Reaction device for preparing o-tolyl isocyanate and reaction method thereof

Abstract

The invention relates to the technical field of isocyanate reaction, and discloses a reaction device for preparing o-tolyl isocyanate and a reaction method thereof.The reaction device comprises a reaction box, a cleaning and stirring mechanism is arranged in the reaction box and used for stirring and cleaning crystals adsorbed on the inner wall, an intermittent conveying mechanism is arranged on one side of the cleaning and stirring mechanism, and the intermittent conveying mechanism is arranged on the other side of the cleaning and stirring mechanism. The phosgene intermittent conveying device is provided with a clean stirring mechanism for intermittently conveying phosgene, the clean stirring mechanism is provided with a pressing discharging mechanism for pushing isocyanate to be rapidly discharged, it is guaranteed that reactants are evenly distributed in the whole reaction mixture through stirring, the local concentration is prevented from being too high or too low, and therefore the overall reaction efficiency and the product quality are improved; according to the reaction device, crystals can be shoveled down from the wall surface during stirring, the service life of the reaction device is prolonged, meanwhile, communication of the exhaust pipe is intermittently cut off, a communication hole in one side of the intermittent rotary table is communicated with the exhaust pipe, and the concentration of reactants in a reaction mixture can be adjusted by intermittently cutting off conveying of phosgene, so that the reaction rate is controlled.

Description

Technical Field

[0001] The invention relates to the technical field of isocyanate reactions, and in particular to a reaction device and a reaction method for preparing o-tolyl isocyanate. Background Art

[0002] Isocyanate is a general term for various esters of isocyanic acid, which are used in household appliances, automobiles, construction, footwear, furniture, adhesives and other industries. If classified by the number of -NCO groups, it includes monoisocyanate R-N=C=O, diisocyanate O=C=N-R-N=C=O and polyisocyanate, etc. Common diisocyanates include toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, lysine diisocyanate.

[0003] By injecting o-toluidine into the reaction device, since the amino group is easily unstable in the subsequent reaction, the amino group needs to be protected through an acylation reaction, and then the phosgene is transported to the reaction device to react with the protected compound. The reaction temperature needs to be strictly controlled to ensure the smooth progress of the reaction and reduce the occurrence of side reactions. It needs to be carried out under a certain pressure to improve the reaction efficiency. After the reaction is completed, the product needs to be purified by distillation, crystallization or chromatography.

[0004] When the above-mentioned reaction device for preparing o-tolyl isocyanate is used, the amino group in o-toluidine is easily unstable in the subsequent reaction, and the amino group needs to be protected by an acylation reaction. When phosgene is transported to the protected compound for reaction to generate isocyanate, the reaction conditions become difficult to control due to the continuous transport of phosgene to the protected compound, which increases the risk of side reactions, affects product quality and reaction efficiency, causes leakage, and triggers poisoning accidents, posing a threat to human health and environmental safety. The isocyanate produced by the reaction is usually liquid at room temperature, but their viscosity is higher than that of water, so their fluidity is not as fast as that of water. If the temperature is reduced, the viscosity of the isocyanate will increase, further slowing down its fluidity, resulting in the purification and unloading process being prolonged and the production efficiency being greatly reduced. Summary of the invention

[0005] 1. Technical issues to be resolved In view of the deficiencies in the prior art, the present invention provides a reaction device and a reaction method for preparing o-tolyl isocyanate, which have the advantages of indirectly conveying phosgene for reaction, and solve the problems of excessive leakage of phosgene caused by quantitative and continuous output of phosgene and difficulty in feeding isocyanate due to its viscosity.

[0006] (II) Technical solution In order to achieve the above purpose of not only solving the problem of excessive leakage of phosgene caused by the quantitative and continuous output of phosgene, but also ensuring the rapid discharge of isocyanate that has reacted well, the present invention provides the following technical solutions: a reaction device for preparing o-tolyl isocyanate and a reaction method thereof, comprising a reaction box, a cleaning stirring mechanism is arranged in the reaction box for stirring and cleaning the crystals adsorbed on the inner wall, an intermittent conveying mechanism is arranged on one side of the cleaning stirring mechanism for intermittently conveying phosgene, a downward pressing discharge mechanism is arranged on the cleaning stirring mechanism for promoting the rapid discharge of isocyanate, the cleaning stirring mechanism comprises a driving disc rotatably connected to the reaction box, ratchet blocks are connected at intervals on the driving disc, a half gear is slidably connected to the ratchet block, a sliding groove is provided on the half gear, a ball that can limit the ratchet block is slidably connected in the half gear, a lifting slide is slidably connected to the ball, a limiting spring sheet is sleeved on the end of the lifting slide away from the ball, the limiting spring sheet is arranged in the sliding groove, and a rotating ring is connected to the upper surface of the half gear.

[0007] As a preferred embodiment of the reaction device for preparing o-tolyl isocyanate described in the present invention, a stirring rod is connected to the upper surface of the rotating ring, a scraper groove is provided on one side of the stirring rod, a reaction tank is sleeved on the rotating ring, a delivery pipe opening is provided on the reaction tank, and a discharge pipe opening is provided at one end of the reaction tank away from the delivery pipe opening.

[0008] As a preferred scheme of the reaction device for preparing o-tolyl isocyanate described in the present invention, an exhaust pipe is arranged in the reaction box, an exhaust pipe is embedded in one side of the reaction tank, one end of the exhaust pipe is connected to a support plate frame 1, a reset spring is sleeved on one side of the support plate frame 1, a sliding sealing head is sleeved on the end of the reset spring away from the support plate frame 1, and a sealing block is connected in the exhaust pipe.

[0009] As a preferred scheme of the reaction device for preparing o-tolyl isocyanate described in the present invention, an exhaust duct is opened on the sealing block, a support plate frame 2 is embedded and installed on the sealing block, one side of the support plate frame 2 is connected to a limiting slide rod, the half gear is connected to a limiting slider, and one side of the limiting slider is slidably connected to a limiting rotating plate.

[0010] As a preferred solution of the reaction device for preparing o-tolyl isocyanate described in the present invention, the lower surface of the limit rotating plate is connected to a driving gear that intermittently meshes with the half gear, the upper surface of the limit rotating plate is connected to a rotating shaft, the end of the rotating shaft away from the limit rotating plate is connected to an intermittent turntable, a connecting hole is provided on the intermittent turntable, a sealing strip is connected to the intermittent turntable, and the end of the exhaust pipe away from the reaction tank is connected to a storage box.

[0011] As a preferred embodiment of the reaction device for preparing o-tolyl isocyanate described in the present invention, the upper surface of the driving disc is connected to a rotating disc, the upper surface of the rotating disc is connected to a spoiler, the upper surface of the rotating disc is connected to a rotating screw, a threaded sleeve is screwed on the rotating screw, and the lower surface of the threaded sleeve is rotatably connected to a discharge plate.

[0012] As a preferred solution of the reaction device for preparing o-tolyl isocyanate described in the present invention, limiting grooves are provided on both sides of the discharge plate, a fixed seat is rotatably connected to the threaded sleeve, a placement cavity is provided in the fixed seat, a snap-on spring is provided in the fixed seat, and a sliding clamping plate is slidably connected in the fixed seat.

[0013] As a preferred solution of the reaction device for preparing o-tolyl isocyanate described in the present invention, a driving slider is slidably connected to the fixed seat, a through groove is provided on the driving slider, the sliding card is slidably connected in the through groove, limiting grooves are provided on both sides of the driving slider, and sliding columns are connected to both sides of the sliding card.

[0014] As a preferred solution of the reaction device for preparing o-tolyl isocyanate described in the present invention, a slot is provided on the threaded sleeve, a sliding column is connected to the fixed seat, the end of the rotating screw away from the rotating disk is connected to a driven gear, a sliding plate is slidably connected to the reaction box, an adjustment slot is provided on the sliding plate, an elastic laminate is embedded and installed at one end of the sliding plate, a sliding rack is slidably connected in the sliding plate, a stop block is connected to one side of the sliding plate, a touch block is slidably connected to the lower surface of the stop block, and the lower surface of the touch block is connected to the upper surface of the driving slider.

[0015] To achieve the above object, the present invention provides the following technical solution: a reaction device for preparing o-tolyl isocyanate, comprising the following reaction method: S1, injecting o-toluidine into the reaction tank through the delivery pipe, and driving the driving disc to rotate clockwise through the motor in the reaction box, which will drive the vertical surface of the ratchet block on the driving disc to fit with the ball in the half gear, and drive the half gear sleeved on the driving disc to rotate clockwise, and the rotating ring will drive the stirring rod on the upper surface to rotate along the inner wall of the reaction tank, and the stirring rod will drive the scraper groove opened on one side to slide along the inner wall of the reaction tank, and scrape off the isocyanate staying on the inner wall of the reaction tank or the crystals adsorbed on the inner wall from the inner wall; S2, drives the half gear to rotate clockwise through the driving disc to intermittently mesh with the driving gear on one side. When the teeth on one side of the half gear rotate through the driving gear, the limit slider at the other end of the half gear will slide along the limit rotating plate on the driving gear to limit the driving gear to prevent shaking. The driving gear drives the intermittent turntable at the other end to rotate 180 degrees in the exhaust pipe through the rotating shaft, intermittently blocking the connection of the exhaust pipe, so that the connecting hole on one side of the intermittent turntable is connected with the exhaust pipe, and the phosgene is transported to the reaction tank along the exhaust pipe through the air pump in the storage box. The phosgene will be transported to the exhaust duct opened on the sealing block along the exhaust pipe. When the air pump is working, high pressure is generated by compressing the gas, and the phosgene will push the sliding sealing head at the other end along the exhaust duct, so that the sliding sealing head slides along the limit sliding rod on one side of the support plate frame 2 to squeeze the reset spring piece. When the intermittent turntable rotates to block the connection of the exhaust pipe, as the air pressure decreases, the compressed reset spring piece will push the sliding sealing head to slide along the limit sliding rod under the reaction force to block the other end of the exhaust duct; S3, because the upper surface of the fixed seat is connected with a sliding column, the sliding card plate in the fixed seat is slidably connected to the card slot on one side of the threaded sleeve, and the rotating disc on the upper surface is driven by the driving disc to rotate clockwise, so that the rotating screw on the upper surface of the rotating disc and the stirring rod on the upper surface of the rotating ring rotate. The clockwise rotation of the rotating screw will drive the discharge plate on the lower surface of the threaded sleeve to move upward along the reaction tank. The driven gear at one end of the rotating screw rotates against the teeth on one side to push the sliding rack and pull the elastic laminate to slide in the adjustment groove. The sliding rack will not mesh with the driven gear. Since the two sides of the discharge plate are provided with limit slots to clamp the stirring rod, the stirring rod will drive the discharge plate to rotate on the lower surface of the threaded sleeve when it rotates. When the rotating screw drives the touch block on the driving slider to contact the stop block on the top of the reaction tank, it will push the driving slider to slide downward along the inside of the fixed seat, and the sliding columns on both sides of the sliding card plate will slide along the limit slots on both sides of the driving slider, so that the sliding card plate moves out of the card slot on the threaded sleeve along the through slot to squeeze the clamping spring in the placement cavity. At this time, the rotating screw will drive the threaded sleeve to rotate but will not drive the fixed seat to move. S4, when the reaction in the reaction tank is completed, when the motor drives the driving disc to rotate counterclockwise, the ball in the half gear will pass along the inclined surface of the ratchet block, and the phosgene delivery and stirring cleaning will stop at the same time. The driving disc drives the rotating screw on the rotating disc to rotate counterclockwise, so that the driven gear at one end of the rotating screw rotates and meshes with the sliding rack on one side. Through the meshing sliding rack, the sliding plate drives the resisting block at one end to move to the right. The compressed card spring will push the sliding columns on both sides of the sliding card plate to slide along the limit groove under the reaction force, pushing the driving slider to rise, so that the sliding card plate slides along the through groove to the self-rotating threaded sleeve and is fixed to the card groove, driving the fixed seat and the discharge plate to move downward along the stationary stirring rods on both sides, squeezing the isocyanate in the reaction tank out of the discharge pipe.

[0016] Compared with the known prior art, the technical solution provided by the present invention has the following beneficial effects: 1. The stirring rod on the upper surface is driven to rotate along the inner wall of the reaction tank by rotating the ring. The stirring rod will drive the scraper groove opened on one side to slide along the inner wall of the reaction tank, and the isocyanate remaining on the inner wall of the reaction tank or the crystals adsorbed on the inner wall will be scraped off from the inner wall. Stirring helps to ensure that the reactants are evenly distributed in the entire reaction mixture, avoiding excessively high or low local concentrations, thereby improving the overall reaction efficiency and product quality. While stirring, the crystals can be scraped off from the wall surface, reducing the accumulation of crystals on the side walls, and extending the service life of the reaction device. At the same time, the connection of the exhaust pipe is intermittently cut off, so that the connecting hole on one side of the intermittent turntable is connected to the exhaust pipe, and the phosgene is transported to the reaction tank along the exhaust pipe through the air pump in the storage box. By intermittently cutting off the transportation of phosgene, the concentration of the reactants in the reaction mixture can be adjusted, thereby controlling the reaction rate; 2. The sliding posts on both sides of the sliding card plate will slide along the limit grooves on both sides of the driving slider, so that the sliding card plate moves out of the card groove on the threaded sleeve along the through groove to squeeze the card spring in the placement cavity. At this time, the rotating screw will drive the threaded sleeve to rotate but will not drive the fixed seat to move. When the discharge plate moves to the top of the reaction tank and stops moving, the discharge amount of the material can be more accurately controlled to avoid excessive discharge or material residue. The stirring rod will continue to rotate and stir in the reaction tank, which helps to keep the material evenly mixed in the reactor and prevent the material from being mixed back due to stopping stirring during the discharge process. 3. By making the sliding card plate slide along the through groove to the self-rotating threaded sleeve and fix it in the card groove, the fixed seat and the discharge plate are driven to move downward along the stationary stirring rods on both sides, and the isocyanate in the reaction tank is squeezed out from the discharge pipe. The rapid discharge of the isocyanate that has reacted well can shorten the production cycle, increase the output per unit time, and thus improve the overall production efficiency. The rapid discharge can make the product leave the reaction environment as soon as possible, reducing the product degradation or quality change that may be caused by staying in the reactor for a long time. The rapid discharge of the isocyanate that has reacted well is helpful for the subsequent separation, purification and processing process, because the fresh reaction product is usually easier to handle. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the prior art descriptions are briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention, and for ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0018] Figure 1 It is a schematic diagram of the overall three-dimensional structure of the present invention; Figure 2 It is a structural schematic diagram of the reaction box of the present invention; Figure 3 It is a schematic diagram of the structure of the half gear of the present invention; Figure 4 It is a structural schematic diagram of an enlarged portion of the half gear A of the present invention; Figure 5 It is a structural schematic diagram of the reaction tank of the present invention; Figure 6 It is a structural schematic diagram of the enlarged portion of the reaction tank B of the present invention; Figure 7 A schematic diagram of the structure of the intermittent conveying mechanism of the present invention; Figure 8 A schematic diagram of the structure of the discharge plate of the present invention; Fig. 9 A schematic diagram of the structure of the discharge plate C of the present invention is enlarged; Fig.10 D is a schematic diagram of the structure of the present invention is an enlarged view of the discharge plate; Fig.11 It is a schematic structural diagram of an enlarged portion of the discharge plate E of the present invention.

[0019] In the figure: 100, reaction box; 200, cleaning and stirring mechanism; 201, driving disc; 202, ratchet block; 203, half gear; 204, sliding groove; 205, ball; 206, lifting slide; 207, limiting spring; 208, rotating ring; 209, stirring rod; 210, scraper groove; 211, reaction tank; 212, conveying pipe mouth; 213, discharge pipe mouth; 300, intermittent conveying mechanism; 301, exhaust pipe; 302, support plate frame 1; 303, reset spring; 304, sliding sealing head; 305, sealing block; 306, exhaust duct; 307, support plate frame 2; 308, limiting slide rod; 309, limiting slide block; 310, limiting rotating plate; 311, driving gear; 3 12. Rotating shaft; 313. Intermittent turntable; 314. Connecting hole; 315. Sealing strip; 316. Storage box; 400. Down-pressing discharging mechanism; 401. Rotating disc; 402. Spoiler; 403. Rotating screw rod; 404. Threaded sleeve; 405. Discharging plate; 406. Limiting groove; 407. Fixed seat; 408. Placement cavity; 409. Snap-on spring piece; 410. Sliding clamping plate; 411. Driving slider; 412. Through groove; 413. Limiting groove; 414. Sliding column; 415. Clamping groove; 416. Sliding column; 417. Driven gear; 418. Sliding plate; 419. Adjusting groove; 420. Elastic laminate; 421. Sliding rack; 422. Stop block; 423. Touch block. DETAILED DESCRIPTION

[0020] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0021] The present invention will be further described below in conjunction with the embodiments.

[0022] Example 1 Reference Figure 1-5 , which is the first embodiment of the present invention, provides a reaction device for preparing o-tolyl isocyanate and a reaction method thereof, including a reaction box 100, a cleaning stirring mechanism 200 is arranged in the reaction box 100, for stirring and cleaning the crystals adsorbed on the inner wall, an intermittent conveying mechanism 300 is arranged on one side of the cleaning stirring mechanism 200, for intermittently conveying phosgene, a downward pressing discharge mechanism 400 is arranged on the cleaning stirring mechanism 200, for promoting the rapid discharge of isocyanate, and the cleaning stirring mechanism 200 includes a driving disc 201 rotatably connected to the reaction box 100, ratchet blocks 202 are connected to the driving disc 201 at intervals, a half gear 203 is slidably connected to the ratchet block 202, a sliding groove 204 is provided on the half gear 203, a ball 205 that can limit the ratchet block 202 is slidably connected in the half gear 203, and a lifting mechanism 400 is slidably connected to the ball 205. The sliding seat 206, the end of the lifting sliding seat 206 away from the ball 205 is sleeved with a limiting spring piece 207, and the limiting spring piece 207 is arranged in the sliding groove 204. The upper surface of the half gear 203 is connected with a rotating ring 208. The shape of the ratchet block 202 is similar to a triangle. One side is provided with an inclined surface so that the ball 205 in the sliding groove 204 can pass through the sliding groove 204 along the surface of the ratchet block 202 to squeeze the sliding groove 204. The vertical plane provided on the other side of the ratchet block 202 is provided with a circular groove that matches the ball 205, which can clamp the ball 205 and place the ball 205 through the ratchet block 202 from the vertical plane. The sliding grooves 204 spaced apart on the half gear 203 have an inward arc support that matches the surface of the ball 205, and can prevent the ball 205 from falling off the sliding groove 204. The lifting sliding seat 206 is in the shape of a cylinder, and one end is provided with a groove that matches the ball 205.

[0023] A stirring rod 209 is connected to the upper surface of the rotating ring 208, a scraper groove 210 is provided on one side of the stirring rod 209, a reaction tank 211 is sleeved on the rotating ring 208, a delivery pipe port 212 is provided on the reaction tank 211, a discharge pipe port 213 is provided at one end of the reaction tank 211 away from the delivery pipe port 212, a stirring rod 209 is fixedly connected to the upper surface of the rotating ring 208, the shape of the stirring rod 209 fits the inner wall of the reaction tank 211, the scraper grooves 210 on the stirring rods 209 on both sides are staggered, a control valve is connected to the delivery pipe port 212 for adding o-toluidine, and a control valve is also connected to the discharge pipe port 213 to control the discharge of isocyanate after the reaction is completed.

[0024] During use, o-toluidine is injected into the reaction tank 211 through the delivery pipe port 212, and the motor in the reaction box 100 drives the driving disc 201 to rotate clockwise, which will drive the vertical surface of the ratchet block 202 on the driving disc 201 to fit with the ball 205 in the half gear 203, and drive the half gear 203 sleeved on the driving disc 201 to rotate clockwise. The rotating ring 208 will drive the stirring rod 209 on the upper surface to rotate along the inner wall of the reaction tank 211, and the stirring rod 209 will drive the scraper groove 210 opened on one side to slide along the inner wall of the reaction tank 211, and scrape off the isocyanate remaining on the inner wall of the reaction tank 211 or the crystals adsorbed on the inner wall from the inner wall.

[0025] Example 2 Reference Figure 1-7 , which is the second embodiment of the present invention, provides a reaction device and a reaction method for preparing o-tolyl isocyanate, wherein an exhaust pipe 301 is arranged in the reaction box 100, and the exhaust pipe 301 is embedded and installed on one side of the reaction tank 211, one end of the exhaust pipe 301 is connected to a support plate frame 302, one side of the support plate frame 302 is sleeved with a reset spring 303, and one end of the reset spring 303 away from the support plate frame 302 is sleeved with a sliding sealing head 304, a sealing block 305 is connected in the exhaust pipe 301, one side of the sealing block 305 is provided with a groove engaged with the sliding sealing head 304, a reset spring 303 is arranged between the sliding sealing head 304 and the support plate frame 302, and the support plate frame 302 is fixedly connected to one end of the exhaust pipe 301.

[0026] An exhaust duct 306 is provided on the sealing block 305, and a support plate frame 307 is embedded and installed on the sealing block 305. A limiting slide bar 308 is connected to one side of the support plate frame 307, and a limiting slider 309 is connected to the half gear 203. One side of the limiting slider 309 is slidably connected to a limiting rotating plate 310. The support plate frame 307 is fixedly connected to one end of the exhaust duct 306 close to the sliding sealing head 304, and one side of the sliding sealing head 304 is fixedly connected to the limiting slide bar 308. A through hole identical to the limiting slide bar 308 is provided on the sliding sealing head 304, and the sliding sealing head 304 slides along the limiting slide bar 308. The limiting slider 309 is fixedly connected to a side of the half gear 203 where no teeth are set. The shape of the limiting rotating plate 310 is a square composed of arcs. The two sides of the limiting rotating plate 310 have the same diameter as the limiting slider 309, so as to limit the driving gear 311.

[0027] The lower surface of the limit rotating plate 310 is connected to a driving gear 311 which intermittently meshes with the half gear 203, the upper surface of the limit rotating plate 310 is connected to a rotating shaft 312, the end of the rotating shaft 312 away from the limit rotating plate 310 is connected to an intermittent rotating disk 313, a connecting hole 314 is provided on the intermittent rotating disk 313, a sealing strip 315 is connected to the intermittent rotating disk 313, the end of the exhaust pipe 301 away from the reaction tank 211 is connected to a storage box 316, a connecting hole 314 is provided on one side of the intermittent rotating disk 313, and a connecting hole 314 is provided on the other side, and a connection between the exhaust pipe 301 and the storage box 316 is blocked, the intermittent rotating disk 313 is rotatably connected between the exhaust pipe 301, and is sealed by the sealing strip 315 on the intermittent rotating disk 313 to prevent air leakage, and the two ends of the rotating shaft 312 are respectively fixedly connected to the limit rotating plate 310 and the intermittent rotating disk 313.

[0028] During use, the driving disc 201 drives the half gear 203 to rotate clockwise and intermittently mesh with the driving gear 311 on one side. When the teeth on one side of the half gear 203 rotate through the driving gear 311, the limiting slider 309 at the other end of the half gear 203 slides along the limiting rotating plate 310 on the driving gear 311 to limit the driving gear 311 to prevent shaking. The driving gear 311 drives the intermittent rotating disk 313 at the other end to rotate 180 degrees in the exhaust pipe 301 through the rotating shaft 312, intermittently blocking the connection of the exhaust pipe 301, so that the connecting hole 314 on one side of the intermittent rotating disk 313 is connected to the exhaust pipe 301, and the air pump in the storage box 316 is connected. The phosgene is transported along the exhaust pipe 301 to the reaction tank 211, and the phosgene is transported along the exhaust pipe 301 to the exhaust duct 306 opened on the sealing block 305. When the air pump is working, high pressure is generated by compressing the gas, and the phosgene will push the sliding sealing head 304 at the other end along the exhaust duct 306, so that the sliding sealing head 304 slides along the limiting slide bar 308 on one side of the support plate frame 307 to squeeze the reset spring piece 303. When the intermittent turntable 313 rotates to cut off the connection of the exhaust pipe 301, as the air pressure decreases, the compressed reset spring piece 303 will push the sliding sealing head 304 to slide along the limiting slide bar 308 under the reaction force to block the other end of the exhaust duct 306.

[0029] The remaining structure is the same as that of Example 1.

[0030] Example 3 Reference Figure 1-11 , which is the third embodiment of the present invention, provides a reaction device for preparing o-tolyl isocyanate and a reaction method thereof, wherein the upper surface of the driving disc 201 is connected to a rotating disc 401, the upper surface of the rotating disc 401 is connected to a spoiler 402, the upper surface of the rotating disc 401 is connected to a rotating screw 403, a threaded sleeve 404 is screwed on the rotating screw 403, the lower surface of the threaded sleeve 404 is rotatably connected to a discharge plate 405, the upper surface of the driving disc 201 is fixedly connected to the rotating disc 401, the rotating disc 401 is spaced apart with spoilers 402, the spoiler 402 is in the shape of an arc-shaped baffle, which can stir the fallen crystals into the surrounding isocyanate during rotation, and the upper surface of the rotating disc 401 is fixedly connected to the rotating screw 403.

[0031] Limiting grooves 406 are provided on both sides of the discharge plate 405, and a fixed seat 407 is rotatably connected to the threaded sleeve 404. A placement cavity 408 is provided in the fixed seat 407, and a snap-on spring piece 409 is provided in the fixed seat 407. A sliding clamping plate 410 is slidably connected in the fixed seat 407. The sliding clamping plate 410 is slidably connected to the placement cavity 408 provided in the fixed seat 407. A snap-on spring piece 409 is provided between the fixed seat 407 and the sliding clamping plate 410. The shape of the limiting groove 406 is consistent with the stirring rod 209.

[0032] A driving slider 411 is slidably connected to the fixed seat 407, a through groove 412 is opened on the driving slider 411, a sliding clamp 410 is slidably connected in the through groove 412, limiting grooves 413 are opened on both sides of the driving slider 411, sliding columns 414 are connected on both sides of the sliding clamp 410, sliding columns 414 are fixedly connected on both sides of the sliding clamp 410, and the sliding columns 414 are slidably connected in the discharge pipe openings 213 opened on both sides of the driving slider 411, and the limiting grooves 413 are shaped as inclined grooves.

[0033] A card slot 415 is provided on the threaded sleeve 404, a sliding column 416 is connected to the fixed seat 407, a driven gear 417 is connected to the end of the rotating screw 403 away from the rotating disc 401, a sliding plate 418 is slidably connected to the reaction box 100, an adjustment slot 419 is provided on the sliding plate 418, an elastic laminate 420 is embedded and installed at one end of the sliding plate 418, a sliding rack 421 is slidably connected in the sliding plate 418, a stop block 422 is connected to one side of the sliding plate 418, a touch block 423 is slidably connected to the lower surface of the stop block 422, and the lower surface of the touch block 423 is connected to the driving On the upper surface of the movable slider 411, the sliding rack 421 is slidably connected in the adjusting groove 419 on the sliding plate 418, and the elastic laminate 420 is embedded between the sliding rack 421 and the sliding plate 418. A stop block 422 is fixedly connected to a part of the sliding plate 418. A touch block 423 is fixedly connected to the upper surface of the driving slider 411. The shape of the card slot 415 opened at a part of the threaded sleeve 404 is the same as that of the sliding card plate 410. The sliding column 416 is a plurality of hollow lifting rods sleeved together, which can slide according to the lifting and lowering of the fixed seat 407. The shape of the adjusting groove 419 is a rectangle with one end wide and the other end narrow.

[0034] During use, since the upper surface of the fixed seat 407 is connected with a sliding column 416, the sliding card plate 410 in the fixed seat 407 is slidably engaged in the card slot 415 on one side of the threaded sleeve 404, and the rotating disc 401 on the upper surface is driven by the driving disc 201 to rotate clockwise, so that the rotating screw rod 403 on the upper surface of the rotating disc 401 and the stirring rod 209 on the upper surface of the rotating ring 208 rotate. The clockwise rotation of the rotating screw rod 403 drives the discharge plate 405 on the lower surface of the threaded sleeve 404 to move upward along the reaction tank 211, and the driven gear 417 at one end of the rotating screw rod 403 rotates to press against the teeth on one side to push the sliding rack 4 21 pulls the elastic laminate 420 to slide in the adjustment groove 419, and the sliding rack 421 will not mesh with the driven gear 417. Since the limiting grooves 406 on both sides of the discharge plate 405 are clamped with the stirring rod 209, the stirring rod 209 will drive the discharge plate 405 to rotate on the lower surface of the threaded sleeve 404 when it rotates. When the rotating screw 403 rotates to drive the touch block 423 on the driving slider 411 to contact the stop block 422 at the top of the reaction tank 211, the driving slider 411 will be pushed to slide downward along the inside of the fixed seat 407, and the sliding columns 414 on both sides of the sliding card plate 410 will move along the limiting grooves 423 on both sides of the driving slider 411. 13 slides, so that the sliding card plate 410 moves out of the card slot 415 on the threaded sleeve 404 along the through groove 412 to squeeze the card spring piece 409 in the placement cavity 408. At this time, the rotating screw rod 403 will drive the threaded sleeve 404 to rotate without driving the fixed seat 407 to move. When the reaction in the reaction tank 211 is completed, the driving disc 201 is driven by the motor to rotate counterclockwise, and the ball 205 in the half gear 203 passes along the inclined surface of the ratchet block 202, and the phosgene delivery and stirring cleaning are stopped at the same time. The rotating screw rod 403 on the rotating disc 401 is driven by the driving disc 201 to rotate counterclockwise, so that one end of the rotating screw rod 403 is moved from The movable gear 417 rotates and meshes with the sliding rack 421 on one side, and the sliding plate 418 drives the stop block 422 at one end to move to the right through the meshing sliding rack 421. The compressed snap-on spring piece 409 will push the sliding columns 414 on both sides of the sliding card plate 410 to slide along the limiting groove 413 under the reaction force, pushing the driving slider 411 to rise, so that the sliding card plate 410 slides along the through groove 412 to the rotating threaded sleeve 404 and is snap-fitted and fixed to the card groove 415, driving the fixed seat 407 and the discharge plate 405 to move downward along the stationary stirring rods 209 on both sides, and the isocyanate in the squeeze reaction tank 211 is discharged from the discharge pipe mouth 213.

[0035] The remaining structure is the same as that of Example 1.

[0036] Reference Figure 1-9 , which is a fourth embodiment of the present invention, provides: a reaction device for preparing o-tolyl isocyanate, comprising the following reaction method, S1, o-toluidine is injected into the reaction tank 211 through the delivery pipe port 212, and the motor in the reaction box 100 drives the driving disc 201 to rotate clockwise, which will drive the vertical surface of the ratchet block 202 on the driving disc 201 to fit with the ball 205 in the half gear 203, and drive the half gear 203 sleeved on the driving disc 201 to rotate clockwise, and the rotating ring 208 will drive the stirring rod 209 on the upper surface to rotate along the inner wall of the reaction tank 211, and the stirring rod 209 will drive the scraper groove 210 opened on one side to slide along the inner wall of the reaction tank 211, and scrape off the isocyanate staying on the inner wall of the reaction tank 211 or the crystals adsorbed on the inner wall from the inner wall; S2, the driving disc 201 drives the half gear 203 to rotate clockwise and intermittently mesh with the driving gear 311 on one side. When the teeth on one side of the half gear 203 rotate through the driving gear 311, the limiting slider 309 at the other end of the half gear 203 will slide along the limiting rotating plate 310 on the driving gear 311 to limit the driving gear 311 to prevent shaking. The driving gear 311 drives the intermittent rotating disk 313 at the other end to rotate 180 degrees in the exhaust pipe 301 through the rotating shaft 312, intermittently blocking the connection of the exhaust pipe 301, so that the connecting hole 314 on one side of the intermittent rotating disk 313 is connected to the exhaust pipe 301, and the air pump in the storage box 316 is used to transfer the air into the exhaust pipe 301. Phosgene is transported to the reaction tank 211 along the exhaust pipe 301, and then transported to the exhaust passage 306 opened on the sealing block 305. When the air pump is working, high pressure is generated by compressing the gas, and the phosgene pushes the sliding sealing head 304 at the other end along the exhaust passage 306, so that the sliding sealing head 304 slides along the limiting slide bar 308 on one side of the supporting plate frame 307 to squeeze the reset spring piece 303. When the intermittent turntable 313 rotates to cut off the connection of the exhaust pipe 301, as the air pressure decreases, the compressed reset spring piece 303 pushes the sliding sealing head 304 to slide along the limiting slide bar 308 under the reaction force to block the other end of the exhaust passage 306. S3, since the upper surface of the fixed seat 407 is connected with a sliding column 416, the sliding card plate 410 in the fixed seat 407 is slidably engaged in the card slot 415 on one side of the threaded sleeve 404, and the rotating disc 401 on the upper surface is driven by the driving disc 201 to rotate clockwise, so that the rotating screw 403 on the upper surface of the rotating disc 401 and the stirring rod 209 on the upper surface of the rotating ring 208 rotate, and the clockwise rotation of the rotating screw 403 will drive the discharge plate 405 on the lower surface of the threaded sleeve 404 to move upward along the reaction tank 211, and the driven gear 417 at one end of the rotating screw 403 rotates against the teeth on one side to push the sliding rack 421 to pull the elastic laminate 420 to slide in the adjustment groove 419, and the sliding rack 421 will not mesh with the driven gear 417. Limiting grooves 406 are provided on both sides of the plate 405 to clamp the stirring rod 209. When the stirring rod 209 rotates, it will drive the discharge plate 405 to rotate on the lower surface of the threaded sleeve 404. When the rotating screw rod 403 rotates and drives the touch block 423 on the driving slider 411 to contact the stop block 422 at the top of the reaction tank 211, it will push the driving slider 411 to slide downward along the inside of the fixed seat 407. The sliding columns 414 on both sides of the sliding card plate 410 will slide along the limiting grooves 413 on both sides of the driving slider 411, so that the sliding card plate 410 moves out of the clamping groove 415 on the threaded sleeve 404 along the through groove 412 to squeeze the clamping spring 409 in the placement cavity 408. At this time, the rotating screw rod 403 will drive the threaded sleeve 404 to rotate but will not drive the fixed seat 407 to move.

[0037] S4, when the reaction in the reaction tank 211 is completed, the motor drives the driving disc 201 to rotate counterclockwise, and the ball 205 in the half gear 203 passes along the inclined surface of the ratchet block 202, and the phosgene delivery and stirring cleaning are stopped at the same time. The driving disc 201 drives the rotating screw 403 on the rotating disc 401 to rotate counterclockwise, so that the driven gear 417 at one end of the rotating screw 403 rotates and meshes with the sliding rack 421 on one side, and the meshing sliding rack 421 drives the sliding plate 418 to The stop block 422 at one end moves to the right, and the compressed snap-on spring piece 409 will push the sliding columns 414 on both sides of the sliding card plate 410 to slide along the limiting groove 413 under the reaction force, pushing the driving slider 411 to rise, so that the sliding card plate 410 slides along the through groove 412 to the rotating threaded sleeve 404 and is snap-fitted and fixed to the card groove 415, driving the fixed seat 407 and the discharge plate 405 to move downward along the stationary stirring rods 209 on both sides, squeezing the isocyanate in the reaction tank 211 to be discharged from the discharge pipe mouth 213.

[0038] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements will not cause the essence of the corresponding technical solutions to deviate from the protection scope of the technical solutions of the embodiments of the present invention.

Claims

1. A reaction device for preparing o-tolyl isocyanate and a reaction method thereof, comprising a reaction box (100), characterized in that: The reaction box (100) is provided with a cleaning stirring mechanism (200) for stirring and cleaning the crystals adsorbed on the inner wall; an intermittent conveying mechanism (300) is provided on one side of the cleaning stirring mechanism (200) for intermittently conveying phosgene; and a downward pressure discharge mechanism (400) is provided on the cleaning stirring mechanism (200) for promoting rapid discharge of isocyanate; The cleaning stirring mechanism (200) comprises a driving disc (201) rotatably connected to a reaction box (100), a ratchet block (202) being connected to the driving disc (201) at intervals, a half gear (203) being slidably connected to the ratchet block (202), a sliding groove (204) being provided on the half gear (203), a ball (205) being slidably connected in the half gear (203) for limiting the ratchet block (202), a lifting slide (206) being slidably connected to the ball (205), a limiting spring sheet (207) being sleeved on one end of the lifting slide (206) away from the ball (205), the limiting spring sheet (207) being arranged in the sliding groove (204), and a rotating ring (208) being connected to the upper surface of the half gear (203).

2. A reaction device and reaction method for preparing o-tolyl isocyanate according to claim 1, characterized in that: The upper surface of the rotating ring (208) is connected to a stirring rod (209), one side of the stirring rod (209) is provided with a scraper groove (210), a reaction tank (211) is sleeved on the rotating ring (208), a delivery pipe opening (212) is provided on the reaction tank (211), and a discharge pipe opening (213) is provided at one end of the reaction tank (211) away from the delivery pipe opening (212).

3. A reaction device and reaction method for preparing o-tolyl isocyanate according to claim 1, characterized in that: An exhaust pipe (301) is arranged in the reaction box (100); an exhaust pipe (301) is embedded in one side of the reaction tank (211); one end of the exhaust pipe (301) is connected to a support plate frame 1 (302); a reset spring sheet (303) is sleeved on one side of the support plate frame 1 (302); an end of the reset spring sheet (303) away from the support plate frame 1 (302) is sleeved on a sliding sealing head (304); and a sealing block (305) is connected in the exhaust pipe (301).

4. A reaction device and reaction method for preparing o-tolyl isocyanate according to claim 3, characterized in that: An exhaust passage (306) is provided on the sealing block (305), a supporting plate frame 2 (307) is embedded and installed on the sealing block (305), one side of the supporting plate frame 2 (307) is connected to a limiting slide bar (308), the half gear (203) is connected to a limiting slide block (309), and one side of the limiting slide block (309) is slidably connected to a limiting rotating plate (310).

5. A reaction device and reaction method for preparing o-tolyl isocyanate according to claim 4, characterized in that: The lower surface of the limit rotating plate (310) is connected to a driving gear (311) that intermittently meshes with the half gear (203); the upper surface of the limit rotating plate (310) is connected to a rotating shaft (312); the end of the rotating shaft (312) away from the limit rotating plate (310) is connected to an intermittent rotating disk (313); a connecting hole (314) is provided on the intermittent rotating disk (313); a sealing strip (315) is connected to the intermittent rotating disk (313); and the end of the exhaust pipe (301) away from the reaction tank (211) is connected to a storage box (316).

6. A reaction device and reaction method for preparing o-tolyl isocyanate according to claim 1, characterized in that: The upper surface of the driving disc (201) is connected to a rotating disc (401), the upper surface of the rotating disc (401) is connected to a spoiler (402), the upper surface of the rotating disc (401) is connected to a rotating screw rod (403), a threaded sleeve (404) is screwed onto the rotating screw rod (403), and a discharge plate (405) is rotatably connected to the lower surface of the threaded sleeve (404).

7. A reaction device and reaction method for preparing o-tolyl isocyanate according to claim 6, characterized in that: Limiting grooves (406) are provided on both sides of the discharge plate (405); a fixing seat (407) is rotatably connected to the threaded sleeve (404); a placement cavity (408) is provided in the fixing seat (407); a clamping spring (409) is provided in the fixing seat (407); and a sliding clamping plate (410) is slidably connected in the fixing seat (407).

8. A reaction device and reaction method for preparing o-tolyl isocyanate according to claim 7, characterized in that: A driving slider (411) is slidably connected to the fixed seat (407), a through slot (412) is provided on the driving slider (411), the sliding card plate (410) is slidably connected in the through slot (412), limiting slots (413) are provided on both sides of the driving slider (411), and sliding columns (414) are connected to both sides of the sliding card plate (410).

9. A reaction device and reaction method for preparing o-tolyl isocyanate according to claim 6, characterized in that: The threaded sleeve (404) is provided with a slot (415), the fixed seat (407) is connected with a sliding column (416), the end of the rotating screw (403) away from the rotating disc (401) is connected with a driven gear (417), the reaction box (100) is slidably connected with a sliding plate (418), the sliding plate (418) is provided with an adjustment slot (419), one end of the sliding plate (418) is embedded with an elastic laminate (420), the sliding plate (418) is slidably connected with a sliding rack (421), one side of the sliding plate (418) is connected with a stop block (422), the lower surface of the stop block (422) is slidably connected with a touch block (423), and the lower surface of the touch block (423) is connected to the upper surface of the driving slider (411).

10. A reaction device for preparing o-tolyl isocyanate as described in any one of 1 to 9, comprising the following reaction method: S1, o-toluidine is injected into the reaction tank (211) through the delivery pipe port (212), and the motor in the reaction box (100) drives the driving disc (201) to rotate clockwise, which drives the vertical surface of the ratchet block (202) on the driving disc (201) to fit with the ball (205) in the half gear (203), driving the half gear (203) sleeved on the driving disc (201) to rotate clockwise, and the rotating ring (208) drives the stirring rod (209) on the upper surface to rotate along the inner wall of the reaction tank (211), and the stirring rod (209) drives the scraper groove (210) provided on one side to slide along the inner wall of the reaction tank (211), so as to scrape off the isocyanate remaining on the inner wall of the reaction tank (211) or the crystals adsorbed on the inner wall from the inner wall; S2, the driving disc (201) drives the half gear (203) to rotate clockwise and intermittently mesh with the driving gear (311) on one side. When the teeth on one side of the half gear (203) rotate through the driving gear (311), the limiting slider (309) on the other end of the half gear (203) slides along the limiting rotating plate (310) on the driving gear (311) to limit the driving gear (311) and prevent it from shaking. The driving gear (311) drives the intermittent rotating disc (313) on the other end to rotate 180 degrees in the exhaust pipe (301) through the rotating shaft (312), intermittently blocking the connection of the exhaust pipe (301), so that the connecting hole (314) on one side of the intermittent rotating disc (313) is connected to the exhaust pipe (301), and the gas in the storage box (316) is discharged. The pump transports phosgene along the exhaust pipe (301) into the reaction tank (211), and the phosgene is transported along the exhaust pipe (301) into the exhaust passage (306) opened on the sealing block (305). When the air pump is working, high pressure is generated by compressing the gas, and the phosgene pushes the sliding sealing head (304) at the other end along the exhaust passage (306), so that the sliding sealing head (304) slides along the limiting slide bar (308) on one side of the supporting plate frame (307) to squeeze the reset spring sheet (303). When the intermittent turntable (313) rotates to cut off the connection of the exhaust pipe (301), as the air pressure decreases, the compressed reset spring sheet (303) pushes the sliding sealing head (304) to slide along the limiting slide bar (308) under the reaction force to block the other end of the exhaust passage (306); S3, since the upper surface of the fixed seat (407) is connected to a sliding column (416), the sliding clamping plate (410) in the fixed seat (407) is slidably clamped in the clamping groove (415) on one side of the threaded sleeve (404), and the rotating disk (401) on the upper surface is driven by the driving disk (201) to rotate clockwise, so that the rotating screw (403) on the upper surface of the rotating disk (401) and the stirring rod (209) on the upper surface of the rotating ring (208) rotate. The screw rod (403) rotates clockwise to drive the discharge plate (405) on the lower surface of the threaded sleeve (404) to move upward along the reaction tank (211). The driven gear (417) at one end of the screw rod (403) rotates against the teeth on one side to push the sliding rack (421) to pull the elastic laminate (420) to slide in the adjustment groove (419). The sliding rack (421) does not mesh with the driven gear (417). 05) The two sides are provided with limit slots (406) to which the stirring rod (209) is clamped. When the stirring rod (209) rotates, it drives the discharge plate (405) to rotate on the lower surface of the threaded sleeve (404). When the rotating screw (403) drives the contact block (423) on the driving slider (411) to contact the stop block (422) at the top of the reaction tank (211), the driving slider (411) is pushed along the inner side of the fixed seat (407). Sliding downward, the sliding posts (414) on both sides of the sliding card plate (410) will slide along the limiting grooves (413) on both sides of the driving slider (411), so that the sliding card plate (410) moves out of the clamping groove (415) on the threaded sleeve (404) along the through groove (412) to squeeze the clamping spring (409) in the placement cavity (408). At this time, the rotating screw (403) will drive the threaded sleeve (404) to rotate without driving the fixed seat (407) to move; S4, when the reaction in the reaction tank (211) is completed, the motor drives the driving disc (201) to rotate counterclockwise, and the ball (205) in the half gear (203) passes along the inclined surface of the ratchet block (202), and the phosgene delivery and stirring cleaning are stopped at the same time. The driving disc (201) drives the rotating screw (403) on the rotating disc (401) to rotate counterclockwise, so that the driven gear (417) at one end of the rotating screw (403) rotates and meshes with the sliding rack (421) on one side, and the sliding plate (418) drives one end through the meshing sliding rack (421). The stop block (422) moves to the right, and the compressed engaging spring sheet (409) pushes the slide posts (414) on both sides of the sliding card plate (410) to slide along the limit groove (413) under the reaction force, pushing the driving slider (411) to rise, so that the sliding card plate (410) slides along the through groove (412) to the self-rotating threaded sleeve (404) and is engaged and fixed with the engaging groove (415), driving the fixing seat (407) and the discharge plate (405) to move downward along the stationary stirring rods (209) on both sides, and the isocyanate in the squeeze reaction tank (211) is discharged from the discharge pipe port (213).

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