A benzofuroxan and its preparation system and preparation method

Abstract

This application relates to the technical field of benzofuroxan preparation, and specifically discloses a benzofuroxan, its preparation system and preparation method, including a resin barrel and a plurality of resin columns. There is a rotating rod on the resin barrel, and a first station, a second station, a third station and a fourth station are also arranged in the resin barrel. When the resin column in this application is located at the first station, the resin column is used to adsorb the organic matter in the waste liquid. When the resin column is located at the second station, methanol is used to elute the adsorbed organic matter in the resin column. When the resin column is located at the third station, the residual methanol in the resin column is centrifugally thrown off. When the resin column is located at the fourth station, the methanol content in the resin column is detected, and the resin in the resin column is poured and replaced. The rotating rod drives the resin column to switch between the first station, the second station, the third station and the fourth station respectively, saving the time consumed for replacing the resin column and the cost required for replacing the resin column.

Description

Technical Field

[0001] The present application relates to the technical field of benzofuroxan preparation, and particularly to a benzofuroxan, its preparation system, and preparation method. Background Art

[0002] Benzofuroxan is an important organic compound, which is widely used in fields such as optical materials, perfumes, and pharmaceutical synthesis. As a light stabilizer, benzofuroxan can absorb ultraviolet light and prevent the aging of plastics and coatings. In addition, it is used as a fragrance ingredient in the perfume industry, imparting specific aromas to products, and also as an intermediate in pharmaceutical synthesis. Its various uses make it play an important role in the chemical industry.

[0003] In the prior art, the preparation system of benzofuroxan includes a synthesis device for benzofuroxan, a centrifugal separation and purification device, and a waste liquid treatment device. The general operation process is to first process the raw materials for synthesizing benzofuroxan successively, and then send them into the synthesis device for reaction. During the synthesis process, the temperature and pressure are controlled to ensure the efficient progress of the reaction. After the reaction is completed, the mixture is separated by the centrifugal separation and purification device to remove unreacted raw materials and by-products, obtaining crude benzofuroxan. Then, the crude product is further purified by distillation or crystallization to obtain high-purity benzofuroxan. Finally, the waste liquid treatment device treats the waste liquid generated during the reaction process. The waste liquid treatment device includes a resin elution column for adsorbing organic substances in the waste liquid, and then the organic substances in the resin elution column are extracted by flushing with methanol, so as to ensure compliance with environmental protection standards and reduce the impact on the environment.

[0004] For the above related technologies, after flushing the resin elution column with methanol, there may be a large amount of methanol remaining in the resin elution column, and some organic substances in the waste liquid may also be dissolved in the methanol, thereby reducing the elution effect of the resin elution column on the organic substances in the waste liquid when it is reused. If the resin elution column is directly replaced, it will cost a large amount, and the adsorption of organic substances by the resin elution column and the flushing of the resin elution column with methanol cannot be carried out simultaneously. When replacing the resin elution column, it is necessary to stop the adsorption of organic substances by the resin elution column and the flushing of the resin elution column with 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 the organic substances in the waste liquid, and to shorten the overall time required for the resin desorption column to adsorb organic substances, flush the resin desorption column with methanol, 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, its preparation system, and preparation method.

[0006] The present application provides a system for preparing benzofuroxan oxide, which adopts the following technical solution:

[0007] 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;

[0008] 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;

[0009] 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;

[0010] 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;

[0011] 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;

[0012] 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;

[0013] 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;

[0014] A connecting component is provided on the liquid inlet pipe and the waste liquid inlet. 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 in the same way as the liquid inlet pipe. The waste liquid outlet, the methanol inlet, the methanol outlet, and the centrifuged liquid outlet are all arranged in the same way as the waste liquid inlet.

[0015] By adopting the above technical solution, the waste liquid is input into the resin barrel from the waste liquid inlet, and then is input into the resin column from the liquid 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 liquid outlet pipe and the waste liquid outlet. When the resin column adsorbs enough organic matter, the first driving motor is started. The first driving motor drives the resin column to rotate around the rotating rod and move to the second station. Methanol is resinized into the resin barrel from the methanol inlet, and then is input into the resin column from the liquid inlet pipe connected to the methanol inlet at the second station, so as to elute the organic matter adsorbed in the resin column. When the elution of the organic matter in the resin column is completed, there will be more methanol remaining in the resin column, which will affect the adsorption effect of the resin column on the organic matter. The first driving motor is started to rotate the resin column to the third station. The centrifugal mechanism at the third station can rotate and centrifuge the resin column, so as to centrifugally throw off the methanol in the resin column, and then output it from the liquid outlet pipe and the centrifuged liquid outlet. When there is still a lot of methanol remaining after the resin column is centrifugally thrown off, more organic matter will be dissolved in the methanol, which means that the resin column needs to be replaced. At this time, the first driving motor is driven again to rotate 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 detection is qualified, the first driving motor will rotate the resin column to the first station for continued use. When the detection is unqualified, the dumping mechanism at the fourth station will dump the resin in the resin column and add new resin, so as to ensure the adsorption effect of the resin column on the organic matter in the waste liquid. The first driving 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, realizing the simultaneous adsorption of organic matter in the waste liquid, the elution of the resin column, the centrifugal separation of the remaining methanol, and the detection and replacement of the resin. The overall time required for the resin desorption column to adsorb organic matter, wash the resin desorption column with methanol, and detect and replace the resin desorption column is shortened. Compared with the prior art of replacing the resin column as a whole, the present application also saves the time and cost required for replacing the resin column, and the centrifugal separation and detection of the remaining methanol can better ensure the use effect of the resin column. The connecting component can ensure the stability of the connection when the liquid inlet pipe and the liquid outlet pipe are connected to each connection port after rotating around the rotating rod.

[0016] Optionally, the centrifugal mechanism includes a second driving motor, a driving gear, a driven gear, a first rotating barrel, a second rotating barrel, a limiting structure, and an extrusion assembly. A fixing plate is arranged inside the resin barrel, and the fixing plate is arranged below the resin column. The second driving motor is arranged on a side of the fixing plate away from the resin column. The driving gear is arranged on a side of the fixing plate close to the resin column and is connected to an output shaft of the second driving motor. The resin column includes a housing. The first rotating barrel is rotatably arranged inside the housing. The second rotating barrel is rotatably arranged inside the first rotating barrel. Resin is arranged inside the second rotating barrel. The driven gear is arranged on a side of the first rotating barrel close to the second driving motor and meshes with the driving gear when in contact with the driving gear. A moving ring groove for the driven gear to rotate around the rotating rod is formed in the fixing plate. Centrifugal holes are formed in both the first rotating barrel and the second rotating barrel. The limiting structure is configured to drive the second rotating barrel to rotate synchronously after relative rotation of the first rotating barrel and the second rotating barrel, so that the centrifugal holes in the first rotating barrel and the second rotating barrel are aligned, and 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 in the first rotating barrel and the second rotating barrel are staggered. The extrusion assembly is arranged inside the second rotating barrel and is configured to extrude the resin.

[0017] By adopting the above technical solution, when the second driving motor is started, the driving gear on the output shaft of the second driving motor drives the driven gear to rotate. Since the driven gear is arranged on a 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, under the action of the limiting structure, the second rotating barrel can be driven to rotate synchronously. When the first rotating body and the second rotating barrel rotate synchronously, the centrifugal holes formed in the first rotating barrel and the second rotating barrel are aligned. At this time, the residual methanol solution in the resin is thrown from the centrifugal holes into the gap between the first rotating barrel and the housing under the action of centrifugation and is output from the liquid outlet on the housing to the centrifugal liquid outlet. Since the centrifugal liquid outlet is communicated with the methanol liquid outlet, the residual methanol liquid separated by centrifugation will also be collected into the methanol recovery barrel, thereby reducing the residual methanol content in the resin column. When the second driving 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 in the first rotating barrel and the second rotating barrel are staggered to restore the initial state for subsequent use of the resin column. The extrusion assembly in the present application can extrude 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.

[0018] Optionally, the limiting structure includes a rotating limiting block and a first reset member. The rotating limiting block is disposed on the inner top wall of the first rotating barrel. An arc-shaped groove is formed on the outer top wall of the second rotating barrel corresponding to the rotating limiting block. When the rotating limiting block is located at both ends of the arc-shaped 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 disposed between the inner top wall of the first rotating barrel and the outer top wall of the second rotating barrel. 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.

[0019] By adopting the above technical solution, in the initial state, the rotating limiting block is located at the middle position of the arc-shaped groove. At this time, the centrifugal holes formed on the first rotating barrel and the second rotating barrel are staggered from 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 relatively, the rotating limiting block rotates to the end of one end of the arc-shaped groove and abuts against the inner wall of the arc-shaped groove, so as to realize 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 reverse direction, the rotating limiting block will move to the end of the other end of the arc-shaped groove. At this time, the separation holes on the first rotating barrel and the second rotating barrel are also aligned, so as to realize that no matter the second driving motor rotates forward or backward, the residual methanol in the resin column can be shaken off, and the adsorption and use effect of the resin column on the organic matter in the waste liquid can be improved.

[0020] Optionally, the extrusion assembly includes a lifting plate, a lead screw and a vertical limiting block. The lifting plate is arranged in the second rotating barrel in a lifting manner. The vertical limiting block is disposed on the lifting plate. A vertical groove is formed on the inner wall of the second rotating barrel corresponding to the vertical limiting block. The lead screw is disposed in the second rotating barrel. One end of the lead screw is rotatably connected to the inner bottom wall of the first rotating barrel, and the other end of the lead screw penetrates through the first rotating barrel and the second rotating barrel and is fixedly connected to the inner top wall of the housing. The lifting plate is disposed on the lead screw and is in threaded connection with the lead screw. When the first rotating barrel drives the second rotating barrel to rotate, under the action of the vertical limiting block and the lead screw, the lifting plate moves up and down.

[0021] By adopting the above technical solution, since one end of the lead screw is fixedly installed on the outer shell and the other end is connected to the inner bottom plate of the first rotating barrel, when the first rotating barrel rotates, the lead screw does not rotate. Because the vertical limiting block on the lifting plate is slidably installed in the vertical groove and the lifting plate is threadedly connected to the lead 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, so as to realize the lifting of the lifting plate on the lead screw. When the height of the lifting plate changes, the resin column in the second rotating barrel can be extruded, thereby further reducing the methanol residue in the resin column and improving the centrifugal effect on the residual methanol in the resin.

[0022] Optionally, the pouring mechanism includes a pouring port, a pouring plate, a clamping block, an electric telescopic rod and a detection component. The pouring port is arranged on the surface of the fixed plate away from the resin column, and a discharge port is formed in the fixed plate corresponding to the position of the pouring port. The clamping block is arranged on the pouring plate, and a clamping groove is formed in the inner bottom wall of the first rotating barrel corresponding to the clamping block. The pouring plate is clamped on the inner bottom wall of the first rotating barrel through the clamping block and the clamping groove. A socket barrel is arranged on the surface of the pouring plate away from the fixed plate. One end of the lead screw close to the fixed plate rotates and is inserted into the socket barrel. The depth of the socket barrel is greater than the height of the lead screw located in the socket barrel. The driven gear is fixedly arranged on the surface of the pouring plate close to the fixed plate. The electric telescopic rod is arranged in the pouring port. The electric telescopic rod includes a first telescopic end and a second telescopic end. When the first telescopic end of the electric telescopic rod extends, it can abut against the surface of the pouring plate close to the fixed plate. When the first telescopic end of the electric telescopic rod extends, the pouring plate is separated from the first rotating barrel, and the resin in the second rotating barrel falls into the pouring port through the gap between the pouring plate and the first rotating barrel. The detection component is used to detect the amount of methanol residue in the resin column.

[0023] By adopting the above technical solution, after the detection component detects the methanol content in the resin column, if the detection is qualified, the first driving motor will transfer the resin column to the first station for adsorbing organic substances in the waste liquid. When the detection result of the methanol content in the resin column by the detection component is too high, the electric telescopic rod is started. The first telescopic end of the electric telescopic rod extends and abuts against the surface of the dumping tray close to the fixing plate. Since the dumping tray is circumferentially clamped and axially inserted between the inner bottom wall of the first rotating barrel through the clamping block, when the first telescopic end extends, the dumping tray can be jacked up to achieve separation from the inner bottom wall of the first rotating barrel. The resin in the second rotating barrel falls into the dumping port through the gap between the dumping tray and the first rotating barrel, thereby realizing the dumping of the resin in the resin column. And when the dumping tray is jacked 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 lead screw located in the socket barrel, interference between the lead screw and the dumping tray can be avoided, and the socket barrel improves the stability of the lead screw at the same time, avoiding the eccentricity of the lead screw after long-term use.

[0024] Optionally, the detection component includes an air pump and a methanol detector. An air inlet and an air outlet are provided on the resin barrel. The air inlet and the air outlet are both arranged in the same way 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, the air outlet is connected to the liquid inlet pipe, a resin addition port is provided on the air inlet, a end cover is provided on the resin addition port, and the methanol detector is electrically connected to the air pump and the electric telescopic rod.

[0025] By adopting the above technical solution, when the resin column is located at the fourth station, the air pump is started, and the air pump conveys 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 it may not be very suitable to continue adsorbing organic substances in the waste liquid. At this time, the methanol detector will send an electric signal to the electric telescopic rod and the air pump, close the air pump and start the electric telescopic rod at the same time, thereby realizing the dumping of the resin. After the dumping is completed, the electric telescopic rod can be closed, and new resin can be added from the resin addition port on the air inlet. Compared with the prior art of replacing the whole resin column, the present application saves the time, the construction period delay and the cost required for replacing the resin column.

[0026] Optionally, a second reset member is provided between the dumping tray and the first rotating barrel. The second reset member includes a spring, a column, and a reset block. The column is disposed on the inner bottom wall of the housing. The reset block is disposed at the end of the column away from the fixed plate and is clamped with the dumping tray. An annular groove for the movement of the reset block is formed on the dumping tray. An installation groove is formed on the bottom wall of the housing. The end of the column away from the dumping tray is located in the installation groove. A limiting plate is provided at the end of the column away from the dumping tray. The spring is disposed on the column and is located between the limiting plate and the top wall of the installation groove.

[0027] By adopting the above technical solution, since the reset block is clamped with the dumping tray and the reset block is installed on the column, when the first telescopic end of the electric telescopic rod drives the dumping tray to rise, the column and the reset column are driven to rise synchronously. The spring is compressed between the limiting plate and the installation groove until the limiting plate abuts against the inner wall of the installation groove. At this time, the dumping tray is completely separated from the inner bottom wall of the first rotating barrel. The resin in the second rotating barrel is dumped through the gap between the first rotating barrel and the dumping tray. When the first telescopic end shortens, the spring elongates between the limiting plate and the installation groove until the inner bottom wall of the first rotating barrel is completely abutted against the dumping tray. The spring can make the dumping tray fit more closely with the end of the first telescopic end during the rising and falling processes of the dumping tray, making the lifting of the dumping tray more stable, and improving the abutting and sealing effect between the inner bottom wall of the first rotating barrel and the dumping tray.

[0028] Optionally, a sealing plate is provided at the bottom of the dumping port. The second telescopic end of the electric telescopic rod is fixedly connected to the sealing plate. When the second telescopic end shortens, the sealing plate is clamped with the bottom of the dumping port to close the bottom of the dumping port. A blanking channel for facilitating the dumping of resin is provided in the dumping port. Both ends of the blanking channel are in a funnel shape that expands outward. The surface of the sealing plate close to the fixed plate is convexly curved. A resin recovery barrel is provided below the dumping port.

[0029] By adopting the above technical solution, while the first telescopic end of the electric telescopic rod elongates, the second telescopic end elongates synchronously. When the second telescopic end elongates, it drives the sealing plate to descend, so that the resin in the dumping port is poured into the resin recovery barrel through the gap between the sealing plate and the dumping port. When the dumping is completed, the second telescopic end shortens until the sealing plate is completely abutted against the dumping port, thereby blocking the connection between the resin recovery barrel and the resin barrel and preventing the methanol in the resin recovery barrel from volatilizing into the resin barrel and affecting the detection of the methanol detector.

[0030] Optionally, the connection component includes a mounting base, a corrugated pipe, a clamping joint, a telescopic member, and a ball head pipe. The mounting base is disposed on the waste liquid inlet, and the clamping joint is disposed on a side of the mounting base away from the waste liquid inlet and is connected by the telescopic member. The corrugated pipe is disposed between the mounting base and the clamping joint, and the ball head pipe is disposed at an end of the liquid inlet pipe away from the resin column.

[0031] By adopting the above technical solution, when the rotating rod drives the resin column to rotate, the ball head pipe on the liquid inlet pipe will abut against the clamping joint. During the abutting process, the telescopic member and the corrugated pipe will contract. After the ball head pipe enters the clamping joint, the telescopic member will drive the corrugated pipe to elongate synchronously until the clamping joint is completely abutted, and the telescopic member will continuously provide a mortgage force when the clamping joint and the ball head pipe are abutted to maintain the connection effect between the clamping joint and the ball head pipe.

[0032] This application also includes a preparation method of benzofuroxan: 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 caustic soda solution and 3000 kg of 10.5% sodium hypochlorite solution, then starting stirring, and at the same time calculating the start time. The temperature is controlled within 52 °C within 3 h. After 3 h, the temperature is raised to 68 - 70 °C, and after keeping warm for 1 h, the jacket is cooled with cooling water. When the temperature drops below 35 °C, crystallization occurs and then the material is discharged for centrifugal separation to obtain benzofuroxan, and finally it is weighed and stored in the warehouse.

[0033] In summary, this application includes at least one of the following beneficial technical effects:

[0034] 1. Using the first driving motor and the rotating rod to switch multiple resin columns at the first station, the second station, the third station, and the fourth station respectively, realizing the simultaneous adsorption of organic substances in the waste liquid, the elution of the resin column, the centrifugal separation of residual methanol, and the detection and replacement of the resin, shortening the overall time required for the resin desorption column to adsorb organic substances, wash the resin desorption column with methanol, and detect and replace the resin desorption column. Compared with the prior art of replacing the resin column as a whole, this application also saves the time and cost required for replacing the resin column, and the centrifugal separation and detection of residual methanol can better ensure the use effect of the resin column;

[0035] 2. Start the second drive motor. 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 one side of the first rotating barrel close to the second drive motor, the second drive motor can drive the first rotating barrel to rotate. When the first rotating barrel rotates, under the action of the limiting structure, it can drive the second rotating barrel to rotate synchronously. 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 residual methanol solution in the resin is thrown from the centrifugal holes into the gap between the first rotating barrel and the outer shell under the action of centrifugation, and is output from the liquid outlet on the outer shell to the centrifugal liquid outlet, thereby reducing 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 from each other to restore the initial state for the subsequent use of the resin column;

[0036] 3. Since one end of the lead screw is fixedly installed on the outer shell and the other end is connected to the inner bottom plate of the first rotating barrel, when the first rotating barrel rotates, the lead screw does not rotate. Because the vertical limiting block on the lifting plate is slidably installed in the vertical groove and the lifting plate is threadedly connected to the lead 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 of the lifting plate on the lead screw. When the height of the lifting plate changes, the resin column in the second rotating barrel can be extruded, thereby further reducing the methanol residue in the resin column and improving the centrifugal effect on the residual methanol in the resin;

[0037] 4. After the detection component detects the methanol content in the resin column, if the detection is qualified, the first drive motor will transfer the resin column to the first station for adsorbing organic substances in the waste liquid. When the detection result of the methanol content in the resin column by the detection component is too high, start the electric telescopic rod. The first telescopic end of the electric telescopic rod extends and abuts against the side of the dumping plate close to the fixed plate. Since the dumping plate is circumferentially clamped and axially inserted between the inner bottom wall of the first rotating barrel through the clamping block, when the first telescopic end extends, it can lift the dumping plate to separate it from the inner bottom wall of the first rotating barrel. The resin in the second rotating barrel falls into the dumping port from the gap between the dumping plate and the first rotating barrel, thereby realizing the dumping of the resin in the resin column. And when the dumping plate is pushed up by the first telescopic end of the electric telescopic rod, the socket barrel improves the stability of the lead screw and avoids the eccentricity of the lead screw after long-term use. When the dumping is completed, the electric telescopic rod can be turned off, and new resin can be added from the resin addition port on the air inlet. Compared with the prior art of replacing the entire resin column, the present application saves the time, the construction period delay, and the cost required for replacing the resin column;

[0038] 5. Since the reset block is clamped with the tipping tray and the reset block is installed on the column, when the first telescopic end of the electric telescopic rod drives the tipping tray to rise, the column and the reset column are driven to rise synchronously. The spring is compressed between the limit plate and the installation groove until the limit plate abuts against the inner wall of the installation groove. At this time, the tipping tray is completely separated from the inner bottom wall of the first rotating barrel, and the resin in the second rotating barrel is poured through the gap between the first rotating barrel and the tipping tray. When the first telescopic end shortens, the spring elongates between the limit plate and the installation groove until the inner bottom wall of the first rotating barrel completely abuts against the tipping tray. The spring can make the tipping tray fit more closely with the end of the first telescopic end during the rising and falling processes of the tipping tray, making the lifting of the tipping tray more stable, and improving the abutting and sealing effect between the inner bottom wall of the first rotating barrel and the tipping tray;

[0039] 6. While the first telescopic end of the electric telescopic rod elongates, the second telescopic end elongates synchronously. While the second telescopic end elongates, it drives the sealing plate to descend, so as to realize that the resin in the pouring port is poured into the resin recovery barrel through the gap between the sealing plate and the pouring port. When the pouring is completed, the second telescopic end shortens until the sealing plate and the pouring port are completely abutted, so as to realize the blocking between the resin recovery barrel and the resin barrel, and avoid 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

[0040] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following will briefly introduce the drawings required for the description of the embodiments. Obviously, the following drawings are only some embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0041] Figure 1 is the overall structural schematic diagram of the embodiment of the present application;

[0042] Figure 2 is Figure 1 partial structural schematic diagram of;

[0043] Figure 3 is Figure 2 partial structural sectional schematic diagram of;

[0044] Figure 4 is Figure 2 partial structural sectional schematic diagram of;

[0045] Figure 5 is Figure 3 enlarged schematic diagram of part A structure of;

[0046] Figure 6 is the structural schematic diagram of the limit structure;

[0047] Figure 7 is Figure 3 an enlarged schematic view of part B structure of

[0048] Figure 8 is Figure 4 an enlarged schematic view of part C structure of

[0049] Figure 9 is Figure 4 an enlarged schematic view of part D structure of

[0050] Reference numerals: 1, resin barrel; 11, waste liquid inlet; 12, methanol inlet; 13, waste liquid outlet; 14, methanol outlet; 15, resin column; 151, inlet pipe; 152, outlet pipe; 153, outer shell; 16, rotating rod; 17, first driving motor; 18, fixing plate; 1a, first working station; 1b, second working station; 1c, third working station; 1d, fourth working station; 2, waste liquid recovery barrel; 3, methanol recovery barrel; 4, centrifugal mechanism; 41, second driving motor; 42, driving gear; 43, driven gear; 44, first rotating barrel; 45, second rotating barrel; 46, limiting structure; 461, rotating limiting block; 462, first resetting member; 463, arc groove; 47, extrusion assembly; 471, lifting plate; 472, lead screw; 473, vertical limiting block; 474, vertical groove; 5, tilting mechanism; 51, tilting opening; 511, sealing plate; 52, tilting 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, connecting assembly; 61, mounting seat; 62, corrugated pipe; 63, connecting head; 64, telescopic member; 65, ball head pipe; 7, second resetting member; 71, spring; 72, column; 73, resetting block; 74, limiting plate; 8, resin recovery barrel. Detailed implementation manners

[0051] The following further describes the present application in detail with reference to Figures 1-9 the accompanying drawings.

[0052] The embodiments of the present application disclose a benzofuroxan and its preparation system and preparation method. Referring to Figure 1 , Figure 2 , Figure 3 and Figure 4, A preparation system for benzofuroxan, comprising a mounting frame, a resin barrel 1, a waste liquid recovery barrel 2 and a methanol recovery barrel 3. The resin barrel 1, the waste liquid recovery barrel 2 and the methanol recovery barrel 3 are all fixedly installed 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. An inlet pipe 151 and an outlet pipe 152 are welded and installed on the resin column 15. The inlet pipe 151 is welded and installed above the 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 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 welded and installed on the rotating rod 16. One end of the connecting rod away from the rotating rod 16 is welded and connected to the top of the resin column 15. The rotating rod 16 drives the resin column 15 to rotate around the rotating rod 16 through the connecting rod.

[0053] A first working position 1a is arranged in the resin barrel 1. When the resin column 15 is located at the first working position 1a, the inlet pipe 151 is connected to the waste liquid inlet 11, and the outlet pipe 152 is connected to the waste liquid outlet 13. A second working position 1b is arranged in the resin barrel 1. When the resin column 15 is located at the second working position 1b, the inlet pipe 151 is connected to the methanol inlet 12, and the outlet pipe 152 is connected to the methanol outlet 14. A third working position 1c is arranged 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 working position 1c, the outlet pipe 152 is connected to the centrifugal liquid outlet. A centrifugal mechanism 4 is arranged at the third working position 1c and on the resin column 15, and the centrifugal liquid outlet is communicated with the methanol outlet 14. A fourth working position 1d is arranged in the resin barrel 1. A dumping mechanism 5 is arranged at the fourth working position 1d and on the resin column 15.

[0054] A plurality of resin columns 15 are provided. The rotating rod 16 drives the positions of the plurality of resin columns 15 to be switched respectively at the first working position 1a, the second working position 1b, the third working position 1c and the fourth working position 1d. A connecting component 6 is arranged on the inlet pipe 151 and the waste liquid inlet 11. The outlet pipe 152 is arranged in the same way as the inlet pipe 151. The waste liquid outlet 13, the methanol inlet 12, the methanol outlet 14 and the centrifugal liquid outlet are all arranged in the same way as the waste liquid inlet 11.

[0055] In this embodiment, the waste liquid is input into the resin barrel 1 from the waste liquid inlet 11, and then enters the resin column 15 through the liquid 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 liquid outlet pipe 152 and the waste liquid outlet 13. When the resin column 15 adsorbs enough organic matter, the first driving motor 17 is started. The first driving motor 17 drives the resin column 15 to rotate around the rotating rod 16 and move to the second station 1b. Methanol enters the resin barrel 1 from the methanol inlet 12, and then enters the resin column 15 through the liquid inlet pipe 151 connected to the methanol inlet 12 at the second station 1b, so as to elute the organic matter adsorbed in the resin column 15. When the elution of the organic matter in the resin column 15 is completed, there will be more methanol remaining in the resin column 15, which will affect the adsorption effect of the resin column 15 on the organic matter. The first driving motor 17 is started to rotate the resin column 15 to the third station 1c. The centrifugal mechanism 4 at 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 pipe 152 and the centrifugate outlet. When there is still a lot of methanol remaining after the resin column 15 is centrifuged and removed, and a lot of organic matter is dissolved in the methanol at the same time, it means that the resin column 15 needs to be replaced. At this time, the first driving 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 driving 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, so as to ensure the adsorption effect of the resin column 15 on the organic matter in the waste liquid. The first driving motor 17 and the rotating rod 16 are used to switch multiple resin columns 15 between the first station 1a, the second station 1b, the third station 1c and the fourth station 1d respectively, realizing the adsorption of organic matter in the waste liquid, the elution of the resin column 15, the centrifugal separation of the residual methanol and the detection of the resin. The detection and replacement are carried out at the same time. Compared with the prior art of replacing the whole resin column 15, this embodiment saves the time and cost consumed by replacing the resin column 15, and the centrifugal separation and detection of the residual methanol can better ensure the use effect of the resin column 15. The connecting component 6 can ensure the connection stability when the liquid inlet pipe 151 and the liquid outlet pipe 152 are connected to each connection port after rotating around the rotating rod 16.

[0056] After the resin in the resin column 15 is rinsed with methanol, the residual methanol 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. Refer to Figure 3 and Figure 5, so the centrifugal mechanism 4 in this embodiment includes a second driving 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 driving motor 41 is fixedly installed on the side of the fixing plate 18 away from the resin column 15. The driving gear 42 is installed on the side of the fixing plate 18 close to the resin column 15 and is welded to the output shaft of the second driving motor 41. The resin column 15 includes a housing 153. The first rotating barrel 44 is rotatably installed in the housing 153, and the second rotating barrel 45 is rotatably installed in the first rotating barrel 44. Resin is placed in the second rotating barrel 45. The driven gear 43 is welded and installed on the side of the first rotating barrel 44 close to the second driving motor 41 and meshes with the driving gear 42 when in contact with the driving gear 42. A moving ring groove is formed on the fixing plate 18 for the driven gear 43 to rotate around the rotating rod 16. Centrifugal holes are formed on both the first rotating barrel 44 and the second rotating barrel 45.

[0057] Start the second driving motor 41. 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. When the first rotating barrel 44 rotates, under the action of the limiting structure 46, it can drive the second rotating barrel 45 to rotate synchronously. When the first rotating body and the second rotating barrel 45 rotate synchronously, the centrifugal holes formed on the first rotating barrel 44 and the second rotating barrel 45 are aligned. At this time, the residual methanol solution in the resin is thrown from the centrifugal holes into the gap between the first rotating barrel 44 and the housing 153 under the action of centrifugation and is output from the liquid outlet on the housing 153 to the centrifugal liquid outlet. Since the centrifugal liquid outlet is communicated with the methanol liquid outlet 14, the residual methanol liquid separated by centrifugation will also be collected into the methanol recovery barrel 3, thereby reducing 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 relatively. At this time, the centrifugal holes on the first rotating barrel 44 and the second rotating barrel 45 are staggered to return to the initial state for the subsequent use of the resin column 15. The extrusion assembly 47 in this embodiment can extrude the resin in the resin column 15, thereby further reducing the methanol residue in the resin column 15 and improving the centrifugal effect on the residual methanol in the resin.

[0058] To align and stagger the centrifugal holes on the first rotating barrel 44 and the second rotating barrel 45, refer to Figure 6 and Figure 7, in this embodiment, the fixed limit structure 46 includes a rotating limit block 461 and a first reset member 462. The rotating limit block 461 is integrally provided 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 limit 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, and the torsion spring is a preferred manner of the embodiment. In other embodiments, the first reset member 462 may be an elastic rubber block installed between the first rotating barrel 44 and the second rotating barrel 45, etc.

[0059] In the initial state, the rotating limit block 461 is located at the middle position of the arc-shaped groove 463. At this time, the centrifugal holes provided on the first rotating barrel 44 and the second rotating barrel 45 are staggered from 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 relatively, the rotating limit block 461 rotates to the end of the arc-shaped groove 463 and abuts against the inner wall of the arc-shaped groove 463, so as to realize the first rotating barrel 44 driving 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 reverse direction, the rotating limit block 461 will move to the other end of the arc-shaped groove 463. At this time, the separation holes on the first rotating barrel 44 and the second rotating barrel 45 are also aligned, so as to realize that no matter the second driving motor 41 rotates forward or backward, the residual methanol in the resin column 15 can be thrown off, improving the adsorption and use effect of the resin column 15 on the organic matter in the waste liquid.

[0060] When the resin in the resin column 15 becomes viscous, the effect of centrifugally throwing off the methanol in the resin may be poor. Refer to Figure 3 and Figure 7 , so the extrusion assembly 47 in this embodiment includes a lifting plate 471, a lead screw 472 and a vertical limit block 473. The lifting plate 471 is installed in the second rotating barrel 45 in a lifting manner. The vertical limit block 473 is integrally provided 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 lead screw 472 is installed in the second rotating barrel 45. One end of the lead screw 472 is rotatably connected to the inner bottom wall of the first rotating barrel 44, and the other end of the lead screw 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 by welding. The lifting plate 471 is installed on the lead screw 472 and is threadedly connected to the lead screw 472.

[0061] 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.

[0062] 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.

[0063] 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 transfer the resin column 15 to the first station 1a for adsorbing organic substances in the waste liquid. When the detection result of the methanol content in the resin column 15 by the detection component 55 is too high, the electric telescopic rod 54 is started. The first telescopic end 541 of the electric telescopic rod 54 extends and abuts against the side of the dumping tray 52 close to the fixed plate 18. Since the dumping tray 52 is circumferentially clamped and axially inserted between the inner bottom wall of the first rotating barrel 44 through the clamping block 53, when the first telescopic end 541 extends, the dumping tray 52 can be lifted to realize the separation from the inner bottom wall of the first rotating barrel 44. The resin in the second rotating barrel 45 drops into the dumping port 51 from the gap between the dumping tray 52 and the first rotating barrel 44, so as to realize the dumping of the resin in the resin column 15. And when the dumping tray 52 is pushed 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 lead screw 472 located in the socket barrel 521, the interference between the lead screw 472 and the dumping tray 52 can be avoided, and the socket barrel 521 improves the stability of the lead screw 472 at the same time, avoiding the eccentricity of the lead screw 472 after long-term use.

[0064] In order to detect the content of residual methanol in the resin column 15, referring to Figure 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 in the same way 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 addition port is arranged on the air inlet, and an end cover is inserted and installed on the resin addition port. The methanol detector 552 is electrically connected to the air pump 551 and the electric telescopic rod 54.

[0065] 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 very suitable for continuing to adsorb organic substances 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, close the air pump 551 and start the electric telescopic rod 54 at the same time, so as to realize the dumping of the resin. After the dumping is completed, the electric telescopic rod 54 can be closed, and new resin can be added from the resin addition port on the air inlet. Compared with the prior art of replacing the whole resin column 15, this embodiment saves the time, construction period and cost required for replacing the resin column 15.

[0066] It is relatively unstable to realize the lifting of the tipping tray 52 only by the abutment between the first telescopic end 541 and the tipping tray 52. Refer to Figure 4 and Figure 8 , so in this embodiment, a second reset member 7 is installed between the tipping 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 housing 153. The reset block 73 is welded to the end of the column 72 away from the fixing plate 18 and is clamped with the tipping tray 52. A ring groove for the movement of the reset block 73 is formed on the tipping tray 52. An installation groove is formed on the bottom wall of the housing 153. The end of the column 72 away from the tipping tray 52 is located in the installation groove. A limiting plate 74 is welded to the end of the column 72 away from the tipping tray 52. The spring 71 is sleeved on the column 72 and is located between the limiting plate 74 and the top wall of the installation groove. In this embodiment, the reset block 73 is a "T"-shaped block, and the cross-section of the ring groove corresponds to the reset block 73 and is also "T"-shaped. The "T"-shaped reset block 73 is a preferred method in this embodiment. In other embodiments, the reset block 73 can be a spherical block, etc.

[0067] Since the reset block 73 is clamped with the tipping tray 52 and the reset block 73 is installed on the column 72, when the first telescopic end 541 of the electric telescopic rod 54 drives the tipping tray 52 to rise, the column 72 and the reset column are driven to rise synchronously. The spring 71 is compressed between the limiting plate 74 and the installation groove until the limiting plate 74 abuts against the inner wall of the installation groove. At this time, the tipping tray 52 is completely separated from the inner bottom wall of the first rotating barrel 44. The resin in the second rotating barrel 45 is poured through the gap between the first rotating barrel 44 and the tipping tray 52. When the first telescopic end 541 shortens, the spring 71 elongates between the limiting plate 74 and the installation groove until the inner bottom wall of the first rotating barrel 44 completely abuts against the tipping tray 52. The spring 71 can make the tipping tray 52 fit more closely with the end of the first telescopic end 541 during the rising and falling processes of the tipping tray 52, making the lifting of the tipping tray 52 more stable, and improving the abutment sealing effect between the inner bottom wall of the first rotating barrel 44 and the tipping tray 52.

[0068] Refer to Figure 1 and Figure 8, in this embodiment, a sealing plate 511 is also 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 sealing plate 511. When the second telescopic end 542 shortens, the sealing plate 511 is clamped with the bottom of the pouring port 51 to seal the bottom of the pouring port 51. A feeding channel is welded and installed in the pouring port 51. Both ends of the feeding channel are in a funnel shape that expands outward. One side of the sealing plate 511 close to the fixing plate 18 is provided with a convex curved surface. A resin recovery barrel 8 is installed below the pouring port 51. While the first telescopic end 541 of the electric telescopic rod 54 extends, the second telescopic end 542 extends synchronously. When the second telescopic end 542 extends, it drives the sealing plate 511 to descend, so as to realize that the resin in the pouring port 51 is poured into the resin recovery barrel 8 through the gap between the sealing plate 511 and the pouring port 51. After the pouring is completed, the second telescopic end 542 shortens until the sealing plate 511 and the pouring port 51 are completely abutted, so as to realize the block between the resin recovery barrel 8 and the resin barrel 1 and avoid the methanol in the resin recovery barrel 8 from volatilizing into the resin barrel 1 and affecting the detection of the methanol detector 552.

[0069] Referring to Figure 9 , the connection component 6 in this embodiment includes a mounting seat 61, a corrugated pipe 62, a clamping joint 63, a telescopic member 64 and a ball head pipe 65. The mounting seat 61 is welded and installed on the waste liquid inlet 11. The clamping joint 63 is movably installed on the side of the mounting seat 61 away from the waste liquid inlet 11 and is connected through the telescopic member 64. The corrugated pipe 62 is installed between the mounting seat 61 and the clamping joint 63. The ball head pipe 65 is welded and installed at the end of the liquid inlet pipe 151 away from the resin column 15. When the rotating rod 16 drives the resin column 15 to rotate, the ball head pipe 65 on the liquid inlet pipe 151 will abut against the clamping joint 63. During the abutting process, the telescopic member 64 and the corrugated pipe 62 will contract. When the ball head pipe 65 enters the clamping joint 63, the telescopic member 64 will drive the corrugated pipe 62 to extend synchronously until the clamping joint 63 is completely abutted, and the telescopic member 64 will continuously provide a mortgage force when the clamping joint 63 and the ball head pipe 65 are abutted to maintain the connection effect between the clamping joint 63 and the ball head pipe 65.

[0070] The implementation principle of the benzofuroxan preparation system in the embodiment of the present application is as follows:

[0071] The waste liquid is input into the resin barrel 1 from the waste liquid inlet 11, and then enters the resin column 15 through the liquid 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 liquid outlet pipe 152 and the waste liquid outlet 13. When the resin column 15 adsorbs enough organic matter, the first driving motor 17 is started, and the first driving motor 17 drives the resin column 15 to rotate around the rotating rod 16 and move to the second station 1b. Methanol enters the resin barrel 1 from the methanol inlet 12, and then enters the resin column 15 through the liquid inlet pipe 151 connected to the methanol inlet 12 at the second station 1b, so as to elute the organic matter adsorbed in the resin column 15;

[0072] When there is a large amount of methanol remaining in the resin column 15, the second driving motor 41 is started. 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 one 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, under the action of the limiting structure 46, it can drive the second rotating barrel 45 to rotate synchronously. 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 holes into 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;

[0073] When it is necessary to further improve the centrifugal throwing effect on the resin, since one end of the lead screw 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 lead screw 472 does not rotate when the first rotating barrel 44 rotates. Because the vertical limiting 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 lead screw 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, so as to realize the lifting of the lifting plate 471 on the lead screw 472. When the height of the lifting plate 471 changes, the resin column 15 in the second rotating barrel 45 can be squeezed, so as to further reduce the methanol residue in the resin column 15 and improve the centrifugal effect on the residual methanol in the resin;

[0074] When it is necessary to detect the methanol content remaining in the centrifuged resin to determine whether replacement is needed, after the detection component 55 detects the methanol content in the resin column 15, if the detection is qualified, the first driving motor 17 will transfer the resin column 15 to the first station 1a for adsorbing organic substances in the waste liquid. When the detection result of the methanol content in the resin column 15 by the detection component 55 is too high, the electric telescopic rod 54 is started. The first telescopic end 541 of the electric telescopic rod 54 extends and abuts against one side of the dumping tray 52 close to the fixing plate 18. Since the dumping tray 52 is circumferentially clamped and axially inserted between the inner bottom wall of the first rotating barrel 44 through the clamping block 53, the extension of the first telescopic end 541 can lift the dumping tray 52 to achieve separation from the inner bottom wall of the first rotating barrel 44. The resin in the second rotating barrel 45 falls into the dumping port 51 through the gap between the dumping tray 52 and the first rotating barrel 44, thereby realizing the dumping of the resin in the resin column 15. After the dumping is completed, the electric telescopic rod 54 can be closed, and new resin can be added through the resin addition port on the air inlet.

[0075] This application also discloses a preparation method of benzofuroxan: Using o-nitroaniline and sodium hypochlorite as raw materials, first weigh 540 kg of o-nitroaniline, put it into a 3000 L enamel kettle, add 180 kg of 33% liquid caustic soda solution and 3000 kg of 10.5% sodium hypochlorite solution, then start stirring, and calculate the start time at the same time. Control the temperature within 52 °C within 3 h. After 3 h, heat up to 68 - 70 °C, keep warm for 1 h, then cool down the jacket with cooling water. When the temperature drops below 35 °C, crystallize and discharge the material for centrifugal separation to obtain benzofuroxan, and finally weigh and store it in the warehouse.

[0076] Unless otherwise defined, the technical terms or scientific terms used in this application shall have the ordinary meanings understood by those with ordinary skills in the field to which this application belongs. The "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. Words such as "a" or "one" do not indicate a quantity limitation either, but indicate that there is at least one. Words such as "including" or "comprising" mean that the elements or objects appearing before "including" or "comprising" cover the elements or objects listed after "including" or "comprising" and their equivalents, and do not exclude other elements or objects. "Up", "down", "left", "right", etc. are only used to represent relative position relationships. When the absolute position of the object being described changes, the relative position relationship may also change accordingly.

[0077] The above are all optional embodiments of this application, and do not limit the protection scope of this application accordingly. Therefore, all equivalent changes made according to the structure, shape and principle of this application should be covered within the protection scope of this 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 oxide 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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