Diflufenican continuous production device

Abstract

The utility model discloses a diflufenican continuous production device which comprises a batching kettle, a metering tank, a continuous etherification tower, a transfer kettle, a recovery kettle, a receiving tank, a flaker and a ton bag, the batching kettle is communicated with a first condenser through a pipeline, a second condenser is arranged on a pipeline between the continuous etherification tower and the transfer kettle, and a third condenser is arranged on a pipeline between the recovery kettle and the receiving tank. According to the continuous etherification device, an amide intermediate and m-trifluoromethylphenol are added through the batching kettle, fully dissolved, stirred and heated, then are introduced into the continuous etherification tower for heating reaction, a catalyst is added through the metering tank for full reaction, reaction liquid is introduced into the transfer kettle for heating and stirring, and the recovered m-trifluoromethylphenol and the catalyst are introduced into the receiving tank. The generated diflufenican is introduced into a flaker to be cooled and flaked and then enters a ton bag to be packaged, continuous production of the diflufenican is achieved, the whole structure is simple, the productivity is high, waste liquid and waste solid cannot be generated, and the production cost is effectively reduced.

Description

TECHNICAL FIELD

[0001] The utility model relates to chemical production equipment technical field, concretely relates to a kind of difenoxuron continuous production device. BACKGROUND

[0002] Difenoxuron belongs to carotenoid biosynthesis inhibitor, the carotenoid content in the plant of being handled plant is reduced, and then chlorophyll is destroyed, cell membrane is broken, and weed shows that sprout is discolored or white;It can form the medicine soil layer of anti-leaching on the table before weed germination, and keep active in the whole growth period of crop;When weed germination, through sprout or root system absorption of reagent finally dies.

[0003] In prior art, mainstream route of preparation difenoxuron is with toluene or xylene as solvent, m-trifluoromethyl phenol is first reacted with potassium hydroxide to form phenolic potassium salt, then etherification reaction with amide intermediate to prepare difenoxuron, this production route will produce a large amount of waste water, waste salt and waste solid, lead to higher production cost. UTILITY MODEL CONTENT

[0004] The utility model aims at: to solve above-mentioned problem, the utility model provides a kind of difenoxuron continuous production device.

[0005] The utility model for realizing above-mentioned purpose specifically adopts following technical scheme, comprising:

[0006] Batching kettle, metering tank, continuous etherification tower, transfer kettle, recovery kettle, receiving tank, flaking machine, ton bag;

[0007] The bottom of the batching kettle and the metering tank are communicated with the bottom of the continuous etherification tower through pipelines, the bottom of the continuous etherification tower is communicated with the top of the transfer kettle through a pipeline, the bottom of the transfer kettle is communicated with the top of the recovery kettle through a pipeline, the bottom of the recovery kettle is communicated with the top of the flaking machine through a pipeline, the top of the recovery kettle is communicated with the top of the receiving tank through a pipeline, the bottom of the receiving tank is communicated with the batching kettle through a pipeline, and the bottom of the flaking machine is communicated with the ton bag through a pipeline.

[0008] The batching kettle is communicated with the first condenser through a pipeline, the second condenser is arranged on the pipeline between the continuous etherification tower and the transfer kettle, and the third condenser is arranged on the pipeline between the recovery kettle and the receiving tank.

[0009] The outer wall of the batching kettle is provided with a first jacket, the outer wall of the continuous etherification tower is provided with a second jacket, the outer wall of the transfer kettle is provided with a third jacket, and the outer wall of the recovery kettle is provided with a fourth jacket.

[0010] As a further description of the above technical scheme, the top of the batching kettle, the metering tank, the continuous etherification tower, the transfer kettle and the recovery kettle is provided with a thermometer on one side and a pressure gauge on the other side, the top of the batching kettle, the transfer kettle and the recovery kettle is provided with a stirring motor, and the stirring motor is connected with a stirring rod.

[0011] As a further description of the above technical scheme, the top of the batching kettle, the metering tank, the continuous etherification tower, the transfer kettle and the recovery kettle is provided with a thermometer on one side and a pressure gauge on the other side, the top of the batching kettle, the transfer kettle and the recovery kettle is provided with a stirring motor, and the stirring motor is connected with a stirring rod.

[0012] As a further description of the above technical scheme, the top of the batching kettle, the metering tank, the continuous etherification tower, the transfer kettle and the recovery kettle is provided with a thermometer on one side and a pressure gauge on the other side, the top of the batching kettle, the transfer kettle and the recovery kettle is provided with a stirring motor, and the stirring motor is connected with a stirring rod.

[0013] As a further description of the above technical scheme, the top of the batching kettle, the metering tank, the continuous etherification tower, the transfer kettle and the recovery kettle is provided with a thermometer on one side and a pressure gauge on the other side, the top of the batching kettle, the transfer kettle and the recovery kettle is provided with a stirring motor, and the stirring motor is connected with a stirring rod.

[0014] As a further description of the above technical scheme, one side of the top of the transfer kettle is provided with a transfer temperature port, the transfer temperature port is connected with the thermometer, the other side of the top of the transfer kettle is provided with a transfer pressure port, the transfer pressure port is connected with the pressure gauge, one side of the transfer temperature port is provided with a transfer feed port, the transfer feed port is communicated with the etherification rising port and the overflow port of the continuous etherification tower through a pipeline, the bottom of the transfer kettle is provided with a transfer discharge port, and the transfer discharge port is communicated with the recovery kettle through a pipeline.

[0015] As a further description of the above technical scheme, one side of the top of the recovery kettle is provided with a recovery temperature port, the recovery temperature port is connected with the thermometer, the other side of the top of the recovery kettle is provided with a recovery pressure port, the recovery pressure port is connected with the pressure gauge, one side of the recovery temperature port is provided with a recovery feed port, the recovery feed port is communicated with the transfer discharge port of the transfer kettle through a pipeline, one side of the recovery pressure port is provided with a recovery rising port, the recovery rising port is communicated with the third condenser through a pipeline, and the bottom of the recovery kettle is provided with a recovery discharge port, and the recovery discharge port is communicated with the flaking machine through a pipeline.

[0016] As a further description of the above technical scheme, the top of the receiving tank is provided with a receiving feed port, the receiving feed port is communicated with the first condenser through a pipeline, the bottom of the receiving tank is provided with a receiving discharge port, the receiving discharge port is communicated with the first batching port of the batching kettle through a pipeline, the top of the flaking machine is provided with a flaking feed port, the flaking feed port is communicated with the recovery discharge port of the recovery kettle, the bottom of the flaking machine is provided with a flaking discharge port, and the flaking discharge port is communicated with the ton bag through a pipeline.

[0017] As a further description of the above technical scheme, the first condenser is provided with a first tube side inlet and a first tube side outlet at both ends, the first condenser is provided with a first shell side inlet and a first shell side outlet in the middle, the first tube side inlet is communicated with the batching rising port of the batching kettle through a pipeline, the second condenser is provided with a second tube side inlet and a second tube side outlet at both ends, the second condenser is provided with a second shell side inlet and a second shell side outlet in the middle, the second tube side inlet is communicated with the etherification rising port of the continuous etherification tower through a pipeline, the second tube side outlet is communicated with the transfer feed port of the transfer kettle through a pipeline, and the third condenser is provided with a third tube side inlet and a third tube side outlet at both ends, the third condenser is provided with a third shell side inlet and a third shell side outlet in the middle, and the third tube side inlet is communicated with the recovery rising port of the recovery kettle through a pipeline.

[0018] As a further description of the above technical scheme, the first jacket top one side is provided with a first water vapor flow through port, the first jacket bottom the other side is provided with a second water vapor flow through port, the second jacket top one side is provided with a third water vapor flow through port, the second jacket bottom the other side is provided with a fourth water vapor flow through port, the third jacket top one side is provided with a fifth water vapor flow through port, the third jacket bottom the other side is provided with a sixth water vapor flow through port, the fourth jacket top one side is provided with a seventh water vapor flow through port, the fourth jacket bottom the other side is provided with an eighth water vapor flow through port.

[0019] The beneficial effects of the present application are as follows:

[0020] The utility model discloses, through the dosing kettle adds amidine intermediate and meta -trifluoromethyl phenol, fully dissolves stirring heating, subsequently passes into continuous etherification tower heating reaction, then through the measuring jar adds catalyst and fully reacts, and the reaction liquid passes into the transfer kettle heating stirring, and the meta -trifluoromethyl phenol and catalyst that the distillation recovery obtains pass into the receiving tank, and the pyrithiobac - sodium that generates passes into the piece -forming machine cooling piece -forming and enters ton bag and is packed after, realize pyrithiobac - sodium continuous production, and the overall structure constitutes simple, and the production capacity is higher, and will not produce waste liquid and waste solid, effectively reduced production cost.

[0021] To make the structure characteristics and the action of the utility model more clear, the utility model is explained in detail below with the specific embodiment and the accompanying drawing. DRAWINGS

[0022] Figure 1 It is the structure schematic diagram of pyrithiobac - sodium continuous production device of the utility model.

[0023] Reference signs:

[0024] 1. Batching vessel; 101. Second batching inlet; 102. First batching inlet; 103. Batching temperature port; 104. Batching pressure port; 105. Batching riser port; 106. Batching discharge port; 2. Metering tank; 201. Metering discharge port; 202. Metering temperature port; 203. Metering pressure port; 3. Continuous etherification tower; 301. Etherification temperature port; 302. Etherification riser port; 303. Etherification pressure port; 304. Overflow port; 305. Temperature measuring port; 306. Etherification inlet; 3 7. Catalytic converter inlet; 4. Transfer vessel; 401. Transfer inlet; 402. Transfer temperature port; 403. Transfer pressure port; 404. Transfer outlet; 5. Recovery vessel; 501. Recovery inlet; 502. Recovery temperature port; 503. Recovery pressure port; 504. Recovery riser; 505. Recovery outlet; 6. Receiving tank; 601. Receiving inlet; 602. Receiving outlet; 7. Flake machine; 701. Flake inlet; 702. Flake outlet; 8. Ton bag; 9. 10. Condenser; 901, First tube side inlet; 902, First shell side inlet; 903, First shell side outlet; 904, First tube side outlet; 11. Second condenser; 1001, Second tube side inlet; 1002, Second shell side outlet; 1003, Second tube side outlet; 1004, Second shell side inlet; 12. Third condenser; 1101, Third tube side inlet; 1102, Third shell side outlet; 1103, Third tube side outlet; 1104, Third shell side inlet; 13. First jacket; 1201, First water vapor inlet; 1202, Second water vapor inlet; 13, Second jacket; 1301, Third water vapor inlet; 1302, Fourth water vapor inlet; 14, Third jacket; 1401, Fifth water vapor inlet; 1402, Sixth water vapor inlet; 15, Fourth jacket; 1501, Seventh water vapor inlet; 1502, Eighth water vapor inlet; 16, Thermometer; 17, Pressure gauge; 18, Stirring motor; 19, Stirring rod; 20, Transfer pump; 21, Flow meter. Detailed Implementation

[0025] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings.

[0026] like Figure 1 As shown, in one embodiment, a continuous production apparatus for pyrfluthrin includes: a batching tank 1, a metering tank 2, a continuous etherification tower 3, a transfer tank 4, a recovery tank 5, a receiving tank 6, a flake generator 7, and a ton bag 8.

[0027] The bottom of the batching kettle 1 and the metering tank 2 are communicated with the bottom of the continuous etherification tower 3 through a pipeline (a conveying pump 20 and a flow meter 21 are arranged on the pipeline), and the bottom of the continuous etherification tower 3 is communicated with the top of the transfer kettle 4 through a pipeline (a conveying pump 20 is arranged on the pipeline); then, the bottom of the transfer kettle 4 is communicated with the top of the recovery kettle 5 through a pipeline (a conveying pump 20 is arranged on the pipeline), the bottom of the recovery kettle 5 is communicated with the top of the flaking machine 7 through a pipeline (a conveying pump 20 is arranged on the pipeline), and the top of the recovery kettle 5 is communicated with the top of the receiving tank 6 through a pipeline; then, the bottom of the receiving tank 6 is communicated with the batching kettle 1 through a pipeline (a conveying pump 20 is arranged on the pipeline), and the bottom of the flaking machine 7 is communicated with the ton bag 8 through a pipeline.

[0028] It can be understood that the materials of the batching kettle 1, the continuous etherification tower 3, the transfer kettle 4, the recovery kettle 5 and the receiving tank 6 are all glass-lined kettles. Glass lining has excellent acid and alkali resistance and can resist the corrosion of these chemical substances. For example, for common acid and alkali solutions such as hydrochloric acid, sulfuric acid and sodium hydroxide, glass lining can remain stable and is not easy to be corroded, so as to ensure the structural integrity of the equipment in long-term production operation, prevent equipment leakage and damage caused by corrosion and other problems, and prolong the service life of the equipment. Compared with ordinary metal materials, glass lining can effectively avoid chemical reaction between metal and material, ensure the chemical stability of amide intermediates and m-trifluoromethylphenol in the mixing process, and has high hardness and wear resistance, can withstand the erosion and friction of the material, and is not easy to appear phenomena such as wear and peeling.

[0029] It needs to be particularly pointed out that the batching kettle 1 is communicated with the first condenser 9 through a pipeline; the pipeline between the continuous etherification tower 3 and the transfer kettle 4 is provided with the second condenser 10, and the pipeline between the recovery kettle 5 and the receiving tank 6 is provided with the third condenser 11, and different condensers correspond to different reaction containers for condensing gas; correspondingly, the outer wall of the batching kettle 1 is provided with the first jacket 12, the outer wall of the continuous etherification tower 3 is provided with the second jacket 13, the outer wall of the transfer kettle 4 is provided with the third jacket 14, and the outer wall of the recovery kettle 5 is provided with the fourth jacket 15, and different heating jackets correspond to different reaction containers for heating or cooling the container.

[0030] It can be understood that the first condenser 9, the second condenser 10 and the third condenser 11 all adopt graphite condensers; graphite has very high thermal conductivity, can quickly transfer heat from the heat medium to the cold medium, greatly improves the heat exchange efficiency, so that the condenser can quickly cool the high-temperature gas into liquid, and in the industry with high heat exchange requirements such as chemical industry, energy consumption and waste gas emission can be effectively reduced; and the surface of graphite is relatively smooth and not easy to attach dirt, so that cleaning and maintenance can be easily carried out when needed, thereby saving maintenance time and labor cost.

[0031] Further, the top of one side of the ingredient kettle 1, the metering tank 2, the continuous etherification tower 3, the transfer kettle 4 and the recovery kettle 5 is provided with a thermometer 16 for measuring the temperature inside the ingredient kettle 1, the metering tank 2, the continuous etherification tower 3, the transfer kettle 4 and the recovery kettle 5, so as to pass steam or cooling circulating water into the corresponding heating jacket to realize the adjustment of the internal temperature; similarly, the top of the other side of the ingredient kettle 1, the metering tank 2, the continuous etherification tower 3, the transfer kettle 4 and the recovery kettle 5 is provided with a pressure gauge 17 for measuring the pressure inside the ingredient kettle 1, the metering tank 2, the continuous etherification tower 3, the transfer kettle 4 and the recovery kettle 5; in addition, the top of the ingredient kettle 1, the transfer kettle 4 and the recovery kettle 5 is provided with a stirring motor 18, the stirring motor 18 is connected with a stirring rod 19, and the stirring motor 18 drives the stirring rod 19 to rotate by adjusting the rotating speed of the stirring motor 18, so that the liquid in the ingredient kettle 1, the transfer kettle 4 and the recovery kettle 5 is fully mixed.

[0032] Please continue to refer to Figure 1 In the embodiment, the top of one side of the ingredient kettle 1 is provided with an ingredient temperature port 103, and the ingredient temperature port 103 is connected with the thermometer 16; correspondingly, the top of the other side of the ingredient kettle 1 is provided with an ingredient pressure port 104, and the ingredient pressure port 104 is connected with the pressure gauge 17. It can be understood that the temperature and pressure in the kettle are monitored by the thermometer 16 and the pressure gauge 17, and the rotating speed of the internal stirring rod 19 is adjusted by adjusting the rotating speed of the motor, so as to adjust the evaporation rate of the internal liquid.

[0033] Further, one side of the ingredient temperature port 103 is provided with a first ingredient inlet port 102 for adding amide intermediates; and one side of the first ingredient inlet port 102 is provided with a second ingredient inlet port 101 for adding meta-trifluoromethyl phenol; in addition, one side of the ingredient pressure port 104 is provided with an ingredient rising port 105, and the ingredient rising port 105 is communicated with the first condenser 9 through a pipeline, so that the generated steam after heating can be condensed through the first condenser 9; in addition, the bottom of the ingredient kettle 1 is provided with an ingredient outlet port 106, and the ingredient outlet port 106 is communicated with the continuous etherification tower 3 through a pipeline, so that the mixed liquid in the ingredient kettle 1 can be continuously introduced into the continuous etherification tower 3 for reaction after heating.

[0034] It needs to be particularly pointed out that the first condenser 9 is provided with a first tube passage inlet 901 and a first tube passage outlet 904 at both ends, and a first shell passage inlet 902 and a first shell passage outlet 903 are arranged in the middle of the first condenser 9, and the first tube passage inlet 901 is communicated with the ingredient rising port 105 of the ingredient kettle 1 through a pipeline. It can be understood that the cooling water ( Figure 1 CWR, Cooling Water Return, represents the circulating cooling water return flow after absorbing heat; Figure 1CWS, Cooling Water Supply, represents the circulation of circulating cooling water flow to be absorbed heat.

[0035] Further, the first jacket 12 is provided with a first steam flow passage 1201 on one side of the top of the first jacket 12, and a second steam flow passage 1202 on the other side of the bottom of the first jacket 12. It can be understood that the steam (steam or water vapor) flows through the first steam flow passage 1201 and the second steam flow passage 1202 of the first jacket 12. Figure 1 LS, Low Pressure Steam, represents low pressure steam; Figure 1 SC, Condensate Water Collection, represents the collection of condensate water (or cooling water) Figure 1 CWR, Cooling Water Return, represents the circulation of circulating cooling water flow after absorbing heat; Figure 1 CWS, Cooling Water Supply, represents the circulation of circulating cooling water flow to be absorbed heat.

[0036] Please continue to refer to Figure 1 In this embodiment, the metering tank 2 is provided with a metering temperature port 202 on one side of the top of the metering tank 2, and the metering temperature port 202 is connected with the thermometer 16; correspondingly, the metering tank 2 is provided with a metering pressure port 203 on the other side of the top of the metering tank 2, and the metering pressure port 203 is connected with the pressure gauge 17. It can be understood that the temperature and pressure in the kettle are monitored by the thermometer 16 and the pressure gauge 17, and then the evaporation rate of the internal liquid is adjusted.

[0037] Further, the metering tank 2 is provided with a metering discharge port 201 at the bottom of the metering tank 2, which is communicated with the continuous etherification tower 3 through a pipeline, and is used for conveying the catalyst to the inside of the continuous etherification tower 3.

[0038] Please continue to refer to Figure 1 In this embodiment, the continuous etherification tower 3 is provided with an etherification temperature port 301 on one side of the top of the continuous etherification tower 3, and the etherification temperature port 301 is connected with the thermometer 16; correspondingly, the continuous etherification tower 3 is provided with an etherification pressure port 303 on the other side of the top of the continuous etherification tower 3, and the etherification pressure port 303 is connected with the pressure gauge 17. It can be understood that the temperature and pressure in the tower are monitored by the thermometer 16 and the pressure gauge 17.

[0039] Further, the continuous etherification tower 3 is provided with an etherification rising port 302 at the top, and the etherification rising port 302 is communicated with the second condenser 10 through a pipeline, so that the steam generated after heating can be condensed through the second condenser 10; in addition, the continuous etherification tower 3 is provided with a catalytic feeding port 307 at one side of the bottom, and the catalytic feeding port 307 is communicated with the metering discharge port 201 of the metering tank 2 through a pipeline, so that the catalyst can be quantitatively fed into the continuous etherification tower 3; in addition, the continuous etherification tower 3 is provided with an etherification feeding port 306 at the bottom, and the etherification feeding port 306 is communicated with the batching rising port 105 of the batching kettle 1 through a pipeline, so that the liquid after the reaction is completed can be fed into the transfer kettle 4; and the continuous etherification tower 3 is further provided with an overflow port 304 at one side of the middle, and the overflow port 304 is communicated with the transfer kettle 4 through a pipeline, and a plurality of temperature measuring ports 305 are equidistantly arranged below the overflow port 304, for monitoring the temperature in the continuous etherification tower 3.

[0040] It needs to be explained in detail that the second condenser 10 is provided with a second tube pass inlet 1001 and a second tube pass outlet 1003 at both ends, and the second condenser 10 is provided with a second shell pass inlet 1004 and a second shell pass outlet 1002 at the middle, the second tube pass inlet 1001 is communicated with the etherification rising port 302 of the continuous etherification tower 3 through a pipeline, and the second tube pass outlet 1003 is communicated with the transfer feeding port 401 of the transfer kettle 4 through a pipeline. It can be understood that the circulation of steam (LS) or cooling water (CWS) is carried out through the second shell pass inlet 1004 and the second shell pass outlet 1002 of the second condenser 10. Figure 1 CWR, Cooling Water Return, represents the circulating cooling water return stream after absorbing heat; Figure 1 CWS, Cooling Water Supply, represents the circulating cooling water inflow stream to be absorbed heat

[0041] Further, the second jacket 13 is provided with a third water vapor flow port 1301 at one side of the top, and a fourth water vapor flow port 1302 at the other side of the bottom. It can be understood that the circulation of steam (LS) or cooling water (CWS) is carried out through the third water vapor flow port 1301 and the fourth water vapor flow port 1302 of the second jacket 13. Figure 1 LS, Low Pressure Steam, represents low pressure steam; Figure 1 SC, Condensate Water Collection, represents condensate water collection Figure 1 CWR, Cooling Water Return, represents the circulating cooling water return stream after absorbing heat; Figure 1 CWS, Cooling Water Supply, represents the circulating cooling water inflow stream to be absorbed heat

[0042] Please continue to refer to Figure 1 In the present embodiment, the transfer kettle 4 is provided with a transfer temperature port 402 on one side of the top thereof, and the transfer temperature port 402 is connected with the thermometer 16; correspondingly, the transfer kettle 4 is provided with a transfer pressure port 403 on the other side of the top thereof, and the transfer pressure port 403 is connected with the pressure gauge 17. It can be understood that the temperature and pressure in the kettle are monitored by the thermometer 16 and the pressure gauge 17.

[0043] Further, the transfer temperature port 402 is provided with a transfer feed port 401 on one side thereof, and the transfer feed port 401 is communicated with the etherification upflow port 302 and the overflow port 304 of the continuous etherification tower 3 through a pipeline, so that the liquid after the reaction is completed can be introduced into the transfer kettle 4; and the bottom of the transfer kettle 4 is provided with a transfer discharge port 404, and the transfer discharge port 404 is communicated with the recovery kettle 5 through a pipeline, for recovering the residual m-trifluoromethylphenol and catalyst after the reaction is completed.

[0044] Further, the third jacket 14 is provided with a fifth water vapor flow port 1401 on one side of the top thereof, and the third jacket 14 is provided with a sixth water vapor flow port 1402 on the other side of the bottom thereof. It can be understood that the steam (steam) or cooling water (condensed water) is circulated through the fifth water vapor flow port 1401 and the sixth water vapor flow port 1402 of the third jacket 14. Figure 1 M-LS, Low Pressure Steam, indicating low pressure steam; Figure 1 M-SC, Condensate Water Collection, indicating condensed water collection) or cooling water (cooling water supply) Figure 1 M-CWR, Cooling Water Return, indicating the circulating cooling water return flow after absorbing heat; Figure 1 M-CWS, Cooling Water Supply, indicating the circulating cooling water inlet flow to be heated)

[0045] Please continue to refer to Figure 1 In the present embodiment, the recovery kettle 5 is provided with a recovery temperature port 502 on one side of the top thereof, and the recovery temperature port 502 is connected with the thermometer 16; correspondingly, the recovery kettle 5 is provided with a recovery pressure port 503 on the other side of the top thereof, and the recovery pressure port 503 is connected with the pressure gauge 17. It can be understood that the temperature and pressure in the kettle are monitored by the thermometer 16 and the pressure gauge 17.

[0046] Further, the recovery temperature port 502 is provided with a recovery feed port 501, and the recovery feed port 501 is communicated with the transfer outlet port 404 of the transfer kettle 4 through a pipeline, so that the liquid in the transfer kettle 4 can be introduced into the recovery kettle 5; and the recovery pressure port 503 is provided with a recovery rising port 504, and the recovery rising port 504 is communicated with the third condenser 11 through a pipeline, thereby recovering the residual meso-trifluoromethylphenol and catalyst after the reaction is completed; in addition, the recovery kettle 5 is provided with a recovery outlet port 505 at the bottom, and the recovery outlet port 505 is communicated with the flaking machine 7 through a pipeline, for conveying the generated fluazolate.

[0047] It needs to be explained in detail that the third condenser 11 is provided with a third tube passage inlet 1101 and a third tube passage outlet 1103 at both ends, and a third shell passage inlet 1104 and a third shell passage outlet 1102 are arranged in the middle of the third condenser 11, and the third tube passage inlet 1101 is communicated with the recovery rising port 504 of the recovery kettle 5 through a pipeline. It can be understood that the cooling water( Figure 1 CWR, Cooling Water Return, represents the circulating cooling water return stream after absorbing heat; Figure 1 CWS, Cooling Water Supply, represents the circulating cooling water inlet stream to be heated) circulation is carried out through the third shell passage inlet 1104 and the third shell passage outlet 1102 of the third condenser 11.

[0048] Further, the fourth jacket 15 is provided with a seventh water vapor flow port 1501 at the top on one side, and an eighth water vapor flow port 1502 at the bottom on the other side. It can be understood that the steam( Figure 1 LS, Low Pressure Steam, represents low pressure steam; Figure 1 SC, Condensate Water Collection, represents condensate water collection) or cooling water( Figure 1 CWR, Cooling Water Return, represents the circulating cooling water return stream after absorbing heat; Figure 1 CWS, Cooling Water Supply, represents the circulating cooling water inlet stream to be heated) circulation is carried out through the seventh water vapor flow port 1501 and the eighth water vapor flow port 1502 of the fourth jacket 15.

[0049] Please continue to refer to Figure 1 In the present embodiment, the receiving tank 6 is provided with a receiving feed port 601 at the top, and the receiving feed port 601 is communicated with the first condenser 9 through a pipeline; and the receiving tank 6 is provided with a receiving outlet port 602 at the bottom, and the receiving outlet port 602 is communicated with the first batching port of the batching kettle 1 through a pipeline.

[0050] Further, the top of the flaking machine 7 is provided with a flaking inlet 701, and the flaking inlet 701 is communicated with the recovery outlet 505 of the recovery kettle 5, so that the generated fluroxydone can be fed into the flaking machine 7 to be cooled and flaked; and the bottom of the flaking machine 7 is provided with a flaking outlet 702, and the flaking outlet 702 is communicated with the ton bag 8 through a pipeline, so that the fluroxydone enters the ton bag 8 for packaging.

[0051] Working principle:

[0052] The circulating cooling water of the first condenser 9 matched with the batching kettle 1 and the circulating steam of the first jacket 12 are opened, then a calculated amount of amide intermediate and meta-trifluoromethyl phenol are added into the batching kettle 1, so that the temperature in the batching kettle 1 can be increased to 85 DEG C, and the amide intermediate can be fully dissolved in the meta-trifluoromethyl phenol; the circulating cooling water of the second condenser 10 matched with the continuous etherification tower 3 and the circulating steam of the second jacket 13 are opened, the dissolved liquid and the catalyst are continuously fed into the continuous etherification tower 3 according to a certain proportion through the metering tank 2 to heat and react, after staying for 1h, the reaction completed liquid is fed into the transfer kettle 4 to heat and stir, the meta-trifluoromethyl phenol and the catalyst recovered by distillation are fed into the receiving tank 6 to heat and stir and are used in the next batch reaction, and the generated fluroxydone is fed into the flaking machine 7 to be cooled and flaked, then enters the ton bag 8 for packaging, so that the continuous production of fluroxydone is realized, the overall structure is simple, the production capacity is high, and no waste liquid and waste solid are generated, so that the production cost is effectively reduced.

[0053] The above description of disclosed embodiments enables those skilled in the art to implement or use the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to these embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A continuous production apparatus for pyrifluquinazon, characterized in that, include: Batching kettle (1), metering tank (2), continuous etherification tower (3), transfer kettle (4), recovery kettle (5), receiving tank (6), flake machine (7), ton bag (8); The bottom of the batching tank (1) and the metering tank (2) are connected to the bottom of the continuous etherification tower (3) through pipelines. The bottom of the continuous etherification tower (3) is connected to the top of the transfer tank (4) through pipelines. The bottom of the transfer tank (4) is connected to the top of the recovery tank (5) through pipelines. The bottom of the recovery tank (5) is connected to the top of the flaking machine (7) through pipelines. The top of the recovery tank (5) is connected to the top of the receiving tank (6) through pipelines. The bottom of the receiving tank (6) is connected to the batching tank (1) through pipelines. The bottom of the flaking machine (7) is connected to the ton bag (8) through pipelines. The batching vessel (1) is connected to the first condenser (9) through a pipeline. A second condenser (10) is installed on the pipeline between the continuous etherification tower (3) and the transfer vessel (4). A third condenser (11) is installed on the pipeline between the recovery vessel (5) and the receiving tank (6). The outer wall of the batching vessel (1) is provided with a first jacket (12), the outer wall of the continuous etherification tower (3) is provided with a second jacket (13), the outer wall of the transfer vessel (4) is provided with a third jacket (14), and the outer wall of the recovery vessel (5) is provided with a fourth jacket (15).

2. The continuous production apparatus for pyrfluthrin according to claim 1, characterized in that, A thermometer (16) is installed on one side of the top of the batching tank (1), the metering tank (2), the continuous etherification tower (3), the transfer tank (4), and the recovery tank (5). A pressure gauge (17) is installed on the other side of the top of the batching tank (1), the metering tank (2), the continuous etherification tower (3), the transfer tank (4), and the recovery tank (5). A stirring motor (18) is installed on the top of the batching tank (1), the transfer tank (4), and the recovery tank (5). A stirring rod (19) is connected through the stirring motor (18).

3. The continuous production apparatus for pyrfluthrin according to claim 2, characterized in that, A batching temperature port (103) is provided on one side of the top of the batching vessel (1), and the batching temperature port (103) is connected to the thermometer (16). A batching pressure port (104) is provided on the other side of the top of the batching vessel (1), and the batching pressure port (104) is connected to the pressure gauge (17). A first batching inlet (102) is provided on one side of the batching temperature port (103), and a second batching inlet (101) is provided on one side of the first batching inlet (102). A batching riser (105) is provided on one side of the batching pressure port (104), and the batching riser (105) is connected to the first condenser (9) through a pipeline. A batching outlet (106) is provided at the bottom of the batching vessel (1), and the batching outlet (106) is connected to the continuous etherification tower (3) through a pipeline.

4. The continuous production apparatus for pyrfluthrin according to claim 2, characterized in that, A metering temperature port (202) is provided on one side of the top of the metering tank (2), and the metering temperature port (202) is connected to the thermometer (16). A metering pressure port (203) is provided on the other side of the top of the metering tank (2), and the metering pressure port (203) is connected to the pressure gauge (17). A metering discharge port (201) is provided at the bottom of the metering tank (2), and the metering discharge port (201) is connected to the continuous etherification tower (3) through a pipeline.

5. The continuous production apparatus for pyrfluthrin according to claim 2, characterized in that, The continuous etherification tower (3) has an etherification temperature port (301) on one side of its top, which is connected to the thermometer (16). The continuous etherification tower (3) also has an etherification pressure port (303) on the other side of its top, which is connected to the pressure gauge (17). The continuous etherification tower (3) also has an etherification riser port (302) at its top, which is connected to the second condenser (10) via a pipeline. The continuous etherification tower (3) also has a catalytic feed inlet (30) on one side of its bottom. 7) The catalytic feed inlet (307) is connected to the metering outlet (201) of the metering tank (2) through a pipeline. The bottom of the continuous etherification tower (3) is provided with an etherification feed inlet (306). The etherification feed inlet (306) is connected to the feeding riser (105) of the batching vessel (1) through a pipeline. An overflow port (304) is provided on one side of the middle part of the continuous etherification tower (3). The overflow port (304) is connected to the transfer vessel (4) through a pipeline. Multiple sets of temperature measuring ports (305) are equidistantly arranged below the overflow port (304).

6. The continuous production apparatus for pyrfluthrin according to claim 2, characterized in that, A transfer temperature port (402) is provided on one side of the top of the transfer vessel (4), and the transfer temperature port (402) is connected to the thermometer (16). A transfer pressure port (403) is provided on the other side of the top of the transfer vessel (4), and the transfer pressure port (403) is connected to the pressure gauge (17). A transfer feed port (401) is provided on one side of the transfer temperature port (402), and the transfer feed port (401) is connected to the etherification riser port (302) and overflow port (304) of the continuous etherification tower (3) through a pipeline. A transfer discharge port (404) is provided at the bottom of the transfer vessel (4), and the transfer discharge port (404) is connected to the recovery vessel (5) through a pipeline.

7. The continuous production apparatus for pyrfluthrin according to claim 2, characterized in that, A recovery temperature port (502) is provided on one side of the top of the recovery vessel (5), and the recovery temperature port (502) is connected to the thermometer (16). A recovery pressure port (503) is provided on the other side of the top of the recovery vessel (5), and the recovery pressure port (503) is connected to the pressure gauge (17). A recovery feed port (501) is provided on one side of the recovery temperature port (502), and the recovery feed port (501) is connected to the transfer outlet (404) of the transfer vessel (4) through a pipeline. A recovery rise port (504) is provided on one side of the recovery pressure port (503), and the recovery rise port (504) is connected to the third condenser (11) through a pipeline. A recovery discharge port (505) is provided at the bottom of the recovery vessel (5), and the recovery discharge port (505) is connected to the flaking machine (7) through a pipeline.

8. The continuous production apparatus for pyrfluthrin according to claim 1, characterized in that, The receiving tank (6) is provided with a receiving inlet (601) at the top, which is connected to the first condenser (9) through a pipeline. The receiving tank (6) is provided with a receiving outlet (602) at the bottom, which is connected to the first batching port of the batching vessel (1) through a pipeline. The flake machine (7) is provided with a flake inlet (701) at the top, which is connected to the recovery outlet (505) of the recovery vessel (5). The flake machine (7) is provided with a flake outlet (702) at the bottom, which is connected to the ton bag (8) through a pipeline.

9. The continuous production apparatus for pyrfluthrin according to claim 1, characterized in that, The first condenser (9) has a first tube-side inlet (901) and a first tube-side outlet (904) at both ends, and a first shell-side inlet (902) and a first shell-side outlet (903) in the middle. The first tube-side inlet (901) is connected to the feeding riser (105) of the batching vessel (1) via a pipeline. The second condenser (10) has a second tube-side inlet (1001) and a second tube-side outlet (1003) at both ends, and a second shell-side inlet (1004) and a second shell-side outlet (1002) in the middle. The second tube inlet (1001) is connected to the etherification riser (302) of the continuous etherification tower (3) through a pipeline, and the second tube outlet (1003) is connected to the transfer feed inlet (401) of the transfer vessel (4) through a pipeline. The third condenser (11) is provided with a third tube inlet (1101) and a third tube outlet (1103) at both ends. The third shell inlet (1104) and a third shell outlet (1102) are provided in the middle of the third condenser (11). The third tube inlet (1101) is connected to the recovery riser (504) of the recovery vessel (5) through a pipeline.

10. The continuous production apparatus for pyrfluthrin according to claim 1, characterized in that, The first jacket (12) has a first water vapor outlet (1201) on one side of its top, a second water vapor outlet (1202) on the other side of its bottom, a third water vapor outlet (1301) on one side of its top, a fourth water vapor outlet (1302) on the other side of its bottom, a fifth water vapor outlet (1401) on one side of its top, a sixth water vapor outlet (1402) on the other side of its bottom, a seventh water vapor outlet (1501) on one side of its top, and an eighth water vapor outlet (1502) on the other side of its bottom.

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