stirring element is activated, the opening and closing element can open the valve pipe to perform a dripping action.

[0011] The temperature control module can drive the regulating component to operate according to the reaction temperature inside the reactor, thereby adjusting the conduction area of ​​the valve tube and thus regulating the dripping speed.

[0012] The above-described automatic phosphorus trichloride-adding trimethyl-m-toluene phosphite synthesis esterification reactor: the stirring component includes a first bevel gear and a third bevel gear mounted on the upper rotating shaft and the lower rotating shaft; a second bevel gear that meshes with both the first bevel gear and the third bevel gear is rotatably mounted on the cover; a motor is mounted on the cover, and a main rotating shaft is mounted on the output end of the motor; the main rotating shaft is connected to the upper rotating shaft through a gear set.

[0013] The above-described automatic phosphorus trichloride-added tri-toluene phosphite synthesis esterification reactor comprises: an opening and closing device including an opening and closing turntable rotatably mounted on the valve pipe, the opening and closing turntable having an opening and closing groove; an opening and closing sliding column mounted on the opening and closing plate, which slidably engages with the opening and closing groove; an opening and closing shaft rotatably mounted on the cover, an opening and closing gear mounted on the opening and closing shaft, a first gear meshing with the opening and closing gear mounted on the opening and closing turntable; an opening and closing column sleeved inside the opening and closing shaft, the opening and closing column having an opening and closing spiral groove; and an opening and closing protrusion mounted inside the opening and closing shaft, which slidably engages with the opening and closing spiral groove.

[0014] The above-described automatic phosphorus trichloride-added tri-m-toluene phosphite synthesis esterification reactor comprises: multiple sets of adjusting plates rotatably mounted on the valve pipe; an adjusting turntable rotatably mounted on the valve pipe, the adjusting turntable having adjusting grooves; adjusting sliding columns mounted on the adjusting plates that slidably engage with the adjusting grooves; a second gear mounted on the adjusting turntable; an adjusting shaft rotatably mounted on the cover, the adjusting shaft having adjusting protrusions and adjusting gears meshing with the second gear; and an adjusting column sleeved inside the adjusting shaft, the adjusting column having adjusting spiral grooves that slidably engage with the adjusting protrusions.

[0015] As described above, in the automatic phosphorus trichloride addition reaction vessel for the synthesis of tri-m-toluene phosphite: the adjusting plate and the opening and closing plate are misaligned. When the opening and closing plates are in contact with each other, the valve tube is in a blocked state; when the opening and closing plates are far apart, the valve tube is in a conductive state. At this time, the adjusting plate rotates to move closer to or further away from the valve tube to increase or decrease the conductive area of ​​the valve tube.

[0016] The above-described automatic phosphorus trichloride-adding trimethyl-m-toluene phosphite synthesis esterification reactor comprises: a centrifugal disc mounted on the main rotating shaft; multiple sets of sliding frames slidably fitted around the centrifugal disc; telescopic sleeves and multiple sets of centrifugal blocks mounted on the sliding frames; a sliding sleeve fitted on the main rotating shaft; a telescopic column mounted on the sliding sleeve that slidably fits with the telescopic sleeve; a return spring fitted on the main rotating shaft; the two ends of the return spring respectively abutting against the sliding sleeve and the cover; and the opening / closing column rotatably connected to the sliding sleeve.

[0017] The above-described automatic phosphorus trichloride-adding trimethyl-m-toluene phosphite synthesis esterification reactor: a lifting plate is slidably installed on the temperature control module, and the temperature control module can adjust the vertical position of the lifting plate according to the temperature inside the reactor; an adjusting spring is provided on the cover, and the two ends of the adjusting spring abut against the lifting plate and the cover respectively.

[0018] The above-described automatic phosphorus trichloride-adding trimethyl-toluene phosphite synthesis esterification reactor: when the upper blade and the lower blade rotate, they can stir the upper reaction solution downwards and stir the lower reaction solution up and down.

[0019] The esterification reactor for the synthesis of trimethyl-m-toluene phosphite by automatically adding phosphorus trichloride as described above: the temperature control module is in contact with the upper reaction solution inside the reactor.

[0020] A method for using the esterification reactor for the synthesis of tri-m-toluene phosphite with automatic phosphorus trichloride addition as described above includes the following steps:

[0021] Step 1: Add the measured amount of m-cresol into the reactor via a transfer pump; start the water jet circulation pump and adjust the pressure inside the reactor;

[0022] Step 2: Start the metering pump to pump phosphorus trichloride to the transition tank, where phosphorus trichloride is pre-stored; the temperature control module continuously monitors the reaction temperature;

[0023] Step 3: Start the agitator to stir the reaction solution in the reactor, and open the valve pipe through the opening and closing device so that the phosphorus trichloride pre-stored in the transition tank drips into the reactor through the drip pipe;

[0024] Step 4: The temperature control module continuously monitors the reaction temperature and can control the action of the regulating components according to the temperature inside the reactor, thereby adjusting the conduction area of ​​the valve tube to control the dripping rate of phosphorus trichloride, and thus control the reaction rate.

[0025] Compared with the prior art, the beneficial effects of the present invention are:

[0026] Through the coordinated operation of the agitator and the opening / closing mechanism, the valve pipe is only fully open after the agitator is activated. If the agitator fails to start, or stops operating due to power failure, shaft breakage, blade jamming, or other malfunctions, the reset spring releases its potential energy, driving the opening / closing mechanism to move in the opposite direction, forcing the opening / closing plate to re-close and seal the valve pipe. This avoids the fatal hidden dangers of dripping before agitation or continuing to drip after agitation stops, and effectively prevents the risk of localized overheating, carbonization, or even material overflow caused by the exothermic accumulation of phosphorus trichloride in the reactor. Attached Figure Description

[0027] Figure 1 A schematic diagram of the structure of the esterification reactor for the synthesis of trimethyl-m-toluene phosphite with automatic addition of phosphorus trichloride.

[0028] Figure 2 A schematic diagram of the structure of the lid in the esterification reactor for the synthesis of trimethyl-m-toluene phosphite with automatic addition of phosphorus trichloride.

[0029] Figure 3 A schematic diagram of the upper and lower rotating shafts in the esterification reactor for the synthesis of trimethyl-m-toluene phosphite with automatic phosphorus trichloride addition.

[0030] Figure 4 A schematic diagram of the temperature control module in the esterification reactor for the synthesis of trimethyl-m-toluene phosphite with automatic phosphorus trichloride addition.

[0031] Figure 5 A schematic diagram of the opening and closing column in the esterification reactor for the synthesis of trimethyl-m-toluene phosphite with automatic phosphoric acid addition.

[0032] Figure 6 A schematic diagram of the regulating column in the esterification reactor for the synthesis of trimethyl-m-toluene phosphite with automatic phosphoric acid addition.

[0033] Figure 7 A schematic diagram of the valve tube in the esterification reactor for the synthesis of trimethyl-m-toluene phosphite with automatic phosphoric acid addition.

[0034] Figure 8 for Figure 7 A structural schematic diagram from a cross-sectional perspective.

[0035] Figure 9 A schematic diagram of the regulating plate in the esterification reactor for the synthesis of trimethyl-m-toluene phosphite with automatic phosphoric acid addition.

[0036] Figure 10 A schematic diagram of the opening and closing plate in the esterification reactor for the synthesis of trimethyl-m-toluene phosphite with automatic phosphoric acid addition.

[0037] In the picture:

[0038] 1. Kettle body;

[0039] 2. Cover;

[0040] 3. Motor;

[0041] 4. Main spindle;

[0042] 5. Upper shaft; 501. Upper blade;

[0043] 6. Lower shaft; 601. Lower blade;

[0044] 7. First bevel gear;

[0045] 8. Second bevel gear;

[0046] 9. Third bevel gear;

[0047] 10. Centrifuge tray;

[0048] 11. Sliding frame; 1101. Telescopic sleeve; 1102. Centrifugal block;

[0049] 12. Sliding sleeve; 1201. Telescopic column;

[0050] 13. Return spring;

[0051] 14. Opening and closing column; 1401. Opening and closing spiral groove;

[0052] 15. Opening and closing shaft; 1501. Opening and closing protrusion; 1502. Opening and closing gear;

[0053] 16. Temperature control module;

[0054] 17. Lifting plate;

[0055] 18. Adjusting spring;

[0056] 19. Adjusting column; 1901. Adjusting spiral groove;

[0057] 20. Adjust the shaft; 2001. Adjust the protrusion; 2002. Adjust the gear;

[0058] 21. Transition tank;

[0059] 22. Valve pipe;

[0060] 23. Turntable for opening and closing; 2301. Inclined sprocket for opening and closing; 2302. First gear;

[0061] 24. Opening and closing plate; 2401. Opening and closing sliding column;

[0062] 25. Adjust the turntable; 2501. Adjust the inclined groove; 2502. Second gear;

[0063] 26. Adjusting plate; 2601. Adjusting slide bar;

[0064] 27. Dropper. Detailed Implementation

[0065] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0066] Furthermore, elements in this invention are referred to as being "fixed to" or "set on" another element, which may be directly on the other element or may also include an intervening element. When an element is considered to be "connected" to another element, it may be directly connected to the other element or may also include an intervening element. The terms "vertical," "horizontal," "left," "right," and similar expressions used herein are for illustrative purposes only and do not represent the only possible implementation.

[0067] Please see Figures 1-10 As an embodiment of the present invention, the automatic phosphorus trichloride addition reaction vessel for the synthesis of tri-m-toluene phosphite includes a vessel body 1 and a cover body 2; an upper rotating shaft 5 and a lower rotating shaft 6 are rotatably mounted on the cover body 2, and the upper rotating shaft 5 and the lower rotating shaft 6 are sleeved together, and multiple sets of upper blades 501 and lower blades 601 are respectively mounted on the two; a temperature control module 16 is also installed on the cover body 2;

[0068] It also includes a drip tube 27 installed on the cover 2, the drip tube 27 being connected to a transition tank 21 for connection with a metering pump via a valve tube 22;

[0069] The valve pipe 22 is provided with an opening and closing component and an adjusting component. The opening and closing component includes multiple sets of opening and closing plates 24 rotatably mounted on the valve pipe 22. The multiple sets of opening and closing plates 24 can rotate to move away from or towards the valve pipe 22.

[0070] The cover 2 is provided with a stirring element, which can drive the upper rotating shaft 5 and the lower rotating shaft 6 to rotate synchronously, thereby driving multiple sets of upper blades 501 and lower blades 601 to rotate, thus performing a stirring action; and after the stirring element is activated, the opening and closing element can open the valve pipe 22 to perform a dripping action.

[0071] The temperature control module 16 can drive the regulating component to operate according to the reaction temperature inside the vessel 1, thereby adjusting the conduction area of ​​the valve tube 22 and thus adjusting the dripping speed.

[0072] In this embodiment, the metered m-cresol is introduced into the reactor 1 via a transfer pump; the water jet circulation pump is started to adjust the pressure inside the reactor; the metering pump is started to pump phosphorus trichloride to the transition tank 21, where phosphorus trichloride is pre-stored; and the temperature control module 16 continuously monitors the reaction temperature.

[0073] The agitator is activated to stir the reaction solution inside the vessel 1. When the upper rotating shaft 5 and the lower rotating shaft 6 rotate, they drive the upper impeller 501 and the lower impeller 601 to rotate, thereby stirring the reaction solution and improving the uniformity of the subsequent reaction. At the same time as the agitator is activated, the valve pipe 22 is opened through the opening and closing device, so that the phosphorus trichloride pre-stored in the transition tank 21 drips into the vessel 1 through the dripping pipe 27. Through the cooperation of the agitator and the opening and closing device, the valve pipe 22 can be opened at the same time as stirring, so that the phosphorus trichloride can drip into the vessel 1 along the dripping pipe 27, avoiding local overheating, violent exothermic reaction, or even material overflow caused by the phosphorus trichloride accumulating in one place, and ensuring the thermal stability of the reaction system.

[0074] The temperature control module 16 continuously monitors the reaction temperature and can control the action of the regulating component according to the temperature inside the vessel 1, thereby adjusting the conduction area of ​​the valve tube 22 to control the dripping rate of phosphorus trichloride, and thus control the reaction rate.

[0075] The temperature control module 16 continuously monitors the reaction temperature inside the vessel 1 and converts the temperature signal into control commands to drive the regulating components: when the temperature rises and approaches the threshold, the conduction area of ​​the valve tube 22 is reduced, thereby reducing the dripping rate of phosphorus trichloride and suppressing the exothermic reaction rate; conversely, when the temperature drops, the dripping rate is restored, thus achieving precise control of the reaction rate and ensuring a stable release of reaction heat.

[0076] As a further embodiment of the present invention, the stirring component includes a first bevel gear 7 and a third bevel gear 9 mounted on the upper rotating shaft 5 and the lower rotating shaft 6, and a second bevel gear 8 rotatably mounted on the cover 2, which meshes with both the first bevel gear 7 and the third bevel gear 9; a motor 3 is mounted on the cover 2, and a main rotating shaft 4 is mounted on the output end of the motor 3, and the main rotating shaft 4 is connected to the upper rotating shaft 5 through a gear set.

[0077] In this embodiment, when the motor 3 operates, it drives the main shaft 4 to rotate, which in turn drives the upper shaft 5 to rotate via the gear set, thereby driving the first bevel gear 7 to rotate. The first bevel gear 7, through meshing with the second bevel gear 8, drives the second bevel gear 8 to rotate around its own axis. The second bevel gear 8 then meshes with and drives the third bevel gear 9 to rotate in the opposite direction, so that the lower shaft 6 obtains a rotation vector opposite to that of the upper shaft 5, thereby driving the upper blade 501 and the lower blade 601 to rotate, so as to force the formation of two circulating vortices in the vessel 1: the upper blade 501 pushes the surface material downward, and the lower blade 601 scoops the bottom material upward. The two opposing flow fields converge violently in the shear zone in the middle of the vessel 1, which not only eliminates the stirring dead zone, but also increases the interphase contact area when the phosphorus trichloride droplets penetrate the shear zone.

[0078] As a further embodiment of the present invention, the opening and closing component includes an opening and closing turntable 23 rotatably mounted on the valve pipe 22, the opening and closing turntable 23 having an opening and closing inclined groove 2301; an opening and closing sliding column 2401 slidably engaged with the opening and closing inclined groove 2301 mounted on the opening and closing plate 24; an opening and closing shaft 15 rotatably mounted on the cover 2, an opening and closing gear 1502 mounted on the opening and closing shaft 15, a first gear 2302 meshing with the opening and closing gear 1502 mounted on the opening and closing turntable 23; an opening and closing column 14 sleeved inside the opening and closing shaft 15, the opening and closing column 14 having an opening and closing spiral groove 1401; and an opening and closing protrusion 1501 slidably engaged with the opening and closing spiral groove 1401 mounted inside the opening and closing shaft 15.

[0079] In this embodiment, in the initial state, multiple sets of opening and closing plates 24 are attached to each other to block the valve pipe 22. At this time, the transition tank 21 and the dripping pipe 27 are in a blocked state, and phosphorus trichloride cannot be added.

[0080] When the agitator operates, it drives the opening and closing column 14 to move upward along the opening and closing shaft 15, thereby driving the opening and closing spiral groove 1401 to move synchronously. During this process, the opening and closing protrusion 1501 slides in the opening and closing spiral groove 1401, thereby driving the opening and closing shaft 15 to rotate. Then, through the meshing of the opening and closing gear 1502 and the first gear 2302, the opening and closing turntable 23 rotates. The rotation of the opening and closing turntable 23 drives the opening and closing inclined groove 2301 to rotate synchronously, so that the opening and closing sliding column 2401 slides in the opening and closing inclined groove 2301, thereby driving multiple sets of opening and closing plates 24 to rotate synchronously and move away from each other, thereby opening the flow section of the valve pipe 22 and allowing phosphorus trichloride to drip smoothly into the reactor.

[0081] Valve 22 is only in the conducting state when the agitator is in operation; once the agitator loses power or stops, the opening and closing plate 24 resets in the opposite direction, forcing the opening and closing plate 24 to close again, thus eliminating the risk of uncontrolled dripping.

[0082] As a further embodiment of the present invention, the adjusting component includes multiple sets of adjusting plates 26 rotatably mounted on the valve pipe 22, an adjusting turntable 25 rotatably mounted on the valve pipe 22, and an adjusting groove 2501 formed on the adjusting turntable 25; an adjusting slide column 2601 slidably engaged with the adjusting groove 2501 is mounted on the adjusting plate 26; a second gear 2502 is mounted on the adjusting turntable 25; an adjusting shaft 20 is rotatably mounted on the cover 2, and an adjusting protrusion 2001 and an adjusting gear 2002 meshing with the second gear 2502 are mounted on the adjusting shaft 20; an adjusting column 19 is sleeved inside the adjusting shaft 20, and an adjusting spiral groove 1901 slidably engaged with the adjusting protrusion 2001 is formed on the adjusting column 19.

[0083] In this embodiment, the temperature control module 16 can control the position of the adjusting column 19 within the adjusting shaft 20 according to the temperature inside the vessel 1. That is, the adjusting column 19 can slide inward or outward along its axis within the adjusting shaft 20, thereby driving the adjusting spiral groove 1901 to move synchronously. Through the sliding engagement of the adjusting protrusion 2001 and the adjusting spiral groove 1901, the adjusting shaft 20 is driven to rotate. Then, through the meshing of the adjusting gear 2002 and the second gear 2502, the adjusting turntable 25 is driven to rotate. The rotation of the adjusting turntable 25 can drive the adjusting inclined groove 2501 to rotate synchronously, so that the adjusting slide column 2601 slides in the adjusting inclined groove 2501, thereby driving multiple sets of adjusting plates 26 to rotate synchronously closer or further away, thereby realizing the adjustment of the conduction area of ​​the valve pipe 22.

[0084] When the temperature control module 16 detects that the reaction temperature is approaching the threshold, the regulating plate 26 converges centripetally, appropriately reducing the dropping rate of phosphorus trichloride without completely cutting off the flow, thus suppressing the exothermic reaction. When the temperature drops back to the safe range, the regulating plate 26 is driven to expand, restoring the dropping rate to maintain reaction efficiency. This achieves dynamic matching between the dropping rate and the reaction temperature, and avoids valve position jitter caused by fluid pulsation, improving the temperature control accuracy and the stability of the reaction process.

[0085] As a further embodiment of the present invention, the adjusting plate 26 and the opening and closing plate 24 are vertically offset. When the opening and closing plates 24 are in contact with each other, the valve pipe 22 is in a blocked state; when the opening and closing plates 24 are far apart, the valve pipe 22 is in a conductive state. At this time, the adjusting plate 26 rotates to move closer to or further away from the valve pipe 22 to increase or decrease the conductive area of ​​the valve pipe 22.

[0086] In this embodiment, when the stirring is started and the opening and closing plate 24 is fully opened, if the reactor temperature is lower than the optimal reaction temperature, the regulating plate 26 is in the maximum open state, the valve pipe 22 is open in full diameter, and phosphorus trichloride is rapidly dripped to shorten the feeding cycle; as the reaction exothermics and the reactor temperature approaches the threshold, the temperature control module 16 gradually drives the regulating plate 26 to slowly close towards the center, reducing the dripping rate without interrupting the feeding, so as to control the rate of reaction exothermics; if extreme conditions such as stirring power failure or shaft breakage occur, regardless of the opening degree of the regulating plate 26, the opening and closing plate 24 will perform a closing action under the action of the opening and closing element, forming a redundant safety protection independent of the regulating system, and improving the operational stability of the device under strong corrosive conditions.

[0087] As a further embodiment of the present invention, a centrifugal disc 10 is mounted on the main rotating shaft 4; multiple sets of sliding frames 11 are slidably fitted around the centrifugal disc 10 in the circumferential direction, and a telescopic sleeve 1101 and multiple sets of centrifugal blocks 1102 are mounted on the sliding frame 11; a sliding sleeve 12 is fitted on the main rotating shaft 4, and a telescopic column 1201 that slidably fits with the telescopic sleeve 1101 is mounted on the sliding sleeve 12; a return spring 13 is fitted on the main rotating shaft 4, and the two ends of the return spring 13 abut against the sliding sleeve 12 and the cover 2 respectively; the opening and closing column 14 is rotatably connected to the sliding sleeve 12.

[0088] In this embodiment, when the main shaft 4 rotates, the stirring component performs a stirring action. During this process, the centrifugal disc 10 rotates synchronously. Due to the center of gravity of the multiple centrifugal blocks 1102 in the circumferential direction of the centrifugal disc 10 being off-center from the axis of the main shaft 4, they slide outward along the radial direction of the centrifugal disc 10 under the action of centrifugal force, thereby driving the sliding frame 11 fixed thereto to extend outward synchronously. Thus, the sliding sleeve 12 is driven to slide through the sliding engagement of the telescopic sleeve 1101 and the telescopic column 1201, thereby compressing the return spring 13. When the sliding sleeve 12 moves, it drives the opening and closing column 14 rotatably connected thereto to move axially synchronously. The opening and closing spiral groove 1401 on the opening and closing column 14 slides relative to the opening and closing protrusion 1501 on the inner wall of the opening and closing shaft 15, converting linear motion into rotational torque. Then, through gear transmission, the multiple opening and closing plates 24 of the opening and closing component are evenly unfolded, opening the valve pipe 22.

[0089] When the agitator starts, the centrifugal force generated by the centrifugal block 1102 is sufficient to completely overcome the resistance of the return spring 13, and the opening and closing plate 24 remains fully open. If the agitator stops, the return spring 13 will push the sliding sleeve 12 back to its original position, thereby driving the opening and closing column 14 to retract synchronously, driving the opening and closing plate 24 to rotate and close, thus sealing the valve pipe 22. Through the cooperation between the agitator and the opening and closing device, the valve pipe 22 can be opened while agitating, allowing phosphorus trichloride to drip into the vessel 1 along the dripping pipe 27, avoiding local overheating, violent exothermic reactions, or even material overflow caused by phosphorus trichloride accumulating in one place, and ensuring the thermal stability of the reaction system.

[0090] As a further embodiment of the present invention, a lifting plate 17 is slidably mounted on the temperature control module 16, and the temperature control module 16 can adjust the vertical position of the lifting plate 17 according to the temperature inside the vessel 1; an adjusting spring 18 is provided on the cover 2, and the two ends of the adjusting spring 18 abut against the lifting plate 17 and the cover 2 respectively.

[0091] In this embodiment, initially, the multiple sets of adjusting plates 26 are in relatively far positions. The temperature control module 16 can drive the lifting plate 17 to rise or fall. When the reaction temperature inside the vessel 1 is lower than the set threshold, the lifting plate 17 is in a high position under the pre-tightening force of the adjusting spring 18. At this time, the adjusting column 19 moves within the adjusting shaft 20, the adjusting plate 26 remains in the maximum open state, the valve tube 22 has the largest conduction area, and the phosphorus trichloride dripping rate is the fastest. When the reaction exothermics and causes the vessel temperature to rise and approach the safety upper limit, the temperature control module 16 overcomes the elasticity of the adjusting spring 18 and pushes the lifting plate 17 to move, thereby driving the adjusting column 19 to move axially in sync. This drives the adjusting plate 26 to retract inward, reducing the conduction area of ​​the valve tube 22 and automatically reducing the dripping rate to suppress exothermics.

[0092] The adjusting spring 18 not only provides a restoring force for the lifting plate 17, but its elasticity can also effectively absorb the mechanical interference caused by stirring vibration or fluid pulsation in the reactor, preventing the temperature control module 16 from malfunctioning due to high-frequency vibration, thus improving the safety level of high-risk processes.

[0093] As a further embodiment of the present invention, when the upper blade 501 and the lower blade 601 rotate, they can stir the upper reaction solution downwards and stir the lower reaction solution up and down.

[0094] In this embodiment, the upper impeller 501 and the lower impeller 601 rotate in opposite directions under the drive of the bevel gear set: the upper impeller 501 pushes the reaction solution downward; at the same time, the lower impeller 601 rotates in the opposite direction, thereby pushing the reaction solution upward. The two fluids with opposite directions and different tangential velocities form a violent shearing and colliding zone in the lower part of the vessel 1, eliminating the dead zone at the bottom and the laminar flow layer in the middle, ensuring that the reaction heat energy is rapidly and evenly distributed in space, avoiding the risk of carbonization or material slugging caused by local overheating, and also improving the interphase mass transfer efficiency, making the esterification reaction more thorough and effectively suppressing the formation of by-products.

[0095] As a further embodiment of the present invention, the temperature control module 16 is in contact with the upper reaction solution inside the vessel 1.

[0096] In this embodiment, the detection end of the temperature control module 16 is directly immersed in the upper reaction solution inside the reactor body 1. This position is located at the interface between the gas phase reflux liquid and the liquid phase bulk, which is the area with the highest heat sensitivity in the reaction system. The temperature control module 16 accurately captures temperature changes in the upper layer and feeds them back to the regulating component, thereby achieving millisecond-level dynamic suppression of the exothermic reaction and providing an extreme temperature control environment for the synthesis of tri-m-toluene phosphite.

[0097] A method for using the esterification reactor for the synthesis of tri-m-toluene phosphite with automatic phosphorus trichloride addition as described above includes the following steps:

[0098] Step 1: Add the measured amount of m-cresol into vessel 1 via a transfer pump; start the water jet circulation pump and adjust the pressure inside the vessel;

[0099] Step 2: Start the metering pump to pump phosphorus trichloride to the transition tank 21, where phosphorus trichloride is pre-stored; the temperature control module 16 continuously monitors the reaction temperature;

[0100] Step 3: Start the agitator to stir the reaction solution in the vessel 1, and open the valve pipe 22 through the opening and closing device so that the phosphorus trichloride pre-stored in the transition tank 21 drips into the vessel 1 through the drip pipe 27;

[0101] Step 4: The temperature control module 16 continuously monitors the reaction temperature and can control the action of the regulating component according to the temperature inside the vessel 1, thereby adjusting the conduction area of ​​the valve tube 22 to control the dripping speed of phosphorus trichloride, and thus control the reaction rate.

[0102] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0103] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. An esterification reactor for the synthesis of tri-m-toluene phosphite with automatic addition of phosphorus trichloride, characterized in that, It includes a vessel body (1) and a cover body (2); an upper rotating shaft (5) and a lower rotating shaft (6) are rotatably mounted on the cover body (2), and the upper rotating shaft (5) and the lower rotating shaft (6) are sleeved together, and multiple sets of upper blades (501) and lower blades (601) are respectively mounted on the two; a temperature control module (16) is also mounted on the cover body (2). It also includes a drip tube (27) installed on the cover (2), the drip tube (27) being connected to a transition tank (21) for connection with a metering pump via a valve tube (22); The valve tube (22) is provided with an opening and closing component and an adjusting component. The opening and closing component includes multiple sets of opening and closing plates (24) rotatably mounted on the valve tube (22). The multiple sets of opening and closing plates (24) can rotate away from or approach each other. The cover (2) is provided with a stirring element, which can drive the upper rotating shaft (5) and the lower rotating shaft (6) to rotate synchronously, thereby driving multiple sets of upper blades (501) and lower blades (601) to rotate, thereby performing a stirring action; and after the stirring element is activated, the opening and closing element can open the valve pipe (22) to perform a dripping action. The temperature control module (16) can drive the regulating component to act according to the reaction temperature inside the vessel (1) to adjust the conduction area of ​​the valve tube (22) and thus adjust the dripping speed.

2. The esterification reactor for the synthesis of tri-m-toluene phosphite with automatic phosphorus trichloride addition according to claim 1, characterized in that, The stirring component includes a first bevel gear (7) and a third bevel gear (9) mounted on the upper rotating shaft (5) and the lower rotating shaft (6). A second bevel gear (8) that meshes with both the first bevel gear (7) and the third bevel gear (9) is rotatably mounted on the cover (2). A motor (3) is mounted on the cover (2). A main rotating shaft (4) is mounted on the output end of the motor (3). The main rotating shaft (4) is connected to the upper rotating shaft (5) through a gear set.

3. The esterification reactor for the synthesis of tri-m-toluene phosphite with automatic phosphorus trichloride addition according to claim 2, characterized in that, The opening and closing components include an opening and closing turntable (23) rotatably mounted on the valve pipe (22), the opening and closing turntable (23) having an opening and closing groove (2301); an opening and closing slide column (2401) slidably engaged with the opening and closing groove (2301) mounted on the opening and closing plate (24); an opening and closing shaft (15) rotatably mounted on the cover (2), an opening and closing gear (1502) mounted on the opening and closing shaft (15), and a first gear (2302) meshing with the opening and closing gear (1502) mounted on the opening and closing turntable (23); an opening and closing column (14) sleeved inside the opening and closing shaft (15), the opening and closing column (14) having an opening and closing spiral groove (1401); and an opening and closing protrusion (1501) slidably engaged with the opening and closing spiral groove (1401) installed inside the opening and closing shaft (15).

4. The esterification reactor for the synthesis of tri-m-toluene phosphite with automatic addition of phosphorus trichloride according to claim 3, characterized in that, The adjusting component includes multiple adjusting plates (26) rotatably mounted on the valve pipe (22), an adjusting turntable (25) rotatably mounted on the valve pipe (22), and an adjusting groove (2501) provided on the adjusting turntable (25); an adjusting slide column (2601) slidably engaged with the adjusting groove (2501) is mounted on the adjusting plate (26); a second gear (2502) is mounted on the adjusting turntable (25); an adjusting shaft (20) rotatably mounted on the cover (2), an adjusting protrusion (2001) and an adjusting gear (2002) meshing with the second gear (2502) are mounted on the adjusting shaft (2); an adjusting column (19) is sleeved inside the adjusting shaft (20), and an adjusting spiral groove (1901) slidably engaged with the adjusting protrusion (2001) is provided on the adjusting column (19).

5. The esterification reactor for the synthesis of tri-m-toluene phosphite with automatic addition of phosphorus trichloride according to claim 4, characterized in that, The adjusting plate (26) and the opening and closing plate (24) are vertically misaligned. When the opening and closing plates (24) are in contact with each other, the valve pipe (22) is in a blocked state. When the opening and closing plates (24) are far apart, the valve pipe (22) is in a conductive state. At this time, the adjusting plate (26) rotates to move closer or further away to increase or decrease the conductive area of ​​the valve pipe (22).

6. The esterification reactor for the synthesis of tri-m-toluene phosphite with automatic addition of phosphorus trichloride according to claim 3, characterized in that, A centrifugal disc (10) is installed on the main rotating shaft (4); multiple sets of sliding frames (11) are slidably fitted around the centrifugal disc (10), and a telescopic sleeve (1101) and multiple sets of centrifugal blocks (1102) are installed on the sliding frame (11). A sliding sleeve (12) is fitted on the main rotating shaft (4), and a telescopic column (1201) is installed on the sliding sleeve (12) and slidably fitted with the telescopic sleeve (1101). A return spring (13) is fitted on the main rotating shaft (4), and the two ends of the return spring (13) abut against the sliding sleeve (12) and the cover (2) respectively. The opening and closing column (14) is rotatably connected to the sliding sleeve (12).

7. The esterification reactor for the synthesis of tri-m-toluene phosphite with automatic addition of phosphorus trichloride according to claim 4, characterized in that, A lifting plate (17) is slidably installed on the temperature control module (16). The temperature control module (16) can adjust the vertical position of the lifting plate (17) according to the temperature inside the vessel (1). An adjusting spring (18) is provided on the cover (2). The two ends of the adjusting spring (18) abut against the lifting plate (17) and the cover (2) respectively.

8. The esterification reactor for the synthesis of tri-m-toluene phosphite with automatic addition of phosphorus trichloride according to claim 2, characterized in that, When the upper blade (501) and the lower blade (601) rotate, they can stir the upper reaction solution downwards and stir the lower reaction solution up and down.

9. The esterification reactor for the synthesis of tri-m-toluene phosphite with automatic addition of phosphorus trichloride according to claim 1, characterized in that, The temperature control module (16) is in contact with the upper reaction solution inside the vessel body (1).

10. A method of using the esterification reactor for the synthesis of tri-m-toluene phosphite with automatic addition of phosphorus trichloride as described in any one of claims 1-9, characterized in that, Includes the following steps, Step 1: Add the measured amount of m-cresol into the reactor body (1) via a transfer pump; start the water jet circulation pump and adjust the pressure inside the reactor; Step 2: Start the metering pump to pump phosphorus trichloride to the transition tank (21) and pre-store phosphorus trichloride in the transition tank (21); the temperature control module (16) continuously monitors the reaction temperature; Step 3: Start the agitator to stir the reaction solution in the vessel (1), and open the valve pipe (22) through the opening and closing device so that the phosphorus trichloride pre-stored in the transition tank (21) drips into the vessel (1) through the drip pipe (27); Step 4: The temperature control module (16) continuously monitors the reaction temperature and can control the action of the regulating component according to the temperature inside the vessel (1), thereby adjusting the conduction area of ​​the valve tube (22) to control the dripping speed of phosphorus trichloride, thereby controlling the reaction rate.

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