Benzofuroxan as well as preparation system and preparation method thereof

Abstract

The invention relates to the technical field of benzofuroxan preparation, and particularly discloses benzofuroxan and a preparation system and a preparation method thereof, the benzofuroxan comprises a resin barrel and a plurality of resin columns, the resin barrel is provided with a rotating rod, and the resin barrel is also internally provided with a first station, a second station, a third station and a fourth station; when the resin column is located at the first station, the resin column is used for adsorbing organic matters in the waste liquid, when the resin column is located at the second station, methanol is used for eluting the adsorbed organic matters in the resin column, when the resin column is located at the third station, the residual methanol in the resin column is centrifugally thrown away, and when the resin column is located at the fourth station, the residual methanol in the resin column is centrifugally thrown away. According to the resin column detection device, the content of methanol in a resin column is detected, resin in the resin column is dumped and replaced, the rotating rod drives the resin column to be switched on the first station, the second station, the third station and the fourth station, and the time consumed for replacing the resin column and the cost needed for replacing the resin column are saved.

Description

Technical Field

[0001] The present application relates to the technical field of benzofuroxan oxide preparation, and in particular to a benzofuroxan oxide and a preparation system and method thereof. Background Art

[0002] Benzofuroxan oxide is an important organic compound, which is widely used in the fields of optical materials, fragrances and drug synthesis. As a light stabilizer, benzofuroxan oxide can absorb ultraviolet rays and prevent the aging of plastics and coatings. In addition, it is used as a flavor ingredient in the fragrance industry to give the product a specific aroma, and is also used as an intermediate in drug synthesis. Its multiple uses make it occupy an important position in the chemical industry.

[0003] In the prior art, the preparation system of benzofurazan oxide includes a benzofurazan oxide synthesis device, a centrifugal separation and purification device, and a waste liquid treatment device. The general operation process is to first treat the raw materials for synthesizing benzofurazan oxide in sequence, and then send them to the synthesis device for reaction. During the synthesis process, the temperature and pressure are controlled to ensure the efficient reaction. After the reaction is completed, the mixture is separated by a centrifugal separation and purification device to remove unreacted raw materials and by-products to obtain crude benzofurazan oxide. Then, the crude product is further distilled or crystallized and purified to obtain high-purity benzofurazan oxide. Finally, the waste liquid treatment device treats the waste liquid generated during the reaction. The waste liquid treatment device will include a resin elution column for adsorbing organic matter in the waste liquid, and then the organic matter in the resin elution column is extracted by methanol washing, thereby ensuring compliance with environmental protection standards and reducing the impact on the environment.

[0004] For the above-mentioned related technologies, after the resin elution column is flushed with methanol, a large amount of methanol may remain in the resin elution column, and methanol will also dissolve some organic matter in the waste liquid, thereby reducing the elution effect of the organic matter in the waste liquid when the resin elution column is used again. If the resin elution column is directly replaced, it will cost a lot, and the adsorption of organic matter by the resin elution column and the flushing of the resin elution column by methanol cannot be carried out at the same time. When replacing the resin elution column, it is necessary to stop the adsorption of organic matter by the resin elution column and the flushing of the resin elution column by methanol. Therefore, the treatment efficiency of the waste liquid is low, so improvements are made. Summary of the invention

[0005] In order to ensure that the resin elution column always has a good adsorption effect on organic matter in the waste liquid, and shorten the overall time required for the resin desorption column to adsorb organic matter, methanol to rinse the resin desorption column and replace the resin desorption column, improve the treatment efficiency of the waste liquid, and reduce the cost of replacing the resin elution column, the present application provides a benzofuroxan oxide and its preparation system and preparation method.

[0006] The present application provides a system for preparing benzofuroxan oxide, which adopts the following technical solution: A preparation system of benzofuroxan oxide, comprising a mounting frame, a resin barrel, a waste liquid recovery barrel and a methanol recovery barrel, wherein the resin barrel, the waste liquid recovery barrel and the methanol recovery barrel are all arranged on the mounting frame, the resin barrel is provided with a waste liquid inlet, a methanol inlet, a waste liquid outlet and a methanol outlet, a resin column is vertically arranged in the resin barrel, and a liquid inlet pipe and a liquid outlet pipe are arranged on the resin column, wherein the liquid inlet pipe is arranged above the liquid outlet pipe; A rotating rod is arranged in the resin barrel, a first driving motor is arranged on the resin barrel, the rotating rod penetrates the top wall of the resin barrel and is connected to the output shaft of the first driving motor, a connecting rod is arranged on the rotating rod, one end of the connecting rod away from the rotating rod is connected to the top of the resin column, and the rotating rod drives the resin column to rotate around the rotating rod through the connecting rod; A first station is provided in the resin barrel. When the resin column is located at the first station, the liquid inlet pipe is connected to the waste liquid inlet, and the liquid outlet pipe is connected to the waste liquid outlet, so as to use the resin column to adsorb organic matter in the waste liquid; A second station is provided in the resin barrel. When the resin column is located at the second station, the liquid inlet pipe is connected to the methanol liquid inlet, and the liquid outlet pipe is connected to the methanol liquid outlet, so as to use methanol to elute the adsorbed organic matter in the resin column; The resin barrel is provided with a third station, the resin barrel is provided with a centrifugal liquid outlet, when the resin column is located at the third station, the liquid outlet pipe is connected to the centrifugal liquid outlet, the third station and the resin column are provided with a centrifugal mechanism for centrifugally removing the methanol remaining in the resin column, and the centrifugal liquid outlet is connected to the methanol liquid outlet; A fourth station is provided in the resin barrel, and a dumping mechanism for detecting the methanol content in the resin column and dumping and replacing the resin in the resin column is provided on the fourth station and the resin column; The resin columns are provided in plurality, and the rotating rod drives the positions of the plurality of resin columns to be switched respectively at the first station, the second station, the third station and the fourth station; The liquid inlet pipe and the waste liquid inlet are provided with a connecting component, and the connecting component is used to connect with the waste liquid inlet after the liquid inlet pipe rotates around the rotating rod. The liquid outlet pipe is arranged with the liquid inlet pipe, and the waste liquid outlet, the methanol inlet, the methanol outlet and the centrifuge liquid outlet are all arranged with the waste liquid inlet.

[0007] By adopting the above technical solution, the waste liquid is input into the resin barrel from the waste liquid inlet, and then input into the resin column from the inlet pipe on the resin column connected to the waste liquid inlet at the first station. After the resin in the resin column adsorbs the organic matter in the waste liquid, the waste liquid is output from the outlet pipe and the waste liquid outlet. When the resin column adsorbs enough organic matter, the first drive motor is started, and the first drive motor drives the resin column to rotate around the rotating rod as the center and move to the second station. Methanol is injected into the resin barrel from the methanol inlet, and then input into the resin column from the inlet pipe connected to the methanol inlet at the second station, thereby adsorbing the resin column. The organic matter adsorbed in the resin column is eluted. When the organic matter in the resin column is eluted, more methanol will remain in the resin column, which will affect the adsorption effect of the resin column on the organic matter. The first drive motor is started to rotate the resin column to the third station. The centrifugal mechanism on the third station can rotate and centrifuge the resin column, so as to centrifugally shake off the methanol in the resin column and then output it from the liquid outlet pipe and the centrifugal liquid outlet. When more methanol still remains after the resin column is centrifuged, more organic matter will be dissolved in the methanol at the same time, which means that the resin column needs to be replaced. At this time, the first drive motor is driven again. The machine rotates the resin column to the fourth station. The dumping mechanism at the fourth station can detect the methanol residue in the resin column. When the test is qualified, the first drive motor will rotate the resin column to the first station for continued use. When the test is unqualified, the dumping mechanism at the fourth station will dump the resin in the resin column and add new resin, thereby ensuring the resin column's adsorption effect on organic matter in the waste liquid. The first drive motor and the rotating rod are used to switch multiple resin columns at the first station, the second station, the third station and the fourth station, respectively, to achieve the adsorption of organic matter in the waste liquid and the elution of the resin column. , the separation and removal of residual methanol and the detection and replacement of the resin are carried out at the same time, which shortens the overall time required for the resin desorption column to adsorb organic matter, rinse the resin desorption column with methanol, and detect and replace the resin desorption column. Compared with the prior art of replacing the entire resin column, the present application also saves the time consumed in replacing the resin column and the cost required for replacing the resin column, and the removal and detection of residual methanol can better ensure the use effect of the resin column, and the connecting component can realize the stability of the connection between the liquid inlet pipe and the liquid outlet pipe when they are connected to each connecting port after rotating around the rotating rod.

[0008] Optionally, the centrifugal mechanism includes a second drive motor, a driving gear, a driven gear, a first rotating barrel, a second rotating barrel, a limiting structure and an extrusion assembly. A fixed plate is provided in the resin barrel, and the fixed plate is provided below the resin column. The second drive motor is provided on a side of the fixed plate away from the resin column. The driving gear is provided on a side of the fixed plate close to the resin column and is connected to an output shaft of the second drive motor. The resin column includes an outer shell, the first rotating barrel is rotatably provided in the outer shell, the second rotating barrel is rotatably provided in the first rotating barrel, the resin is provided in the second rotating barrel, and the driven gear is provided on a side of the first rotating barrel close to the second drive motor and is connected to the output shaft of the second drive motor. When the gears abut, they mesh with the driving gear. A movable annular groove is provided on the fixed plate for the driven gear to rotate around the rotating rod. Centrifugal holes are provided on the first rotating barrel and the second rotating barrel. The limiting structure is used to drive the second rotating barrel to rotate synchronously after the first rotating barrel and the second rotating barrel rotate relative to each other, so that the centrifugal holes on the first rotating barrel and the second rotating barrel are aligned, and is used to reset the first rotating barrel and the second rotating barrel after the first rotating barrel and the second rotating barrel stop rotating, so that the centrifugal holes on the first rotating barrel and the second rotating barrel are staggered. The extrusion assembly is arranged in the second rotating barrel for extruding resin.

[0009] By adopting the above technical solution, the second driving motor is started, and the driving gear on the output shaft of the second driving motor drives the driven gear to rotate. Since the driven gear is installed on the side of the first rotating barrel close to the second driving motor, the second driving motor can drive the first rotating barrel to rotate. While the first rotating barrel is rotating, the second rotating barrel can be driven to rotate synchronously under the action of the limiting structure. When the first rotating body and the second rotating barrel rotate synchronously, the centrifugal holes opened on the first rotating barrel and the second rotating barrel are aligned. At this time, the methanol solution remaining in the resin is thrown from the centrifugal hole to the gap between the first rotating barrel and the shell under the action of centrifugation, and is discharged from the liquid outlet on the shell. The first rotating barrel and the second rotating barrel are connected to each other, and the centrifugal holes on the first rotating barrel and the second rotating barrel are staggered to restore the initial state, so as to facilitate the subsequent use of the resin column. The extrusion assembly in the present application can realize the extrusion of the resin in the resin column, thereby further reducing the residual methanol in the resin column and improving the centrifugal effect on the residual methanol in the resin.

[0010] Optionally, the limiting structure includes a rotation limit block and a first reset member, the rotation limit block is arranged on the inner top wall of the first rotating barrel, and an arc groove corresponding to the rotation limit block is opened on the outer top wall of the second rotating barrel, when the rotation limit blocks are located at both ends of the arc groove, the first rotating barrel drives the second rotating barrel to rotate synchronously, and the centrifugal holes on the first rotating barrel and the second rotating barrel are aligned with each other, the first reset member is arranged between the inner top wall of the first rotating barrel and the outer top wall of the second rotating barrel, and the first reset member is used to reset the first rotating barrel and the second rotating barrel when the first rotating barrel and the second rotating barrel stop rotating, so that the centrifugal holes on the first rotating barrel and the second rotating barrel are staggered.

[0011] By adopting the above technical scheme, in the initial state, the rotation limit block is located in the middle position of the arc groove, at this time, the centrifugal holes opened on the first rotating barrel and the second rotating barrel are staggered with each other, when the second driving motor is started, the second driving motor drives the first rotating barrel to rotate, after the first rotating barrel and the second rotating barrel rotate relative to each other, the rotation limit block rotates to one end of the arc groove and abuts against the inner wall of the arc groove, so that the first rotating barrel drives the second rotating barrel to rotate synchronously, at this time, the centrifugal holes on the first rotating barrel and the second rotating barrel are aligned with each other, when the second driving motor rotates in the opposite direction, the rotation limit block will move to the other end of the arc groove, at this time, the separation holes on the first rotating barrel and the second rotating barrel are also aligned, so that no matter whether the second driving motor is rotating forward or reverse, the residual methanol in the resin column can be shaken off, thereby improving the adsorption effect of the resin column on organic matter in waste liquid.

[0012] Optionally, the extrusion assembly includes a lifting plate, a screw rod and a vertical limit block, the lifting plate is lifted and arranged in the second rotating barrel, the vertical limit block is arranged on the lifting plate, a vertical groove is opened on the inner wall of the second rotating barrel corresponding to the vertical limit block, the screw rod is arranged in the second rotating barrel, one end of the screw rod is rotatably connected to the inner bottom wall of the first rotating barrel, the other end of the screw rod passes through the first rotating barrel and the second rotating barrel and is fixedly connected to the inner top wall of the outer shell, the lifting plate is arranged on the screw rod and is threadedly connected to the screw rod, and when the first rotating barrel drives the second rotating barrel to rotate, the lifting plate is lifted and lowered under the action of the vertical limit block and the screw rod.

[0013] By adopting the above technical solution, since one end of the screw rod is fixedly mounted on the outer shell and the other end is connected to the inner bottom plate of the first rotating barrel, the screw rod does not rotate when the first rotating barrel rotates. Since the vertical limit block on the lifting plate is slidably mounted in the vertical groove, and the lifting plate and the screw rod are threadedly connected, when the first rotating barrel drives the second rotating body to rotate synchronously, the second rotating barrel can drive the lifting plate to rotate synchronously, thereby realizing the lifting and lowering of the lifting plate on the screw rod. When the height of the lifting plate changes, the resin column in the second rotating barrel can be squeezed, thereby further reducing the methanol residue in the resin column and improving the centrifugal effect on the residual methanol in the resin.

[0014] Optionally, the dumping mechanism includes a dumping port, a dumping pan, a clamping block, an electric telescopic rod and a detection assembly, the dumping port is arranged on a surface of the fixed plate away from the resin column, and the fixed plate is provided with a discharge port at a position corresponding to the dumping port, the clamping block is arranged on the dumping pan, a clamping groove is arranged on the inner bottom wall of the first rotating barrel corresponding to the clamping block, the dumping pan is clamped with the clamping block and the clamping groove on the inner bottom wall of the first rotating barrel, a socket barrel is arranged on the surface of the dumping pan away from the fixed plate, the screw rod rotates at one end close to the fixed plate and is socketed in the socket barrel, and the depth of the socket barrel The driven gear is fixedly arranged on a side of the pouring tray close to the fixed plate, the electric telescopic rod is arranged in the pouring port, the electric telescopic rod comprises a first telescopic end and a second telescopic end, the first telescopic end of the electric telescopic rod is extended to abut against a side of the pouring tray close to the fixed plate, the first telescopic end of the electric telescopic rod is extended to separate the pouring tray from the first rotating barrel, and the resin in the second rotating barrel falls into the pouring port from the gap between the pouring tray and the first rotating barrel, and the detection component is used to detect the amount of residual methanol in the resin column.

[0015] By adopting the above technical scheme, after the detection component detects the methanol content in the resin column, if the detection is qualified, the first drive motor will transport the resin column to the first station for adsorption of organic matter in the waste liquid. When the detection result of the detection component for the methanol content in the resin column is too high, the electric telescopic rod is started, and the first telescopic end of the electric telescopic rod is extended to abut against a side of the pouring plate close to the fixed plate. Since the pouring plate is circumferentially clamped and axially socket-connected with the inner bottom wall of the first rotating barrel through the clamping block, the extension of the first telescopic end can lift the pouring plate to achieve separation from the inner bottom wall of the first rotating barrel, and the resin in the second rotating barrel falls into the pouring port from the gap between the pouring plate and the first rotating barrel, thereby realizing the pouring of the resin in the resin column, and when the pouring plate is lifted up by the first telescopic end of the electric telescopic rod, since the depth of the socket barrel is greater than the height of the screw rod in the socket barrel, interference between the screw rod and the pouring plate can be avoided, and the socket barrel also improves the stability of the screw rod, thereby avoiding the eccentricity of the screw rod after long-term use.

[0016] Optionally, the detection component includes an air pump and a methanol detector, the resin barrel is provided with an air inlet and an air outlet, the air inlet and the air outlet are both arranged at the same time as the waste liquid inlet, the air pump is arranged on the air inlet, and the methanol detector is arranged on the air outlet. When the resin column is located at the fourth station, the air inlet is connected to the liquid outlet pipe, and the air outlet is connected to the liquid inlet pipe. A resin adding port is provided on the air inlet, and an end cover is provided on the resin adding port. The methanol detector is electrically connected to the air pump and the electric telescopic rod.

[0017] By adopting the above technical solution, when the resin column is located at the fourth station, the air pump is started to transport air into the resin column. When the methanol detector located on the air outlet detects that the methanol content in the output gas exceeds the standard, it means that the methanol residue in the resin exceeds the standard and may not be suitable for continuing to adsorb organic matter in the waste liquid. At this time, the methanol detector will send an electrical signal to the electric telescopic rod and the air pump, turn off the air pump and turn on the electric telescopic rod at the same time, so as to dump the resin. When the dumping is completed, the electric telescopic rod can be closed, and new resin can be added from the resin adding port on the air inlet. Compared with the prior art of replacing the entire resin column, the present application saves the time consumed in replacing the resin column, the delayed construction period and the cost required for replacing the resin column.

[0018] Optionally, a second reset member is provided between the pouring tray and the first rotating barrel, the second reset member comprising a spring, a column and a reset block, the column is provided on the inner bottom wall of the outer shell, the reset block is provided at the end of the column away from the fixed plate and is clamped with the pouring tray, the pouring tray is provided with an annular groove for movement of the reset block, the bottom wall of the outer shell is provided with a mounting groove, the end of the column away from the pouring tray is located in the mounting groove, the end of the column away from the pouring tray is provided with a limiting plate, the spring is provided on the column and is located between the limiting plate and the top wall of the mounting groove.

[0019] By adopting the above technical scheme, since the reset block and the pouring plate are clamped together and the reset block is installed on the column, when the first telescopic end of the electric telescopic rod drives the pouring plate to rise, it drives the column and the reset column to rise synchronously, and the spring is compressed between the limit plate and the mounting groove until the limit plate abuts against the inner wall of the mounting groove. At this time, the pouring plate and the inner bottom wall of the first rotating barrel are completely separated, and the resin in the second rotating barrel is poured through the gap between the first rotating barrel and the pouring plate. When the first telescopic end is shortened, the spring extends between the limit plate and the mounting groove until the inner bottom wall of the first rotating barrel is completely abutted against the pouring plate. The spring can make the pouring plate fit more closely with the end of the first telescopic end during the rising and falling process of the pouring plate, so that the lifting and lowering of the pouring plate is more stable, and the abutment sealing effect between the inner bottom wall of the first rotating barrel and the pouring plate can be improved.

[0020] Optionally, a sealing plate is provided at the bottom of the pouring port, and the second telescopic end of the electric telescopic rod is fixedly connected to the sealing plate. When the second telescopic end is shortened, the sealing plate and the bottom of the pouring port are clamped together to close the bottom of the pouring port. A discharge channel for facilitating the pouring of resin is provided in the pouring port, and both ends of the discharge channel are funnel-shaped extending outward. The sealing plate has a convex curved surface on one side close to the fixed plate, and a resin recovery bucket is provided below the pouring port.

[0021] By adopting the above technical solution, while the first telescopic end of the electric telescopic rod is extended, the second telescopic end is extended synchronously, and the second telescopic end is extended while driving the sealing plate to descend, so that the resin in the pouring port is poured into the resin recovery barrel from the gap between the sealing plate and the pouring port. When the pouring is completed, the second telescopic end is shortened until the sealing plate and the pouring port are completely abutted, thereby achieving blocking between the resin recovery barrel and the resin barrel, preventing the methanol in the resin recovery barrel from volatilizing into the resin barrel and affecting the detection of the methanol detector.

[0022] Optionally, the connecting assembly includes a mounting seat, a bellows, a clamping joint, a telescopic piece and a ball head tube, the mounting seat is arranged on the waste liquid inlet, the clamping joint is arranged on the side of the mounting seat away from the waste liquid inlet and is connected through the telescopic piece, the bellows is arranged between the mounting seat and the clamping joint, and the ball head tube is arranged at the end of the inlet pipe away from the resin column.

[0023] By adopting the above technical solution, when the rotating rod drives the resin column to rotate, the ball head tube on the liquid inlet pipe will abut against the card joint, and the telescopic part and the bellows will shrink during the abutment process. When the ball head tube enters the card joint, the telescopic part will drive the bellows to extend synchronously until the card joint is fully abutted, and the telescopic part will continue to provide a mortgage force when the card joint and the ball head tube abut, so as to maintain the connection effect between the card joint and the ball head tube.

[0024] The present application also includes a method for preparing benzofurazan oxide: using o-nitroaniline and sodium hypochlorite as raw materials, first weighing 540 kg of o-nitroaniline, putting it into a 3000 L enamel kettle, adding 180 kg of 33% liquid alkali solution and 3000 kg of 10.5% sodium hypochlorite solution, and starting stirring, while calculating the starting time, controlling the temperature within 52°C within 3 hours, raising the temperature to 68-70°C after 3 hours, keeping the temperature for 1 hour, and using cooling water to cool the jacket, when it drops below 35°C, crystallizes, discharges the material for centrifugal separation, and finally weighs and puts into storage.

[0025] In summary, the present application includes at least one of the following beneficial technical effects: 1. The first driving motor and the rotating rod are used to switch the multiple resin columns at the first station, the second station, the third station and the fourth station respectively, so that the adsorption of organic matter in the waste liquid, the elution of the resin column, the separation of the residual methanol and the detection and replacement of the resin are realized at the same time, which shortens the overall time required for the resin desorption column to adsorb organic matter, the methanol to wash the resin desorption column and the detection and replacement of the resin desorption column. Compared with the prior art of replacing the resin column as a whole, the present application also saves the time consumed by replacing the resin column and the cost required for replacing the resin column, and the removal and detection of the residual methanol can better ensure the use effect of the resin column; 2. Start the second drive motor, and the driving gear on the output shaft of the second drive motor drives the driven gear to rotate. Since the driven gear is installed on the side of the first rotating barrel close to the second drive motor, the second drive motor can drive the first rotating barrel to rotate. While the first rotating barrel is rotating, it can drive the second rotating barrel to rotate synchronously under the action of the limiting structure. When the first rotating body and the second rotating barrel rotate synchronously, the centrifugal holes opened on the first rotating barrel and the second rotating barrel are aligned. At this time, the methanol solution remaining in the resin is thrown from the centrifugal hole to the gap between the first rotating barrel and the shell under the action of centrifugation, and is output from the liquid outlet on the shell to the centrifugal liquid outlet, so as to reduce the residual methanol content in the resin column. When the second drive motor is turned off and the first rotating barrel and the second rotating barrel stop rotating, under the action of the limiting structure, the first rotating barrel and the second rotating barrel rotate relatively. At this time, the centrifugal holes on the first rotating barrel and the second rotating barrel are staggered to restore the initial state for the subsequent use of the resin column; 3. Since one end of the screw is fixedly mounted on the outer shell and the other end is connected to the inner bottom plate of the first rotating barrel, the screw does not rotate when the first rotating barrel rotates. Since the vertical limit block on the lifting plate is slidably mounted in the vertical groove, and the lifting plate is threadedly connected to the screw, when the first rotating barrel drives the second rotating body to rotate synchronously, the second rotating barrel can drive the lifting plate to rotate synchronously, thereby realizing the lifting and lowering of the lifting plate on the screw. When the height of the lifting plate changes, the resin column in the second rotating barrel can be squeezed, thereby further reducing the methanol residue in the resin column and improving the centrifugal effect on the residual methanol in the resin; 4. After the detection component detects the methanol content in the resin column, if the detection is qualified, the first drive motor will transport the resin column to the first station to adsorb organic matter in the waste liquid. When the detection result of the detection component on the methanol content in the resin column is too high, the electric telescopic rod is started, and the first telescopic end of the electric telescopic rod is extended to abut against the side of the pouring plate close to the fixed plate. Since the pouring plate is circumferentially clamped and axially socket-connected with the inner bottom wall of the first rotating barrel through the clamping block, the extension of the first telescopic end can lift up the pouring plate to separate it from the inner bottom wall of the first rotating barrel. The resin in the barrel falls into the pouring port from the gap between the pouring plate and the first rotating barrel, thereby realizing the pouring of the resin in the resin column. When the pouring plate is lifted up by the first telescopic end of the electric telescopic rod, the socket barrel improves the stability of the screw rod, thereby preventing the screw rod from being eccentric after long-term use. When the pouring is completed, the electric telescopic rod can be closed, and new resin can be added from the resin adding port on the air inlet. Compared with the prior art of replacing the entire resin column, the present application saves the time consumed in replacing the resin column, the delayed construction period and the cost required for replacing the resin column. 5. Since the reset block and the dumping plate are clamped and the reset block is installed on the column, when the first telescopic end of the electric telescopic rod drives the dumping plate to rise, the column and the reset column are driven to rise synchronously, and the spring is compressed between the limit plate and the mounting groove until the limit plate abuts against the inner wall of the mounting groove. At this time, the dumping plate and the inner bottom wall of the first rotating barrel are completely separated, and the resin in the second rotating barrel is dumped through the gap between the first rotating barrel and the dumping plate. When the first telescopic end is shortened, the spring extends between the limit plate and the mounting groove until the inner bottom wall of the first rotating barrel is completely abutted against the dumping plate. The spring can make the dumping plate and the end of the first telescopic end fit more closely during the rising and falling process of the dumping plate, so that the lifting and lowering of the dumping plate is more stable, and the abutment and sealing effect between the inner bottom wall of the first rotating barrel and the dumping plate can be improved; 6. While the first telescopic end of the electric telescopic rod is extended, the second telescopic end is extended synchronously, and the second telescopic end is extended while driving the sealing plate to descend, so that the resin in the pouring port is poured into the resin recovery barrel from the gap between the sealing plate and the pouring port. When the pouring is completed, the second telescopic end is shortened until the sealing plate and the pouring port are completely abutted, thereby blocking the resin recovery barrel and the resin barrel, preventing the methanol in the resin recovery barrel from volatilizing into the resin barrel and affecting the detection of the methanol detector. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0027] Figure 1 It is a schematic diagram of the overall structure of an embodiment of the present application; Figure 2 yes Figure 1 A partial structural diagram of Figure 3 yes Figure 2 A schematic cross-sectional view of a partial structure of Figure 4 yes Figure 2 Schematic diagram of the cross-section structure of some structures; Figure 5 yes Figure 3 An enlarged schematic diagram of the structure of part A; Figure 6 It is a structural schematic diagram of the limiting structure; Figure 7 yes Figure 3 An enlarged schematic diagram of the structure of part B; Figure 8 yes Figure 4An enlarged schematic diagram of the structure of part C; Fig. 9 yes Figure 4 An enlarged schematic diagram of the structure of part D.

[0028] Figure numerals: 1, resin barrel; 11, waste liquid inlet; 12, methanol inlet; 13, waste liquid outlet; 14, methanol outlet; 15, resin column; 151, liquid inlet pipe; 152, liquid outlet pipe; 153, shell; 16, rotating rod; 17, first drive motor; 18, fixed plate; 1a, first station; 1b, second station; 1c, third station; 1d, fourth station; 2, waste liquid recovery barrel; 3, methanol recovery barrel; 4, centrifugal mechanism; 41, second drive motor; 42, driving gear; 43, driven gear; 44, first rotating barrel; 45, second rotating barrel; 46, limiting structure; 461, rotation limiting block; 462, first reset member; 4 63. arc groove; 47. extrusion assembly; 471. lifting plate; 472. screw rod; 473. vertical limit block; 474. vertical groove; 5. dumping mechanism; 51. dumping mouth; 511. sealing plate; 52. dumping plate; 521. socket barrel; 53. clamping block; 54. electric telescopic rod; 541. first telescopic end; 542. second telescopic end; 55. detection assembly; 551. air pump; 552. methanol detector; 6. connection assembly; 61. mounting seat; 62. bellows; 63. clamping joint; 64. telescopic member; 65. ball head tube; 7. second reset member; 71. spring; 72. column; 73. reset block; 74. limit plate; 8. resin recovery barrel. DETAILED DESCRIPTION

[0029] The following is combined with Figure 1-9 This application is described in further detail.

[0030] The present application discloses a benzofuroxan oxide and a preparation system and method thereof, referring to Figure 1 , Figure 2 , Figure 3 and Figure 4A preparation system of benzofuroxan oxide comprises a mounting frame, a resin barrel 1, a waste liquid recovery barrel 2 and a methanol recovery barrel 3, wherein the resin barrel 1, the waste liquid recovery barrel 2 and the methanol recovery barrel 3 are all fixed on the mounting frame, a waste liquid inlet 11, a methanol inlet 12, a waste liquid outlet 13 and a methanol outlet 14 are welded and installed on the resin barrel 1, a resin column 15 is vertically installed in the resin barrel 1, a liquid inlet pipe 151 and a liquid outlet pipe 152 are welded and installed on the resin column 15, and the liquid inlet pipe 151 is welded and installed above the liquid outlet pipe 152, a rotating rod 16 is rotatably installed in the resin barrel 1, a first driving motor 17 is fixedly installed on the resin barrel 1, the rotating rod 16 penetrates the top wall of the resin barrel 1 and is connected to the output shaft of the first driving motor 17, a connecting rod is welded and installed on the rotating rod 16, and an end of the connecting rod away from the rotating rod 16 is welded and connected to the top of the resin column 15, and the rotating rod 16 drives the resin column 15 to rotate around the rotating rod 16 through the connecting rod.

[0031] A first station 1a is provided in the resin barrel 1. When the resin column 15 is located at the first station 1a, the liquid inlet pipe 151 is connected to the waste liquid inlet 11, and the liquid outlet pipe 152 is connected to the waste liquid outlet 13; a second station 1b is provided in the resin barrel 1. When the resin column 15 is located at the second station 1b, the liquid inlet pipe 151 is connected to the methanol inlet 12, and the liquid outlet pipe 152 is connected to the methanol outlet 14; a third station 1c is provided in the resin barrel 1. A centrifugal liquid outlet is welded and installed on the resin barrel 1. When the resin column 15 is located at the third station 1c, the liquid outlet pipe 152 is connected to the centrifugal liquid outlet. A centrifugal mechanism 4 is provided on the third station 1c and the resin column 15, and the centrifugal liquid outlet is connected to the methanol outlet 14; a fourth station 1d is provided in the resin barrel 1. A dumping mechanism 5 is provided on the fourth station 1d and the resin column 15.

[0032] There are multiple resin columns 15, and the rotating rod 16 drives the positions of the multiple resin columns 15 to switch respectively at the first station 1a, the second station 1b, the third station 1c and the fourth station 1d; a connecting component 6 is provided on the liquid inlet pipe 151 and the waste liquid inlet 11, the liquid outlet pipe 152 is arranged at the same time as the liquid inlet pipe 151, and the waste liquid outlet 13, the methanol inlet 12, the methanol outlet 14 and the centrifugal liquid outlet are all arranged at the same time as the waste liquid inlet 11.

[0033] In this embodiment, the waste liquid is input into the resin barrel 1 from the waste liquid inlet 11, and then input into the resin column 15 from the inlet pipe 151 on the resin column 15 connected to the waste liquid inlet 11 at the first station 1a. After the resin in the resin column 15 adsorbs the organic matter in the waste liquid, the waste liquid is output from the outlet pipe 152 and the waste liquid outlet 13. When the resin column 15 adsorbs enough organic matter, the first drive motor 17 is started, and the first drive motor 17 drives the resin column 15 to rotate around the rotating rod 16 to the second station 1b. Methanol is resinated into the resin barrel 1 from the methanol inlet 12, and then the inlet pipe 151 connected to the methanol inlet 12 at the second station 1b is output. 151 is input into the resin column 15, so as to elute the organic matter adsorbed in the resin column 15. After the organic matter in the resin column 15 is eluted, more methanol will remain in the resin column 15, thereby affecting the adsorption effect of the resin column 15 on the organic matter. The first drive motor 17 is started to rotate the resin column 15 to the third station 1c. The centrifugal mechanism 4 on the third station 1c can rotate and centrifuge the resin column 15, so as to centrifuge and remove the methanol in the resin column 15, and then output it from the liquid outlet 152 and the centrifuge outlet. When more methanol still remains after the resin column 15 is centrifuged, more organic matter will be dissolved in the methanol at the same time, then This indicates that the resin column 15 needs to be replaced. At this time, the first drive motor 17 is driven again to rotate the resin column 15 to the fourth station 1d. The dumping mechanism 5 at the fourth station 1d can detect the methanol residue in the resin column 15. When the detection is qualified, the first drive motor 17 will rotate the resin column 15 to the first station 1a for continued use. When the detection is unqualified, the dumping mechanism 5 at the fourth station 1d will dump the resin in the resin column 15 and add new resin, thereby ensuring the adsorption effect of the resin column 15 on organic matter in the waste liquid. The first drive motor 17 and the rotating rod 16 are used to rotate multiple resin columns 15 at the first station 1a and the second station 1d respectively. 1b, the third station 1c and the fourth station 1d are switched to realize the adsorption of organic matter in the waste liquid, the elution of the resin column 15, the separation of the residual methanol and the detection of the resin, and the replacement is carried out at the same time after the detection. Compared with the prior art that replaces the resin column 15 as a whole, this embodiment saves the time consumed in replacing the resin column 15 and the cost required for replacing the resin column 15, and the separation of the residual methanol can better ensure the use effect of the resin column 15, and the connecting component 6 can realize the stability of the connection when the liquid inlet pipe 151 and the liquid outlet pipe 152 are connected to each connecting port after rotating around the rotating rod 16.

[0034] After the resin in the resin column 15 is washed with methanol, the methanol remaining in the resin and the organic matter dissolved in the methanol will reduce the adsorption effect of the resin column 15 on the organic matter in the waste liquid. Figure 3 and Figure 5Therefore, the centrifugal mechanism 4 in this embodiment includes a second drive motor 41, a driving gear 42, a driven gear 43, a first rotating barrel 44, a second rotating barrel 45, a limiting structure 46 and an extrusion assembly 47. A fixing plate 18 is welded and installed in the resin barrel 1, and the fixing plate 18 is welded and installed below the resin column 15. The second drive motor 41 is fixedly installed on a side of the fixing plate 18 away from the resin column 15, and the driving gear 42 is installed on a side of the fixing plate 18 close to the resin column 15, and is welded to the output shaft of the second drive motor 41. The resin column 15 includes a housing 153, a first rotating barrel 44 is rotatably mounted in the housing 153, a second rotating barrel 45 is rotatably mounted in the first rotating barrel 44, resin is placed in the second rotating barrel 45, a driven gear 43 is welded and mounted on a surface of the first rotating barrel 44 close to the second driving motor 41, and meshes with the driving gear 42 when abutting against the driving gear 42, a movable annular groove is provided on the fixed plate 18 for the driven gear 43 to rotate around the rotating rod 16, and centrifugal holes are provided on the first rotating barrel 44 and the second rotating barrel 45.

[0035] The second driving motor 41 is started, and the driving gear 42 on the output shaft of the second driving motor 41 drives the driven gear 43 to rotate. Since the driven gear 43 is installed on the side of the first rotating barrel 44 close to the second driving motor 41, the second driving motor 41 can drive the first rotating barrel 44 to rotate. While the first rotating barrel 44 is rotating, the second rotating barrel 45 can be driven to rotate synchronously under the action of the limiting structure 46. When the first rotating body and the second rotating barrel 45 rotate synchronously, the centrifugal holes opened on the first rotating barrel 44 and the second rotating barrel 45 are aligned. At this time, the methanol solution remaining in the resin is thrown from the centrifugal hole to the gap between the first rotating barrel 44 and the outer shell 153 under the action of centrifugation, and is output from the liquid outlet on the outer shell 153 to The centrifugal liquid outlet is connected to the methanol outlet 14, so the residual methanol liquid separated by centrifugation will also be collected into the methanol recovery barrel 3, so as to reduce the residual methanol content in the resin column 15. When the second driving motor 41 is turned off and the first rotating barrel 44 and the second rotating barrel 45 stop rotating, under the action of the limiting structure 46, the first rotating barrel 44 and the second rotating barrel 45 rotate relative to each other. At this time, the centrifugal holes on the first rotating barrel 44 and the second rotating barrel 45 are staggered to restore the initial state, so as to facilitate the subsequent use of the resin column 15. The extrusion assembly 47 in this embodiment can realize the extrusion of the resin in the resin column 15, so as to further reduce the residual methanol in the resin column 15 and improve the centrifugal effect on the residual methanol in the resin.

[0036] In order to achieve the alignment and staggering of the centrifugal holes on the first rotating barrel 44 and the second rotating barrel 45, refer to Figure 6 and Figure 7In this embodiment, the fixed limiting structure 46 includes a rotation limiting block 461 and a first reset member 462. The rotation limiting block 461 is integrally arranged on the inner top wall of the first rotating barrel 44. An arc groove 463 is provided on the outer top wall of the second rotating barrel 45 corresponding to the limiting block. The first reset member 462 is installed between the inner top wall of the first rotating barrel 44 and the outer top wall of the second rotating barrel 45. In this embodiment, the first reset member 462 is a torsion spring, which is a preferred embodiment. In other embodiments, the first reset member 462 can be an elastic rubber block installed between the first rotating barrel 44 and the second rotating barrel 45.

[0037] In the initial state, the rotation limit block 461 is located in the middle position of the arc groove 463. At this time, the centrifugal holes on the first rotating barrel 44 and the second rotating barrel 45 are staggered with each other. When the second driving motor 41 is started, the second driving motor 41 drives the first rotating barrel 44 to rotate. After the first rotating barrel 44 and the second rotating barrel 45 rotate relative to each other, the rotation limit block 461 rotates to one end of the arc groove 463 and abuts against the inner wall of the arc groove 463, so that the first rotating barrel 44 drives the second rotating barrel 45 to rotate synchronously. At this time, the centrifugal holes on the first rotating barrel 44 and the second rotating barrel 45 are aligned with each other. When the second driving motor 41 rotates in the opposite direction, the rotation limit block 461 will move to the other end of the arc groove 463. At this time, the separation holes on the first rotating barrel 44 and the second rotating barrel 45 are also aligned, so that no matter whether the second driving motor 41 is rotating forward or reverse, the residual methanol in the resin column 15 can be shaken off, thereby improving the adsorption effect of the resin column 15 on organic matter in the waste liquid.

[0038] When the resin in the resin column 15 is sticky, the effect of removing the methanol in the resin by centrifugation may be poor. Figure 3 and Figure 7 Therefore, the extrusion assembly 47 in this embodiment includes a lifting plate 471, a screw rod 472 and a vertical limit block 473. The lifting plate 471 is lifted and installed in the second rotating barrel 45. The vertical limit block 473 is integrally arranged on the lifting plate 471. A vertical groove 474 is provided on the inner wall of the second rotating barrel 45 corresponding to the vertical limit block 473. The screw rod 472 is installed in the second rotating barrel 45. One end of the screw rod 472 is rotatably connected to the inner bottom wall of the first rotating barrel 44. The other end of the screw rod 472 passes through the first rotating barrel 44 and the second rotating barrel 45 and is welded and fixedly connected to the inner top wall of the shell 153. The lifting plate 471 is installed on the screw rod 472 and is threadedly connected to the screw rod 472.

[0039] Since one end of the screw rod 472 is fixedly mounted on the outer shell 153 and the other end is connected to the inner bottom plate of the first rotating barrel 44, the screw rod 472 does not rotate when the first rotating barrel 44 rotates. Since the vertical limit block 473 on the lifting plate 471 is slidably mounted in the vertical groove 474, and the lifting plate 471 is threadedly connected to the screw rod 472, when the first rotating barrel 44 drives the second rotating body to rotate synchronously, the second rotating barrel 45 can drive the lifting plate 471 to rotate synchronously, thereby realizing the lifting and lowering of the lifting plate 471 on the screw rod 472. When the height of the lifting plate 471 changes, the resin column 15 in the second rotating barrel 45 can be squeezed, thereby further reducing the methanol residue in the resin column 15 and improving the centrifugal effect on the residual methanol in the resin.

[0040] After the resin is centrifugally squeezed and shaken off, if there is still a lot of methanol left in the resin, there will also be organic matter dissolved in the methanol. Figure 4 and Figure 8 , thus reducing the adsorption effect of organic matter in the waste liquid, the dumping mechanism 5 in this embodiment includes a dumping port 51, a dumping pan 52, a clamping block 53, an electric telescopic rod 54 and a detection assembly 55, the dumping port 51 is welded and installed on the side of the fixed plate 18 away from the resin column 15, and the fixed plate 18 is provided with a discharge port at a position corresponding to the dumping port 51, the clamping block 53 is integrally arranged on the dumping pan 52, and a clamping groove is provided on the inner bottom wall of the first rotating barrel 44 corresponding to the clamping block 53, and the dumping pan 52 is clamped on the inner bottom wall of the first rotating barrel 44 through the clamping block 53 and the clamping groove. A socket barrel 521 is welded on the side of the plate 52 away from the fixed plate 18, the end of the screw rod 472 close to the fixed plate 18 rotates and is socket-installed in the socket barrel 521, the depth of the socket barrel 521 is greater than the height of the screw rod 472 in the socket barrel 521, the driven gear 43 is fixedly welded and installed on the side of the dumping plate 52 close to the fixed plate 18, the electric telescopic rod 54 is installed in the dumping mouth 51, the electric telescopic rod 54 includes a first telescopic end 541 and a second telescopic end 542, and the first telescopic end 541 of the electric telescopic rod 54 can be extended to abut against the side of the dumping plate 52 close to the fixed plate 18.

[0041] After the detection component 55 detects the methanol content in the resin column 15, if the detection is qualified, the first drive motor 17 will transport the resin column 15 to the first station 1a for adsorption of organic matter in the waste liquid. When the detection result of the detection component 55 on the methanol content in the resin column 15 is too high, the electric telescopic rod 54 is started, and the first telescopic end 541 of the electric telescopic rod 54 is extended to abut against the side of the pouring plate 52 close to the fixed plate 18. Since the pouring plate 52 is circumferentially clamped and axially socket-connected with the inner bottom wall of the first rotating barrel 44 through the clamping block 53, the first telescopic end 541 is extended to lift the pouring plate 52. The resin in the second rotating barrel 45 is separated from the inner bottom wall of the first rotating barrel 44, and falls into the pouring port 51 from the gap between the pouring plate 52 and the first rotating barrel 44, so that the resin in the resin column 15 is poured out. When the pouring plate 52 is lifted up by the first telescopic end 541 of the electric telescopic rod 54, since the depth of the socket barrel 521 is greater than the height of the screw rod 472 in the socket barrel 521, interference between the screw rod 472 and the pouring plate 52 can be avoided. At the same time, the socket barrel 521 improves the stability of the screw rod 472, thereby avoiding eccentricity of the screw rod 472 after long-term use.

[0042] In order to detect the content of residual methanol in the resin column 15, refer to Fig. 9 The detection component 55 in this embodiment includes an air pump 551 and a methanol detector 552. An air inlet and an air outlet are welded and installed on the resin barrel 1. The air inlet and the air outlet are both arranged at the same time as the waste liquid inlet 11. The air pump 551 is installed on the air inlet, and the methanol detector 552 is installed on the air outlet. When the resin column 15 is located at the fourth station 1d, the air inlet is connected to the liquid outlet pipe 152, and the air outlet is connected to the liquid inlet pipe 151. A resin adding port is arranged on the air inlet, and an end cover is installed on the resin adding port in a socket manner. The methanol detector 552 is electrically connected to the air pump 551 and the electric telescopic rod 54.

[0043] When the resin column 15 is located at the fourth station 1d, the air pump 551 is started, and the air pump 551 conveys air into the resin column 15. When the methanol detector 552 located on the air outlet detects that the methanol content in the output gas exceeds the standard, it means that the methanol residue in the resin exceeds the standard and may not be suitable for continuing to adsorb organic matter in the waste liquid. At this time, the methanol detector 552 will send an electrical signal to the electric telescopic rod 54 and the air pump 551, and turn off the air pump 551 and turn on the electric telescopic rod 54 at the same time to realize the dumping of the resin. When the dumping is completed, the electric telescopic rod 54 can be closed, and new resin can be added from the resin adding port on the air inlet. Compared with the prior art of replacing the resin column 15 as a whole, this embodiment saves the time consumed in replacing the resin column 15, the delayed construction period and the cost required for replacing the resin column 15.

[0044] The lifting and lowering of the pouring tray 52 is relatively unstable only by the contact between the first telescopic end 541 and the pouring tray 52. Figure 4 and Figure 8 Therefore, in this embodiment, a second reset member 7 is installed between the dumping tray 52 and the first rotating barrel 44. The second reset member 7 includes a spring 71, a column 72 and a reset block 73. The column 72 is movably installed on the inner bottom wall of the shell 153. The reset block 73 is welded and installed at the end of the column 72 away from the fixed plate 18 and is clamped with the dumping tray 52. ​​The dumping tray 52 is provided with an annular groove for the reset block 73 to move. The bottom wall of the shell 153 is provided with a mounting groove. The end of the column 72 away from the dumping tray 52 is located in the mounting groove. The end of the column 72 away from the dumping tray 52 is welded and installed with a limiting plate 74. The spring 71 is sleeved on the column 72 and is located between the limiting plate 74 and the top wall of the mounting groove. In this embodiment, the reset block 73 is a "T"-shaped block, and the cross-section of the annular groove corresponds to the reset block 73 is also "T"-shaped. The "T"-shaped reset block 73 is a preferred embodiment of this embodiment. In other embodiments, the reset block 73 can be a spherical block, etc.

[0045] The cam 72 is pressed against the bottom wall of the first rotating barrel 44 and the first rotating barrel 44 is pressed against the bottom wall of the first rotating barrel 44. The resin in the rotating barrel 45 is poured out. When the first telescopic end 541 is shortened, the spring 71 extends between the limit plate 74 and the mounting groove until the inner bottom wall of the first rotating barrel 44 is completely in contact with the pouring plate 52. The spring 71 can make the pouring plate 52 fit more closely with the end of the first telescopic end 541 during the rising and falling process of the pouring plate 52, so that the rising and falling of the pouring plate 52 is more stable, and the abutment sealing effect between the inner bottom wall of the first rotating barrel 44 and the pouring plate 52 can be improved.

[0046] Reference Figure 1 and Figure 8In this embodiment, a blocking plate 511 is installed at the bottom of the pouring port 51. The second telescopic end 542 of the electric telescopic rod 54 is fixedly connected to the blocking plate 511. When the second telescopic end 542 is shortened, the blocking plate 511 and the bottom of the pouring port 51 are clamped to close the bottom of the pouring port 51. A material discharge channel is welded and installed in the pouring port 51. The two ends of the material discharge channel are funnel-shaped and expand outward. The side of the blocking plate 511 close to the fixed plate 18 is set as a convex curved surface. A resin recovery barrel 8 is installed below the pouring port 51; the first telescopic end 541 of the electric telescopic rod 54 is extended As the second telescopic end 542 grows, it simultaneously extends. When the second telescopic end 542 extends, it drives the sealing plate 511 to descend, thereby realizing that the resin in the pouring port 51 is poured into the resin recovery barrel 8 from the gap between the sealing plate 511 and the pouring port 51. When the pouring is completed, the second telescopic end 542 shortens until the sealing plate 511 and the pouring port 51 are completely abutted, thereby realizing the blockage between the resin recovery barrel 8 and the resin barrel 1, and preventing the methanol in the resin recovery barrel 8 from volatilizing into the resin barrel 1 and affecting the detection of the methanol detector 552.

[0047] Reference Fig. 9 In this embodiment, the connecting assembly 6 includes a mounting seat 61, a bellows 62, a clamping joint 63, a telescopic member 64 and a ball head tube 65. The mounting seat 61 is welded and mounted on the waste liquid inlet 11. The clamping joint 63 is movably mounted on the side of the mounting seat 61 away from the waste liquid inlet 11 and connected by the telescopic member 64. The bellows 62 is mounted between the mounting seat 61 and the clamping joint 63. The ball head tube 65 is welded and mounted on the end of the liquid inlet pipe 151 away from the resin column 15. When the rotating rod 16 drives When the resin column 15 rotates, the ball head tube 65 on the liquid inlet pipe 151 will abut against the card joint 63. During the abutment process, the telescopic part 64 and the bellows 62 will shrink. When the ball head tube 65 enters the card joint 63, the telescopic part 64 will drive the bellows 62 to extend synchronously until the card joint 63 is fully abutted. The telescopic part 64 will continue to provide a mortgage force when the card joint 63 and the ball head tube 65 abut, so as to maintain the connection effect between the card joint 63 and the ball head tube 65.

[0048] The implementation principle of a preparation system of benzofuroxan oxide in the present application example is: The waste liquid is input into the resin barrel 1 from the waste liquid inlet 11, and then input into the resin column 15 from the inlet pipe 151 on the resin column 15 connected to the waste liquid inlet 11 at the first station 1a. After the resin in the resin column 15 adsorbs the organic matter in the waste liquid, the waste liquid is output from the outlet pipe 152 and the waste liquid outlet 13. When the resin column 15 adsorbs enough organic matter, the first drive motor 17 is started, and the first drive motor 17 drives the resin column 15 to rotate around the rotating rod 16 to the second station 1b. Methanol is injected into the resin barrel 1 from the methanol inlet 12, and then input into the resin column 15 from the inlet pipe 151 connected to the methanol inlet 12 at the second station 1b, thereby eluting the organic matter adsorbed in the resin column 15. When a large amount of methanol remains in the resin column 15, the second drive motor 41 is started, and the driving gear 42 on the output shaft of the second drive motor 41 drives the driven gear 43 to rotate. Since the driven gear 43 is installed on the side of the first rotating barrel 44 close to the second drive motor 41, the second drive motor 41 can drive the first rotating barrel 44 to rotate. While the first rotating barrel 44 is rotating, the second rotating barrel 45 can be driven to rotate synchronously under the action of the limiting structure 46. When the first rotating body and the second rotating barrel 45 rotate synchronously, the centrifugal holes opened on the first rotating barrel 44 and the second rotating barrel 45 are aligned. At this time, the methanol solution remaining in the resin is thrown from the centrifugal hole to the gap between the first rotating barrel 44 and the outer shell 153 under the action of centrifugation, and is output from the liquid outlet on the outer shell 153 to the centrifugal liquid outlet; When it is necessary to further improve the centrifugal separation effect of the resin, since one end of the screw rod 472 is fixedly installed on the outer shell 153 and the other end is connected to the inner bottom plate of the first rotating barrel 44, the screw rod 472 does not rotate when the first rotating barrel 44 rotates. Since the vertical limit block 473 on the lifting plate 471 is slidably installed in the vertical groove 474, and the lifting plate 471 is threadedly connected to the screw rod 472, when the first rotating barrel 44 drives the second rotating body to rotate synchronously, the second rotating barrel 45 can drive the lifting plate 471 to rotate synchronously, thereby realizing the lifting and lowering of the lifting plate 471 on the screw rod 472. When the height of the lifting plate 471 changes, the resin column 15 in the second rotating barrel 45 can be squeezed, thereby further reducing the methanol residue in the resin column 15 and improving the centrifugal effect on the residual methanol in the resin; When it is necessary to detect the methanol content remaining in the centrifuged resin to determine whether it needs to be replaced, the detection component 55 detects the methanol content in the resin column 15. If the detection is qualified, the first drive motor 17 will transport the resin column 15 to the first station 1a for adsorption of organic matter in the waste liquid. When the detection result of the detection component 55 on the methanol content in the resin column 15 is too high, the electric telescopic rod 54 is started, and the first telescopic end 541 of the electric telescopic rod 54 is extended to abut against the side of the dumping plate 52 close to the fixed plate 18, and the resin column 15 is transported to the first station 1a by the first drive motor 17. The pouring pan 52 is circumferentially clamped and axially socket-connected to the inner bottom wall of the first rotating barrel 44 through the clamping block 53, so the first telescopic end 541 is extended to lift the pouring pan 52 to achieve separation from the inner bottom wall of the first rotating barrel 44, and the resin in the second rotating barrel 45 falls into the pouring port 51 from the gap between the pouring pan 52 and the first rotating barrel 44, so as to realize pouring of the resin in the resin column 15. When the pouring is completed, the electric telescopic rod 54 can be closed, and new resin can be added from the resin adding port on the air inlet.

[0049] The present application also discloses a method for preparing benzofurazan oxide: using o-nitroaniline and sodium hypochlorite as raw materials, first weighing 540 kg of o-nitroaniline, putting it into a 3000 L enamel kettle, adding 180 kg of 33% liquid alkali solution and 3000 kg of 10.5% sodium hypochlorite solution, and starting stirring, while calculating the starting time, controlling the temperature within 52°C within 3 hours, raising the temperature to 68-70°C after 3 hours, keeping the temperature for 1 hour, and using cooling water to cool the jacket, when it drops below 35°C, crystallize and discharge the material for centrifugal separation to obtain benzofurazan oxide, and finally weighing and storing.

[0050] Unless otherwise defined, the technical terms or scientific terms used in this application should be understood by people with ordinary skills in the field to which this application belongs. The words "first", "second", "third" and similar words used in the specification and claims of this application do not indicate any order, quantity or importance, but are only used to distinguish different components. "One" or "one" and similar words do not indicate a quantitative limit, but indicate the existence of at least one. "Include" or "comprise" and similar words mean that the elements or objects appearing before "include" or "comprise" include the elements or objects listed after "include" or "comprise" and their equivalents, and do not exclude other elements or objects. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0051] The above are all optional embodiments of the present application, and are not intended to limit the protection scope of the present application. Therefore, any equivalent changes made based on the structure, shape, and principle of the present application should be included in the protection scope of the present application.

Claims

1. A system for preparing benzofuroxan, comprising a mounting frame, a resin barrel (1), a waste liquid recovery barrel (2) and a methanol recovery barrel (3), characterized in that: The resin barrel (1), the waste liquid recovery barrel (2) and the methanol recovery barrel (3) are all arranged on the mounting frame; the resin barrel (1) is provided with a waste liquid inlet (11), a methanol inlet (12), a waste liquid outlet (13) and a methanol outlet (14); a resin column (15) is vertically arranged in the resin barrel (1); the resin column (15) is provided with a liquid inlet pipe (151) and a liquid outlet pipe (152); the liquid inlet pipe (151) is arranged above the liquid outlet pipe (152); A rotating rod (16) is arranged in the resin barrel (1), a first driving motor (17) is arranged on the resin barrel (1), the rotating rod (16) passes through the top wall of the resin barrel (1) and is connected to the output shaft of the first driving motor (17), a connecting rod is arranged on the rotating rod (16), one end of the connecting rod away from the rotating rod (16) is connected to the top of the resin column (15), and the rotating rod (16) drives the resin column (15) to rotate around the rotating rod (16) through the connecting rod; A first workstation (1a) is provided in the resin barrel (1); when the resin column (15) is located at the first workstation (1a), the liquid inlet pipe (151) is connected to the waste liquid inlet port (11), and the liquid outlet pipe (152) is connected to the waste liquid outlet port (13), so as to use the resin column (15) to adsorb organic matter in the waste liquid; A second workstation (1b) is provided in the resin barrel (1). When the resin column (15) is located at the second workstation (1b), the liquid inlet pipe (151) is connected to the methanol liquid inlet (12), and the liquid outlet pipe (152) is connected to the methanol liquid outlet (14), so as to use methanol to elute the adsorbed organic matter in the resin column (15); A third station (1c) is provided in the resin barrel (1), and a centrifugal liquid outlet is provided on the resin barrel (1); when the resin column (15) is located at the third station (1c), the liquid outlet pipe (152) is connected to the centrifugal liquid outlet; a centrifugal mechanism (4) for centrifugally removing the methanol remaining in the resin column (15) is provided on the third station (1c) and the resin column (15); and the centrifugal liquid outlet is connected to the methanol liquid outlet (14); A fourth workstation (1d) is provided in the resin barrel (1), and a dumping mechanism (5) for detecting the methanol content in the resin column (15) and dumping and replacing the resin in the resin column (15) is provided on the fourth workstation (1d) and the resin column (15); A plurality of the resin columns (15) are provided, and the rotating rod (16) drives the positions of the plurality of resin columns (15) to be switched respectively at the first station (1a), the second station (1b), the third station (1c) and the fourth station (1d); A connecting assembly (6) is provided on the liquid inlet pipe (151) and the waste liquid inlet port (11). The connecting assembly (6) is used to connect to the waste liquid inlet port (11) after the liquid inlet pipe (151) rotates around the rotating rod (16). The liquid outlet pipe (152) is provided on the same side as the liquid inlet pipe (151). The waste liquid outlet port (13), the methanol inlet port (12), the methanol outlet port (14) and the centrifugal liquid outlet are all provided on the same side as the waste liquid inlet port (11).

2. A system for preparing benzofuroxan according to claim 1, characterized in that: The centrifugal mechanism (4) comprises a second drive motor (41), a driving gear (42), a driven gear (43), a first rotating barrel (44), a second rotating barrel (45), a limiting structure (46) and an extrusion assembly (47). A fixing plate (18) is arranged in the resin barrel (1), and the fixing plate (18) is arranged below the resin column (15). The second drive motor (41) is arranged on a side of the fixing plate (18) away from the resin column (15). The driving gear (42) is arranged on a side of the fixing plate (18) close to the resin column (15) and connected to an output shaft of the second drive motor (41). The resin column (15) comprises a housing (153). The first rotating barrel (44) is rotatably arranged in the housing (153). The second rotating barrel (45) is rotatably arranged in the first rotating barrel (44). The resin is arranged in the second rotating barrel (45). The driven gear (43) is arranged on a side of the first rotating barrel (44) close to the second drive motor (41). 1), and meshes with the driving gear (42) when abutting against the driving gear (42); a movable annular groove is provided on the fixed plate (18) for the driven gear (43) to rotate around the rotating rod (16); centrifugal holes are provided on the first rotating barrel (44) and the second rotating barrel (45); the limiting structure (46) is used to drive the second rotating barrel (45) to rotate synchronously after the first rotating barrel (44) and the second rotating barrel (45) rotate relative to each other, so that the centrifugal holes on the first rotating barrel (44) and the second rotating barrel (45) are aligned; and is used to reset the first rotating barrel (44) and the second rotating barrel (45) after the first rotating barrel (44) and the second rotating barrel (45) stop rotating, so that the centrifugal holes on the first rotating barrel (44) and the second rotating barrel (45) are staggered; the extrusion assembly (47) is arranged in the second rotating barrel (45) and is used to extrude the resin.

3. A system for preparing benzofuroxan according to claim 2, characterized in that: The limiting structure (46) comprises a rotation limiting block (461) and a first restoring member (462); the rotation limiting block (461) is arranged on the inner top wall of the first rotating barrel (44); an arc-shaped groove (463) is provided on the outer top wall of the second rotating barrel (45) corresponding to the rotation limiting block (461); when the rotation limiting blocks (461) are located at both ends of the arc-shaped groove (463), the first rotating barrel (44) drives the second rotating barrel (45) to rotate synchronously; the first rotating barrel (44) and the second rotating barrel (45) rotate synchronously. The centrifugal holes on the second rotating barrel (45) are aligned with each other, the first resetting member (462) is arranged between the inner top wall of the first rotating barrel (44) and the outer top wall of the second rotating barrel (45), and the first resetting member (462) is used to reset the first rotating barrel (44) and the second rotating barrel (45) when the first rotating barrel (44) and the second rotating barrel (45) stop rotating, so that the centrifugal holes on the first rotating barrel (44) and the second rotating barrel (45) are staggered.

4. A system for preparing benzofuroxan according to claim 2, characterized in that: The extrusion assembly (47) comprises a lifting plate (471), a screw rod (472) and a vertical stop block (473); the lifting plate (471) is lifted and arranged in the second rotating barrel (45); the vertical stop block (473) is arranged on the lifting plate (471); a vertical groove (474) is provided on the inner wall of the second rotating barrel (45) corresponding to the vertical stop block (473); the screw rod (472) is arranged in the second rotating barrel (45); one end of the screw rod (472) is connected to the first rotating barrel The first rotating barrel (44) is rotatably connected to the inner bottom wall of the housing (153); the other end of the screw rod (472) passes through the first rotating barrel (44) and the second rotating barrel (45) and is fixedly connected to the inner top wall of the housing (153); the lifting plate (471) is arranged on the screw rod (472) and is threadedly connected to the screw rod (472); when the first rotating barrel (44) drives the second rotating barrel (45) to rotate, the lifting plate (471) is lifted and lowered under the action of the vertical limit block (473) and the screw rod (472).

5. A system for preparing benzofuroxan according to claim 4, characterized in that: The pouring mechanism (5) comprises a pouring port (51), a pouring tray (52), a clamping block (53), an electric telescopic rod (54) and a detection assembly (55); the pouring port (51) is arranged on a surface of the fixing plate (18) away from the resin column (15); a discharge port is provided on the fixing plate (18) at a position corresponding to the pouring port (51); the clamping block (53) is arranged on the pouring tray (52); the inner bottom of the first rotating barrel (44) A clamping groove is provided on the wall corresponding to the clamping block (53); the pouring plate (52) is clamped and arranged on the inner bottom wall of the first rotating barrel (44) through the clamping block (53) and the clamping groove; a socket barrel (521) is provided on the side of the pouring plate (52) away from the fixed plate (18); the end of the screw rod (472) close to the fixed plate (18) is rotated and socket-arranged in the socket barrel (521); the depth of the socket barrel (521) is large. At a height at which the screw rod (472) is located in the socket barrel (521), the driven gear (43) is fixedly arranged on a surface of the pouring tray (52) close to the fixed plate (18), and the electric telescopic rod (54) is arranged in the pouring opening (51). The electric telescopic rod (54) comprises a first telescopic end (541) and a second telescopic end (542). The first telescopic end (541) of the electric telescopic rod (54) is extended to abut against a surface of the pouring tray (52) close to the fixed plate (18). The first telescopic end (541) of the electric telescopic rod (54) is extended to separate the pouring tray (52) from the first rotating barrel (44), and the resin in the second rotating barrel (45) falls from the gap between the pouring tray (52) and the first rotating barrel (44) into the pouring opening (51). The detection component (55) is used to detect the amount of residual methanol in the resin column (15).

6. A system for preparing benzofuroxan according to claim 5, characterized in that: The detection component (55) comprises an air pump (551) and a methanol detector (552). The resin barrel (1) is provided with an air inlet and an air outlet. The air inlet and the air outlet are both provided at the same location as the waste liquid inlet (11). The air pump (551) is provided on the air inlet. The methanol detector (552) is provided on the air outlet. When the resin column (15) is located at the fourth station (1d), the air inlet is connected to the liquid outlet pipe (152), and the air outlet is connected to the liquid inlet pipe (151). The air inlet is provided with a resin adding port, and the resin adding port is provided with an end cap. The methanol detector (552) is electrically connected to the air pump (551) and the electric telescopic rod (54).

7. A system for preparing benzofuroxan oxide according to claim 5, characterized in that: A second reset member (7) is provided between the pouring tray (52) and the first rotating barrel (44), the second reset member (7) comprising a spring (71), a column (72) and a reset block (73), the column (72) being provided on the inner bottom wall of the housing (153), the reset block (73) being provided at the end of the column (72) away from the fixing plate (18) and being engaged with the pouring tray (52), the pouring tray (52) being provided with an annular groove for movement of the reset block (73), the bottom wall of the housing (153) being provided with a mounting groove, the end of the column (72) away from the pouring tray (52) being located in the mounting groove, the end of the column (72) away from the pouring tray (52) being provided with a limiting plate (74), the spring (71) being provided on the column (72) and being located between the limiting plate (74) and the top wall of the mounting groove.

8. A system for preparing benzofuroxan oxide according to claim 5, characterized in that: A blocking plate (511) is provided at the bottom of the pouring port (51), and the second telescopic end (542) of the electric telescopic rod (54) is fixedly connected to the blocking plate (511). When the second telescopic end (542) is shortened, the blocking plate (511) and the bottom of the pouring port (51) are clamped together to seal the bottom of the pouring port (51). A material discharge channel for conveniently pouring resin is provided in the pouring port (51), and both ends of the material discharge channel are funnel-shaped and expand outwardly. A side of the blocking plate (511) close to the fixed plate (18) is provided with a convex curved surface, and a resin recovery bucket (8) is provided below the pouring port (51).

9. A system for preparing benzofuroxan according to claim 1, characterized in that: The connecting assembly (6) comprises a mounting seat (61), a bellows (62), a clamping joint (63), a telescopic member (64) and a ball head tube (65); the mounting seat (61) is arranged on the waste liquid inlet (11); the clamping joint (63) is arranged on a side of the mounting seat (61) away from the waste liquid inlet (11) and is connected via the telescopic member (64); the bellows (62) is arranged between the mounting seat (61) and the clamping joint (63); and the ball head tube (65) is arranged at an end of the liquid inlet pipe (151) away from the resin column (15).

10. A method for preparing benzofurazan oxide, according to a system for preparing benzofurazan oxide according to any one of claims 1 to 9, characterized in that: Take o-nitroaniline and sodium hypochlorite as raw materials, first weigh 540kg of o-nitroaniline, put it into a 3000L enamel kettle, add 180kg of 33% liquid alkali solution and 3000kg of 10.5% sodium hypochlorite solution, start stirring, and calculate the starting time at the same time. The temperature is controlled within 52°C within 3h, and then raised to 68-70°C after 3h. After keeping warm for 1h, use cooling water to cool the jacket, and when it drops below 35°C, crystallize and discharge the material for centrifugal separation to obtain benzofuroxan, which is finally weighed and put into storage.

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