Production device of 2-methylsulfonyl-5-trifluoromethyl-1, 3, 4-thiadiazole

Abstract

The utility model discloses a production device of 2-methylsulfonyl-5-trifluoromethyl-1, 3, 4-thiadiazole, and belongs to the technical field of herbicide intermediate production devices. Comprising a kettle body, a material injection assembly and a filtrate assembly, wherein a kettle cover is fixed at the top of the kettle body; a first feeding flange and a second feeding flange are arranged on the kettle cover, a driving motor is fixed in the center of the kettle cover, and the driving motor is connected to a stirring paddle on the inner side of the kettle body through a coupler; the material injection assembly is composed of two material injection units, each material injection unit comprises a bent pipe flange, and one end of each bent pipe flange is connected to a first feeding flange or a second feeding flange. The other ends of the two bent pipe flanges are connected to a first feeding main pipe or a second feeding main pipe; according to the production device of the 2-methylsulfonyl-5-trifluoromethyl-1, 3, 4-thiadiazole, disclosed by the utility model, the front-end reaction can be completed in one kettle body, so that a front-end product of the 2-methylsulfonyl-5-trifluoromethyl-1, 3, 4-thiadiazole is obtained.

Description

Technical Field

[0001] The utility model specifically relates to a production device for 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole, belonging to the technical field of herbicide intermediate production devices. Background Art

[0002] 2-Methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole is an intermediate in the synthesis of flufenacet and is the step with the lowest yield. The production equipment of 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole in the traditional original process has low production efficiency, and the production process is divided into multiple stages of production, which reduces the continuity of production, and the final yield of the product is not high, which is not suitable for large-scale industrial production applications. Therefore, Chinese Patent Publication No.: CN216137204U discloses a production device for 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole, including a primary reactor, a separation device, a secondary reactor, a primary distillation tower, a secondary distillation tower, a tertiary reactor and other structures. The device can improve the production efficiency, but when the front end of the device reacts, the reaction material flow needs to pass through multiple reactors. During the flow process, solid material is easily trapped, which affects the subsequent reaction, thereby reducing the product yield, and multiple reactors and reaction tube groups need to be configured. Utility Model Content

[0003] In order to solve the above problems, the utility model proposes a production device for 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole, which can complete the front-end reaction in a kettle to obtain the front-end product of 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole.

[0004] The utility model discloses a production device for 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole, comprising:

[0005] A kettle body, wherein a temperature control jacket is arranged on the outside of the kettle body, and a kettle cover is fixed on the top of the kettle body; a first feed flange and a second feed flange are arranged on the kettle cover, and a drive motor is fixed at the center of the kettle cover, and the drive motor is connected to a stirring paddle inside the kettle body through a coupling; the kettle body is equipped with a temperature control jacket and a stirring paddle, which can realize reaction temperature control and mixed stirring, and the first feed flange on the kettle cover can realize the feeding of a primary reaction component, and the second feed flange can realize the feeding of a secondary reaction component;

[0006] Injection assembly, the injection assembly includes two groups of injection units, the two groups of injection units each include an elbow flange, one end of the two elbow flanges is connected to the first feed flange or the second feed flange; the other end of the two elbow flanges is connected to the first feed main pipe or the second feed main pipe; a dripping pipe is provided through the top of the outer side of the elbow flange, a plurality of flow channels are provided inside the dripping pipe, and a dripping liquid inlet flange is screwed on the top surface of each flow channel; the dripping liquid inlet flange is used to feed the reaction liquid that needs to be continuously dripped for a long time into the kettle body, and the first feed main pipe or the second feed main pipe completes the feeding of the primary reaction component and the feeding of the secondary reaction component respectively;

[0007] The filtrate assembly comprises a bottom valve fixed to the bottom of the kettle body, a side pipe seat is arranged above the bottom valve, an annular groove is opened on the inner side of the side pipe seat, a filter plate is arranged on the inner side of the annular groove, and a drain valve is screwed on the inner side of the side pipe seat; the drain valve is tightly pressed against the filter plate; the filter plate is pressed between the annular groove and the drain valve, and when the filter plate needs to be replaced and cleaned, the filter plate can be taken out by screwing down the drain valve; the filter plate discharges the filtrate separated by solid and liquid through the drain valve, and the bottom valve can inject the reaction liquid that has completed the secondary reaction into the next processing flow.

[0008] Furthermore, the first material supply main pipe is connected to the first three-way valve through a first flow meter, and the other two ends of the first three-way valve are respectively connected to the first storage tank and the second storage tank; the second material supply main pipe is connected to the second three-way valve through a second flow meter, and the other two ends of the second three-way valve are respectively connected to the third storage tank and the fourth storage tank.

[0009] Furthermore, the dripping liquid inlet flange is connected to the switch valve through a dripping valve, and the switch valve is connected to a high-position dripping liquid storage tank; the dripping liquid storage tank is connected to the liquid replenishing tank through a metering valve; the liquid replenishing tank injects a certain amount of dripping liquid into the dripping liquid storage tank through the metering valve, and then when the kettle body reacts, the switch valve is opened, and the dripping liquid is continuously fed into a certain flow channel in the dripping tube through the dripping valve and the dripping liquid inlet flange, and then the dripping liquid enters the kettle body to participate in the reaction.

[0010] During operation, after hydrazine hydrate and water are fully mixed in the first storage tank, a certain amount of premixed liquid is injected into the kettle body through the first three-way valve, the first flowmeter and the first feeding pipe; then, the toluene in the second storage tank is injected into the kettle body through the first three-way valve, the first flowmeter and the first feeding pipe, and mixed with the premixed liquid, and the first three-way valve is closed. Then, the temperature control jacket is opened, and the premixed liquid in the kettle body reacts under temperature control and stirring. During the reaction, the switch valve is opened, and the certain amount of carbon disulfide and dimethyl sulfate in the two drip storage tanks enter the drip valves respectively, and carbon disulfide and dimethyl sulfate are continuously injected into the flow channel in the drip pipe through the drip valve; and the reacting premixed liquid is dripped until the reaction time is reached, and the switch valve is closed; then, the drain valve is opened, and the liquid that has completed the reaction in the kettle body enters the drain valve through the filter plate, and is finally collected in the wastewater tank; after the drainage is completed, the drain valve is closed;

[0011] Next, after trifluoroacetic acid and toluene are fully mixed in the third storage tank, the mixed liquid is pumped into the kettle body through the second three-way valve, the second flowmeter and the second feed pipe, and mixed with the crystallized material in the kettle body. Then, the temperature control jacket is opened, and the catalyst in the fourth storage tank is pumped into the kettle body through the second three-way valve, the second flowmeter and the second feed pipe, the drive motor is turned on, and the stirring paddle is driven to fully stir and mix the reaction. When the reaction is connected, the switch valve is opened, and a certain amount of catalyst in the drip storage tank enters the drip valve respectively, and enters the flow channel in the drip pipe through the drip valve, so as to continuously supplement the catalyst to the mixed liquid; until the reaction time is reached, the switch valve is closed; finally, the mixed liquid is pumped into the distillation tower through the bottom valve for distillation, and subsequent reactions are carried out.

[0012] Furthermore, the dropper extends above the stirring paddle, and the dropper can deliver the reaction droplets close to the reaction liquid surface, thereby preventing the droplets from being agitated on the reaction liquid surface or staying on the inner wall of the kettle.

[0013] Furthermore, a spiral tube is integrally formed at the outer top of the elbow flange, and the drip tube is screwed to the spiral tube. The elbow flange and the drip tube can be assembled into one through the spiral tube, thereby realizing the assembly of the injection unit to the first feed flange or the second feed flange; the injection unit is convenient for disassembly and cleaning.

[0014] Compared with the prior art, the production device of 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole of the utility model can continuously inject quantitative reaction components into the kettle body, and can realize solid-liquid separation for waste discharge. After the waste discharge is completed, the secondary reaction continues, and the front-end reaction can be completed in one kettle body, so that the front-end reaction product of 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole is prepared by a one-pot method. The front-end reaction product is a flowing mixed liquid, and the highly fluid mixed liquid can smoothly enter the distillation tower for distillation and carry out subsequent reactions. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a schematic diagram of the overall structure of the utility model.

[0016] Figure 2 For the utility model Figure 1 Schematic diagram of the local enlarged structure at point A in the middle.

[0017] Figure 3 For the utility model Figure 1 Schematic diagram of the local enlarged structure at point B in the middle.

[0018] Figure 4 It is a schematic diagram of the axial cross-section structure of the dropper of the utility model.

[0019] Figure 5 This is a schematic diagram of the structure of the connecting components on the first feed flange of the utility model.

[0020] Figure 6 It is a schematic diagram of the structure of each connecting component on the second feed flange of the utility model.

[0021] Figure numerals: 1, kettle body, 2, temperature control jacket, 3, kettle cover, 4, first feed flange, 5, second feed flange, 6, drive motor, 7, stirring paddle, 8, elbow flange, 9, first feed main pipe, 10, second feed main pipe, 11, dripping pipe, 12, flow channel, 13, dripping inlet flange, 14, bottom valve, 15, side pipe seat, 16, filter plate, 17, drain valve, 18, first flow meter, 19, first three-way valve, 20, first storage tank, 21, second storage tank, 22, second flow meter, 23, second three-way valve, 24, third storage tank, 25, fourth storage tank, 26, dripping valve, 27, switch valve, 28, dripping storage tank, 29, spiral tube. DETAILED DESCRIPTION

[0022] like Figures 1 to 6 The production device of 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole shown comprises:

[0023] A kettle body 1, wherein a temperature control jacket 2 is arranged outside the kettle body 1, and a kettle cover 3 is fixed on the top of the kettle body 1; a first feed flange 4 and a second feed flange 5 are arranged on the kettle cover 3, and a drive motor 6 is fixed at the center of the kettle cover 3, and the drive motor 6 is connected to a stirring paddle 7 inside the kettle body 1 through a coupling; the kettle body 1 is equipped with a temperature control jacket 2 and a stirring paddle 7, which can realize reaction temperature control and mixed stirring, and the first feed flange 4 on the kettle cover 3 can realize the feeding of a primary reaction component, and the second feed flange 5 can realize the feeding of a secondary reaction component;

[0024] Injection assembly, the injection assembly includes two groups of injection units, the two groups of injection units include elbow flanges 8, one end of the two elbow flanges 8 is connected to the first feed flange 4 or the second feed flange 5; the other end of the two elbow flanges 8 is connected to the first supply main pipe 9 or the second supply main pipe 10; a dripping pipe 11 is provided through the top of the outer side of the elbow flange 8, a plurality of flow channels 12 are provided inside the dripping pipe 11, and a dripping liquid inlet flange 13 is screwed on the top surface of each flow channel 12; the dripping liquid inlet flange 13 is used to feed the reaction liquid that needs to be dripped for a long time into the kettle body 1, and the first supply main pipe 9 or the second supply main pipe 10 completes the feeding of the primary reaction component and the feeding of the secondary reaction component respectively;

[0025] The filtrate assembly includes a bottom valve 14 fixed to the bottom of the kettle body 1, a side pipe seat 15 is arranged above the bottom valve 14, an annular groove is opened on the inner side of the side pipe seat 15, a filter plate 16 is arranged on the inner side of the annular groove, and a drain valve 17 is screwed on the inner side of the side pipe seat 15; the drain valve 17 is tightly pressed against the filter plate 16; the filter plate 16 is pressed between the annular groove and the drain valve 17, and when the filter plate 16 needs to be replaced and cleaned, the drain valve 17 only needs to be unscrewed to take out the filter plate 16; the filter plate 16 discharges the filtrate separated by solid and liquid through the drain valve 17, and the bottom valve 14 can inject the reaction liquid that has completed the secondary reaction into the next processing flow.

[0026] The first material supply main pipe 9 is connected to the first three-way valve 19 through the first flowmeter 18, and the other two ends of the first three-way valve 19 are respectively connected to the first storage tank 20 and the second storage tank 21; the second material supply main pipe 10 is connected to the second three-way valve 23 through the second flowmeter 22, and the other two ends of the second three-way valve 23 are respectively connected to the third storage tank 24 and the fourth storage tank 25.

[0027] The dripping liquid inlet flange 13 is connected to the switch valve 27 through the dripping valve 26, and the switch valve 27 is connected to the high-position dripping liquid storage tank 28; the dripping liquid storage tank 28 is connected to the liquid replenishing tank through the metering valve; the liquid replenishing tank injects a certain amount of dripping liquid into the dripping liquid storage tank 28 through the metering valve, and then when the kettle body 1 reacts, the switch valve 27 is opened, and the dripping liquid is continuously fed into a certain flow channel 12 in the dripping tube 11 through the dripping valve 26 and the dripping liquid inlet flange 13, and then the dripping liquid enters the kettle body 1 to participate in the reaction.

[0028] During operation, after hydrazine hydrate and water are fully mixed in the first storage tank 20, a certain amount of premixed liquid is pumped into the kettle body 1 through the first three-way valve 19, the first flowmeter 18 and the first feed pipe 9; then, toluene in the second storage tank 21 is pumped into the kettle body 1 through the first three-way valve 19, the first flowmeter 18 and the first feed pipe 9, and mixed with the premixed liquid, the first three-way valve 19 is closed, and then the temperature control jacket 2 is opened, and the premixed liquid in the kettle body 1 reacts under temperature control and stirring. During the reaction, Open the switch valve 27, and the quantitative carbon disulfide and dimethyl sulfate in the two dripping tanks 28 enter the dripping valve 26 respectively, and the carbon disulfide and dimethyl sulfate are continuously injected into the flow channel 12 in the dripping tube 11 through the dripping valve 26; and the premixed liquid being reacted is dripped until the reaction time is reached, and the switch valve 27 is closed; then, the drain valve 17 is opened, and the liquid that has completed the reaction in the kettle body 1 enters the drain valve 17 through the filter plate 16, and is finally collected in the waste water tank; after the drainage is completed, the drain valve 17 is closed;

[0029] Next, after trifluoroacetic acid and toluene are fully mixed in the third storage tank 24, the mixed liquid is pumped into the kettle body 1 through the second three-way valve 23, the second flowmeter 22 and the second feed pipe 10, and mixed with the crystallized material in the kettle body 1. Then, the temperature control jacket 2 is opened, and the catalyst in the fourth storage tank 25 is pumped into the kettle body 1 through the second three-way valve 23, the second flowmeter 22 and the second feed pipe 10, the drive motor 6 is turned on, and the stirring paddle 7 is driven to fully stir and mix the reaction. When the reaction is connected, the switch valve 27 is opened, and the quantitative catalyst in the drip storage tank 28 enters the drip valve 26 respectively, and enters the flow channel 12 in the drip pipe 11 through the drip valve 26, so as to continuously supplement the catalyst to the mixed liquid; until the reaction time is reached, the switch valve 27 is closed; finally, the mixed liquid is pumped into the distillation tower through the bottom valve 14 for distillation, and subsequent reactions are carried out.

[0030] The dropper 11 extends above the stirring paddle 7 , and can deliver the reaction droplets to a place close to the reaction liquid surface, thereby preventing the droplets from being agitated on the reaction liquid surface or staying on the inner wall of the kettle body 1 .

[0031] The outer top of the elbow flange 8 is integrally formed with a spiral tube 29, and the drip tube 11 is screwed to the spiral tube 29. The elbow flange 8 and the drip tube 11 can be assembled into one through the spiral tube 29, thereby realizing the assembly of the injection unit to the first feed flange 4 or the second feed flange 5; the injection unit is convenient for disassembly and cleaning.

[0032] The above embodiments are only preferred implementations of the present invention, so any equivalent changes or modifications made according to the structures, features and principles described in the scope of application of the present invention are included in the scope of application of the present invention.

Claims

1. A production device for 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole, characterized in that: include: A kettle body, wherein a temperature control jacket is arranged outside the kettle body, and a kettle cover is fixed on the top of the kettle body; a first feed flange and a second feed flange are arranged on the kettle cover, and a driving motor is fixed at the center of the kettle cover, and the driving motor is connected to a stirring paddle inside the kettle body through a coupling; The injection assembly comprises two groups of injection units, each of which comprises an elbow flange, one end of each of the two elbow flanges is connected to the first feed flange or the second feed flange; the other end of each of the two elbow flanges is connected to the first feed main pipe or the second feed main pipe; a dripping pipe is provided through the top of the outer side of the elbow flange, a plurality of flow channels are provided inside the dripping pipe, and a dripping inlet flange is screwed on the top surface of each flow channel; The filtrate assembly comprises a bottom valve fixed to the bottom of the kettle body, a side pipe seat is arranged above the bottom valve, an annular groove is opened on the inner side of the side pipe seat, a filter plate is arranged on the inner side of the annular groove, a drain valve is screwed on the inner side of the side pipe seat; the drain valve is tightly pressed against the filter plate.

2. The production device of 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole according to claim 1, characterized in that: The first material supply main pipe is connected to the first three-way valve through a first flow meter, and the other two ends of the first three-way valve are respectively connected to the first storage tank and the second storage tank; the second material supply main pipe is connected to the second three-way valve through a second flow meter, and the other two ends of the second three-way valve are respectively connected to the third storage tank and the fourth storage tank.

3. The production device of 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole according to claim 1, characterized in that: The dripping liquid inlet flange is connected to the switch valve through a dripping valve, and the switch valve is connected to a high-position dripping liquid storage tank; the dripping liquid storage tank is connected to the liquid replenishing tank through a metering valve.

4. The production device of 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole according to claim 1, characterized in that: The drip tube extends above the stirring paddle.

5. The production device of 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole according to claim 1, characterized in that: A spiral tube is integrally formed on the top of the outer side of the elbow flange, and the drip tube is screwed to the spiral tube.

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