Preparation device and process of triazinone

Abstract

The invention discloses a triazinone preparation device and process, and relates to the technical field of triazinone preparation, the triazinone preparation device comprises a base, one side of the base is provided with a support, and the base is provided with a hydrolysis kettle, an oxidation kettle and a cyclization kettle; electromagnetic control valves are respectively arranged on the outer sides of the hydrolysis kettle and the cyclization kettle; a butt joint transmission mechanism is arranged on the outer side of the oxidation kettle and is used for transmitting materials; materials are subjected to a hydrolysis reaction in the hydrolysis kettle, are conveyed into the oxidation kettle through the butt joint conveying mechanism for an oxidation reaction, and then are conveyed into the cyclization kettle for a cyclization reaction; an executing mechanism is arranged on the support and comprises an installation frame installed on the support in a sliding mode, a deflection plate is rotationally arranged on the installation frame, and a scraping piece, a checking piece and a removing piece are further sequentially arranged on the installation frame. A stirring shaft is telescopically arranged on the deflection plate and is used for stirring treatment; according to the invention, preparation of triazinone can be efficiently realized, and material transmission is convenient, so that subsequent maintenance operation is more convenient.

Description

Technical Field

[0001] The present invention relates to the technical field of triazone preparation, and in particular to a triazone preparation device and process. Background Art

[0002] Triazine is a chemical name, usually referring to compounds containing triazine rings and ketone groups. Triazine is a six-membered heterocyclic compound composed of three nitrogen atoms and three carbon atoms, with strong chemical stability and wide application. Triazine compounds have certain applications in chemistry, pesticides, medicine, and materials science. Many triazine compounds are used as herbicides and insecticides. Common triazine herbicides such as cyhalothrin are widely used triazine compounds. Triazine compounds have a broad spectrum of herbicidal effects and can effectively inhibit the growth of a variety of grass plants; in addition, triazine compounds also have certain applications in the medical field, especially in the development of some antiviral and anti-tumor drugs. Triazine ketone compounds may be used as one of the structural skeletons to combine with other drug molecules to exert biological activity. As a compound containing a triazine ring and a ketone group, triazine ketone has a variety of chemical properties and has broad application prospects, especially in the fields of pesticides, photocatalysis, medicine, and materials science. Due to its special molecular structure, it can participate in a variety of chemical reactions, providing important support for research and industrial development in related fields. The preparation process of triazone is currently generally carried out through hydrolysis, oxidation, cyclization and other reactions. During the reaction at each stage, the materials need to be transferred in sequence, and between the reactors, they are generally transferred through fixed pipelines, or after unloading, they are transferred externally, resulting in low efficiency and making subsequent maintenance operations inconvenient. Based on this, the present invention proposes a preparation device that can efficiently realize the preparation of triazone, and the material transmission is convenient, making subsequent maintenance operations more convenient. Summary of the invention

[0003] In view of the above technical problems, the present invention can efficiently realize the preparation of triazone, and the material transmission is convenient, making the subsequent maintenance operation more convenient.

[0004] The use scheme of the present invention is as follows: a triazone preparation device comprises a base, a bracket is arranged on one side of the base, a hydrolysis kettle, an oxidation kettle and a cyclization kettle are arranged on the base; electromagnetic control valves are arranged on the outer sides of the hydrolysis kettle and the cyclization kettle respectively for material transportation; a docking transmission mechanism is arranged on the outer side of the oxidation kettle, the docking transmission mechanism comprises a steering ring rotatably mounted on the oxidation kettle, a transmission pump is arranged on the steering ring, a telescopic connecting pipe is connected to the transmission pump, a fixing mechanism is arranged at the end of the telescopic connecting pipe, and the fixing mechanism is sealed and docked with the electromagnetic control valves on the hydrolysis kettle and the cyclization kettle to transmit material; discharge holes are symmetrically provided on both sides of the oxidation kettle, and a control mechanism is provided on the inner side of the oxidation kettle and at the discharge holes to control the release of the material; the material undergoes a hydrolysis reaction in the hydrolysis kettle, is transmitted to the oxidation kettle through a docking transmission mechanism for an oxidation reaction, and then is transmitted to the cyclization kettle for a cyclization reaction; an actuator is provided on the bracket, and the actuator includes a mounting frame slidably mounted on the bracket, a deflection plate is rotatably provided on the mounting frame, and a scraper, an inspection member and a cleaning member are also provided on the mounting frame in sequence; a stirring shaft is telescopically provided on the deflection plate for stirring treatment.

[0005] Furthermore, the hydrolysis kettle, oxidation kettle and cyclization kettle are all provided with a top plate motor and a top plate, and the top plate motor is used to drive the top plate to rotate for sealing; the hydrolysis kettle, oxidation kettle and cyclization kettle are also provided with a control panel and an air outlet valve; a bottom plate is provided at the bottom of the hydrolysis kettle, oxidation kettle and cyclization kettle, and a control cylinder is provided on the base, and the control cylinder is used to control the movement of the bottom plate; a steam transmission box is provided on one side of the base for transmitting steam; the hydrolysis kettle, oxidation kettle and cyclization kettle are respectively provided with steam chucks, and the steam chucks are connected to the steam transmission box for temperature regulation.

[0006] Furthermore, a matching turntable is rotatably arranged on the top plate, a socket is opened on the matching turntable, and a blocking motor is arranged on the matching turntable, and a baffle is arranged on the output shaft of the blocking motor, and the baffle is used to block the socket; an electromagnetic fixing rod is arranged on the top plate and located on the outside of the matching turntable, which is used to fix the matching turntable; the stirring shaft on the actuator passes through the socket and enters the hydrolysis kettle, oxidation kettle and cyclization kettle for stirring treatment.

[0007] Furthermore, the actuator includes a moving belt and a moving motor arranged on the bracket, the moving motor is used to drive the moving belt, the moving belt is used to control the movement of the mounting frame, the mounting frame includes a moving frame attached to the moving belt, a support plate is arranged on the top of the moving frame, and a deflection motor is arranged on the moving frame, the deflection motor is used to drive the deflection plate; the scraping member, the inspection member and the cleaning member are respectively arranged on the support plate.

[0008] Furthermore, an extension motor is provided on the deflection plate, a belt structure is provided on the output shaft of the extension motor, and an extension screw and an extension guide rod are movably provided on the deflection plate, the ends of the extension screw and the extension guide rod are connected to an extension seat, the belt structure on the output shaft of the extension motor and the extension screw form a spiral pair, a mounting platform is provided on the extension seat, a turntable is rotatably installed on the mounting platform, a stirring motor is also fixedly provided on the mounting platform, a stirring gear is provided on the output shaft of the stirring motor, and the stirring gear is meshed with the turntable; a connecting guide rod is fixedly provided on the turntable, and a transfer screw is rotatably provided, a screw motor is provided on the top of the connecting guide rod, and the screw motor is used to drive the transfer screw; the stirring shaft is slidably connected to the connecting guide rod, and the top of the stirring shaft and the transfer screw form a spiral pair; a transfer hole is opened at the bottom of the stirring shaft, and the transfer hole is respectively fixed with a scraper and an inspection member to drive the scraper and the inspection member to extend into the hydrolysis kettle, the oxidation kettle and the cyclization kettle; the stirring shaft extends into the cleaning member for cleaning treatment.

[0009] Furthermore, the cleaning member includes an adsorption control box and a cleaning cylinder arranged on the support plate, an adsorption part is arranged inside the cleaning cylinder, an adsorption part is provided on the adsorption part, the adsorption part is connected with the adsorption part, and the stirring shaft extends through the adsorption hole on the adsorption part to perform adsorption treatment on the surface of the stirring shaft; the scraping member includes a scraping ring, and the inspection member includes an inspection seat, and an inspection instrument is arranged on the outer side of the inspection seat; the scraping ring and the inspection seat are both provided with magnetic holes, and a magnetic seat is arranged on the support plate, and the magnetic seat cooperates with the magnetic hole for magnetic fixation; fixed electric cylinders are both provided on the scraping ring and the inspection seat, and matching holes are opened on the scraping ring and the inspection seat, and the stirring shaft is docked and matched with the matching hole, and fixed by matching the telescopic rod of the fixed electric cylinder with the transfer hole.

[0010] Furthermore, the docking transmission mechanism includes a steering motor arranged on the oxidation kettle, a steering gear is arranged on the output shaft of the steering motor, and the steering gear is meshed with the steering ring; a telescopic control electric cylinder is arranged on the steering ring, and the telescopic control electric cylinder is used to control the movement of the fixing mechanism; the fixing mechanism includes a docking tube connected to the telescopic connecting pipe, and the docking tube is connected to the telescopic rod of the telescopic control electric cylinder; a fixed motor is arranged on the docking tube, a fixed gear is arranged on the output shaft of the fixed motor, and a control gear ring is rotatably installed on the docking tube, and the control gear ring is meshed with the fixed gear; a fixed shaft is telescopically arranged on the docking tube, and a spring is connected between the fixed shaft and the docking tube; a pressure plate is arranged on the end face of the control gear ring, and the pressure plate contacts with the end of the fixed shaft to push the fixed shaft to move; a spring is arranged on the electromagnetic control valve, and a fixing hole is arranged on the valve docking part, and the fixing hole is docked with the fixed shaft for fixing, and a sealing ring is arranged on the inner side of the valve docking part, and the valve docking part is docked with the docking tube for sealing.

[0011] Furthermore, the control mechanism includes a ring gear rotatably mounted on the inner side of the oxidation kettle, an incomplete gear tooth portion is arranged on the ring gear, and a release control motor is arranged on the inner side of the oxidation kettle, a release control gear is arranged on the output shaft of the release control motor, and the release control gear is meshed with the ring gear; a control release cylinder is arranged on the inner side of the oxidation kettle and located at the discharge hole, the control release cylinder is connected with the discharge hole, a control rotating part is rotatably mounted inside the control release cylinder, a torsion spring is connected between the top of the control rotating part and the control release cylinder; a connecting gear is arranged at the bottom of the control rotating part, and the connecting gear is meshed with the ring gear.

[0012] A preparation process of triazone, using 95% dichloropinacolone and 50% sodium hydroxide as starting main raw materials, the production process mainly consists of hydrolysis, oxidation, cyclization and other reactions, and has the following steps:

[0013] S10: Hydrolysis reaction

[0014] The hydrolysis kettle is kept at room temperature, and a certain amount of 50% sodium hydroxide and a certain amount of 95% dichloropinacolone are dripped from the metering tank. The jacket is heated to 60°C by steam, and the temperature is evenly stirred and kept warm for 3 hours. The temperature is then raised to 80°C and kept warm for 1 hour. After the insulation is completed, 31% hydrochloric acid is added to remove impurities and the material is discharged to the oxidation kettle;

[0015] S20: Oxidation reaction

[0016] In the oxidation kettle, add a certain amount of hydrolyzate, add a certain amount of sodium hypochlorite solution at 55°C and normal pressure, and keep warm for 2 hours. After the end of the heat preservation, discharge the material into the cyclization kettle;

[0017] S30: Cyclization reaction

[0018] In the cyclization kettle, add a certain amount of oxidation liquid, slowly add a certain amount of 31% hydrochloric acid, stir for 1 hour after adding, heat to 50-70℃, transfer sulfur card to the cyclization kettle, and continuously add a certain amount of 31% hydrochloric acid at the same time, keep warm for 1 hour;

[0019] S40: The material is discharged to the washing kettle through a circulation pump, water is added for rinsing, the material is unloaded to a transfer tank, and then discharged to a centrifuge and a vacuum rake dryer for drying. After drying, the material is transferred to a mixer for packaging.

[0020] Compared with the prior art, the present invention has the following advantages: (1) stirring treatment can be carried out at each stage through the actuator, with high execution efficiency and convenient subsequent maintenance. At the target stirring position, the stirring shaft is extended to the hydrolysis kettle, oxidation kettle and cyclization kettle to carry out stirring treatment in sequence; (2) the materials can be transmitted in sequence through the docking transmission mechanism, which is a telescopic docking type, replacing the fixed connection type and the external transmission method, which is convenient for subsequent maintenance; the telescopic control electric cylinder controls the movement of the docking tube, the telescopic connecting pipe can be telescoped, the docking tube is docked with the valve docking part on the electromagnetic control valve, and then sealed and fixed by the fixing mechanism; (3) before the stirring treatment of each stage begins, the stirring shaft can be cleaned, that is, the deflection plate is controlled by the deflection motor to deflect to the position of the cleaning member, and the stirring shaft is controlled to extend into the cleaning tube. Through the operation of the adsorption control box, the adsorption part adsorbs and cleans the surface of the stirring shaft, that is, removes the attached materials; (4) The hydrolysis kettle, oxidation kettle, and cyclization kettle can be maintained and the inside of the telescopic connecting pipe can be cleaned. Specifically, the steering ring is deflected to the cleaning area, that is, the fixing mechanism is not in a docking state, and the operator can easily clean the inside of the telescopic connecting pipe; (5) The scraping ring contacts the inner wall of the hydrolysis kettle, oxidation kettle, and cyclization kettle to achieve the scraping operation. The bottom plate can be controlled by controlling the oil cylinder to move and achieve separation from the hydrolysis kettle, oxidation kettle, and cyclization kettle, which is convenient for the cleaning operation; (6) After each stage of reaction, the corrosion of the inner wall of the hydrolysis kettle, oxidation kettle, and cyclization kettle is inspected. Specifically, the inspection part is transferred, that is, transferred to the hydrolysis kettle, oxidation kettle, and cyclization kettle, and its inner wall surface is inspected by the inspection instrument. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0022] Figure 2 It is a schematic diagram of the overall structure of the present invention from another angle.

[0023] Figure 3 It is a schematic diagram of the installation structure on the deflection plate of the present invention.

[0024] Figure 4 It is a schematic diagram of the installation structure on the turntable of the present invention.

[0025] Figure 5 It is a schematic diagram of the stirring shaft structure of the present invention.

[0026] Figure 6 It is a schematic diagram of the installation structure of the scraping member and the inspection member of the present invention.

[0027] Figure 7 It is a schematic diagram of the installation structure of the hydrolysis kettle, oxidation kettle and cyclization kettle of the present invention.

[0028] Figure 8This is a schematic diagram of the structure of the turntable of the present invention.

[0029] Fig. 9 It is a schematic diagram of the structure of the docking transmission mechanism of the present invention.

[0030] Fig.10 It is a schematic diagram of the installation structure of the turning ring of the present invention.

[0031] Fig.11 It is a schematic diagram of the installation structure of the fixing mechanism of the present invention.

[0032] Fig.12 It is a schematic diagram of the internal structure of the oxidation kettle of the present invention.

[0033] Fig.13 It is a schematic diagram of the control mechanism structure of the present invention.

[0034] Fig.14 It is a schematic diagram of the installation structure of the electromagnetic control valve and the docking transmission mechanism of the present invention.

[0035] Figure numerals: 1-base; 2-bracket; 3-hydrolysis kettle; 4-oxidation kettle; 5-cyclization kettle; 6-steam chuck; 7-steam transmission box; 8-moving belt; 9-moving motor; 10-moving frame; 11-deflection motor; 12-support plate; 1201-magnetic seat; 1202-scraping ring; 1203-inspection seat; 1204-inspection instrument; 1205-fixed electric cylinder; 1206-magnetic hole; 13-adsorption control box; 14-clearing cylinder; 15-adsorption part; 16-deflection plate; 17-extension motor; 18-extension screw rod; 19-extension guide rod; 20-extension seat; 21-stirring motor; 22-stirring gear; 23-mounting table; 24-turntable; 25-screw motor; 26-connection guide rod; 27-transfer screw rod; 28-stirring shaft; 2801 -transfer hole; 29-control oil cylinder; 30-bottom plate; 31-control panel; 32-exhaust valve; 33-electromagnetic fixing rod; 34-matching turntable; 3401-jack; 35-baffle; 36-blocking motor; 37-steering motor; 38-steering gear; 39-steering ring; 40-telescopic control electric cylinder; 41-transmission pump; 42-telescopic connecting pipe; 4201-docking tube; 43-fixed gear; 44-fixed motor; 45-control gear ring; 46-top plate motor; 47-top plate; 48-pressure plate; 49-fixed shaft; 50-spring; 51-gear ring; 52-control release tube; 53-connecting gear; 54-torsion spring; 55-control rotating part; 56-release control motor; 57-release control gear; 58-electromagnetic control valve; 59-valve docking part. DETAILED DESCRIPTION

[0036] Example: Figures 1 to 14As shown, a bracket 2 is provided on one side of the base 1, and a hydrolysis kettle 3, an oxidation kettle 4, and a cyclization kettle 5 are provided on the base 1; electromagnetic control valves 58 are provided on the outer sides of the hydrolysis kettle 3 and the cyclization kettle 5 for material transportation; a docking transmission mechanism is provided on the outer side of the oxidation kettle 4, and the docking transmission mechanism includes a steering ring 39 rotatably mounted on the oxidation kettle 4, and a transmission pump 41 is provided on the steering ring 39, and a telescopic connecting pipe 42 is connected to the transmission pump 41, and a fixing mechanism is provided at the end of the telescopic connecting pipe 42, and the fixing mechanism is sealed and docked with the electromagnetic control valves 58 on the hydrolysis kettle 3 and the cyclization kettle 5 to transmit materials; Discharge holes are symmetrically provided on both sides of the oxidation kettle 4, and a control mechanism is provided on the inner side of the oxidation kettle 4 and at the discharge hole to control the release of the material; the material undergoes a hydrolysis reaction in the hydrolysis kettle 3, is transmitted to the oxidation kettle 4 through a docking transmission mechanism for an oxidation reaction, and then is transmitted to the cyclization kettle 5 for a cyclization reaction; an actuator is provided on the bracket 2, and the actuator includes a mounting frame slidably mounted on the bracket 2, a deflection plate 16 is rotatably provided on the mounting frame, and a scraper, an inspection member and a cleaning member are also provided on the mounting frame in sequence; a stirring shaft 28 is telescopically provided on the deflection plate 16 for stirring treatment.

[0037] The hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5 are all provided with a top plate motor 46 and a top plate 47, and the top plate motor 46 is used to drive the top plate 47 to rotate for capping; the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5 are also provided with a control panel 31 and an air outlet valve 32; a bottom plate 30 is provided at the bottom of the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5, and a control cylinder 29 is provided on the base 1, and the control cylinder 29 is used to control the movement of the bottom plate 30; a steam transmission box 7 is provided on one side of the base 1 for transmitting steam; the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5 are respectively provided with steam chucks 6, the steam chuck 6 is connected to the steam transmission box 7 for temperature regulation; a matching turntable 34 is rotatably arranged on the top plate 47, a socket 3401 is opened on the matching turntable 34, and a blocking motor 36 is arranged on the matching turntable 34, and a baffle 35 is arranged on the output shaft of the blocking motor 36, and the baffle 35 is used to block the socket 3401; an electromagnetic fixing rod 33 is arranged on the top plate 47 and located on the outside of the matching turntable 34, which is used to fix the matching turntable 34; the stirring shaft 28 on the actuator passes through the socket 3401 and enters the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5 for stirring treatment.

[0038] The actuator includes a moving belt 8 and a moving motor 9 arranged on the bracket 2, the moving motor 9 is used to drive the moving belt 8, the moving belt 8 is used to control the movement of the mounting frame, the mounting frame includes a moving frame 10 attached to the moving belt 8, a support plate 12 is arranged on the top of the moving frame 10, and a deflection motor 11 is arranged on the moving frame 10, and the deflection motor 11 is used to drive the deflection plate 16; the scraping member, the inspection member and the cleaning member are respectively arranged on the support plate 12; the deflection plate 16 is provided with an extension motor 17, the output shaft of the extension motor 17 is provided with a belt structure, and an extension screw rod 18 and an extension guide rod 19 are movably arranged on the deflection plate 16, and the extension screw rod 18, the extension guide rod 19 and the extension guide rod 19 are movably arranged on the deflection plate 16, and the extension screw rod 18, the extension guide rod 19 and the extension guide rod 19 are movably arranged on the deflection plate 16. The end of the extension guide rod 19 is connected to an extension seat 20, the belt structure on the output shaft of the extension motor 17 and the extension screw rod 18 form a spiral pair, a mounting platform 23 is provided on the extension seat 20, a turntable 24 is rotatably mounted on the mounting platform 23, a stirring motor 21 is also fixedly arranged on the mounting platform 23, a stirring gear 22 is arranged on the output shaft of the stirring motor 21, and the stirring gear 22 is meshed with the turntable 24; a connecting guide rod 26 is fixedly arranged on the turntable 24, and a transfer screw rod 27 is rotatably arranged, a screw motor 25 is arranged on the top of the connecting guide rod 26, and the screw motor 25 is used to drive the transfer screw rod 27; a stirring shaft 28 is slidably connected to the connecting guide rod 26, and the stirring shaft The top of the stirring shaft 28 and the transfer screw 27 form a spiral pair; a transfer hole 2801 is provided at the bottom of the stirring shaft 28, and the transfer hole 2801 is respectively fixed with the scraper and the inspection member to drive the scraper and the inspection member to extend into the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5; the stirring shaft 28 extends into the cleaning member to perform cleaning treatment; the cleaning member includes an adsorption control box 13 and a cleaning cylinder 14 arranged on the support plate 12, and an adsorption part 15 is arranged inside the cleaning cylinder 14, and an adsorption hole is opened on the adsorption part 15, and the adsorption control box 13 is connected with the adsorption part 15, and the stirring shaft 28 extends through the adsorption hole on the adsorption part 15 to perform adsorption treatment on the surface of the stirring shaft 28 ; The scraping part includes a scraping ring 1202, and the inspection part includes an inspection seat 1203. An inspection instrument 1204 is arranged on the outer side of the inspection seat 1203; The scraping ring 1202 and the inspection seat 1203 are both provided with magnetic holes 1206, and a magnetic seat 1201 is provided on the support plate 12, and the magnetic seat 1201 cooperates with the magnetic hole 1206 for magnetic fixation; A fixed electric cylinder 1205 is provided on the scraping ring 1202 and the inspection seat 1203, and matching holes are opened on the scraping ring 1202 and the inspection seat 1203, and the stirring shaft 28 is docked with the matching hole, and the telescopic rod of the fixed electric cylinder 1205 cooperates with the transfer hole 2801 for fixation.

[0039] The docking transmission mechanism includes a steering motor 37 arranged on the oxidation kettle 4, and a steering gear 38 is arranged on the output shaft of the steering motor 37, and the steering gear 38 is meshed with a steering ring 39; a telescopic control electric cylinder 40 is arranged on the steering ring 39, and the telescopic control electric cylinder 40 is used to control the movement of the fixing mechanism; the fixing mechanism includes a docking tube 4201 connected to the telescopic connecting pipe 42, and the docking tube 4201 is connected to the telescopic rod of the telescopic control electric cylinder 40; a fixed motor 44 is arranged on the docking tube 4201, and a fixed gear 43 is arranged on the output shaft of the fixed motor 44, and a control gear 43 is rotatably installed on the docking tube 4201. The gear ring 45 controls the gear ring 45 to mesh with the fixed gear 43; a fixed shaft 49 is telescopically arranged on the docking tube 4201, and a spring 50 is connected between the fixed shaft 49 and the docking tube 4201; a pressure plate 48 is arranged on the end face of the control gear ring 45, and the pressure plate 48 contacts the end of the fixed shaft 49 to push the fixed shaft 49 to move; a spring 50 is arranged on the electromagnetic control valve 58, and a fixing hole is arranged on the valve docking part 59, and the fixing hole is docked with the fixed shaft 49 for fixing, and a sealing ring is arranged on the inner side of the valve docking part 59, and the valve docking part 59 is docked with the docking tube 4201 for sealing.

[0040] The control mechanism includes a ring gear 51 rotatably mounted on the inner side of the oxidation kettle 4, an incomplete gear portion is arranged on the ring gear 51, and a release control motor 56 is arranged on the inner side of the oxidation kettle 4, a release control gear 57 is arranged on the output shaft of the release control motor 56, and the release control gear 57 is meshed with the ring gear 51; a control release cylinder 52 is arranged on the inner side of the oxidation kettle 4 and at the discharge hole, the control release cylinder 52 is connected to the discharge hole, a control rotating part 55 is rotatably mounted inside the control release cylinder 52, and a torsion spring 54 is connected between the top of the control rotating part 55 and the control release cylinder 52; a connecting gear 53 is arranged at the bottom of the control rotating part 55, and the connecting gear 53 is meshed with the ring gear 51.

[0041] A preparation process of triazone, using 95% dichloropinacolone and 50% sodium hydroxide as starting main raw materials, the production process mainly consists of hydrolysis, oxidation, cyclization and other reactions, and has the following steps:

[0042] S10: Hydrolysis reaction

[0043] The hydrolysis kettle 3 is kept at room temperature, and a certain amount of 50% sodium hydroxide and a certain amount of 95% dichloropinacolone are dripped from the metering tank. The jacket is heated to 60°C by steam, and the mixture is stirred and kept warm for 3 hours. The mixture is then heated to 80°C and kept warm for 1 hour. After the heat preservation is completed, 31% hydrochloric acid is added to remove impurities, and the mixture is discharged to the oxidation kettle 4.

[0044] S20: Oxidation reaction

[0045] In the oxidation kettle 4, add a certain amount of hydrolyzate, add a certain amount of sodium hypochlorite solution at 55°C and normal pressure, add the sodium hypochlorite solution dropwise, keep warm for 2 hours, and discharge the solution to the cyclization kettle 5 after the end of the heat preservation;

[0046] S30: Cyclization reaction

[0047] In the cyclization kettle 5, add a certain amount of oxidation liquid, slowly add a certain amount of 31% hydrochloric acid, stir for 1 hour after adding, heat to 50-70°C, transfer sulfur card to the cyclization kettle 5, and continuously add a certain amount of 31% hydrochloric acid at the same time, and keep warm for 1 hour;

[0048] S40: The material is discharged to the washing kettle through a circulation pump, water is added for rinsing, the material is unloaded to a transfer tank, and then discharged to a centrifuge and a vacuum rake dryer for drying. After drying, the material is transferred to a mixer for packaging.

[0049] The specific working principle is as follows: the main raw materials are added into the hydrolysis kettle 3, the top plate motor 46 can control the opening and closing of the top plate 47, and the steam is transmitted to the steam chuck 6 through the steam transmission box 7, so that the temperature can be adjusted; during stirring, the moving motor 9 can be operated, and the moving belt 8 can drive the moving frame 10 to move. At the target stirring position, the extension motor 17 can be operated to extend the screw rod 18 and the extension guide rod 19, that is, the mounting platform 23 is moved to the top of the hydrolysis kettle 3, and the baffle 35 can be controlled to move by the blocking motor 36, that is, the socket 3401 is exposed, and the electromagnetic fixing rod 33 releases the pressing fixation of the mating turntable 34, and then the screw motor 25 works to rotate the transfer screw 27 to move the stirring shaft 28, and the stirring shaft 28 extends into the hydrolysis kettle 3, and the stirring motor 21 works to rotate the turntable 24, and then the stirring shaft 28 rotates to carry out stirring treatment.

[0050] After the first stage reaction is completed, the material is transferred through the docking transmission mechanism. Specifically, the telescopic control electric cylinder 40 controls the movement of the docking tube 4201, and the telescopic connecting tube 42 can be extended and retracted. The docking tube 4201 is docked with the valve docking part 59 on the electromagnetic control valve 58. The fixed motor 44 is operated to rotate the control gear ring 45, and then the pressure plate 48 pushes the fixed shaft 49, and the fixed shaft 49 cooperates with the fixed hole on the valve docking part 59 to perform sealing and fixing. At this time, the electromagnetic control valve 58 controls the release of the material, and the transmission pump 41 pumps the material, that is, pumps the material into the oxidation kettle 4. Specifically, in the oxidation kettle 4, the release control motor 56 is operated, and the gear ring 51 rotates, so that the control rotating part 55 on one side rotates, that is, the transmission hole on the control rotating part 55 is connected with the transmission hole on the control release tube 52 to transfer the material, and the control rotating part 55 on the other side is in a blocked state. The rotation of the gear ring 51 can be controlled to rotate on both sides to perform unilateral transmission control of the material.

[0051] In the oxidation kettle 4, the material can be stirred through the above steps. After the reaction is completed, the steering ring 39 is rotated by the steering motor 37, that is, the fixing mechanism is directed toward the cyclization kettle 5. Through the above process, the fixing mechanism and the electromagnetic control valve 58 on the cyclization kettle 5 are sealed and matched to transfer the material to the cyclization kettle 5, and then the corresponding stirring treatment is carried out; before the stirring treatment of each stage begins, the stirring shaft 28 can be cleaned, that is, the deflection plate 16 is controlled by the deflection motor 11 to deflect to the position of the cleaning member, and the stirring shaft 28 is controlled to extend into the cleaning cylinder 14. The adsorption control box 13 works, and the adsorption part 15 adsorbs and cleans the surface of the stirring shaft 28, that is, removes the attached material.

[0052] Subsequently, the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5 can be maintained, and the inside of the telescopic connecting pipe 42 can be cleaned. Specifically, the steering ring 39 is deflected to the cleaning area, that is, the fixing mechanism is not in a docking state, and the operator can easily clean the inside of the telescopic connecting pipe 42; for the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5, the deflection plate 16 can be controlled to deflect to the position of the scraper, the stirring shaft 28 is matched with the matching hole, and the telescopic rod of the fixed electric cylinder 1205 is matched with the transfer hole 2801 for fixing, and the magnetic seat 1201 releases the adsorption of the magnetic hole 1206, which can drive the scraper The movable part moves, and the scraping part is transferred to the inner side of the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5. The scraper ring 1202 contacts the inner wall thereof to realize the scraping operation. The bottom plate 30 can be controlled to move by controlling the oil cylinder 29 to realize the separation from the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5, so as to facilitate the cleaning operation. For the inspection operation, after each stage of reaction, it is necessary to inspect the corrosion of the inner wall of the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5. Specifically, through the above operation, the inspection part is transferred, that is, transferred to the hydrolysis kettle 3, the oxidation kettle 4, and the cyclization kettle 5, and the inner wall surface is inspected by the inspection instrument 1204.

Claims

1. A triazone preparation device, comprising a base (1), a support (2) being provided on one side of the base (1), characterized in that: A hydrolysis kettle (3), an oxidation kettle (4), and a cyclization kettle (5) are arranged on the base (1); electromagnetic control valves (58) are arranged on the outside of the hydrolysis kettle (3) and the cyclization kettle (5) for material transportation; a docking transmission mechanism is arranged on the outside of the oxidation kettle (4), the docking transmission mechanism comprises a steering ring (39) rotatably mounted on the oxidation kettle (4), a transmission pump (41) is arranged on the steering ring (39), a telescopic connecting pipe (42) is connected to the transmission pump (41), and a fixing mechanism is arranged at the end of the telescopic connecting pipe (42), and the fixing mechanism is sealed and docked with the electromagnetic control valves (58) on the hydrolysis kettle (3) and the cyclization kettle (5) to transmit materials; Discharge holes are symmetrically provided on both sides of the oxidation kettle (4), and a control mechanism is provided inside the oxidation kettle (4) and at the discharge hole to control the release of the material; the material undergoes a hydrolysis reaction in the hydrolysis kettle (3), is transmitted to the oxidation kettle (4) through a docking transmission mechanism to undergo an oxidation reaction, and then is transmitted to the cyclization kettle (5) to undergo a cyclization reaction; an actuator is provided on the bracket (2), the actuator comprising a mounting frame slidably mounted on the bracket (2), a deflection plate (16) is rotatably provided on the mounting frame, and a scraper, an inspection member and a cleaning member are also provided on the mounting frame in sequence; a stirring shaft (28) is telescopically provided on the deflection plate (16) for stirring treatment.

2. A triazone preparation device according to claim 1, characterized in that: The hydrolysis kettle (3), oxidation kettle (4) and cyclization kettle (5) are all provided with a top plate motor (46) and a top plate (47), and the top plate motor (46) is used to drive the top plate (47) to rotate for sealing; the hydrolysis kettle (3), oxidation kettle (4) and cyclization kettle (5) are also provided with a control panel (31) and an air outlet valve (32); a bottom plate (30) is provided at the bottom of the hydrolysis kettle (3), oxidation kettle (4) and cyclization kettle (5), and a control oil cylinder (29) is provided on the base (1), and the control oil cylinder (29) is used to control the movement of the bottom plate (30); a steam transmission box (7) is provided on one side of the base (1) for transmitting steam; the hydrolysis kettle (3), oxidation kettle (4) and cyclization kettle (5) are respectively provided with a steam chuck (6), and the steam chuck (6) is connected to the steam transmission box (7) for temperature regulation.

3. A triazone preparation device according to claim 2, characterized in that: A matching turntable (34) is rotatably arranged on the top plate (47), a socket (3401) is provided on the matching turntable (34), a blocking motor (36) is arranged on the matching turntable (34), a baffle (35) is arranged on the output shaft of the blocking motor (36), and the baffle (35) is used to block the socket (3401); an electromagnetic fixing rod (33) is arranged on the top plate (47) and located outside the matching turntable (34), and is used to fix the matching turntable (34); a stirring shaft (28) on the actuator passes through the socket (3401) and enters the hydrolysis kettle (3), the oxidation kettle (4), and the cyclization kettle (5) to perform stirring treatment.

4. A triazone preparation device according to claim 3, characterized in that: The actuator comprises a moving belt (8) and a moving motor (9) arranged on a bracket (2); the moving motor (9) is used to drive the moving belt (8); the moving belt (8) is used to control the movement of a mounting frame; the mounting frame comprises a moving frame (10) attached to the moving belt (8); a support plate (12) is arranged on the top of the moving frame (10); a deflection motor (11) is arranged on the moving frame (10); the deflection motor (11) is used to drive the deflection plate (16); and a scraping member, an inspection member and a cleaning member are respectively arranged on the support plate (12).

5. A triazone preparation device according to claim 4, characterized in that: The deflection plate (16) is provided with an extension motor (17), the output shaft of the extension motor (17) is provided with a belt structure, and an extension screw rod (18) and an extension guide rod (19) are movably provided on the deflection plate (16), the ends of the extension screw rod (18) and the extension guide rod (19) are connected to an extension seat (20), the belt structure on the output shaft of the extension motor (17) and the extension screw rod (18) form a spiral pair, the extension seat (20) is provided with a mounting platform (23), a turntable (24) is rotatably mounted on the mounting platform (23), a stirring motor (21) is also fixedly provided on the mounting platform (23), a stirring gear (22) is provided on the output shaft of the stirring motor (21), and the stirring gear (22) and the turntable (24) are connected to each other. 4) engagement; a connecting guide rod (26) is fixedly arranged on the turntable (24), and a transfer screw rod (27) is rotatably arranged, a screw motor (25) is arranged on the top of the connecting guide rod (26), and the screw motor (25) is used to drive the transfer screw rod (27); the stirring shaft (28) is slidably connected to the connecting guide rod (26), and the top of the stirring shaft (28) and the transfer screw rod (27) form a spiral pair; a transfer hole (2801) is opened at the bottom of the stirring shaft (28), and the transfer hole (2801) is respectively fixed with a scraper and an inspection member to drive the scraper and the inspection member to extend into the hydrolysis kettle (3), the oxidation kettle (4), and the cyclization kettle (5); the stirring shaft (28) extends into the cleaning member to perform cleaning treatment.

6. A triazone preparation device according to claim 5, characterized in that: The cleaning member comprises an adsorption control box (13) and a cleaning cylinder (14) arranged on the support plate (12); an adsorption portion (15) is arranged inside the cleaning cylinder (14); an adsorption hole is provided on the adsorption portion (15); the adsorption control box (13) is connected to the adsorption portion (15); the stirring shaft (28) extends through the adsorption hole on the adsorption portion (15) to perform adsorption treatment on the surface of the stirring shaft (28); the scraping member comprises a scraping ring (1202); the inspection member comprises an inspection seat (1203); an inspection instrument (1204) is arranged on the outer side of the inspection seat (1203); the scraping ring (1202) is connected to the adsorption portion (15); the inspection member comprises an inspection seat (1203); an inspection instrument (1204) is arranged on the outer side of the inspection seat (1203); the scraping ring (1202) is connected to the adsorption portion (15); the inspection member comprises an inspection seat (1203); the inspection device (1204) is arranged on the outer side of the inspection seat (1203); the scraping ring (1202) is connected to the adsorption portion (15 ... adsorption hole is provided on the adsorption portion (15); the adsorption control box (13) is connected to the adsorption portion (15); the adsorption hole is provided on the adsorption portion (15); the adsorption control box (13) is 02) and the inspection seat (1203) are both provided with magnetic holes (1206), a magnetic seat (1201) is provided on the support plate (12), and the magnetic seat (1201) cooperates with the magnetic hole (1206) to perform magnetic fixation; a fixed electric cylinder (1205) is provided on the scraper ring (1202) and the inspection seat (1203), and matching holes are opened on the scraper ring (1202) and the inspection seat (1203), the stirring shaft (28) is docked with the matching hole, and the telescopic rod of the fixed electric cylinder (1205) cooperates with the transfer hole (2801) to perform fixation.

7. The preparation device of triazone according to claim 1, characterized in that: The docking transmission mechanism comprises a steering motor (37) arranged on the oxidation kettle (4), a steering gear (38) being arranged on the output shaft of the steering motor (37), and the steering gear (38) being meshed with a steering ring (39); a telescopic control electric cylinder (40) being arranged on the steering ring (39), and the telescopic control electric cylinder (40) being used to control the movement of the fixing mechanism; the fixing mechanism comprises a docking sleeve (4201) connected to the telescopic connecting pipe (42), and the docking sleeve (4201) is connected to the telescopic rod of the telescopic control electric cylinder (40); a fixing motor (44) is arranged on the docking sleeve (4201), a fixing gear (43) being arranged on the output shaft of the fixing motor (44), and a control gear (43) being rotatably mounted on the docking sleeve (4201). A ring (45) is provided, the control gear ring (45) is meshed with the fixed gear (43); a fixed shaft (49) is telescopically arranged on the docking tube (4201), and a spring (50) is connected between the fixed shaft (49) and the docking tube (4201); a pressure plate (48) is provided on the end surface of the control gear ring (45), and the pressure plate (48) contacts the end of the fixed shaft (49) to push the fixed shaft (49) to move; a spring (50) is provided on the electromagnetic control valve (58), and a fixing hole is provided on the valve docking part (59), and the fixing hole is docked with the fixed shaft (49) for fixing, and a sealing ring is provided on the inner side of the valve docking part (59), and the valve docking part (59) is docked with the docking tube (4201) for sealing.

8. The preparation device of triazone according to claim 1, characterized in that: The control mechanism comprises a gear ring (51) rotatably mounted on the inner side of the oxidation kettle (4), an incomplete gear portion being arranged on the gear ring (51), and a release control motor (56) being arranged on the inner side of the oxidation kettle (4), a release control gear (57) being arranged on the output shaft of the release control motor (56), and the release control gear (57) being meshed with the gear ring (51); a control release cylinder (52) being arranged on the inner side of the oxidation kettle (4) and at the discharge hole, the control release cylinder (52) being connected with the discharge hole, a control rotating portion (55) being rotatably mounted inside the control release cylinder (52), a torsion spring (54) being connected between the top of the control rotating portion (55) and the control release cylinder (52); and a connecting gear (53) being arranged at the bottom of the control rotating portion (55), and the connecting gear (53) being meshed with the gear ring (51).

9. A process for preparing triazone, using 95% dichloropinacolone and 50% sodium hydroxide as the starting main raw materials, the production process mainly consists of hydrolysis, oxidation, cyclization and other reactions; characterized in that: The following steps are required: S10: Hydrolysis reaction The hydrolysis kettle (3) is kept at room temperature, and a certain amount of 50% sodium hydroxide and a certain amount of 95% dichloropinacolone are dripped into the measuring tank, and the jacket is heated to 60°C by steam, and the mixture is stirred evenly and kept warm for 3 hours, and then the temperature is raised to 80°C and kept warm for 1 hour. After the heat preservation is completed, 31% hydrochloric acid is added to remove impurities, and then the mixture is discharged to the oxidation kettle (4); S20: Oxidation reaction In the oxidation kettle (4), add a certain amount of hydrolyzate, add a certain amount of sodium hypochlorite solution at 55°C and normal pressure, add the sodium hypochlorite solution dropwise, keep warm for 2 hours, and discharge the solution to the cyclization kettle (5) after the end of the heat preservation; S30: Cyclization reaction In the cyclization kettle (5), add a certain amount of oxidation liquid, slowly add a certain amount of 31% hydrochloric acid, stir for 1 hour after adding, raise the temperature to 50-70°C, transfer the sulfur card to the cyclization kettle (5), and continuously add a certain amount of 31% hydrochloric acid at the same time, and keep warm for 1 hour; S40: The material is discharged to the washing kettle through a circulation pump, water is added for rinsing, the material is unloaded to a transfer tank, and then discharged to a centrifuge and a vacuum rake dryer for drying. After drying, the material is transferred to a mixer for packaging.

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